X-ray Photon Correlation Spectroscopy Beamline (XPCS) X-ray Diffraction Beamline A SAXS/ WAXS Beamline Environmental Soft X-ray

XANES Beamline Hard X-ray Environmental XAS Spectroscopy Beamline The Materials Science Beamline

The Imaging and Tomography Beamline A Short-Pulse Facility for Time-Resolved X-ray Science at MAX IV

X-ray photon correlation spectroscopy beamline (XPCS) Spokespersons: Aleksandar Matic (Chalmers University of Technology), Per Jacobsson (Chalmers University of Technology), Johan Mattsson (University of Leeds, UK), Anders Palmqvist (Chalmers University of Technology), Adrian Rennie (Uppsala University) The X-ray Photon Correlation Spectroscopy (XPCS) beamline at the 3GeV ring at MAX IV will be outstanding thanks to the extraordinary specifications of the synchrotron source concerning emittance and brilliance. Examples of research areas that can be addressed are: Systems with a heterogeneous microstructure and/or dynamics, polymers, non-Newtonian fluids, colloids, liquid crystals, capillary waves polymer surfaces and of thin polymer films, protein and bio-membrane dynamics, charge density waves, and dynamic critical phenomena. Thus, the expected user community is broad and includes researchers from physics, chemistry, biotechnology, and biology. In XPCS the partial coherence of the X-ray beam is utilized to study dynamics in time domain by following the intensity fluctuation of the scattered light. The intensity-intensity autocorrelation function calculated from the scattering is directly related to the intermediate scattering function S(Q,t) reflecting the dynamics in the material. XPCS provides information on mesoscopic dynamics (10-3 1 -1) over large time scales (10-8-103 s), a region not accessible by any other technique. The low emittance of the MAX IV 3 GeV ring results in an increase in the beam coherence with more than one order in magnitude. Thus we can expect scientific breakthroughs based on the experiments performed at the XPCS beamline at MAX IV. The significant improvement of the contrast in the experiment enabling studies of weakly scattering processes and systems, complex geometries and sample environments and smaller beam/sample sizes. In particular the increased coherence can be used to exploit higher energies and so avoid beam damage of fragile samples, such as biological materials. These increased capabilities of XPCS at MAX IV will also attract a new user community and wider range of experiments. A co-location of the XPCS beamline with a coherent imaging/diffraction station, thus having one beamline dedicated to coherent scattering, could be of high interest forming a critical mass for exploitation of coherent X-ray scattering techniques at MAX IV. In addition to scientific synergies there are also technical synergies such as collimation and stability of the beam that cannot be found in other constellations. Main constellations committed to the beamline project Applied Physics, Chalmers University of Technology: Aleksandar Matic and Per Jacobsson Physics and Astronomy, University of Leeds, UK: Johan Mattsson Chemistry and Biotechnology, Chalmers University of Technology: Anders Palmqvist Physics, Uppsala University: Adrian Rennie Scientific Motivation A general feature of all condensed matter is complex dynamics; as noticed in for example protein folding, polymer reptation, viscoelastic flow, phase transitions, magnetic domain switching, coarsening and other collective processes that show fast and slow responses over vast time and length scales. The dynamic processes can cover time scales from femtoseconds to kiloseconds and involve length scales from ngstrms to microns and more. They are generally sensitive to external perturbations like temperature, pressure, applied fields, and are thus crucial for material function. The complex dynamics can be probed with time- or energy-resolved scattering techniques, most commonly scattering of photons, neutrons, and electrons. Light scattering (photons) is by far the most common and is available in-house in most laboratories. With a combination of specific light scattering techniques (Raman, Brillouin and Photon Correlation Spectroscopy) the full range of time scales involved can be probed provided that the optical quality of the sample permits. However, as these conventional techniques are based on visible and near visible light sources, they probe length scales around 1000 or more, i.e. the length scale of the wavelength or longer. This is far more distant than the intermolecular interactions ( - nm) important in most condensed matter and also longer than for example the polymer-polymer interactions in polymer melts and solutions, the ferroelectric alignment and the liquid state molecular orientational alignment. Accordingly these techniques reveal the macroscopic dynamics but cannot access the fundamental process the dynamics on the nanoor mesoscale.

Large scale facility based neutron scattering techniques, like Quasi and Inelastic Neutron Scattering (QENS and INS) and Neutrons Spin-Echo (NSE) techniques complement the accessible time and length scales. With neutron scattering fast dynamics can be probed from the mesoscale all the way down to atomic resolution (see figure 1 below). However, time scales longer than 100 ns seconds can not be reached. There has recently also been a development of high resolution inelastic X-ray scattering [1] covering a dynamical range in the THz and nm-1 range. Thus there is, or at least has been, a white spot in the frequency-wave vector plane, not accessible to conventional scattering techniques and where dynamics of considerable interest takes place. X-ray Photon Correlation Spectroscopy (XPCS) is a recent technique, covering the white spot of dynamics in the sub-microsecond to kilosecond range at the mesoscale [2]. Correlation spectroscopy is a technique based on the coherence properties of light and how this coherence is changed after interaction with matter. Visible light PCS, or dynamic light scattering, was thus first made possible when lasers where developed in the sixties. XPCS is now made possible with the third generation synchrotron radiation sources in their capability of producing coherent X-ray beams several orders of magnitude more intense than previously available. XPCS covers approximately the same time range as PCS but on submicron to meso/nano-scales. Furthermore, it is not restricted to samples with high optical quality; to X-rays most matter is transparent and therefore not sensitive to multiple scattering, a problem often encountered in visible light PCS.

Fig. 1. Frequencywave vector space covered by XPCS in comparison to other scattering techniques: Photon correlation spectroscopy with coherent visible light, Raman and Brillouin scattering, inelastic neutron scattering and neutron spin-echo. Adopted from ref. 3. XPCS, as ordinary PCS, measures the dynamics in time domain by recording the intensity fluctuations of the scattered light. The intensity-intensity autocorrelation function, calculated from the scattering, is directly related to the intermediate scattering function S(Q,t) reflecting the dynamics in the material. Compared to PCS using visible light XPCS is much more challenging due to two main reasons: the X-ray beam is only partially coherent and with less brilliance than a laser the scattering cross section is much smaller in the X-ray regime.

Thus, XPCS experiments are severely limited in contrast and the signal to noise ratio needs to be optimised as much as possible. Increasing the brilliance and coherence from the source, and optimizing the beamline optics to preserve these, is crucial for successful experiments. XPCS is ideally suited to investigate dynamic processes at the meso/nano-scale in a number of systems where one can expect dynamic signatures to be different on different length scales. Obvious examples are systems with a heterogeneous microstructure and/or dynamics; polymers, nonNewtonian fluids, colloids, liquid crystals and many more. So far XPCS beamlines are operating at the European Synchrotron Radiation Facility (ESRF) in Grenoble, at the Advanced Photon Source (APS) in Argonne, and at the Swiss Light Source (SLS) at PSI. The new storage ring designed for MAX IV will improve the coherence of the produced X-rays even further, about an order of magnitude better than any other synchrotron existing or planned, see further in the section on beamline characteristics.

There are a number of problems that can be addressed on a new XPCS beamline operating at MAX IV. To review them all is outside the scope of this proposal. But, some enlightening examples taken from recent literature [4] are given below to show the broad scope of problems that can be addressed with the XPCS technique. Opaque Colloidal Systems Colloidal systems at low concentration have been studied with visible light PCS for many years. However, at higher concentration, where a transition from weakly to strongly interacting particles can be expected, the optical properties and problems with multiple scattering have limited the usefulness of visible light PCS. XPCS have recently been shown to overcome these problems in e.g. magnetic colloids and carbon black [5]. Polymers Entanglement and repetitive dynamics Polymers are another class of materials in which equilibrium motions are not well understood. For example, important aspects of the repetition model are still untested after almost three decades since the dynamics have been too slow for neutron scattering experiments and occurring on too short length scales to be covered by visible light PCS [6]. Also the capillary waves and other properties of polymer surfaces and thin polymer films can be explored using XPCS in diffuse reflectivity mode. Such studies will likely help to solve the long standing question concerning the reported dramatic decrease (more than 50 K) of the glass transition temperature in thin polymer films [7]. Glass formers Vibrational and relaxational modes in the mesoscopic space-time regime. Many liquids, when rapidly cooled below their freezing points, form glassy or amorphous phases. Glassy materials (among them metal alloys, oxides, polymers) are among the least understood materials at a fundamental level [8]. Conventional statistical mechanics does not predict the existence of the amorphous phase although it can explain most other states of matter like basic superconductivity and super-fluidity. Glasses show a very rich dynamic response with primary processes linked to the viscosity and other faster, secondary processes near the glass transition. The region of frequencywave vector space covered by XPCS is very important in understanding the structural nature of the dynamics in glass-forming systems at the nanoscale [9]. Slow dynamics in hard condensed matter systems XPCS can probe dynamics also in hard condensed matter systems. Phenomena of interest involve the dynamics accompanying for example domain formation and phase separation in alloys [10] or gold precipitation in iron films [11]. Recently very intriguing results very obtained on slow atomic diffusion in alloys revealing the symmetry of these fundamental processes [12]. As seen from the above there are many possible experiments to suggest for a XPCS beamline at MAX IV and the list can easily be made much longer by including for example: Complex Liquids Symmetry of local structure and slow dynamics [13] Dynamic Critical Phenomena Order fluctuations in alloys, liquid crystals, etc. [14] Charge Density Waves Direct observation of sliding dynamics [2]. Quasicrystals Nature of phason and phonon dynamics [2]. Surfaces Dynamics of adatoms, islands and steps during growth and etching [15]. Defects in Crystals Diffusion, dislocation glide, domain dynamics. Ferroelectrics Order-disorder vs. displacive nature; anisotropic correlations and size effect [16]

Thus a beamline for X-ray photon correlation spectroscopy (XPCS) at MAX IV will be of high national interest. All larger Swedish Universities run research programs directly related to the areas where XPCS will have an impact. The expected user community for the XPCS beamline at MAX IV spans a large spectrum from physics to biology, including hard matter, surface physics, soft matter, microfluidics and bio-applications. These topics well reflect the research at several universities in Sweden, and there are leading groups in all topics and several Linneaus and VINN Excellence centres which could benefit from this research, e.g. Organizing Molecular Matter (Linn/Lund University), Bioinspired Supramolecular Function and Design (Linn/Chalmers), and Supramolecular Biomaterials (VINN Excellence/Chalmers). In addition there are strong activities in the other Nordic countries, especially in Denmark, which would benefit from this facility and we also expect at strong international

user community considering that the beamline will have a world-class performance. Thus, we can foresee a large user community for the beamline and that the research will be state-of-the-art. Several of the research topics are closely connected to applications, such as drug delivery systems, food stuffs, electrolytes, and polymeric materials. Thus, it impacts the areas of importance for society, Energy-Health-Sustainability, and there is a strong possibility also for industrial users once the technique is established at MAX IV. As the technique is new for MAX-lab and there are also just a few instruments in the world there is also a need for education of the user community. A first step is here taken this year when Chalmers Graduate School for Soft Matter organizes a summer school on New X-ray and neutron scattering techniques for soft matter where XPCS will be one of the topics. During the construction phase of the beamline further schools and workshops should be organized and Swedish scientists given the opportunity to learn about the technique at the present instruments at PETRA III and ESRF. References [1] F. Sette et al., Science 280, 1550 (1998) [2] Soft Matter Characterization, chapter 18; X-ray Photon Correlation Spectroscopy. And references therein. (Springer, Netherlands, 2008) [3] G. Grbel et al., Alloys Compd. 362, 3 (2004). [4] See the recent review by Mark Sutton in C.R. Physique 9 657-667 (2008) and references therein. [5] A. Robert et al. Journal of Magnetism and Magnetic Materials 289, 47 (2005); V. Trappe et al., Phys. Rev. E 76, 051404 (2007). [6] P. Pincus, J. Chem Phys. 75, 1996 (1981). [7] J. Matsson et al. Phys. Rev. B 62, 5187 (2000). [8] see e.g. Science 309, 1st July (2205) 125 Questions: What dont we know? [9] C. Caronna, Y. Chushkin, A. Madsen and A. Cupane, Phys. Rev. Lett. 100, 055702 (2008) [10] Stadler L-M. et al. Phys.Rev E 74, 041107 (2006) [11] N. Spiridis et al. Surf. Sci. 135, 507 (2002) [12] M. Leitner et al. Nature Materials 8, 717 (2009) [13] P. Wochner et al. Proc. Nat. Acad. Sci. 106, 11511 (2009); Y. Chushkin et al. EPL 83, 36001 (2008); Z. Jiang et al. Phys rev Lett 101, 246104 (2008) [14] D. Constantin et al. Phys. Rev E 74, 031706 (2006) [15] R. Reitinger et al. Defect and Diffusion Forum, 263, 177-182 (2007) [16] G. Grbel et al. Nuclear Instruments and Methods in Physics Research B 262, 357367 (2007)

Beamline characteristics The XPCS beamline is planned to be located at the 3 GeV storage ring at MAX IV, taking advantage of the low emittance and high brilliance. The performance of the 3 GeV storage ring is approaching the theoretical limit for storage rings, thus, the facility will be world leading for long time to come for photon energies up to some 20 keV. In this range the emittance will be extremely low, 0.24 nmrad for MAX IV to be compared with for instance ESRF, currently the premier source in Europe, which has an emittance of 3.9 nmrad, or the recently opened PETRA III with an emittance around 1 nmrad. The low emittance, which transfers to a high brilliance (B), is of particular importance for techniques requiring a coherent beam such as XPCS and coherent imaging. The coherent flux from the source, Ic, at a given wave length, , is following the relation

IC B2 .
Thus, the high brilliance of MAX IV, at least an order of magnitude better than for current or planned sources in the range 5-20 keV leads to an order of magnitude increase in the coherent flux of the XPCS beamline. The increased flux leads to that the contrast in the experiments is significantly improved and in general enables studies of: weakly scattering processes and systems complex geometries and sample environments smaller beam/sample sizes studies over larger parameter space (concentration, temperature, pH, etc.)

In particular this allows us to work with higher energies that will reduce beam damage. Current XPCS beamlines work with incident energies around 8 keV which causes beam damage in biological and other organic materials. Due to the very high brilliance the XPCS beamline at MAX IV will be able to work at higher energies and still have a higher fraction of coherent flux than the best beamlines today. The energy range 12-20 keV will be a unique range for the XPCS beamline at MAX IV and enable studies that cannot be performed at any other beamline. Since the performance of the MAX IV 3 GeV ring is truly unique concerning the emittance the exact design of the XPCS beamline has to be fully optimized to take advantage of this. Thus, there is a need for detailed design studies rather than just adapting the concepts from existing beamlines. This work will be made in the detailed design phase of the beamline during building of the facility. In particular there is today a rapid technology development concerning for instance X-ray optics and detectors which we plan to take full advantage of to obtain the best beamline in the world. Some guiding beamline specifications can be summarised as: The source for the XPCS beamline should be a long in-vacuum undulator providing high flux in the energy range 5-20 keV. Theoretical calculations (published in Insertion Devices for the MAX IV 3 GeV Ring, Erik Walln, 2010-02-15) on a 3.8 m in-vacuum undulator gives a coherent fraction of 9 % and 0.15% for the energies 5 and 20 keV, respectively. The corresponding flux is 1013 and 1011 photons/s, respectively, see figure 2. This can be compared to the flux at the current most productive beamline ID10A at ESRF which is 1010 photons/s at 8 keV. Thus, a significant, order of magnitude, increase in flux is expected for XPCS at MAX IV. The X-ray optics should be optimized for preserving the coherence from the source. This is crucial in order not to loose the coherence on the way from the source to the sample. The creation of an X-ray optics group at MAX-lab is high on the agenda and this would be very valuable for optimizing the components for the XPCS beamline. The spot-size on the sample should be matched to the coherence length in the beam. Typically it will fall in the 10-20 m range. Overall it is important to have a high stability of the whole set-up to ensure precise experiments. The scattering geometry should allow for both small and wide angle scattering experiments in order to cover a momentum transfer range of 10-3 to 1 -1. It should also allow for measurements in either transmission or reflectance mode. The latter of importance for studying surface processes. Typical sample environments are cryostats and furnaces but also other more complex environments can be envisaged such as flow cells, shear cells, or in situ chambers. The sample detector distance should be optimized to match the speckle size with the pixel size of the particular detector used.

The detection system will be a high-efficiency fast 2D detector (currently the most common are CCDs and pixel detectors). The short time limit is determined by the detector performance (rise time) and the long time limit is determined by the patience of the experimentalist and more importantly by the stability of the set-up. There is here a rapid development on the detector side, driven by the need of fast and efficient detectors for X-rays at synchrotrons and XFELs, and one can foresee much more rapid detectors being available in the near future, why there is little point in specifying a particular detector at this stage.

Fig. 2. Coherent flux of a 3.8m undulator for MAX IV Exclusion of vibrations and drift in the beam is crucial, in particular to look at long time correlations (for example for speckle analysis). In the design of the instrument and in the location of the beamline it is vital to consider constraints such as isolation of auxiliary equipment as well as other instruments. As these factors are also crucial for coherent imaging it is a very good strategy to co-locate such beamlines rather than having them as end stations on other set-ups. In addition there is obvious synergies in optics, detectors and know how. In particular it is important to build a critical mass of scientists in techniques utilizing coherence.

Description of the main constellation involved in the project The XPCS beamline is proposed by Aleksandar Matic and Per Jacobsson from Dept. of Applied Physics, Chalmers University of Technology (Sweden) Johan Mattsson from Dept. of Physics and Astronomy, University of Leeds (UK) Anders Palmqvist from Dept. of Chemical and Biological Engineering, Chalmers University of Technology (Sweden) Adrian Rennie, Dept. of Applied Physics, Uppsala University (Sweden) We have a long standing experience within the field of Soft Matter physics working with glasses and super cooled liquids, polymer solutions and gels, surfactant solutions, and colloidal dispersions. We have realized the large potential in applying coherent X-ray scattering techniques to our research problems with the recent development of the third generation synchrotron sources. With MAX IV we see the potential for a leap in the performance of the technique and breakthroughs in our field can be expected Our current research is both fundamental and applied towards materials for energy applications (new electrolytes for Li-batteries and fuel cells, catalysis, and thermoelectrics). In our research we use both in-house spectroscopic techniques (Photon Correlation Spectroscopy, Brillouin and Raman Scattering, and Dielectric Spectroscopy) and X-ray and neutron scattering methods at large scale facilities. Recently a part of the team (Matic, Jacobsson and Mattsson) has initiated studies using XPCS at ESRF together with the group of Anders Madsen at the ID10A beamline. These studies concern slow local dynamics in glass forming systems near the glass transition. To realize this beamline there is a need to build up competence at MAX-lab since this is a new technique for the facility. An experienced beamline scientist should be recruited and lead the detailed design and together with us develop the detailed science case. Furthermore, a collaboration on the development of the XPCS beamline at MAX IV with the leading centers in the world should be established to draw on the experience and exchange knowledge, for instance groups at PETRA III and at ESRF.

Budget, staffing and time plan An overview budget for the beamline is presented in Table 1, including estimates for source, optics, end-station and infrastructure. One should note that if one chooses to have a full coherent scattering beamline (XPCS and coherent imaging) the total cost will not increase significantly as all the majors parts are also contained in the present budget. Table 1. Overview budget for the XPCS beamline Description Source Undulator, front end, optical & experimental hutches incl. personal safety system, etc. Optics Monochromator, focusing optics (coherence preserving), beam diagnostics, slits, etc. End station Sample environment, positioning systems, detector systems, etc. Infrastructure Electronics, controls & computing, vacuum, liq-N2, fluids, etc. Others Control room & sample preparation lab. Total Amount (MSEK) 22 21 25 10 2 80

The project can be realized during a three year period for construction and installation of the full beamline. It will require a beamline responsible, a second beamline scientist, and a technician/electrician (the latter can most likely be shared with another beamline). For the design of the beamline we plan to have an extensive collaboration with leading groups for instance at PETRA III and at ESRF to draw on their experience and expertise. We also plan to collaborate and closely follow the detector development taking place at various sources, e.g. the XFEL in Hamburg.

X-ray Diffraction Beamline Spokespersons: Kristina Edstrm, Materials Chemistry, Uppsala University; Sven Lidin, Polymer- and Materials Chemistry, Lund University; Jens Birch, Thin Film Physics, IMF, Linkping University. It is proposed to build a diffraction facility by using three high resolution diffractometers each optimized for powder, single crystal and surface experiments. This combination will allow the study of materials ranging from amorphous, powders and single crystals, to advanced interface structures. A wide energy range, very high angular resolution, good count rates combined with controlled environmental conditions will enable detailed structural analysis of complex materials that are of importance in many areas of the physical, life and environmental sciences. The facility will employ a 4-circle single-crystal diffractometer with kappa geometry, capable of collecting high precision data for electron density studies. It will have the high resolution and counting statistics necessary for studying weak diffraction phenomena such as satellites from modulated structures and structured diffuse scattering from disordered materials. It will also be able to perform fast data collections on crystals that are too small to be studied using standard home laboratory instrumentation. For powder diffraction a state-of-the-art 3 circle instrument (two 2 axes and one axis) with two detector systems, one for each 2 axis, will be employed. The detectors will be a multichannel analyzer system for high resolution data (better than 0.003 in 2) and a fast strip detector covering 120 in 2 with a resolution of 0.004. This instrument will be equipped with a range of sample environment stages allowing different temperatures, gas mixtures, pressures, and relative humidity. For the surface diffraction, a multi-purpose 6-circle diffractometer equipped with a hexapod, will be installed. Apart from surface diffraction, this diffractometer allows for in situ studies of dynamic processes in dedicated chambers for various environments. A large carrying capacity with a large collision-free space for sample geometries will facilitate design and implementation of environmental chambers. The high performance of the MAX IV source will provide a beam that is coherent on a micrometer size. This opens up the possibility to perform measurements without configurational average. To allow development of experiments and techniques taking full advantage of this unique source, the optics of the beamline will be optimized to preserve the coherence. Main constellations committed to the beamline project: Materials Chemistry, Uppsala University Materials and Environmental Chemistry, Stockholm University Polymer- and Materials Chemistry, Lund University Thin Film Physics, IMF, Linkping University Joined research groups in Denmark Dedicated user groups: Division of Synchrotron Radiation Research, Lund University, - Catalysts at Work - Edvin Lundgren Competence center for Catalysis, Chalmers, Gteborg, - Catalysts at Work - M. Skoglund Max-Planck-Institut fr Metallforschung, Stuttgart, Germany - Catalysts at Work - A. Stierle ngstrm Advanced Battery Centre, Uppsala Univ. - Li-ion batteries - T. Gustafsson and K. Edstrm Polymer & Materials Chemistry, Lund University - Clay Minerals - Staffan Hansen SKB AB, Oskarshamn; -Clay Minerals - Daniel Svensson, Numerical Analysis, Lund University; - Clay Minerals - Eskil Hansen Clay Technology AB, Lund. Clay Minerals Materials Physics Division, Uppsala Univ.-Low-dimensional structures and nanomaterials - Adrian Rennie and Bjrgvin Hjrvarsson Department of Chemistry, Aarhus University - Nano Particles - Bo Brummerstedt Iversen Department of Chemistry, Aarhus University - Gas/solid Liquid/solid reactions - Torben R. Jensen Department of Chemistry, Aarhus University - Non-Ambient Conditions - Jens Erik Jrgensen Department of Chemistry, Aarhus University - Biominerals - Henrik Birkedal Department of Chemistry, Aarhus University - Energy Materials - Mogens Christensen RWTH Aachen University - Molecular containers as reaction vessels - Markus Albrecht University Mnster - Molecular containers as reaction vessels - Roland Frhlich University Helsinki - Molecular containers as reaction vessels - Martin Nieger, Markku Leskel

Department of Physics and Chemistry, University of Southern Denmark - Pharmaceutical solid forms Andrew D. Bond Faculty of Pharmaceutical Sciences, University of Copenhagen - Pharmaceutical solid forms - Jukka T. Rantanen Materials Research Division, Ris DTU - In-situ Powder Diffraction - Poul Norby Department of Chemistry, DTU - Temperature-Pressure - Kenny Sthl Haldor Topse A/S - Catalysts at Extreme Conditions - Alfons Molenbroeck H. Lundbeck A/S - Pharmaceutical polymorphs - Anette Frost Jensen Karlsruhe Institute of Technology, Germany; - Chiral Porous 3-D Networks - Stefan Brse Helsinki University - Chiral Porous 3-D Networks - Markku Leskel, Martin Nieger University Mnster - Metal-Organic-Frameworks - Frank Glorius, Roland Frhlich Helsinki University. - Metal-Organic-Frameworks - Markku Leskel, Martin Nieger Berzelii Center EXSELENT on Porous Materials, Dept. of Materials and Environmental Chemistry, Stockholm University - Porous materials and organo- and organometallic catalysts - Prof. Xiaodong Zou, Director Dept. of Materials and Environmental Chemistry, Stockholm University - New microporous materials Xiaodong Zou, Junliang Sun Dept. Materials and Environmental chemistry, Stockholm University, - Transition Metal Oxides Gunnar Svensson

Powder Diffraction (PD) Powder diffraction has for a long time been the principal technique for determining the structure of materials that do not readily form large ordered crystals. It is the technique of choice for the analysis of novel materials where synthesis is undeveloped or where international competition is strong. It is also preferred for highly strained materials and materials inherent to twinning. It has been vastly improved by the development of intense sources of synchrotron radiation and advances in data analysis using modeling, direct methods and global optimization methods. It is a preferred technique for timeresolved studies of irreversible reactions. The properties of real materials are often to a large extend determined by defects in their microstructure. It is also most often as a powder that advanced materials will be used in real applications. Powder diffraction, as a method to characterize microstructure, or follow changes during operational conditions therefore belongs to the heart of the realm of materials science, and solid state chemistry and physics. The outline design is a heavy-duty three-circle diffractometer (two 2 axes, one for each detector system) equipped with an analyzer stage for accurate structural analysis and a position-sensitive detector for rapid recording of phase transitions. Easy-to-use environmental stages will be used with state-of-the-art automation to achieve high sample throughput. The exceptionally high angular resolution of 0.003, together with improved detectors and the control over the ambient conditions of temperature, pressure and humidity will enable new ground breaking studies to be made on complex materials in different states and as a function of time. It will attract many users from academia and industry. The strip detector will facilitate rapid data collection and readout of large angular range data. It should be possible to collect high angular data in a matter of seconds, with virtually no readout time between collections. This is especially important during in situ measurements as it is likely that states observed during such measurements are not stable and thus cannot be studied in any other way. Therefore it is important that the data is of a quality good enough for structure solution and refinement. With the very high angular resolution now becoming available, it is possible to investigate much more complex materials. One area that could benefit from this is macromolecular crystallography. It is often a challenge to grow single crystals suitable for structure determination so the possibility to collect data from powders would be a vast improvement. Also by using the position sensitive detector, complete data could be collected in seconds or minutes, thereby dramatically reducing the effects of radiation damage. To take full advantage of these new possibilities, easy wavelength control would be essential to allow for collection of data at several wavelengths for MAD structure solution. The challenge has already been addressed by the USA team of Von Dreele who achieved the solution and refinement of two protein structures from synchrotron powder diffraction data, and the method is currently being developed at two other synchrotrons (ESRF, APS). One interesting potential is to study protein crystallization in situ, studying pH dependencies, salt concentration dependencies etc. to determine the optimal crystallization parameters. The importance of powder diffraction as a technique used in Swedish research is huge; it is the work horse in most laboratories, and an indispensable tool for research in high performance ceramics, hydrogen storage materials, anode and cathode materials for new high powder density batteries, micro- and meso-porous materials, solid state catalysts and pharmaceuticals. All are areas where Swedish groups are performing world leading research. The advantages of powder diffraction are enhanced by synchrotron radiation as the very narrow vertical resolution of the beam is well suited for high angular resolution studies, (e.g. profile analysis, microstrains studies), and ab initio determination of complex structures. The obtained instrumental resolution decreases peak overlaps, which is a determinant factor in the process of indexing a powder diagram and extracting the diffracted intensities. Short wavelengths give the possibility to work in transmission geometry even with compounds containing heavy elements, which considerably simplifies the problems of absorption corrections. Studies on compounds containing 2nd series transition metals or rare earth elements are thus possible. To summarize, synchrotron radiation combines simultaneously four important features for structure determination on powders: Large range in reciprocal space (completeness of the data set for accurate determination of atomic displacement parameters).

High angular resolution which allows the separation of neighboring contributions (weak distortions and pseudo symmetries) and well-defined peak shapes (quality of the Rietveld refinement). Good signal to noise ratio (precision of the measurement, weak intensities e.g. satellite reflections in incommensurate structures) Energy tunability for the collection of Multi wavelength Anomalous Diffraction (MAD) data for phasing.

Powder diffraction is also an area in which the complementarity of neutron and X-ray techniques is significant, and one in which the natural synergy created by co-locating MAX IV and ESS can have immediate and significant benefits to Swedish science. The proposed instrumentation will be able to probe the properties of condensed matter on length scales ranging from sub-ngstrm, through the nanometer regime, to the micron level; at temperatures ranging from 80 to 2500 K; on timescales ranging from the order of seconds to tens of minutes; under conditions of ambient and applied pressure; under varying degrees of humidity or chemical environment; and in situ studies of synthesis of materials. Over this range of conditions, the instrument will be capable of probing the atomic arrangement of microcrystalline and amorphous materials, thus giving key insight into their properties and hence to the technological or biological applications. The Danish constellation committed to this beamline project is at present preparing an application on a dedicated multipurpose powder diffraction beamline to be presented to several Danish financiers. Depending on the outcome, the powder diffraction from this proposal should be coordinated with the dedicated beamline. Single Crystal Diffraction (SC) A main argument for using synchrotron radiation is the high photon flux available. This allows for structure and charge density studies of very small crystals for which the size is the limiting factor of the scattering power. This topic is important in chemistry (complex molecular structures, supramolecular chemistry, porous materials, catalysis) and mineralogy The small beam size, high intensity and small sphere of confusion, enables the study of mineral samples using single crystal diffraction. By cutting and polishing thin plates and mount them on a glass slide, it is possible to select single crystallites in the sample for diffraction experiments. At SNBL at ESRF it has recently been demonstrated that this method is feasible by collecting data on a triclinic feldspar sample. The study of small crystals is greatly aided by the small beam size possible with the low emittance of the MAX IV 3 GeV ring.

Fig. 1: Illustration of small single crystals of a micro-porous material. The structure is not yet solved. Furthermore the high flux aids the study of unstable crystals or crystals very sensitive to radiation damages, needing short recording times. It is also needed to study aperiodic crystals (incommensurate structures, quasicrystals), for which weak reflections are rich in information and for

measurements of the intensity diffracted by crystal planes of low reflecting power: systems containing heavy and light elements (for example, contrast problems in actinide-based organo-metallic systems), and highly symmetric systems with pseudo-extinctions. Single crystal diffraction will also benefit from the easy and fast energy tunability for anomalous scattering experiments for multiple elements in the same sample, suggested for powder diffraction. The energy range between 5 and 30 keV is wide enough to reach at least one of the K, L or M edges of the elements from titanium to uranium. By exploiting the tunability of the photon energy several diffraction experiments unique to synchrotron radiation can be performed. One option is to combine or complete data sets measured at different energies around the absorption edge of a relevant element. The fast data acquisition times at a synchrotron (complete data sets in a couple of hours) open up the possibility to refine simultaneously different data sets, for example in order to improve the electron density modeling. Furthermore, when the energy of the incident X-rays is close to the absorption edge of one of the chemical element in the crystal, forbidden reflections may appear and give a unique insight into structural properties. Particularly for modulated structures the atomic contrast of resonant diffraction can be used for the analysis of complex features: The energy dependence of the intensity of satellite reflections gives specific information about contributions of a given atom, and therefore also information about which atomic positions are modulated. For disordered structures with mixed atomic species on a position, the combination of multiple data sets measured at the absorption edges of the concerned elements, makes possible the disentanglement the mixed occupancy at a certain position. Especially in situations with more than two elements involved this can otherwise be a difficult task. The proposed diffractometer has already been financed by VR and will be installed at the beamline I711 on the existing MAX II ring during the summer 2010. The diffractometer is an ultimate performance instrument for performing high resolution structure determination, and in situ experiments on single crystals. The experiences and expertise accumulated during the next 3 years will be invaluable for making the diffractometer perform to its limits as a state-of-the-art single crystal instrument at the MAX IV beamline. We also expect to build up a significant user community during these 3 years, and it is important to ensure a smooth transition to the MAX IV facility. The proposed upgrade with a fast pixel detector will improve the study of diffuse scattering and make time resolved diffraction experiments a possibility Surface Diffraction (SD) Surfaces and interfaces are often the key to materials properties as this is where the interaction with the surroundings takes place. X-ray diffraction is a powerful technique for the determination of structural arrangements of low dimensional materials, such as surfaces and interfaces. It can be used in a wide range of environments including solid surfaces, solid-solid and liquid-solid interfaces. The brightness of modern storage ring insertion devices means that many, often weak, reflections can be recorded giving the high information content necessary to characterize complex structures. It is becoming more and more common that the systems of interest are complex or occur in buried interfaces. Diffraction from such samples results in many peaks in reciprocal space or weak features due to absorption by the material that the X-rays must penetrate (e.g. solids or liquids). The choice of placing the diffractometer at a hard X-ray beamline that goes to energies as high as 30keV will give increased penetration, and allow for the study of buried interfaces. Most Surface Diffraction facilities are build for the solid-vacuum studies using the energy range 10-14 keV. The increased penetration and reduced radiation damage of harder X-rays, together with accurate diffractometers will make surface diffraction at MAX IV a world leading facility to study more complex structures (by allowing more access to reciprocal space) and buried interfaces. The proposed instrument is at present installed at the I811 beamline on the MAX II ring. This is well known by the user groups and there are a number of existing experimental chambers available already. In addition the goniometer is a heavy load multipurpose type useful for many types of materials science experiments such as nano-structures, thin films and semiconductors. The large carrying capacity with a large collision-free space for sample geometries will facilitate design and implementation of environmental chambers for in situ studies of dynamic processes. Depending on what beamlines are financed in phase 1, this instrument could also be placed at a wiggler based materials science beamline.

Beamline characteristics, general beamline layout and technical solutions Energy (wavelength) range Photon source Monochromator Energy stability Band pass (E/E) Position stability Optics Polarization Spot size on sample 5 -30 keV (2.5 - 0.4 ) In-vacuum undulator EXAFS-quality double crystal monochromator with channel-cut Si(111) and Si(311) crystals. 0.1 eV ~10-4 (low bandpass monochromator) 1% r.m.s. on 5s time scale 3% r.m.s. on 1hr time scale Refractive lenses or mechanically bend KB mirrors Linear PD: 1 x 0.5 mm2 SC: down to 5 x 5 m2 SD: down to 5 x 5 m2

Source To fulfill the purpose of the beamline, the source will have to deliver X-rays within the range 5-30 keV. This requires a small gap, short period undulator source operating at high harmonics. Such devices are successfully used at several 3rd generation synchrotron beamlines today. The proposed device is the undulator pmu18p5. The on-axis power density is 97.108 kW/mrad2 and the total emitted power is 13.306 kW. The brilliance at peak energy is shown in figure 2. All energies below 5keV will be removed by a diamond window before the monochromator. The chosen undulator is also characterized by not having dramatic changes in brilliance when changing from one harmonic to the next; this should ease the energy tunability of the beamline. The maximal brilliance is above 11021 at 5keV and even at 30keV the brilliance is 71019 100 times more than the similar beamline at SOLEIL.

Fig. 2: The brilliance at peak energy from the pmu18p5 undulator

Optics For the purpose of anomalous diffraction experiments it is important that the energy tunability is reproducible and user friendly, therefore a EXAFS-quality double crystal monochromator with two channel-cut monochromator crystals (Si(111) and Si(311)) is required. For energies less than 20 keV a Si(111) crystal will be used, and for higher energies a Si(311) crystal will be used. The device must provide a fixed beam exit. Due to the high power of the undulator beam, the first crystal must be cooled with liquid nitrogen. This kind of device is well known and no design problems are anticipated. To allow easy and fast changes between setups it is proposed to use individual focusing optics for each instrument, this has the further advantage of a short distance to the sample allowing for microfocusing. The focusing optics should preserve the brilliance and coherence of the beam and be easily and reproducibly energy tunable. Several ways of focusing exist such as zone plates, refractive lenses, and KB mirrors. The choice is left for the detailed design phase with ray tracing calculations, but it is expected that it will be between a lens system and mechanically bend KB mirrors. The KB arrangement has become the favoured option in terms of performance at other synchrotrons, and at the moment presents the best solution when it comes to energy tunability. One option is to have KB mirrors on the single crystal diffractometer and a lens system optimized for a narrower energy interval for the surface diffractometer. In case of a KB mirror setup the mirrors should have three tracks: Si for energies less than 15 keV; Rh for energies less than 24 keV; Pt for energies less than 38 keV. Change of wavelength For the optimal user-friendly wavelength change a unified control system is needed to couple the undulator and the monocromator movements. For automation on the powder diffractometer this movement should even be coupled to the tuning of the analyzer crystals. Both solutions are currently in operation on the Diamond Light Source in UK. Change between setups For optimal performance of each instrument it is important to insert vacuum flight tubes on the entire beam path leading up to the instrument in use. This requires the individual focusing optics to be easily moved out of the beam path when not in use. It also requires some modifications to the existing single crystal diffractometer. No issues are expected with any of these solutions. Powder sample changer For fast scanning of many samples we propose to have a sample changer system with a capacity of 200 samples. The system will be similar to that operating on the I11 powder beamline at Diamond Light Source. The mounting socket should also be the same standard used at Diamond and ESRF

Fig. 3: Schematic beamline layout

Catalysts at work. We propose to perform in situ Surface X-Ray Diffraction (SXRD) studies of catalysts under near industrial working conditions. These investigations require a diffractometer, a flow reactor cell developed for SXRD as well as an advanced gas system. For many years there has been little overlap between the catalytic industry and surface science and surface chemistry, largely because of the simplified catalytic model systems and low pressures used in fundamental studies. However, during the last decade a number of new experimental techniques have emerged allowing for atomic scale studies at conditions much closer to real catalysts at work. One of those techniques is SXRD, which may probe the phase or compound present on a surface or in nanoparticles down to single layers, while being insensitive to the presence of the reactant gas atmosphere. If the composition of the reactant gas is simultaneously analyzed by mass spectroscopy or laser means, the reactivity and selectivity of a catalyst can be related to the presence of certain formed compounds. In this way we plan to study the oxidation of methane using compounds such as oxides and carbides of Co and Fe, the reduction of NO by novel Ag catalysts, and gas induced shape changes and segregation of alloy nanoparticles. Research constellation: E. Lundgren, J. Gustafson, Division of Synchrotron Radiation Research, Lund University, Lund, Sweden.M. Skoglund, Competence Center for Catalysis, Chalmers, Gteborg, Sweden.A. Stierle, Max-Planck-Institut fr Metallforschung, Stuttgart, Germany Li-ion batteries Rechargeable lithium batteries are today the prime choice for energy intensive mobile applications like laptops and mobile phones. Despite the commercial success during the last decades there is an ever increasing demand for new materials for Li-ion batteries. There are demands for higher capacities, higher power, better stability, longer lifetime and higher safety. A core activity within the ngstrm Advanced Battery Centre is to synthesise and characterise such materials. High quality diffraction studies from micron (or even sub micron) sized single crystals are needed to identify lithium atom positions within transition metal compounds. High resolution powder diffraction data is needed to characterise materials with complicated phase diagrams and intrinsic impurities. High speed in-situ diffraction at temperatures between 230 K and 350 K is needed when studying charge and discharge mechanisms in these materials under realistic conditions. From our frequent use of beam lines I711 and I911-5 at MAX II we have experience of such studies. For the next step we need: 1) Higher intensity and better tunability of the primary beam, 2) Much better resolution for the powder diffraction set up and 3) A 2D-detector insensitive to overload or with a very high dynamic range. Research constellation:T. Gustafsson and K. Edstrm, ngstrm Advanced Battery Centre, Uppsala University. The unit consists of approximately 10 senior staff members and 20 junior staff members. The main areas of activity are related to bulk, surfaces, interfaces, and nanostructures of electrochemically active materials. Clay Minerals The KBS-3 concept for a Swedish repository for high-level radioactive waste includes three barriers: copper canister, swelling clay and suitable rock. It is vital that the clay retains its properties over a long period of time. Available clay materials are evaluated under repository-like conditions in the alternative buffer materials experiment (ABM), which was started at the sp Hard Rock Laboratory in 2006. The first of the three ABM parcels, containing 11 different clay materials each, was retrieved in May 2009. The aim of our project is to study fundamental processes of importance in this context. In order to investigate the swelling kinetics of the layer silicates and the time-dependent transport of water, we use powder X-ray diffraction. Short measuring times and good counting statistics are necessary for this type of study. Another point of interest is to characterize and quantify the minor minerals in the clays and the prospect of collecting powder patterns with superior angular resolution sounds very promising. Research constellation: Staffan Hansen, Polymer & Materials Chemistry, Lund University; Daniel Svensson, SKB AB, Oskarshamn; Eskil Hansen, Numerical Analysis, Lund University; Clay Technology AB, Lund.

Low-dimensional structures and nanomaterials Many interesting effects are found when the size of a material is limited (e.g. quantum confinement) or a sample is restricted in to 1 or 2 spatial dimensions. In soft matter, nanomagnetism and other areas dynamic properties, for example responses to external fields (stress, electric/magnetic) and phase transitions are dominated by these effects. Structural determination is the first step in characterisation of such novel materials and both high resolution and high throughput synchrotron radiation diffraction is an essential supplement to laboratory X-ray facilities for a range of projects. For example, powder diffraction from samples as they grow in liquid media can be used to understand the mechanisms that control directed and anisotropic growth. Responses of samples, specially prepared as thin films, to hydrogen loading over a wide range of momentum transfer can give information about the relative effects of lattice distortion, role of boundaries and introduction of defects in overall properties. Wide angle diffraction is also key to studying orientation in many soft materials. Research constellation: Adrian Rennie and Bjrgvin Hjrvarsson lead the Materials Physics Division at the ngstrm Laboratory, Uppsala University with about 30 researchers (about 10 seniors and 20 juniors) working on soft matter, magnetic materials and hydrogen in metals. The work explores the effects of restrictions in size and dimensions on physical properties. There is extensive support from national funding bodies and the division participates in a wide number of international co-operations. Nano Particles In situ characterization of nano-particle nucleation and growth under super- and subcritical conditions. In situ investigation of energy materials (e.g. fuels cell materials, thermoelectric materials, battery materials, cement materials, catalysts). High resolution powder diffraction for structure solution, Rietveld refinement and maximum entropy method charge density studies. Studies of structural and magnetic phase transitions. Research constellation: Bo Brummerstedt Iversen, Director, Professor, dr. scient., DG Centre for Materials Crystallography, iNANO and Department of Chemistry, Aarhus Universitet Gas/solid Liquid/solid reactions Studies of chemical reactions at high pressure (gas/solid and liquid/solid), crystal structures of new compounds, preparation of new energy materials for hydrogen storage, in situ studies of cement materials. Research constellation: Torben R. Jensen, Lektor, Ph.D., DG Centre for Materials Crystallography, iNANO and Department of Chemistry, Aarhus Universitet Non-ambient conditions Structural studies at high and low temperatures as well as high pressure including studies of structural phase transitions and magnetic structures. Synthesis of inorganic materials. In situ studies of chemical reactions at elevated temperatures and hydro/solvo-thermal conditions. Research constellation: Jens Erik Jrgensen, Associate Professor, Ph.D., Department of Chemistry, Aarhus University Biominerals Studies of biomineralization and synthesis of bioinspired materials. Studies of kinetics of crystallization of nanoparticles and higher order hierarchical aggregates in water and/or organic solvents. Phase transformations of polymorphs and amorphous precursors. Kinetics of gel formation, e.g. induced by coordination chemistry of metals. Lattice strain and its correlation with nanoparticle size and the presence of included organic additives. Research constellation: Henrik Birkedal, Associate Professor, Ph.D., Department of Chemistry and iNANO, Aarhus University

Energy Materials In situ characterization of crystallization of nanoparticles under super- and subcritical conditions. Insitu investigation of functional materials such as solid oxide fuel cells, thermoelectric materials, and battery materials. Research constellation: Mogens Christensen, Assistant Professor, Ph.D., DG Center for Materialekrystallografi, iNANO, Department of Chemistry, Aarhus University Molecular containers as reaction vessels Cavities on a molecular level are important for the specific binding of guest molecules and for subsequent chemical reactions. This is observed in nature (enzymes and enzyme catalysis) but is also used in industrial processes (zeolites, MOFs). Homogeneous systems in which a soluble container molecule can act as a novel type of receptor for substrates and is able to initialize chemical reactions were developed during the last decade. Our aim in this field is to prepare and characterize metallosupramolecular containers bearing a negative charge and therefore act as hosts for cationic species or promote reactions involving cationic intermediates. The systems are characterized in solution by NMR and ESI MS or by Small Angle Scattering. However, for the structural understanding of the system (cavity size, size of pores, orientation of guests in the cavity) solid phase structural investigations are crucial. Due to the porosity of the corresponding crystals and disorder of encapsulated solvent molecules and guests conventional X-ray does not lead to sufficient diffraction data. The use of synchrotron radiation is a great chance to overcome these problems. Research constellation: Markus Albrecht, RWTH Aachen University, Roland Frhlich, University Mnster, Martin Nieger, Markku Leskel, University Helsinki. The group of scientists is well chosen in order to generate synergism by combining the expertises in the fields of supramolecular chemistry, organometallic chemistry and structural chemistry. From pharmaceutical solid forms to optimal medicinal products To create optimal medicinal products requires understanding and control of structural aspects of pharmaceutical solids. The aim of this research project is to establish firm links between molecularlevel structure of pharmaceutical solid forms and the functionality of resulting medicinal products. For this purpose, it is vital to characterize the wide variety of molecular solid forms that result from pharmaceutical solid-form screening experiments, without hindrance for the most challenging cases. At a basis level, synchrotron facilities are required for cases where home-lab instrumentation cannot achieve diffraction of sufficient intensity. This includes small single crystals and microcrystalline powders. One more challenging aspect of this project is to target semi-crystalline solid forms, with differing degrees of long range order. Here, the high intensity of the synchrotron source is required to measure effectively structured diffuse scattering, for complete characterization of local structure. The opportunity to combine these diffraction experiments with non-ambient sample conditions (especially relative humidity) is particularly valuable for these studies. Research constellation: Andrew D. Bond, Department of Physics and Chemistry, University of Southern Denmark; Jukka T. Rantanen, Faculty of Pharmaceutical Sciences, University of Copenhagen. This constellation combines two Danish research groups, with expertise in structural and experimental aspects of pharmaceutical solid forms. In-situ powder diffraction In situ studies of materials for energy technology: Synthesis, transformation and operation. Examples are materials for lithium batteries, superconductors and catalysts. High resolution powder diffraction for structure solution and Rietveld refinement. Research constellation: Poul Norby, Senior Scientist, Ph.D., Materials Research Division, Ris, DTU.

Temperature-Pressure In situ characterization of new materials: high-temperature, high-pressure behaviour, phase transitions. Biological materials as bone tissue and protein conformations. Research constellation: Kenny Sthl, Associate Professor, Ph.D., Dept. of Chemistry, DTU. Catalysts at extreme conditions In situ anomalous powder diffraction of catalysts under working conditions: high-temperature, up to 100 bar pressure, in gas flow. High resolution powder diffraction for phase identification and Rietveld refinement. Research constellation: Alfons Molenbroeck, General Manager, Dr. Ir., Characterization Department, Haldor Topse A/S. Pharmaceutical polymorphs Ab initio crystal structure determination of compounds in pharmaceutical development and their polymorphs, and studies of phase transitions between such polymorphs. Research constellation: Anette Frost Jensen, Ph.D., Analytical Chemist, Preformulation, Analytical R&D, H. Lundbeck A/S. Chiral Porous 3-D Networks The proposed research programme, bringing together two complementary teams, focuses on novel highly porous chiral self-assembled molecular materials offering controlled (dimension and space orientation) cavities, channels and other three dimension structures. These highly porous solids will be generated upon combining enantiomerically pure organic tectons based on chiral spacers of different lengths and appropriate metal ions. The organic spacers will either bear two or more monodentate coordinating sites or e.g. will be attached to a C60 Buckminster fullerene core which holds and orientates them in defined directions. In both cases, higher periodic assemblies will be generated in the presence of suitable metal ions. These networks will in term be used to specifically functionalize surfaces in order to built device prototypes with high technical potential. The material obtained would need sophisticated spectroscopic evaluation (XPS, XAS). For the structural understanding of the systems (cavity size, size of channels) solid phase structural investigations are crucial. Due to the porosity of the corresponding crystals and disorder of encapsulated solvent molecules in many cases conventional X-ray does not lead to sufficient diffraction data. The use of synchrotron radiation is a great chance to overcome these problems. Research constellation: Stefan Brse, Karlsruhe Institute of Technology, Karlsruhe, Germany; Markku Leskel, Martin Nieger, Helsinki University. This constellation combines the groups and expertise of three senior researchers. The constellation is worked now for nearly eight years.

Design and synthetic modifications of Metal-Organic-Frameworks (MOFs) for catalytic applications The recent advent of metal-organic frameworks (MOFs), rigid coordination polymers formed from metals and organic linkers (mostly, aromatic carboxylic acids or pyridines) has created a lot of interest into these materials in many different research fields. The modular design principle, the endless diversity and the attractive properties like being highly ordered, crystalline and highly porous, tuneable pore size, low density, catalytic activity and ability for gas storage (e.g. H2) add to the attractiveness of these materials. More than 4000 different MOFs have been reported already, and recent reports on the postsynthetic modifications of MOFs (synthetic modifications after the MOF formation) expand the scope even further. However, so far all of these postsynthetic modifications are quite limited in scope and rely on rather simple functional group manipulations (e.g. acylation of a NH2-funtionalized MOF). With our research program we want to develop new and efficient postsynthetic modification methods. A successful implementation would potentize the structural possibilities. Besides this, we are involved in the de novo synthesis of new chiral MOFs and their application in catalysis. Heterogeneous asymmetric catalysis employing chiral highly porous MOF catalysts is highly attractive. In both projects the structural characterization of the MOF materials is key to success and a sound crystal structure analysis is essential. Unfortunately, due to the structural complexity and dimensions of MOF, in many cases more traditional X-ray spectroscopic methods fail and the use of a synchrotron is the method of choice. Research constellation: Frank Glorius, Roland Frhlich, University Mnster, Markku Leskel, Martin Nieger, University Helsinki. This constellation combines the groups and expertise of four senior researchers. Structure characterization of porous materials and organo- and organometallic catalysts Berzelii Center EXSELENT on Porous Materials is a center of excellence initiated by VR and VINNOVA. The consortium consists of 55 researchers from SU, YKI and industrial partners working in four research areas: heterogeneous catalysis, gas separation and storage, biomaterials, new porous materials and characterization. We design and synthesize porous crystalline materials with novel framework structures with high surface area and unique pore structures. We develop new organometallic catalysts and immobilize them in the pores. X-ray diffraction has been the most important technique for determining the structures of our new materials and catalysts. Our structure determination requires routinely high coherent and high flux synchrotron sources since the porous materials and catalysts often form micro-sized crystals, too small for in-house X-ray diffractometers. High-resolution powder X-ray diffraction has been important for structure determination of nano-sized crystals. We have a unique competence in new method development to push the limit of the structure determination, for example combining powder X-ray diffraction with electron crystallography, which resulted in several publications in Nature and Science. The different sample environment stages will allow us to perform in situ experiments to study the crystallization, structural dynamics, gas adsorption properties and catalytic reactions. We are also seeking new possibilities of using the proposed X-ray diffraction beam-line for our research in developing new porous materials and new catalysts. Research constellation: Prof. Xiaodong Zou, Director of Berzelii Center EXSELENT on Porous Materials, Dept. of Materials and Environmental Chemistry, Stockholm University.

Design and synthesis of new microporous inorganic and metal-organic framework materials Porous materials are of scientific and technological interest because of their ability to interact with guest atoms, ions and molecules not only at their surfaces, but throughout the bulk of the material. They are important for applications in catalysis, gas storage and separation and controlled delivery. The project is to design and synthesis of porous crystalline materials with novel framework structures with high surface area and unique pore structures. Our group has synthesized more than 80 new microporous inorganic and metal-organic framework materials such as extra-large pores, pores with unique shapes and chiral or helical channels. X-ray diffraction has been the most important technique for determining the structures of our new materials. Our structure determination requires routinely high coherent and high flux synchrotron sources since the porous materials often form micro-sized crystals, too small for in-house X-ray diffractometers. High-resolution powder X-ray diffraction has been important for structure determination of nano-sized crystals. We have a unique competence in new method development to push the limit of the structure determination, for example combining powder X-ray diffraction with electron crystallography, which resulted in several publications in Nature and Science. The different sample environment stages will allow us to make in-situ experiments to study the crystallization, structural dynamics, gas adsorption properties and catalytic reactions. We are also seeking new possibilities of using the proposed X-ray diffraction beam-line for MAX IV for our research in developing new porous materials and new catalysts. Research constellation: Prof. Xiaodong Zou, Assistant Prof. Junliang Sun, Dept. of Materials and Environmental Chemistry, Stockholm University. Transition Metal Oxides Our research concerns the synthesis and characterization of novel transition metal oxide compounds. Some of these compounds will have new and novel structures others will have know type structures, which are distorted. The structural refinements of these structures can be a challenge and then high intensity high resolution data, which can be obtained at a high performance X-ray Diffraction beamline as that suggested at MAX IV are of great value. It is of course also important that this instrument has facilities such as cryostats, a furnace, reaction chambers so that structural studies can be made in a number of environments. Such set up would also make it possible to study chemical reactions in situ which is of interest for us as several of the materials we study are possible candidates as electrode or electrolyte materials in fuel cells. Research constellation: Gunnar Svensson, Dept. Materials and Environmental Chemistry, Stockholm University.

Main Constellations Committed to the Beamline Project Materials Chemistry, Uppsala Univ. represented by Kristina Edstrm, Professor at Inorganic Chemistry The research in inorganic chemistry is directed towards the chemistry of both thin films and bulk solid materials. The long-range objective is to obtain a deeper understanding of dynamics and mechanisms of reactions at interfaces as well as relationships between properties and atomic, defect and electronic structures of the materials. The ngstrm Advanced Battery and Fuel Cell Centre is today established as one of Europes leading basic research environments for the development of electrochemical energy storage and conversion materials for the battery and fuel-cell technologies of tomorrow. The unit consists of approximately 10 senior staff members and 20 junior staff members. Materials and Environmental Chemistry, Stockholm University represented by Xiaodong Zou, Professor and Head of Inorganic and structural chemistry, Director of Berzelii Center EXELENT The research activities include new methods of synthesis, preparation of new compounds and materials, developing and implementing structural investigation methods by using X-ray, electron and neutron diffraction, scanning and transmission electron microscopy and various spectroscopic methods. Examples of current research areas are synthesis and characterization of porous crystals, complex oxides, oxynitrides, metal hydrides, low-dimensional compounds, intermetallic compounds and ceramic materials. We study the physical, chemical and mechanical properties of the materials and explore their applications for example in catalysis, energy storage and generation, molecule separation and as thermoelectric materials. Our competence on structural characterization is important for exploring the relationship between structure and properties. Polymer- and Materials Chemistry, Lund University represented by Sven Lidin, Professor. Materials characterisation and structure determination is carried out using techniques such as high resolution transmission electron microscopy (HRTEM) for nanoscale materials at atomic resolution, scanning electron microscopy in combination with energy dispersive X-ray analysis (EDX) or electron energy loss spectroscopy (EELS) for determining chemical composition at nanometer resolution and various X-ray diffraction techniques. Materials that are investigated include nano structured semiconductors (in collaboration with the Lund nanometer structure consortium), catalysts (in collaboration with the Department of Chemical Engineering), clay minerals for nuclear waste storage and thermoelectric compounds. The latter are also synthesised at the division. Thin Film Physics, IMF, Linkping University represented by Jens Birch, Professor Our aim is to increase the fundamental understanding of vapor phase growth and reactions in thin films on an atomistic level, and to explore physical properties of structures unique to thin solid films. The strategy is to carry out basic research studies for describing the relationships between growth parameters, structure/composition and physical properties of thin films. The research covers several materials and growth techniques, and often forms the basis for new materials & processes of interest for future applications. Joined research groups in Denmark represented by Kenny Sthl, Associate Professor Department of Chemistry, DTU The constellation consists of researchers from Department of Chemistry, Aarhus University; Materials Research Division, Ris; Department of Chemistry, DTU; Haldor Topse A/S; H. Lundbeck A/S. The researchers from Aarhus University covers five research groups, two research centers and approximately 70 people, who each year have about 4 months of beamtime at synchrotrons around the world of which ca. 2 months are at MAX II. The constellation routinely performs advanced characterization of crystalline materials, this is important for a broad range of materials technologies such as development of new materials within nano-, environmental, and energy technologies, studies of pharmaceutical products and fundamental research. Danish research has a long tradition in experimental research at world leading synchrotron facilities. Several of the researchers have much experience in the development of in-situ, and environmental cells for powders and single crystals. Advisory Comity Phil Pattison, Senior Beamline Scientist, Deputy Director SNBL, ESRF Chiu Tang, Principal Beamline Scientist I11 (High Resolution Powder Diffraction) Diamond Lighsource Ltd. Sten Eriksson, Professor, Environmental Inorganic Chemistry, Chalmers.

Budget Item Undulator insertion device Front end Radiation shielding & PSS Monochromator system Vacuum system Slits & diagnostics Infrastructure Electronics & controls & computing Control room & prep. lab. Focusing optics 4-circle diffractometer kappa geometry moved from I711 2D pixel detector Heavy-duty 3-circle diffractometer (incl. sample stages, motors and controls) Multi-analyser stage (48 double bounce channel cut crystals, rotary tables, and detectors) Position sensitive detector (pixel type) Environmental stages Sample changer & robot (powder diffraction) 6-circle diffractometer moved from I811 Total Table 1: Time plan 2011 2012

Price ( in 1000 SEK) 12.000 5.000 5.000 4.000 2.000 4.000 5.000 5.000 2.000 4.000 200 5.000 4.500 5.500 10.000 2.000 2.500 200 77.900

2013 2014 2015 2016 Detailed design Undulator + FE design Undulator + FE Hutches + infrastructure tender call build Undulator + FE production Undulator + FE inst. Beamline + optics tender call Beamline + optics production Beamline + optics inst. PD goniostat + detector tender call PD goniostat + detector construction PD goniostat inst. PD commissioning SC goniostat inst. SC commissioning . SD goniostat inst SD commissioning beamline External work end stations

Paperwork

Based on Table 1 we estimate the following personnel requirements during construction and commissioning, assuming that the beamline components will be installed by the manufacturer. Table 2: Man-years to be financed 2011 2012 2013 2014 2015 2016 Man-years 1 2 3 4 6 6 The main constellations committed to the beamline will contribute with expertise during the design phase and as friendly users during the commissioning phase. There will also be a development of experiment specific environmental stages.

A SAXS/ WAXS beamline Spokespersons: Yngve Cerenius MAX-lab, Ulf Olsson, Physical Chemistry, Lund University, Jan-Skov Pedersen, Dept. of Chemistry, Aarhus University, Denmark, Adrian Rennie, Materials Physics Division, Uppsala University An undulator based beamline for small angle X-ray scattering (SAXS) experiments with simultaneous wide angle X-ray scattering (WAXS) capacity. The unique low emittance on the MAX IV 3 GeV ring will permit a design where a small X-ray spot size can be combined with a very small divergence. It permits keeping a small spot size on the sample while extending the sample to detector distance to be able to measure very small scattering angles. This flexible set-up will enable obtaining structural information (size, shape and inter-particle interactions) on length scales ranging from 0.1 to almost 1000 nm. The studies will include a large range of materials, and the multipurpose SAXS/WAXS instrument will have a very broad user community coming from different fields of science and technology, as well as industry. A very wide range of samples will be studied under a range of different conditions and experiments. In all cases the experiments will be able to exploit the high quality X-ray light produced at the MAX IV 3 GeV ring : the high brilliance, the low divergence, the tunable photon energy and the high fraction of coherence. The SAXS set-up will be of a pinhole camera type where the sample to detector distance can be varied to up to 10 m. A separate detector system for simultaneous WAXS measurements will be mounted next to the sample. The continuously tunable energy will allow anomalous SAXS (ASAXS). There will be possibilities for windowless measurements which are essential for weakly scattering samples. The experimental set-up will be equipped with a generous amount of different sample environments including temperature control, flow, stopped flow and a rheometer. The set up will permit the use of an additional goniostat for grazing incidence SAXS (GISAXS) measurements to study surfaces. The high fraction of coherence will allow for the performance of X-ray photon correlation spectroscopy (XPCS) and coherent diffraction imaging. To exploit this option fully particular care will be devoted to the detection system of the instrument. Main constellations committed to the beamline project: Physical Chemistry, Lund University Dept. of Chemistry, Aarhus University Materials Physics Division, Uppsala University Dedicated user groups: Dept. of Molecular Biophysics, Lund University Salam Al-Karadaghi Dept. of Chemistry, Biochemistry & Biophysics, University of Gothenburg - Richard Neutze Dept.of Chemistry, University of Gothenburg Johan Bergenholtz Biomedical Laboratory Science & Biomedical Technology, Malm University Johan Engblom Materials Physics Division, Uppsala University Adrian Rennie Dept. of Physics, NTNU, Trondheim, Norway Jon Otto Fossum Polymers and Materials, Lund University Clays Staffan Hansen Dept. of Materials and Environmental Chemistry, Stockholm University Niklas Hedin Dept. of Physics, Institute for Energy Technology, Norway - Matti Knaapila Dept. Physical Chemistry, Lund University, - Ulf Olsson Dept. of Chemistry, Aarhus University, Denmark Jan-Skov Pedersen Div. of Combustion Physics, Lund University Frederik Ossler Div. of Surface and Corrosion Science, School of Chemical Science and Engineering, KTH, Stockholm - Per Claesson Eka Chemicals AB, Caterina Camerani Faculties of Life & Pharmaceutical Science, University of Copenhagen Lise Arleth Diabetes Protein Engineering, Novo Nordisk A/S Proteins/ peptides Gerd Schluckebier Dept. of Physics, Helsinki University Polymers & Proteins - Ritva Serimaa Dept. of Medical Physics/ Karolinska University Hospital; Dept. of Oncology-Pathology, Karolinska Institute - Albert Siegbahn

Scientific Motivations In soft matter, colloid science and biological systems one typically deals with structures occurring on the so called colloidal length scale ranging from approximately a nanometer up to a micrometer. Examples are many: polymers, gels, rubbers, proteins, bio-membranes, nanoparticles, and viruses. In addition, many hard materials, like metals and alloys, have textures on this particular length scale.

Fig 1. A very large number of systems share the colloidal length scale. [1] Small angle X-ray scattering (SAXS), often combined with additional wide angle (WAXS) detection, is ideally suited to investigate structures on the colloidal length or nanometer scale.[2]. Hence, a SAXS instrument has a large and broad user community from essentially the whole range of scientific disciplines: Physics, chemistry, biology and medicine including the related technology or engineering areas. Indeed, The Colloidal Domain is probably the arena where all these disciplines meet. [3] Soft matter and colloidal materials have for several decades been a very strong Swedish and Nordic research area with roots back to the pioneering work of e.g. Per Ekwall and Theodor Svedberg. In these research areas there is often only a tiny step between basic science and applications. Hence one finds significant collaborations between industry and academia today and we can foresee an increased demand for synchrotron SAXS from various industry groups in the future. Because of the very broad user community, the primary SAXS/WAXS instrument at MAX IV needs to be a multipurpose instrument. A large variety of systems will be investigated under a wide range of conditions in different kinds of experiments. In order to secure the state-of-the-art performance for such a wide range of experiments, the instrument has to be carefully designed and, furthermore, it requires a significant staff of beamline scientists and engineers to provide the necessary range of competence. However, the fact that these ambitious goals of broad applications are achievable, has been proven elsewhere, for example, at the high brilliance beamline ID02 at the European Synchrotron Radiation Facility (ESRF) in Grenoble [4]. The issues of the broad range of applications and the demand for highly qualified staff are explicitly addressed in the beamline design and annual budget.

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O. Ikkala and G. ten Brinke, Chem. Comm., 2131 (2004) T. Narayanan Curr. Opinion Colloid Interface Sci. 14, 409 (2009) 3 nd D. F. Evans and H. Wennerstrm The Colloidal Domain, 2 ed. Wiley-VCH, New York (1999) 4 http://www.esrf.eu/UsersAndScience/Experiments/SoftMatter/ID02/

Experiments performed at the proposed SAXS/WAXS beamline will be able to use the particular and, in some cases, unique properties of the MAX IV X-ray beam: (1) The high brilliance, (2) the low divergence and (3) the high coherence of the beam. Below we will describe, by using examples, projects/experiments that will benefit from the high quality of the X-ray beam. Making use of the high brilliance The highly brilliant X-ray beam allows definition of a very small well-collimated beam that readily permits measurements at very small angles, which in combination with the variable sample-to-detector distance, typically 0.5-10 m, results in a very wide range of scattering vectors, q. Using the low-q region With the large detector distance the low q limit will be <0.01 nm-1, corresponding to a real space length scale of almost 1 m. This will allow studies of significantly larger structures (orders of magnitude) compared to those studied, for example, at the existing MAX II SAXS beamline, and in particular compared with general lab source instruments. Examples of systems for which the extended q-range is essential are peptide self-assembly, viruses and other protein complexes, amyloids, clays, emulsions, only to mention a few. Using the small spot size The small spot size allows experiments with small samples/volumes. This is important because in particular many biological materials can only be obtained in very small quantities. Here, we can foresee an extensive use of microfluidic devices [5] that can mix, pump, and, in the near future, also shear very small liquid volumes. For samples sensitive to radiation damage, one also needs to flow samples in order to bring down the exposure time per unit sample volume. [6] Here again microfluidics is useful in keeping the total sample volume to a minimum. Another important application of the small spot size is that it allows for scanning heterogeneous samples/specimens with the X-ray beam. In fact the scanning SAXS option at this beamline will be a very important complement to a nanofocus beamline. In many materials, like bone [7], the hierarchical structure that covers many orders of magnitude in length scale makes it necessary to employ both micro- and nanofocus beams, as well as wider beams. Using the brilliance for time resolution The high brilliance allows short exposure times, which in turn opens up the possibility for time resolved experiments. [8] A sample is rapidly perturbed away from equilibrium, and scattering profiles are recorded in separate frames, time resolved, following the return to equilibrium. Typical perturbations, include composition (stopped flow), temperature and pressure jump. The dead time in all these perturbations are typically a few ms, although for stopped flow it can be significantly reduced (order of magnitude) when turning to microfluidic manipulations of small volumes. This means that it is possible to follow dynamic processes typically with ms resolution. With this time resolution there are many interesting processes like dissolution and self-assembly, precipitation and spinodal decomposition that can be studied. A recent study on block copolymer micellization by Lund et al. [9] illustrates the current state of the art of the stopped flow approach. A study that exploited the full potential of high brilliance was a time resolved study of muscle contraction, elucidating the molecular basis of muscle braking and its rapid control.[10] Solution scattering With a high photon flux, small or weakly scattering samples can be studied. However, soft matter and biological systems are strongly susceptible to radiation damage and having high photon flux is not
K. Nrgaard Toft, B. Vestergaard, S. S. Nielsen, D. Snakenborg, M. G. Jeppesen, J. K. Jacobsen, L. Arleth, and J. P. Kutter, Anal. Chem. 80, 3648 (2008) 6 J. S. Lamb, B. D. Zoltowski, S. A. Pabit, B. R. Crane, L. Pollack, J. Am. Chem. Soc. 130, 12226 (2008) 7 P. Fratzl, R. Weinkamer, Prog. Mater. Sci. 52, 1263 (2007) 8 P. Panine, S. Finet, T. M. Weis, T. Narayanan, Adv. Colloid Interface Sci. 127, 9 (2006) 9 R. Lund, L. Willner, M. Monkenbusch, P. Panine, T. Narayanan, J. Colmenero, D. Richter Phys. Rev. Lett. 102, 188301 (2009) 10 E. Brunello, M. Reconditi, R. Elangovan, M. Linari, Y. B. Sun, T. Narayanan, P. Panine, G. Piazzesi, M. Irving and V. Lombardi Proc. Natl. Acad. Sci. USA 104, 20114 (2007)
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sufficient. In order to keep the exposure time short, the scattered intensities need to be detected with highest possible efficiency and the background has be kept to a minimum. With a properly designed instrument, high-quality data can be obtained on an absolute scale and analyzed even though the signal may be more than 90 % composed of background [11]. For very weak signals, background subtraction becomes extremely crucial. This is illustrated in Figure 2 (top) where a WAXS pattern recorded from a dilute vesicle dispersion below the chain melting temperature is shown together with the water background. The bottom figure shows the scattering pattern after the background had been subtracted. Now a Bragg-like peak resulting from the ordered alkyl chains is clearly seen. [12]

Fig 2 (Top) WAXS pattern from sample and the water background. Essentially only the water scattering is observed. (Bottom) Difference pattern obtained after background subtraction resolving the Bragg-like peak associated with the ordered alkyl chains.

A rapidly growing field within solution scattering is the application to dilute solutions of biomacromolecules. [13] SAXS is almost the only structural technique for studying the structure of large complexes and flexible structures. Also in cases where the atomic structure can be obtained by other techniques, SAXS is widely used for checking for artifacts from crystal packing [14] or for studying association, aggregation and fibrillation of biomolecules [15]. Using the low divergence The low divergence of the beam gives a high q-resolution which is useful for example in doing crystallography of soft mesoscale liquid crystalline samples. Examples of studies that in addition rely
A. Shukla, T. Narayanan, D. Zanchi, Soft Matter 5, 2884 (2009) P. Saveyn, P. van der Meeren, M. Zackrisson, T. Narayanan and U. Olsson, Soft Matter 5, 1735 (2009) 13 D. I. Svergun and M. H. J. Koch Rep. Prog. Phys. 66, 1735 (2003) 14 (C. B. F. Andersen et al. Nature 443, 663 (2006) 15 C. L. P. Oliveira, M. A. Behrens, J. Sondergaard Pedersen, K. Erlacher, D. Otzen, J. Skov Pedersen J. Mol. Biol. 387, 147 (2009)
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on the high brilliance can be found in the work of Tiberg and his coworkers at Camurus AB in Lund in their studies of internally structured lipid nanoparticles, developed for the formulation of drugs and related compounds.[16] and in studies of colloidal crystals [17] [18] In many of those studies the use of synchrotron SAXS is essential. Using the tunable wavelength ASAXS In anomalous small angle X-ray scattering (ASAXS) one can, by carefully varying the photon energy around the absorption edge of an atom, perform contrast variation experiments that highlights the scattering coming from a particular element in a multicomponent mixture. [19] The approach is similar to the contrast variation often performed in neutron experiments by specific deuteriation. The technique has been recently used for example to probe the counter-ion concentration profile around nucleic acids [20] and studying bimetallic nanoparticles [21]. Using the coherence A unique property of the X-rays produced at MAX IV is the high fraction of coherence which will allow for X-ray photon correlation spectroscopy (XPCS) experiments [22] as well as coherent diffraction imaging (CDI) [23]. Such experiments will exploit the unique properties of the MAX IV light source and the demand is expected to increase significantly in the near future. The XPCS method is complementary to neutron spin-echo and is typically well suited to study e.g. internal mode dynamics in biopolymer and membrane systems although particular care has to be taken concerning radiation damage. A portfolio of sample environments The general or multipurpose SAXS/WAXS beamline will host a significant portfolio of sample environments, many of which are expected to be developed in collaboration with users. It also needs to allow for users to bring in and mount their own specialized equipment, when appropriate. The portfolio of sample environments will develop over time depending on the demands of the user community. Sample environments that will be available already at the initial state includes: (i) Peltier controlled flow through cells and capillary holders for solution scattering and also sample holders for pastes and solids, (ii) a stopped-flow system, (iii) a rheometer for rheo-SAXS and (iv) equipment for Grazing incidence SAXS (GiSAXS). In addition, we expect that sample environments based on microfluidic manipulations will develop fast and play a significant role in the near future. Many soft matter systems show a complex rheological behavior because of structural and even phase transformations may be induced by the shear. SAXS is an ideal technique to study such structural transformations using transparent shear tools (often Couette flow) in the rheometer. Determining near surface structure is of major interest as many applications require a balance of surface and bulk properties. GiSAXS is rapidly growing as it allows studies of organization in thin films. It complements reflectivity measurements that provides data about the average of structure in a direction normal to the surface by providing data on lateral structure. Examples range from surface hardened metals, through co-extruded polymer films to models of drug delivery materials. Although many people have used both SAXS and GiSAXS in a qualitative (or pictorial) manner it is now evident that advances in calculations allow quantitative interpretation.[24] This scattering is now attracting attention to investigate lithographic nanonostructures, copolymers, composites and biological materials.

J. Barauskas, M. Johnsson, F. Tiberg, Nano Lett. 5, 1615 (2005) A. V. Petukhov, D. van der Beek, R.P.A. Dullens, I.P. Dolbnya, G.J. Vroege and H. N. W. Lekkerkerker, Phys. Rev. Lett. 95, 077801 (2005) 18 A. B. D. Brown, C. Ferrero, T. Narayanan and A. R. Rennie European Physical Journal B 11, 481 (1999) 19 M. Ballauff, A. Jusufi Colloid Polym. Sci. 284, 1303 (2006) 20 S. A. Pabit, K. D. Finkelstein, and L Pollack, Methods in Enzymology 469, 391 (2009) 21 J. Haug, H. Kruth, M. Dubiel, H. Hofmeister, S. Haas, D. Tatchev and A. Hoell, Nanotechnology 20, 505705 (2009) 22 F. Westermeier, T. Autenrieth, C. Gutt, O. Leupold, A. Duri, A. Menzel, I. Johnsson, C. Broennimann and G. Grbel, J. Synchrotron Rad. 16, 687 (2009) 23 E. Lima, L. Weigart, P. Pernot, M. Howells, J. Timmins, F. Zontone and A. Madsen, Phys. Rev. Lett. 103, 198102 (2009) 24 S. Frster et al. J. Phys. Chem. B 109, 1347 (2005)
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Beamline Description Beamline Summary Energy (wavelength) range Photon Source Optics Spot Size Experimental Techniques 5 30 keV (0.4 2.5) In-vacuum Undulator (pmuA) Channel cut Si(111) and Si(311) monochromator & focusing optics that could either consist of compound refractive lenses or KB mirrors. Down to 30 m (dep on acceptable divergence) Structural analysis over lengths scales between ~ 1 to greater than 5000 . Techniques: SAXS, ASAXS, GISAXS, XPCS, coherent diffraction imaging

Source and Front end The planned insertion device for the beamline is an in-vacuum undulator of hybrid type on the MAX IV 3 GeV ring. The most important parameters are listed in Table 1. Undulator (Hybride type) Length [mm] Magnetic Gap [mm] Period Length [mm] Peak Field [T] Total Power [kW] On Axis Power Density [kW/mrad2] Table 1 Undulator parameters The total power and especially the on axis power density of the synchrotron beam require precautions to be taken to avoid failure of the first crystal in the monochromator. In this study a 150 micron diamond window has been added in the front end. In addition there will also be a water cooled aperture, beam monitors and a white beam safety shutter. Optics Hutch At 22.5 m from the source is the front end flange situated just on the outer side of the MAX IV storage ring shielding wall. The rather generous space in the MAX IV hall permits a flexible optical solution where different types of optics can be used for different types of experiments or space is set aside for possible upgrade scenarios. Monochromator For beam stability reasons the preferred monochromator would be a liquid nitrogen cooled channel-cut Si(111) & Si(311). Another option is a standard fixed exit double crystal monochromator (DCM) equipped with Si(111) and (311) crystals with liquid N2 cooling. The Si(111) crystals will be used for energies below 20 keV while the Si(311) crystals are intended for higher energies. Focusing optics The other main optical element of the beamline is a focusing or collimating optics situated after the monochromator. The purpose is to focus the beam onto the detector while changing the sample to detector distance up to 10 meter. When extending the sample to detector distance it is critical to keep a small divergence of the incoming X-ray beam to have a small spot size on the sample. The optics must therefore permit focusing down to a spot size of 30 m when high spatial resolution is required but for most applications the preferred options would be a more parallel beam and accepting a slightly larger beam size. Several optical schemes would provide this possibility. A number of SAXS beamlines with similar design have chosen a bimorph KB mirror pair. With this type of mirrors it is possible to change the geometry from a more focusing to a collimating one depending on the requirements. However, a thorough survey of the performance of these types of mirrors must be done before any decision. 3783.25 4.2 18.5 1.24 13.3 97.1

Another attractive option would be to use a set of compound refractive lenses in combination with a flat mirror for harmonic rejection. Coherence The small emittance of the MAX IV 3 GeV ring will give a very high degree of coherence on the emitted radiation. That could be used for X-ray Photon Correlation Spectroscopy experiments. However, precautions must be made in order to preserve the coherence until the experimental set-up. Neither reflective (unless produced with extreme tight tolerances) nor refractive optics will preserve this property. Therefore it should be an option to move out the focusing optics and only define the beam with slits, thus accepting less intensity but having a higher degree of coherence. Experimental Hutch The components inside the experimental hutch include a slit system to exclude any parasitic scattering and a fast shutter. For normal transmission SAXS measurements a large area 2D detector will be mounted inside a long vacuum chamber, see fig. 3. Although technically challenging this could be solved with different techniques, i.e. as at the Swing beamline at Soleil using a vacuum compatible detector or as on ID2 at ESRF where the detector is placed inside a submarine inside the large vacuum chamber. This will ensure the needed flexibility for rapid camera length changes. It should be noted that to ensure the possibilities for XPCS measurements requirements must be made on the area detector for small pixel size, high dynamic range, low background and fast read out. For instance the Pilatus detector from Dectris is expected to fulfill all these demands. The variable length of the vacuum chamber will enable sample to detector distances up to 10 meters. In addition a WAXS detector will be mounted close to the sample so it covers scattering angles up to 90.

Fig 3 The experimental set-up of the SAXS/WAXS beamline including a 10 m long vacuum chamber with a movable area detector inside Sample Environment The experimental set-up where the complete vacuum system can be moved back and forth on a rail system would permit the usage of a wide range of different sized samples and sample cells. A generous amount of sample environments must be incorporated from the beginning both hard- and software wise. These include flow, stop-flow, shear and temperature controlled cells. A goniostat for GISAXS (gracing incidence SAXS) for surface analysis will also be added. It is essential that the system will permit windowless measurements on weakly scattering samples, e.g. low concentration of proteins in solution.

From single molecules to oligomeric complexes: Function through self-assembly & dynamics Frataxin plays a central role in the storage and detoxification of surplus mitochondrial iron through oxygen-dependent oxidation of Fe2+ to Fe3+ and its storage in the form of a ferrihydrite mineral. Frataxin oligomers also play a key role in controlling metal specificity of iron requiring reactions in mitochondria, among which are heme biosynthesis and the generation of iron-sulphur clusters (ISC). Several human diseases are related to disorders in iron trafficking. One of them is the neurodegenerative disease Friedreich ataxia that is linked to frataxin deficiency and defects (mutations). Using the SAXS beamline I711 at MAX-lab, we have recently performed several studies on metal-dependence of yeast frataxin self-assembly. These studies have resulted in two manuscripts under preparation. Currently we plan to extend these studies to the human frataxin to understand the role that the different oligomeric states play in iron delivery, storage and detoxification in mitochondria. AAA+ ATPases constitute a large class of proteins involved in diverse functions among which are proteolysis, DNA synthesis, membrane trafficking, cytoskeletal regulation and protein folding. Cobaltochelatase and magnesium chelatase are two enzymes from the AAA+ class of proteins. They function in the cobalamin (vitamin B12) and chlorophyll biosynthesis pathways and catalyse the insertion of cobalt and magnesium into a ring contracted tetrapyrrole hydrogenobyrinic acid a,cdiamide (HBAD) and protoporphyrin IX, respectively. The catalytic reaction is ATP-dependent and has been found to require 15 ATP molecules/ catalytic cycle, as determined in the case of magnesium chelatase. Our earlier and recent studies have demonstrated that magnesium chelatase and cobaltochelatase, have unique structural features not found in any other members of the AAA+ family. Within this project we will continue the study of the structural organisation and dynamics of cobalto- and magnesium chelatase subunits and their complexes. Research constellation: Salam Al-Karadaghi, Molecular Biophysics, Lund University Time-resolved wide angle X-ray scattering studies of membrane proteins Retinal proteins such as bacteriorhodopsin, sensory rhodopsin and visual rhodopsin are integral membrane proteins that harvest both the energy and information content of light to create chemical energy essential for the cell, and to provide information on the environment through photo-taxis and vision. We have recently developed a new approach to study the structural biology of light sensitive membrane proteins using time-resolved wide angle X-ray scattering. This work was performed at the dedicated time-resolved station of the European Synchrotron Radiation Facility and enabled us to visualize the entire history of protein conformational changes in light-driven retinal proteins from a time-scale of nanoseconds to milliseconds (Andersson et al., Structure 17, 1265 (2009)). We have also demonstrated how this method can be applied at a standard, monochromatic X-ray scattering beamline (cSAXS of the Swiss Light Source), where a time resolution of 10 milliseconds was achieved using a rapid-readout X-ray detector (Pilatus). We anticipate exploiting the two-orders of magnitude higher flux expected at the multi-purpose X-ray scattering beamline of MAX IV in combination with developments in X-ray detector readout rates, to push this temporal-resolution of this approach into the microsecond domain. We also foresee a tremendous growth in the method of time-resolved wide angle X-ray scattering applied to proteins during the next decade. In particular these advancements in combination with advanced nano-fluidic devices will enable the structural dynamics of irreversible, chemically triggered reactions to be probed with microsecond resolution. These studies will be complemented by the capabilities of the proposed short pulse facility at MAX IV, for which a sub-picosecond temporal resolution will be achievable for light-driven systems. Research constellation: Richard Neutze, Gergeley Katona, Sebastian Westenhoff, Dept. of Chemistry, Biochemistry & Biophysics, University of Gothenburg.

Fundamental studies of colloidal interactions and non-equilibrium microstructures A small-angle X-ray scattering (SAXS) instrument at MAX IV is essential for the study of macromolecules and colloidal-size structures in solution. At the University of Gothenburg studies of this sort are underway on well-characterized, often in-house-made, model systems in an effort to understand the coupling between many-body interactions, structures adopted in solution, and bulk system properties. Current interest is focused on interactions among fluorinated or partially fluorinated nanoscopic particles bearing grafted polymer. Such colloidal dispersions exhibit gel transitions under marginal solvent conditions where they produce highly random, ramified microstructures. The response of these structures to the application of a flow is of particular interest and has seen little systematic study so far. In situ SAXS under flow or rheo-SAXS are ideal probes of the connection between short- and longer-range microstructure and the rheological properties. Related systems without polymer sheaths are exemplary model systems for studies of long-range electrostatic interactions and their effect on structures under flow. These particles interact strongly even under dilute conditions and serve as a proving ground for non-equilibrium statistical mechanical theory for mirostructures under flow. In addition, the particles used in these studies can be refractive index matched, which allow for the rheo-SAXS measurements to be complemented by rheo-small-angle light scattering, available in house. Johan Bergenholtz is a senior staff member of the Dept. of Chemistry at the Universty of Gothenburg. Ongoing research projects utilizing small angle scattering are currently pursued together with Jan Skov Pedersen of Aarhus University and Malin Zackrisson of Lund University. Projects to be started in this area include a collaboration with Peter Holmqvist and Gerhard Ngele of FZ Jlich.

Lipid morphology in nature Understanding lipid morphology in nature is one core focus in our research at Malm University. The activities orient to structure of biological interfaces (like skin, mucosa, blood vessels, bone tissue, leafs), barrier functions, interactions with formulations or implants, transport mechanisms (e.g., of drugs), etc. A primary request for MAX IV would be a combined SWAXD beamline, where both SAXS and WAXS spectra could be obtained simultaneously. Below is a list of ongoing and planned projects where access to a SAXS/WAXS beamline at MAX IV would be highly valued: 1. Water a crucial factor in regulating biomembrane permeability (Malm University/HS & Lund University/Phys Chem1, funded by FLK, LU) 2. Humectants and their effects on skin barrier function - a mechanistic approach (Malm University/HS, YKI AB, ACO Hud Nordic AB & Eviderm AB, funded by KKs) 3. Hydration of mucous gel (Malm University/HS, funded by Mah) 4. Mucoadhesion: Drug carrier interactions at biologically relevant interfaces (Malm University/HS, Camurus AB, funded by KKs) 5. Adjuvants for products used in agriculture (Malm University/HS & AkzoNobel Surface Chemistry AB, funded by KKs) 6. Increased understanding of temporary forearm cutaneous anesthetisia aiming at improved hand sensibility (Malm University/HS & Lund University/Handsurgery, funded in part by Mah) 7. Screening of phase behaviour in the DOPS/DOPE/water system and effects on lipid morphology from a decrease in water chemical potential (Malm University/HS, funded by CLRF) 8. Symptomatic vs. asymptomatic atherosclerotic plaques (Malm University/HS & Lund University/CRC, funded in part by Mah) 9. The influence of biochemical coat for implant bone incorporation (Malm University/HS, OD & Promimic AB, funded by KKs) 10. A novel microemulsion for nasal drug delivery mucoadhesion and barrier response (Malm University/HS, Bioglan AB & Nares AB) 11. Attachable Diagnostic Devices with Individualised Referencing (ADDIR) (Malm University/HS) 12. Importance of cell membrane lipid composition for microbial acid tolerance adaptation of Streptococci (Malm University/HS, OD). Research constellation: Johan Engblom, Malm University and see above for individual projects

Colloidal Materials under External Fields interplay of structure and properties Colloidal materials consist of both self-assembled molecules and particles, as well as specifically prepared dispersions such as polymer lattices and inorganic particles. The physical properties are strongly correlated with structure and this is the focus of our research. High performance SAXS is a key technique to determine the structure on a nanometre scale and the correlations between particles. The technique complements laboratory tools and allows in-situ observation of the bulk of samples under the influence of applied fields such as shear or elongational flow, as well as electric and magnetic fields. The use of synchrotron SAXS allows temporal evolution of structures to be followed, both directly on a scale of milliseconds but also faster using stroboscopic techniques. Several sub-projects led by Adrian Rennie, Max Wolff and Vassilios Kapaklis can exploit this potential both for investigation of the materials prepared in the laboratory but for studies of the preparation process. Developments include use of structural evolution with copolymers as tools for templating nanodevices. Our vision is to use the continuum of scattering and spectroscopy with real time and real space resolution to probe materials. Research constellation: Adrian Rennie and Bjrgvin Hjrvarsson lead the Materials Physics Division at the ngstrm Laboratory, Uppsala University with approximately 30 researchers (about 10 seniors and 20 juniors) working on soft matter and interfaces, magnetic materials and hydrogen in metals. There is extensive support from national funding bodies and the division participates in a wide number of international co-operations. The scattering centre at ngstrm run by Adrian Rennie is a centre of expertise in these experiments. Complex Physical Phenomena in Clays and related Soft Matter Systems The long-term aim of this project is to develop basic understanding on how clay nano particles and related systems behave in various confined environments including under the influence of applied mechanical, electrical or magnetic fields. Among physical phenomena studied are self-organization of anisotropic nanoparticles, fluid transport through porous media, fracture and avalanche dynamics in colloidal gel systems, clay-polymer nanocomposite phenomena etc. These and other phenomena are studied using complementary experimental techniques such as microscopy, rheometry, imaging, magnetic resonance, SANS and synchrotron SAXS/WAXS including microbeams. Research constellation: Jon Otto Fossum, Dept. of Physics, The Norwegian University of Science and Technology, Trondheim, Norway; Kenneth D. Knudsen and Geir Helgesen, Physics Dept., Institute for Energy Technology, Kjeller, Norway, Knut Jrgen Mly, Physics Dept., University of Oslo, Norway.Marie. This constellation combines the groups and expertise of four senior researchers. The constellation is part of the Complex network in Norway (www.complexphysics.org), which includes collaboration financed through several grants from the Research Council of Norway. Study of clay minerals using X-ray techniques The KBS-3 concept for a Swedish repository for high-level radioactive waste includes three barriers: copper canister, swelling clay and suitable rock. It is vital that the clay retains its properties over a long period of time. Available clay materials are evaluated under repository-like conditions in the alternative buffer materials experiment (ABM), which was started at the sp Hard Rock Laboratory in 2006. The first of the three ABM parcels, containing 11 different clay materials each, was retrieved in May, 2009. The aim of our project is to study fundamental processes of importance in this context. In order to investigate the swelling kinetics of the layer silicates we use powder X-ray diffraction. Under certain conditions, the clay minerals intercalate water molecules to form hydrates with basal spacings of 40-100 , i.e. small angle methods must be used. It would be of great interest to study the temperature-dependence of these hydrates in the interval -30 to + 90 C. Research constellation: Staffan Hansen, Polymer & Materials Chemistry, Lund University; Daniel Svensson, SKB AB, Oskarshamn; Clay Technology AB, Lund.

Studies of biomineralized and biomimetic calcium carbonates and silica Small angle X-ray scattering and diffraction have been very important to the understanding of biomimetic silica chemistry and its representations on the colloidal length scale. We study biomimetic silica and calcium carbonate chemistries and typically use polymers or surfactants to template or direct the structuring of these complex solids. SAXS data can enable the understanding of the events in liquid state before and during the formation of the solids, SAXS data from the solids may resolve details in the structure of the solids. In addition SAXS, we apply a multipronged approach with the used of solid-state NMR spectroscopy and AFM and EM. We hope to reveal intricate details in the formation of silica and calcium carbonates in living systems, which clearly involves both equilibrium and out-of-equilibrium dependencies. Research constellation: Niklas Hedin, Dept. of Materials and Environmental Chemistry, Stockholm University. Collaborations with the groups of Mattias Edn and Lennart Bergstrm at Stockholm University. Collaboration with Denis Gebauer (presently at SU)

Phase behaviour and structure formation of conjugated polymers and supramolecules The long-term aim of this project is to understand phase behaviour and self-organized structure formation of selected conjugated polymers and their complexes in solution and the solid state. This information is utilized both in the design of new polymers and in the design of opto-electronic devices. The emphasis is on the archetypical conjugated polymers such as polyfluorenes which act as model molecules for generic physical understanding; as well as on the water soluble conjugated polymers which are candidates for biosensors. As these polymers show ordered structures in many length scales from the crystalline level to the submicron level clusters and as they many times scatter weakly, synchrotron radiation and preferentially simultaneous SAXS/WAXS with large q-range are essential experimental tools for our studies. The X-ray scattering experiments are connected to neutron scattering experiments as well as to photo spectroscopy. Most of the measurements are done at ambient or nearly ambient conditions but with I711 beamline staff (MAX-lab) we are also performing high pressure XRD measurements. Research constellation: Matti Knaapila, Dept. of Physics, Institute for Energy Technology, Norway; Andrew Monkman, Dept. of Physics, University of Durham, UK; Ullrich Scherf, Dept. of Chemistry, University of Wuppertal, Germany; Hugh Burrows, Dept. of Chemistry, University of Coimbra, Portugal. The main areas of this constellation are related to optically active organic materials.

Organizing Molecular Matter The Linnaeus centre Organizing Molecular Matter (OMM, www.omm.lu.se) consists of research groups from Physical, (PC) Theoretical (TC) and Biochemistry (BC) at Lund University. The work of the centre is focused on intermolecular interactions and how they lead to an organization of matter on the colloidal length scale, often using a combination of theoretical and experimental methods. On the experimental side, small (and wide) angle X-ray scattering (SAXS/WAXS) is a very important method that consequently is used in a large number of the projects. The use of scattering methods is indeed growing rapidly within the centre and we are currently recruiting a new associate professor to further strengthen our profile in small angle scattering area. In fact, the centre has the clear strategy towards MAX IV: Being a world leading soft matter laboratory we will be a key local academic support structure of the multipurpose SAXS/WAXS beamline at MAX IV with a strong involvement also in future developments of this beamline. Current or starting projects that will benefit from the unique performance of the MAX IV SAXS/WAXS beamline include: Intefacial stuctures of ionic liquids (Jan Forsman, Ulf Olsson) Peptide self-assembly (Ulf Olsson, Mikael Lund) Complex polymeric salts (Karin Schilln, Lennart Picullel) Anomalous swelling of Ca-clays (Bo Jnsson, Ulf Olsson) Formation mechanism of mesoporous silica (Viveka Alfredsson) Phase Transitions in shear flow (Ulf Olsson) Protein-Protein Interactions (Mikael Lund, Sara Linse, Ulf Olsson) Responsive membranes (Emma Sparr) Biopolymer/protein-lipid interactions (Tommy Nylander, Emma Sparr, Sara Linse) At the MAX IV beamline the following experiments are expected to be central for the activities at the centre: state-of-the art solution SAXS/WAXS, ASAXS, GISAXS, rheo-SAXS, time-resolved SAXS/WAXS experiments and XPCS. Research constellation: U. Olsson, T. Nylander, V. Alfredsson, M. Lund,, K. Schilln, L. Piculell, E. Sparr, J. Forsman, S. Linse, B. Jnsson. External collaborations include: B. Cabane (ESPCI, Paris), T. Narayanan (ESRF, Grenoble), J. Skov Pedersen (Aarhus Univ.) P. Schurtenberger (Univ. Fribourg)

Kinetics of micelle formation in out-of-equilibrium surfactants solutions The scope of this project is to investigate non-equilibrium kinetics in surfactant solutions by doing time-resolved solution scattering with a stopped-flow setup. The structures of surfactant micelles have been the topic of numerous scientific studies over the last several decades. Many different equilibrium micelle shapes and sizes have been observed upon varying the molecular properties of the surfactant, concentration, temperature, pH, solvent, ionic strength etc. However, the kinetics of the formation of micelles or transitions from one equilibrium structure to another is much harder to access, and studies have only recently become possible. In this project, low molecular weight surfactant solutions will be studied. By performing a rapid mixing of a surfactant solution with either another solvent, a salt solution or another surfactant solution, one can end up in a non-equilibrium state from where relaxation to a new equilibrium can be followed. The use of small-angle x-ray scattering at a high brilliance x-ray source allows for a good time resolution within the millisecond range to follow changes in micellar properties and also for identifying intermediate states on the way to equilibrium. One type of project that will be carried out is a study of the formation of micelles by mixing surfactant solutions below the critical micelle concentration (cmc) with another solvent of higher selectivity. Morphology changes in micellar solutions induced upon mixing micelles of different surfactants, or by mixing a micelle solution with an aqueous salt solution can also be studied. The changes could, e.g., be transitions from spherical to cylindrical micelles. In all cases, the mixed solutions will be out of equilibrium, and since the equilibration kinetics is expected to be fast, time resolved synchrotron small-angle x-ray scattering with millisecond time resolution is needed. Research constellation: Jan Skov Pedersen, Aarhus University, Denmark and Reidar Lund, Donostia International Physics Center, San Sebastin, Spain. Jan Skov Pedersen is leader of the Soft Matter Group at Aarhus University. The group's main research areas are colloidal and polymer science, complex self-assembling systems, solution structure of macromolecular complexes. The systems are studied by small angle X-ray, neutron and light scattering.

Combining small angle and wide angle X-ray scattering to combustion systems: Today much is still unknown about the mechanisms that control particle formation in combustion. Nanoparticles of a few nanometers have lately drawn much attention due to the high-risk factors for human health and the radiation balance in the atmosphere. Today there are hardly any techniques that can identify these particles with sufficient resolution to describe them physically and chemically. There are also important issues in fuels economy since the carbon contain in particles are deviated from the energy conversion processes and fuel economy is reduced. We are strongly interested in continuing the developments we have previously done at beamline D611 and applying studies to real combustion condition in line with the prospective for the coming MAX IV. There are special requirements on the beam line properties such as: High Brilliance High Coherence (lateral and longitudinal) Vertical polarization of the radiation in the range 5 keV 20 keV. Tunable energy. Research constellation: Frederik Ossler, Combustion Physics, Physics Dept., Lund University Self-assembly of surfactant-surfactant, surfactant-lipid and surfactant-polyelectrloyte mixtures in bulk and at interfaces We want to characterize the microstructure of aggregates and complexes formed in different surfactant-surfactant, surfactant-lipid and surfactant-polyelectrolyte mixtures (SAXS, ASAXS). In surfactant mixtures we are mainly interested in exploring the size and geometrical shape of micelles, vesicles, bilayers etc, and its dependence on molecular architecture and composition. Studying polyelectrolyte-surfactant mixtures also include the characterization of internal microstructure in dispersed liquid crystal colloidal particles using SAXS in the high q-regime or WAXS. We also want to study fast and slow kinetics in our non-equilibrium systems and its dependence on sample preparation using, for instance, rapid mixing and T-jump techniques. Investigating microstructural behaviour at interfaces with GISAXS include the adsorption of polyelectrolyte-surfactant complexes and polyelectrolyte multilayers at surfaces and interfaces as well as anti-corrosive coatings formed by conductive polymers and nanoparticles. Incorporation of heavy metals in polyelectrolyte complexes is particularly suitable to study with x-rays. The bulk measurements will be complemented with static light scattering data that gives information in a regime of low q-values partly overlapping with the SAXS data available at MAX IV. Interfaces will be pre-examined with the numerous surface characterizations techniques (QCM, ellipsometry, AFM etc) available at the Surface Chemistry Laboratory at the Royal Institute of Technology. Research constellation: Per Claesson, Magnus Bergstrm, Andra Ddinait and Eva Blomberg are all senior scientists at the Division of Surface and Corrosion Science, School of Chemical Science and Engineering, Royal Institute of Technology, Stockholm.

Activation of hydrocarbons using surface-bonded molecular catalyst The main objective of this project is to develop models for describing the formation via aggregation of gels in concentrated colloidal silica dispersions. Gelling suspensions have a big industrial importance as they can be used as a grouting material or as a soil stabilizer, the silica monolith can be used as a solid state electrochemical device or as a catalyst support. The stability and morphology of the aggregates formed in the initial stages of the aggregation will affect the overall morphology of the contiguous gel network which in turn affects important parameters of solid gel such as strength and permeability. To investigate pre-aggregated morphology and/or dimension change and cluster growth during gelation, we will use a combination of time resolved Synchrotron Radiation Small Angle X-ray Scattering (SR-SAXS) and ElectroSpray and Scanning Mobility Particle Sizer (ES-SMPS) techniques. Due to the considerable size of the forming aggregates (up to several hundreds nm) very low q will required for this investigation, in the USAXS range. In order to fully characterise the behaviour and to capture the very onset of gelation, a stopped flow cell will be needed. Research constellation: Caterina Camerani and Inger Jansson Eka Chemicals AB, Bohus, Sweden; Ann Catrin Johansson, Dept. Chemistry, Gteborg Univerisity; Ann Terry, ISIS Facility, Rutherford Appleton Lab., UK. This constellation combines the groups and expertise of four senior researchers. The constellation is a long-term collaboration between an industrial company, one university and one research institute. Investigation of biomolecules in solution using solution Small-Angle X-ray Scattering A wide range of biomolecules, e.g. proteins, DNA and amphiphilic aggregates as well as complexes formed by these constituents, can only be studied by solution based techniques. Here, solution smallangle scattering is by far the most optimal technique for answering crucial questions about the 3-D structure of the systems and their interactions. In several cases, these systems are optimally investigated with special sample environments, for example microfluidics based mixing devices to allow for hi-throughput screening of a wide range of buffer conditions. In other cases, the samples need to be investigated at biologically extreme temperatures, i.e. close to the freezing and boiling points of the buffer solutions. In both cases we need access to a relatively flexible SAXS instrument, with focus on providing the best quality SAXS data for a wide range of sample environments. For the microfludics applications, the very high source intensity combined with the very small beamsize at the proposed MAX IV, will be close to optimal as this presently constitutes a central limiting factor for the optimal combination of microfluidics and SAXS. Research constellation: L. Arleth, K. Mortensen, L. Lo Leggio, B. Vestergaard, University of Copenhagen. The SAXS commutiny at University of Copenhagen (KU) is presently quickly expanding at all four Natural Science faculties (KU-Life, KU-Farma, KU-Science, and KU-Medicine). The core SAXS users presently consists of 4 senior staff members and at least 15 junior staff members (Ph.D. students and Post Docs). The main areas of activity are related to either studies of biomolecules in solution or soft condensed matter studies. The Copenhagen user groups are already very well established large scale facility users at several international X-ray and Neutron Scattering facilities.

SAXS activities at Novo Nordisk Novo Nordisk is a healthcare company and a worldwide market leader in diabetes care and has a leading position in haemophilia, growth hormone disorders and hormone replacement therapy. Our current R&D activities are focused on development of therapeutic proteins and peptides and improved proteins delivery routes. With our product portfolio focused on therapeutic proteins we find small angle X-ray scattering (SAXS) a very useful tool for characterisation of proteins/peptides with respect to molecular weight, oligomeric state, size and shape in solution under varying conditions. Furthermore, we routinely use SAXS for characterisation of larger protein complexes and protein-protein interactions. This information is important for our understanding of the stability and modes of action of our proteins/peptides and thus provides a rational basis for design of pharmaceutical formulations with the desired properties, i.e. chemical and physical stability and therapeutic profile. With the expected orders of magnitudes in improvements with regards to beam geometry, intensity and stability on the proposed SAXS/WAXS beamline at MAX IV we expect much more detailed and accurate characterisation of our pharmaceutical formulations. We find it very attractive and definitely believe that we would benefit from it. Research constellation: Gerd Schluckebier & Mathias Norrman, SC Formulation and Biophysics, Novo Nordisk A/S, Diabetes Protein Engineering, Novo Nordisk Park, DK-2760 Mlv, Denmark Hierarchically ordered natural polymer based materials The research aims at development of new nanocomposite materials from natural polymers, cellulose, hemicelluloses, starch, and surface active proteins. Nanocomposites based on cellulose or starch have applications in paper making, biodegradable films, or food industry. In the plant cell wall cellulose forms microfibril bundles which tend to be present also in isolated nanocellulose. We have studied microfibril structures in cellulose isolated from both conventional sources like wood and unconventional sources like needles and rice husks previously at MAX-lab. In the current research we have focused on enzymatic hydrolysis of cellulose for production of bioethanol. For instance, the physico-chemical interactions between the enzymes and the cellulosic substrate and their effects on the rate of the hydrolysis are not fully understood. The lamellar structure of starch granules may also be present in e.g. cereal extrudates even thought the granules are mainly broken in the process. In this project in situ studies on natural polymer composite formation and properties, and cellulose degradation using combined WAXS and SAXS experiments are of interest. Results are to be combined with those obtained using USAXS and x-ray microtomography. Research constellation: Ritva Serimaa, Mika Torkkeli, Helsinki University, Dept. of Physics, Maija Tenkanen, Liisa Viikari, University of Helsinki, Dept. of Applied Chemistry and Microbiology. The unit consists of 4 senior staff members and about 10 junior members. At Dept. of Physics, several inhouse setups for both wide- and small-angle scattering experiments and x-ray microtomography, atomic force microscopy, and setups for ultrasonic and mechanical testing of materials are available for basic characterization of the materials.

S-layer protein self-assembly The surface (S) layer is the outermost structure of the bacterial cell wall. S-layer proteins form a crystalline coating on the cell wall and can be reassembled also on other solid supports or at the airwater interface. This research aims at understanding the structure, properties and function of S-layer proteins of probiotic Lactobacillus bacteria on the cell wall and in biochemical applications. We have already shown that diffraction peaks arising from the two-dimensional order of the proteins on the cell wall may be seen in SAXS patterns of concentrated samples of native bacterial cells. In this project studies of concentrated solutions of self-assembled S-layers and dilute solutions of isolated proteins are planned. One aim would be to determine the shape of the protein or its aggregate in dilute solution. The samples will also be studied using transmission electron microscopy for obtaining complementary information on the protein structures. Research constellation: Mika Torkkeli, Ritva Serimaa, Helsinki University, Dept. of Physics, Airi and Ilkka Palva, University of Helsinki, Dept. of Basic Veterinary Sciences. The unit consists of 5 senior staff members and about 10 junior members. Laboratory facilities for the biomaterial production and characterization are available including several in-house setups for both wide- and small-angle scattering experiments and x-ray microtomography, atomic force microscopy, and electron microscopy at Helsinki area. Small-angle X-ray scattering of tissue samples Elastic scattering in angles smaller than 5 degrees, with respect to the direction of the incident X-ray, is called small-angle X-ray scattering (SAXS). The SAXS pattern can be used to study the structures of biological tissue at the molecular level, which can be to weakly ordered to be determined by crystallographic techniques. By studying the patterns created by elastically scattered X-rays from different types of tissue we can attempt to distinguish SAXS patterns for cancerous tissue from healthy tissue and in that way use the SAXS technique as a diagnostic tool. Research constellation: Albert Siegbahn, Dept. of Medical Physics, Karolinska University Hospital; Dept. of Oncology-Pathology, Karolinska Institute.

The main constellations contributing to the project are: Prof. Ulf Olsson and the division of Physical Chemistry, Lund University. Prof. Adrian Rennie and the Materials Physics Division, Uppsala University Prof. Jan Skov Pedersen and the Soft Matter Group at the Chemistry Dept., University of Aarhus. These three groups are all very experienced users of small angle scattering and represent strong research in the soft matter and biophysical areas. All three groups are also very active in the complementary use of neutron scattering. Hence they will also be able to ensure that the SAXS/WAXS activities at MAX IV will be suitably connected to the corresponding activities and relevant beamlines at the European Spallation Source (ESS) The SAXS/WAXS project will also benefit from an Advisory Group, consisting of: Prof. Peter Schurtenberger, University of Fribourg, Switzerland, Prof. Kell Mortensen, Copenhagen University Dr. Theyencheri Narayanan, European Synchrotron Radiation Facility (ESRF), Grenoble, France. The members of the advisory group each will focus on different parts of the project and have been selected particularly for this. Peter Schurtenberger will focus on the scientific program where his experience in various studies of soft condensed matter will be particularly useful. In addition he has experience from the SAXS instrument at the Swiss Light Source where one has taken particular care to exploit the use of the beam coherence. Kell Mortensen has among other things a long experience of neutron research. He is active in the ESS project and will here, in particular, focus on optimizing the synergy between MAX IV and the ESS. Theyencheri Narayanan has developed the high brilliance SAXS/WAXS beamline ID02 at the ESRF into a world leading beamline. His advice regarding beamline design and optimization will be of outmost importance for the project.

Budget, Staffing and Time Plan Budget

Table 2 : Budget Description Undulator Frontend Optical & Experimental Hutches incl. Personal Safety System Optics Monochromator Focusing Optics (KB mirrors or refractive lenses) Beam Diagnostics incl. Slits Endstation SAXS detector WAXS detector Sample Environment Vacuum system (inside experimental hutch) Miscellaneous Infrastructure Electronics, controls & computing Vacuum Misc. incl. AC, fluids & liq. Nitrogen Others Control room + sample prep lab. 2 5 2 5 8 4 2 3 Amount (MSEK) 12 5 5

4 5 4

Total Time Plan

2011

66

Table 3: Time plan 2012 2013 2014 2015 Beamline design Purchase Procedure FE & und design Installation of hutches and infrastructure Production of bl components Installation of beamline components Installation front end & und. Commissioning front end & und. Commissioning beamline Commissioning sample environment Operation

Paperwork Staffing

Beamline

External work

End stations

Based on Table 3 we estimate the following personnel requirements during construction and commissioning. Out of these the committed user constellations will contribute with in total two manyears over the total construction period.
Table 4: Man-years during construction 2012 2013 1 3

Man-years

2011 1

2014 4

2015 4

In operation, this beamline will require three beamline scientists, one of which being primarily focused on the solution SAXS/bioSAXS community. In addition, there will be one beamline engineer/technician, and support, corresponding to one third staff member from the MAX-lab computer group, is also required. Extensive postdoc and PhD programs in collaboration with the main constellations involved in this project are also foreseen.

Environmental Soft X-ray XANES Beamline Spokespersons: Katarina Norn, Ingmar Persson, SLU, Uppsala, Per Persson, Ume University, Ume, Ulf Skyllberg, SLU, Ume, Britt-Marie Steenari, Chalmers, Gteborg, Sophie Canton, Lund University, Lund, Anna Puig Molina and Alfons Molenbroek, Haldor Topsoe A/S, Denmark, Jan-Dierk Grunwaldt, KIT, Germany and DTU, Denmark, David Nicholson, NTNU, Norway The beamline design is optimized for XANES spectroscopy measurements in the soft X-ray energy range 1-4 keV. This beamline is in the process to be built at the MAX II 1.5 GeV ring on a bending magnet, and will be relocated to an undulator source on the 1.5 GeV ring at the MAX IV facility. The technical design of this beamline will allow for in-situ XAFS measurements within the energy range 1-4 keV, which covers the K absorption edges of magnesium, aluminium, silicon, phosphorus, sulfur, chlorine and potassium. These elements, which often are regarded to be spectroscopically quiet, are significant for scientific applications ranging from catalysis and materials science to biological, environmental, geological and archaeological research. In order to fully utilize the flux generated by the light source the beamline is windowless up to the experimental station, where one 8 m thin Be-window is inserted to separate UHV conditions of the beamline from the ambient pressure at the experimental station. Such design allows for in-situ measurements and variation in atmosphere, pressure and temperature environment around the sample. The design of the beamline on the bending magnet at the MAX II ring only allows for construction of a XAFS experimental station with fully focused beam size of 0.1 x 0.4 mm2 (v x h). Upon relocation of the beamline to the 1.5 GeV ring at the MAX IV facility an upgrade of the beamline to include one more station for XANES measurements with microfocused beam up to 10 x 12 m2 (v x h), is incorporated in the design. Microfocus XANES combined with XRF element mapping is foreseen to be important techniques for the XANES community. The possibility to include a STXM station will be looked into. Main constellations committed to the beamline project: Chemistry, SLU, Uppsala - Ingmar Persson Forest Ecology & Management, SLU, Ume - Ulf Skyllberg Chemistry, Ume University, Ume - Per Persson Chemical and Biological Engineering, Chalmers, Gteborg - Britt-Marie Steenari Chemical and Biochemical Engineering, DTU, Denmark and Chemical Technology, Karlsruhe Institute of Technology (KIT), Germany - Jan-Dierk Grunwaldt Chemistry, NTNU, Norway - David Nicholson Dedicated user groups: Ume University: Per Persson SLU, Ume: Ulf Skyllberg SLU, Uppsala: Ingmar Persson, Dan Berggren Kleja, Gunnar Almkvist, Anke Herrman, Kristina Boye, Ingvar Nilsson, Magnus Simonsson, Barbro Uln and Ararso Etana Uppsala University: Dimitri Arvanitis, Torbjrn Gustafsson and Kristina Edstrm KTH: Jon Petter Gustafsson and Gunno Renman Chalmers University of Technology: Britt-Marie Steenari Lund University: Staffan Hansen, Villy Sundstrm, Sophie Canton Technical Univeristy of Denmark, Denmark: Kenny Sthl, Pernille Harris, NTNU, Norway: David Nicholson, Magnus Rnning, Karina Mathisen

Scientific motivation Synchrotron radiation techniques are increasingly used to study natural systems in their normal environments rather than model systems. A strongly developing field using element specific techniques such as XAFS spectroscopy is to study speciation and perform structure analysis of trace elements in natural systems. It is of importance to perform in-situ measurements, without any pretreatment, as e.g. up-concentration, as it might change both speciation and structure. The high X-ray intensity at MAX IV will make it possible to perform studies on natural systems, independent of state of aggregation. At energies below 4 keV experiments need to be done in either vacuum or helium atmosphere. Having helium atmosphere around the sample enables the environmentally interesting elements like for example sulfur to be studied in-situ in natural samples and in solution. The success of using S K-edge XANES for characterisation of sulfur compounds in various types of environmental samples have resulted in an increased pressure on the few existing properly equipped beamlines for soft X-ray determinations. There is currently only a few beamlines available in the world for XAFS measurements of low mass elements such as Mg, Al and Si. Also the number of beamlines for collection of XAFS data for P, S and Cl is highly restricted. Because these low mass elements are highly abundant, studies of the most fundamental biogeochemical processes are limited by access to proper research facilities. This means that the unprecedented photon flux and stability of environmental soft X-ray beamline at MAX IV is expected to attract the most excellent in situ research within the field of biogeochemistry and molecular environmental science. Biogeochemistry and molecular environmental science In situ studies of complex biogeochemical or molecular environmental processes require a multitechnique approach. A combination of both hard X-rays and soft X-rays are needed to cover central atoms and their associated ligands. In soils, sediments and waters C, N, O, Al, Si, P and S serve as both the most abundant building block elements of the organic (C,N,O) and inorganic (Al, Si) matrices, as well as the most important elements in ligands and functional groups binding metals and metalloids. This means that studies of fundamental biogeochemical processes in the environment is dependent on a state-of-the-art soft X-ray beamline. One classical problem in terrestrial and aquatic sciences is the chemical characterization of natural organic matter (NOM). The task has proven extremely difficult because of the inherent heterogeneity of NOM. Applied analytical techniques often includes destructive extraction and purification steps. As a consequence proposed structures of NOM are inevitably biased by artifacts. Because interactions with soft X-rays are non-destructive, they could be used to reveal structures, as well as be used to improve the understanding of the mechanisms behind the turnover rate of soil organic matter, and the associated changes in chemical speciation of essential plant nutrient elements, which originate from the degradation of low or high molecular NOM. There is often a rather close connection between the chemical speciation of a nutrient element and the plant uptake and use of that particular nutrient. The majority of plant nutrients is taken up either as inorganic cations or anions, although some charged low molecular organic compounds such as the amino acids, which contain nutrient elements nitrogen and sulfur, can also be taken up by plant roots. The conversion of a nutrient element from an organic to an inorganic chemical form is controlled by the activity of soil microorganisms. Sulfur is an element of particular environmental importance, e.g. as atmospheric gas pollutant, in acidification of natural waters, essential in many enzymes and an important fertilizer, but the transformations of sulfur species in natural samples are very difficult to follow with conventional techniques. While the total sulfur concentration can be easily determined, the difficulty to characterize sulfur species in a mixture represents a real challenge. Speciation of sulfur is preferably determined by combining XANES spectroscopy with -focused XRF element mapping. The composition of sulfur is extremely important for speciation of virtually all metals under anoxic conditions in soils and sediments. Another environmentally important element is phosphorus. Even though it is a nutrient, phosphorus may however occur in elevated levels in lakes and in the Baltic Sea, and thus causing euthrophication. Optimizing the processes that affects removal of phosphorus in wastewater treatment is a research area of interest that would benefit from measurements with the XANES spectroscopy technique. Determination of phosphorus phases on wastewater treatment media is necessary to increase the understanding of phosphorus speciation. Increased knowledge on phosphorus speciation on sewage sludge in order to determine the phase composition will help to understand the processes that affect

phosphorus transformation on the sludge, and hence help to determine the availability of bound phosphorus. Other very important research areas that would take immediate advantage of the proposed beamline are studies of naturally and anthropogenically derived chlorinated organic substances occurring in the environment and weathering processes of Mg, Al and Si in soils and sediments. Magnesium is an essential, major nutrient, Al is potentially toxic and Si the most important element in silicate minerals. The beamline would open up new possibilities for a quantitative determination of Al-hydrolyses (formation of Al-hydroxides) in presence of organic matter in natural environments, an issue that has been in debate for 100 years and still is not solved. This process is of fundamental importance for acidification of soils and waters. Archaeology Synchrotron radiation studies of archeological artifacts provides important information on chemical speciation in the objects, which among other things help to formulate more effective and scientifically based conservation strategies. Furthermore, the detailed chemical and structural information give the historians a deeper understanding of the origin and technology behind the objects. A Swedish example is from marine-archaeological wood, where measurements on sulfur K-edge XANES revealed that large amounts of reduced sulfur species had accumulated in the timbers of the Vasa, which was found to develop acidity and cause preservation problems in the Vasa Museum. The sulfur accumulation originates from hydrogen sulfide produced by sulfate-reducing bacteria in seawater, and its reactions with lignin expose an environmentally important mechanism of incorporating sulfur into organic matter, in competition with reactive iron that forms sulfides. The acidity problems were found to be quite general for marine-archaeological wooden objects preserved in seawater, and methods to remove iron and sulfur species are being developed in an international project. Bulk and -focus XANES spectroscopy combined with XRF element mapping are synchrotron radiation techniques required to monitor the efficiency of the improved removal procedures by determining the distribution and physical state of the reduced sulfur and iron compounds in the marine-archaeological wood. Catalysis research Light elements are important in heterogeneous catalysis as they are the main component of carriers in supported catalysts. Typical carriers Al2O3 and SiO2 are composed of high surface area oxides which provide mechanical strength and thermal stability to the active nanoparticles, while facilitating a high dispersion of the active catalytic phase. The anchoring of the supported particle on the carrier depends to a large extent on the carrier. A good anchoring prevents sintering of the supported particles and loss of surface area. Light elements can also be added to promote catalysts. When added in relatively small amounts, the activity, selectivity or stability of the catalyst might improve. Some elements though can also act as poisons and decrease the catalyst activity by blocking active sites. In order to design improved catalysts it is crucial to know the physico-chemical properties of these light elements and understand their role in the catalytic reaction. While oxide forms of Al, Si and Mg are typically used as carriers, P and Na can give promoting effects. On the other hand, S, Cl and Na are known to poison some catalyst systems. By studying the chemical state and local environment of light element a better understanding of the particle-substrate interaction and promotion and poisoning effects can be achieved. In-situ XANES measurements are fundamental in order to obtain realistic information. Energy research Experience from practical use and applied research in full scale and laboratory studies have shown that an efficient use of biomasses in combustion and gasification is strongly dependent on the quality of the feedstock. A critical factor in this context is the content of different ash forming nutrients in the raw material. During utilization of biomass for energy conversion purposes these ash elements cause technical concerns, e.g. clinkering or slagging on grates, bed agglomeration in fluidized beds and deposit formation through condensation of volatilized material on rear walls and heat exchange tubes. The amount and composition of the ash forming elements in different parts of the raw material varies in wide ranges depending of origin, harvesting and transportation. The most important elements to contribute to these ash chemical issues are Si, Al, Ca, Mg, Na, K, Cl, S and P. They may be present in the ash in various chemical forms, such as silicates, oxides, chlorides, and sulfates as well as amorphous melts. Biomass contains high concentrations of volatile ash material of which K and Na are known to promote in principal all ash related. Different mechanisms of alkali metal release have

been identified depending on fuel composition and combustion temperature. Accordingly, the presence of macro and micro nutrient elements is associated with different technical and environmentally related issues during combustion and gasification. The broad variation of different ash forming elements between different feedstocks will significantly influence the presence and severeness of these different problems. The limiting factors for the end of use of different assortments are therefore connected to the prerequisites for different types of energy conversion systems and detailed information concerning critical ash elements and chemical transformation processes is therefore needed to avoid or minimize these potential problems. Spectromicroscopy of nanobio interfaces The importance of understanding nano-bio interfaces and their modifications under external conditions has emerged from the growing number of practical applications found for nanomaterials in biophysics, biochemistry and medicine over the past decade The detailed characterization of these interfaces requires the correlation of experimental results from many techniques that can monitor in situ several length scales. X ray Absorption Spectroscopy (XAS) is a versatile, element specific analytical tool capable of delivering accurate information about geometric and electronic local environment of the absorbing atom. Thanks to unprecedented beam size and flux, the new XAS beamline at MAXIV will enable spectromicroscopy. Although a steady state behavior is usually assumed for analyzing this type of samples, it is already recognized that transient chemical states play an important but largely unknown role. As the beamline develops, several detector designs and sample handling systems will be investigated in order to increase the temporal resolution of these measurements and explore the dynamics of the nano-bio interface

Technical description An application for funding of this beamline has been submitted to the Knut and Alice Wallenberg foundation. The beamline is planned to be constructed on the bending magnet at the 1.5 GeV MAX II ring. The entire beamline, the dedicated endstation and the suite of spectrometers have been designed so that they can be moved without any modifications to an undulator beamline at MAX IV. The significant gain in flux and photon beam size will readily enable the implementation of soft X-ray spectromicroscopy. The increased sensitivity will make it possible to perform 2D mapping on dilute environmental and biological samples based on chemical contrast, free from spatial averaging on the aggregate or colloid length scale. Building upon the knowledge acquired during the operation of beamline at MAX II, it will eventually be possible to perform both spatially and temporally resolved studies of heterogeneous samples. These experiments will answer some of the outstanding questions that are hampering progress in many fields. One line of research will also focus on the implementation of time-resolved capabilities, from microreactor type fuel cells to laser initiated photoreactions. Construction of the beamline at the MAX II ring With a front end opening angle of 0.33 x 3.5 mrad (v x h) on the bending magnet at MAX II ring 1.5 GeV, the size of the source is 0.1 x 0.8 mm2 (v x h). A beam position monitor is placed in front end for monitoring the beam quality. The first optical element after the front end is Cr-coated water cooled toroidal mirror, which is positioned 10 m from the source and has a mirror pitch of 8 mrad. The mirror provides horizontal focusing of the beam at the sample position at 3.82 m from the mirror, where the beam size is 0.92 x 0.6 mm2 (v x h) and flux is 1.2*1011 (ph/s/0.1%BW). Following the toroidal mirror is a set of Cr-coated water cooled flat mirrors for harmonic rejection with variable pitch values (8-20 mrad). These mirrors acts as a lowpass filter, which minimizes the contamination by higher order harmonics delivered by the source, and reduces the thermal load received on the monochromator crystals. The position of the beam entering the monochromator is monitored by the second beam position monitor, which is placed in front of the monochromator. The double crystal monochromator is equipped with three sets of crystals, KTiOPO4, KTP, (011), InSb(111) and Si(111), in order to cover the energy range 1-4 keV. The crystals are easily exchanged in vacuum, and the first crystals are water cooled. The entire beamline, up to the sample chamber, is windowless in order to get thorough as high flux as possible. This means that the beamline, as well as the ring, is operated under ultra high vacuum (UHV). In order to separate the sample environment from the UHV conditions a differential pump is positioned between the monochromator and the sample chamber. Differential pumping allows for samples to be run in low vacuum environment, but there is also 8 m thick beryllium window mounted on the sample chamber for the in situ measurements at atmospheric pressure. The position and the size of the beam at the sample position are monitored with the third beam position monitor, which is positioned in front of the sample chamber. The monochromator To obtain beam divergence limited energy resolution a double-crystal monochromator is the easiest and most economical option. The monochromator must incorporate three exchangeable crystal sets to cover the entire energy range. In order to cover the Mg (1.30 keV) and Al (1.56 keV) K-edges several crystals such as beryl (1010), quartz (1010), potassium titanyl phosphate (KTP) (011) and YB66 (400) are available. However, the energy range of beryl (1010) and quartz (1010) is limited since they contain Al and Si, respectively. For the YB66 (400) crystal, there are no adsorption edges present between 1200 eV and the Y L3-edge at 2.08 keV. However, the YB66 (400) crystal has two dominating glitches at 1.39 keV and 1.44 keV caused by significant increase in reflectivity of the (600) reflection of the Y L-edges. The KTP (011) crystals can instead be used up to P (2.14 keV) K-edge, including Mg, Al and Si (1.84 keV) K-edges. In order to cover energies above Si K-edge the InSb (111) crystals can be used. The InSb (111) can be used from Si K-edge up to 3.7 keV where the In L3 edge starts to interfere. It is recommended to use Si (111) crystals above 2.1 keV, due to the better energy resolution of the Si (111) crystals over InSb (111) crystals (Fig 1).

350 300 250 200

InSb (111) KTP (011)

Rocking curve width Darwin curve width

150 100 50
Si (111)

Fig. 1. Rocking curve width (solid) and Darwin curve width (dashed) for different Bragg reflexes on KTP(011) crystal, InSb(111) crystal and Si(111) crystal as a function of photon energy. Darwin curve or diffraction curve means -polarized one crystal rocking curve. Rocking curve means two-crystal rocking curve (with only one crystal rocking), calculated by convolution of the diffraction curve with itself. The rocking curves were obtained using XCrystal/XOP.

0 1100 1600 2100 2600 3100 3600 4100 4600 5100 Energy (eV)

Relocation of the beamline to the MAX IV facility The entire beamline is designed so that it can be moved without any changes of the optical elements to an undulator beamline at the MAX IV facility. The MAX IV facility will have two synchrotron rings, a 1.5 GeV ring and a 3 GeV ring. The calculations have showed that moving the beamline to the bigger 3 GeV ring will, due to the high power density of 93 kW/mrad2 produced by the source, have a damaging affect on the optical elements on the beamline. This power density would require that all the optical elements be cooled with liquid nitrogen instead of water. But what would be even more worrying is that, since the KTP (011) and InSn (111) monochromator crystals are known to be much more prone to radiation damage than the conventional Si (111) crystals, the performance of the beamline and quality of the beam would significantly degrade. Hence, the best would be to move the beamline to the 1.5 GeV ring at the MAX IV facility. The power density of 0.72 kW/mrad2 produced by the undulator source at the 1.5 GeV ring at the MAX IV is manageable with the same water cooling system that will used for this beamline on the bending magnet at the MAX II ring. One big advantage of moving the beamline to the MAX IV facility will be the significant gain in flux from 1.2*1011 (ph/s/0.1%BW) at MAX II ring to 4.8*1013 (ph/s/0.1%BW) at the MAX IV facility. The size of the beam at the sample position will change from 0.92 x 0.6 mm2 (v x h) at the MAX II ring to the 0.1 x 0.4 mm2 (v x h) at the MAX IV facility. Furthermore, an upgrade of the beamline to include two experimental XAFS stations is planned, upon relocation to the MAX IV facility. The first experimental station will be dedicated for bulk XANES measurements, and the second one will be the new upgraded station for focused XANES and XRF element mapping. (Fig. 2)

Fig. 2. Overall layout of the beamline at the 1.5 GeV ring at the MAX IV facility

The beamline is proposed to be relocated to a 1.5 m long in-vacuum permanent magnet undulator with 65 periods and a period length of 23 mm. In order utilize high flux over the entire energy range 14 keV the 3rd, 5th , 7th and 9th harmonics can be used (Fig. 3). Fig. 3. Flux of protons in the harmonics of the emitted synchrotron radiation. The toroidal mirror focuses the beam to a spot size of 0.1 x 0.4 mm2 (v x h) at the sample position on the XANES station, 25 m from the source, with flux 4.8*1013 (ph/s/0.1%BW). Following this station a pair of slits is installed before two Cr-coated KB mirrors for horizontal and vertical focusing at the -XANES station to a spot size of 10 x 12 m2 (v x h) and flux 9.2*109 (ph/s/0.1%BW) The equipment at the beamline including sample chamber and detectors will easily be movable between the two experimental stations, so that users can conduct experiments at both stations during allocated beamtime. Equipment Since the entire beamline needs to be windowless in the 1-4 keV energy range in order to obtain sufficient flux, a differential pump needs to be positioned before the sample chamber so that the UHV conditions at the beamline can be separated from the vacuum conditions in the sample chamber or the in-situ measurements at atmospheric pressure. The design of the sample chamber will allow for conducting in-situ measurements. The sample chamber will consist of a vacuum chamber and an insitu sample cell. A Cu-mesh will be positioned inside the vacuum chamber, as close as possible to the sample cell so that the I0 (intensity of the incoming beam) current from Cu-mesh can be measured. The vacuum chamber will also be designed to allow easy assessment for mounting and connecting in situ sample cell. The in situ sample cell will be designed so that measurements can be performed in gaseous environment at maximum pressure of 1 bar and at temperatures ranging from 80 to 750 K. Pre-treatment can be performed at 5 bar and 750 K in the same sample cell, after which XANES measurements can be done without exposing the sample to ambient air. For measurements in the soft X-ray range nitrogen cooled Germanium fluorescence detector is required, which is optimized for measuring in the soft X-ray energy range. Electron yield detection can be used simultaneously by measuring total electron yield. The sample chamber and the detectors will, like the optical elements, be relocated from the MAX-lab facility. The Germanium fluorescence detector will be used to measure both bulk and -focused XANES, but it can also be used for XRF element mapping at the -XANES station. At the later phase of beamline upgrade a STXM station is planned to be installed, which would be an excellent complimentary technique to XANES and XRF measurements.

Research project proposals from dedicated user groups Biogeochemistry of phosphorus: Molecular-scale studies of key processes Phosphorus occurs in nature mostly as inorganic phosphates or as organophosphates. A unique property of phosphates is the unusually large reactivity towards solid particles in the natural aquatic environment. Thus, reactions at environmental interfaces govern the fate of phosphorus and greatly influence biomass production in ecosystems. Our research project is concerned with key species and processes at these interfaces and the overall objectives are: 1) to determine the structures and reactivities of phosphate species formed at naturally occurring Fe(III) phases/complexes; 2) to determine the mechanisms and rates of enzymatic and mineral-promoted hydrolysis of adsorbed organophosphates; 3) to characterize the micro-chemical environments of P uptake at interfaces between microorganisms/fungi and adsorbed phosphate phases. We use a novel experimental approach that combines state-of-the-art spectroscopic and imaging techniques, including synchrotron-based XANES and EXAFS and vibration spectroscopy, with methods from soil microbiology in microcosm experiments. This research provides unique, molecular-scale information that enhances the fundamental knowledge about the transfer mechanisms between various biogeochemical pools of phosphorus. Lead PI: Prof. Per Persson, Department Of Chemistry, UmU. The research group consists of 3 senior and 6 junior staff. Focus is on molecular-level studies of processes at mineral, organic, and bacterial surfaces that influence the biogeochemical cycles of elements. The main objective is to provide fundamental understanding of chemical speciation, mechanisms and rates of reactions in the inherently heterogeneous aquatic and terrestrial environments. Biogeochemical processes of trace metals (mercury) under varying redox conditions in soils and sediments We combine the state-of-the-art analytical techniques such as species-specific isotope dilution, SR spectroscopic, electron microscopic and isotope labeled microbial activity experiments to link the chemical speciation of trace metals to their biotic and abiotic transformations in natural environments. One example is the transformation of Hg to the highly toxic and bioaccumulating MeHg molecule. We apply hard X-rays for studies of the metal and soft X-rays for studies of the ligands. Sulfur, oxygen and nitrogen are the three most important elements in organic and inorganic ligands. The high photon flux and stability of the proposed environmental soft X-ray beamline at MAX IV will give us possibilities to go into unprecedented detail about the chemical speciation of trace metals under in situ conditions. This will help us to understand and explain conditions and factors in control of transformations of trace metals to toxic, bioaccumulating forms which in turn can lay the ground for societal decisions regarding local and more widespread contaminations. Research constellation: Lead PI: Prof. Ulf Skyllberg, Department of Forest Ecology and Management, Swedish University of Agricultural Sciences, Ume and Ass. Prof. Erik Bjrn, Chemistry Department, Ume University. The research group in addition includes 3 PhD students and 2 Post-Docs. The objective is to provide fundamental understanding of chemical speciation, mechanisms and rates of reactions of mainly mercury but also other trace metals in aquatic and terrestrial environments

Understanding reactions between metals and organic matter in soils and natural waters Organic matter generally plays a central role in governing the mobility and bioavailability of metals in soils and waters. If present as a solid phase metals can be immobilized, whereas the opposite is true if metals are being bound to dissolved organic matter. Furthermore, organic matter can also shuttle electrons to metals like iron, chromium, selenium; thus affecting their redox state and thereby their mobility and toxicity. X-ray absorption spectroscopy is a very powerful tool to study environmental processes involving interactions between metals and natural organic matter, such as redox and complex formation reactions. Since many reactions are concentration dependent, the environmental beam line at MAX-lab IV offers improved possibilities to move towards more environmental relevant conditions. The possibility of measuring elements like Al, will be another major advantage. I have been involved in four research projects financed the Swedish Research Council, where we used the synchrotron facility at MAX-lab, the last two are on-going projects. All projects are collaboration with Professor Ingmar Persson, Department of Chemistry, SLU, and Professor Jon Petter Gustafsson, Department of Land and Water Resources Engineering, KTH. New to the group is Dr Anke Herrmann, Department of Chemistry, SLU, Sweden, SLU, Uppsala. Research constellation: Dan Berggren Kleja, Department of Soil and Environment SLU; Ingmar Persson, Department of Chemistry SLU; Jon Petter Gustafsson, Department of Land and Water Resources Engineering, KTH; Anke Herrmann, Department of Chemistry, SLU, Sweden, SLU, Uppsala.

Speciation and mobility of phosphorus in soil and aquifers To alleviate the eutrophication envisaged in many South Swedish lakes and in the Baltic Sea, Swedens emissions of phosphorus (P) to natural waters have to be substantially reduced. Leaching of P from agricultural land is a major source of P emissions, and counter-measures to mitigate these P losses is a priority field of research. A major proportion of the lost P is adsorbed onto various mineral phases, or resides as esterbound P in organic molecules. Colloids of these materials may be suspended and lost with the run-off water. The subsequent mobilization of orthophosphate species (directly responsible for eutrophication) is highly dependent on the chemical nature of the bound P; detailed information on this is needed to assess risks associated with P losses. In an intended project, we plan to study the transport of P-forms from agricultural watersheds, which are monitored by the Dep. of Soil and Environment, SLU, under the auspices of the Swedish EPA (Obervationsflt p jordbruksmark). Our objective is to estimate the efficiency of counter-measures against P losses already undertaken in these areas. To do this, we need to assess size distribution and elemental composition of P-carrying particles from soil, drainage water, sedimentation ponds, and filtering wetlands. Intended techniques include SEM-EDS, light scattering, and field flow fractionation. In this context, a XANES method for P would be a higly valuable tool to observe the bonding environment of P directly. One strength of XANES is its versatility regarding state of aggregation and concentration of the sample; thanks to it, different materials (dissolved, colloidal, sedimented) could be investigated with the same method. Research constellation: Magnus Simonsson, Ararso Etana and Barbro Uln, Department of Soil and Environment, SLU, Uppsala

Speciation of sulfur compounds in natural matrices using sulfur XANES Sulfur K edge XANES (X-ray Absorption Near Edge Structure) spectroscopy is an excellent tool to determine the speciation of sulfur compounds in complex matrices. A new method has been developed to quantitatively determine the kinds of sulfur species in natural samples using internally calibrated reference spectra of model compounds. Quantitative measurements can only be performed on samples with the sulfur compounds homogenously separated in the sample at low concentrations, less than 0.3-0.5 %. Samples containing particles are very difficult to determine quantitatively due to high self-absorption in the individual particles. The method is applied on a wood sample from the historic warship and Vasa and a soil sample. Sulfur speciation in preserved water-logged archaeological wood from the Vasa In the studies of wood from the Swedish warship Vasa have shown that organic sulfur compounds are accumulated in the surface. Inorganic compounds as elemental sulfur, gypsum and iron sulfates are often present as particles, and that these are more frequent in the surface than deeper into the material. The organic sulfur is evenly distributed in the wooden matrix dominated by reduced forms of sulfur, mainly bound to lignin in the middle lamellae. Sulfur mineralization in arable soils One classical problem in soil science is how to make a satisfactory chemical characterization of soil organic matter and how such a characterization can be used to improve the understanding of the mechanisms behind the turnover rates of soil organic C, N, P and S, and the associated changes in chemical speciation of these essential plant nutrient elements. This study has shown that newly developed XANES data treatment method with inclusion of post-edge structure and calibration between model samples, as well as the use of diluted solutions instead of solid samples for the model compounds and thus avoiding the problem with self-adsorption, has greatly improved the possibility to achieve reliable quantitative results for contributing sulfur compounds in soil samples and soil extracts. It is shown that farmyard manure application generally shifts the sulfur chemistry to the more reduced end of the spectrum, but that the effect is masked in soils with a high sulfur turnover rate. A conclusion of this in turn is that the sulfur turnover rate is generally determined by other factors than the chemical composition of the organic sulfur, such as microbial activity, other nutrient deficiencies, physical properties of the soil etc. Research constellation: Ingmar Persson and Gunnar Almkvist, Department of Chemistry, SLU, Uppsala; Kristin Boye and Ingvar Nilsson, Department of Soil and Environmental, SLU, Uppsala

Investigation of solid phase speciation of P and Al in environmental samples using K-edge XANES spectroscopy The overall aim of this research project is to gain increased knowledge into the phosphorus and aluminium speciation of soils and wastewater treatment media, and XANES spectroscopy is a very useful tool. Determination of P and Al phases on soils and treatment media is necessary to increase the understanding of factors influencing P release and eutrophication. Important tasks include: To determine phosphorus phases in filter materials used in small-scale wastewater treatment. This is essential for designing process-based models for the determination of filter life spans, and to determine the availability of bound P when used filters are recycled to agriculture. Phosphorus speciation studies on sewage sludge/biosolids and soil infiltration systems (using K-edge XANES spectroscopy) to determine the phase composition of bound P. Use of P-XANES to accurately determine the forms of P that accumulate in soils, information that may prove to be essential for risk assessments for eutrophication in lakes and seas. Complementary studies using Al K-edge XANES to determine the crystallinity/identity of formed Al-P phases in environmental samples.

Research constellation: J.P. Gustafsson, G. Renman and E. Plaza, Land and Water Resources Engineering, KTH, D. B. Kleja and M. Simonsson, SLU. The units consist of about 8 senior staff members and about 5-10 PhD students active in this research field.

Development of new materials for lithium ion batteries Our research is based on studying the mechanism of lithium insertion of a number of different new or already existing materials. Today, there is a hunt for introducing lighter and lighter materials in the lithium-ion batteries that will be the future for HEV and EV vehicles. One example that we work with is the replacement of the commercially used graphite for silicon. Silicon can increase the energy density for the negative electrode in the battery about 10 times. There are, however, lithium-silicon structural phases that appear that cannot be studied with conventional X-ray diffraction techniques. This is only one example of a system where the use of a new XAFS beam-line can contribute to the fundamental understanding that will have an impact on one important application. A second example is the trend to move from oxides to poly anion compounds as positive electrode materials for lithium-ion batteries. The most important factors driving this trend is safety and environmental concern. Lithium iron phosphate and lithium iron silicate are two of the most promising new cathode materials. Still a large number of questions about mechanism and stability remain to be studied for these materials. The new XAFS beam-line will be important in this work. Research constellation: Professor Kristina Edstrm and Associate Professor Torbjrn Gustafsson, Department of Material Chemistry, Uppsala University. Element specific magnetism beyond 1 keV: The rare earths, induced moments, magnetic EXAFS The project complements soft X-ray investigations with circular polarized X-ray light at the new magnetism dedicated, soft X-ray PGM based beam line of MAX IV. We want to focus on X-ray absorption spectroscopy using circular light with harder X-rays. Here due to the use of KMCs circular X-rays can be produced with high energy resolution and high photon flux in the spectral range 1-2 keV important for the M edges of the rare earth elements (from La to Lu). These can be conveniently addressed within an energy range where the dispersive power and performance of the PGMs is limited. Within an element specific view of magnetism investigations, using hard X-rays one is also interested on the role, played in alloys and multi component systems, of the passive magnetic elements (such as Cu, Ga, Sb, As, Zn, Te, Pt, Au) in magnetic semiconductor systems, spin valves, magnetic interfaces and metallic multilayers. Harder X-rays have allowed in the past to characterize successfully the contribution to magnetism from p states for a variety of non ferromagnetic elements in the bulk. Magnetic EXAFS is a technique that complements magnetic investigations, allowing to characterize the local magnetic environment around the photo excited atom. Below 1 keV due to the small spin orbit energy of the initial states the EXAFS analysis presents complications. With harder Xrays one can easily disentangle the magnetic from the real space part of the electron scattering in an EXAFS experiment and disentangle ferromagnetic from non-ferromagnetic local order. Research constellation: Dimitri Arvanitis, Physics and Astronomy, Uppsala University; Iwona Kowalik, IFPAN Warsaw, Poland; Juanjo de Miguel, Universidad Autonoma de Madrid, Spain. This collaboration is supported by national funds and funds targeting transnational collaborations, following bilateral agreements between the countries involved.

Possibilities to do XAFS analysis of Al, Si, Cl and P in material samples and samples of combustion residues One central issue in the research work in our group is the chemistry of metals in combustion of solid fuels, such as biomass, coal and waste. We have used synchrotron based X-ray spectroscopy methods (XANES and EXAFS) in this work and specifically studied the chemical speciation of Cd, Zn and Cu. The mix of fuels used in the combustion units becomes more and more complex as new fuels are introduced and the result is that even the chemical speciation of main elements becomes less predictable and more investigations are required. Aluminium, silicon, phosphorous, sulfur and chlorine are very important components of the incombustible part of the fuels and they also have a strong influence of the trace metal chemistry of the resulting ash. Another important line of work for us is investigations of the basic chemistry of the cement system. In addition, this work is coupled to the work on combustion residues since ashes may, in some cases, be utilized as components in cement and concrete mixtures. Also in the cement system, aluminium and silicon are central chemical components and speciation investigations are necessary. Some reactions can be followed by FTIR measurements, but the possibility to make detailed investigations of the chemical surroundings of S, Si and Al atoms in the structures would be very valuable. Research constellation: B-M. Steenari, Environmental Inorganic Chemistry; Industrial Materials Recycling, Chalmers University of Technology. Melanin photochemistry and function Melanins are a family of ubiquitous natural pigments found in melanocytes in the skin, hair follicles, eyes and inner ear, of humans and other animals, and in neurons of the substantia nigra in the human brain. The melanin in the skin is believed to have both photo-protective and photo-toxic functions, but the underlying molecular mechanisms are largely unknown. Through a combination of time resolved spectroscopy and quantum chemical calculations we are trying to establish a detailed mechanistic understanding of the UV-induced processes in melanin. Understanding of the UV-light induced processes in melanin may help the development of therapies and drugs against skin cancer. X-ray spectroscopy providing local structural probes would greatly contribute to increased understanding of structure-function relationships. Research constellation: V. Sundstrm, S. Canton, J. Uhlig, G. Smolentsev, N. Gador, P. Chabera, Chemical Physics, Lund University. Approx 30 scientists working on molecular dynamics in chemistry, biology and material science, using ultrafast spectroscopy techniques probing the electromagnetic spectrum from the far infrared (THz) to the X-rays.

Study of clay minerals using X-ray absorption spectroscopy The current Swedish concept (KBS-3) for a repository for the high-level radioactive waste produced by nuclear power plants includes three barriers to protect the environment. These are copper canister, swelling clay and rock of suitable quality. In this context, it is of great importance that the clay retains it mechanical properties and its function as a diffusion barrier over a long period of time. The most tested clay material so far has been a Wyoming bentonite, containing the swelling clay mineral montmorillonite as the main phase. Other available clay materials need to be evaluated under repository-like conditions and such an experiment (Alternative buffer materials, ABM) was started at the sp Hard Rock Laboratory in 2006. In this connection an industrial doctorate project was also initiated. The aim of the project is to study fundamental crystal chemical processes that might be of importance under these conditions and the first of the three parcels containing 11 different clay materials was retrieved in May, 2009. To obtain a more complete picture of how the montmorillonite atomic structure is affected by the reduction of its iron, it would be very useful to be able to monitor the X-ray absorption K-edges of the lighter elements like Mg, Al and Si and we are thus strongly in favour of adding such a facility to MAX IV. The possibility of monitoring changes in the oxidation state of iron and its effect on the environment of the lighter elements has great potential in connection with studies of other types of synthetic and natural silicates as well. Research constellation: Staffan Hansen, Polymer & Materials Chemistry, Lund University; Daniel Svensson, SKB AB, Oskarshamn; Clay Technology AB, Lund. X-ray absorption spectroscopy studies of phospholipids-nanoparticles interfaces A beamline in the 1-3 keV range will open up the possibility to perform combined near edge XAS experiments on phospholipids-Al2O3 and phospholipids-SiO2 nanometer complexes at the P edge (i.e. on the bio part of the interface) and Al/Si edges (i.e. on the solid part of the interface). The impact of suspending medium composition, concentration and pH will be investigated. These two systems are good models of pro-inflammatory and membrane disruption precursors. The planned capability for handling wet samples in a He atmosphere, which will be unique in Europe, will be essential for assessing the implications of the findings for in-vivo processes. These experiments will be complemented by SAXS, WAXS and hard X-ray XAS data obtained on other beamlines at MAX IV that will quantify concurrent particle aggregation and surface modification through wrapping. Although a steady state behavior is usually assumed for analyzing this type of samples, it is already recognized that transient chemical states play an important but largely unknown role. As the future D811 beamline develops, several detector designs and sample handling systems will be investigated in order to increase the temporal resolution of these measurements and explore the dynamics of the nano-bio interface. Research constellation: S. E. Canton, MAX-lab. The unit consists of approximately 1 senior staff members and 2 students (beginning 2010). The main areas of activity are related to implementation of dedicated instrumentation at synchrotron facilities.

Structure and function of proteins We are interested in the structure and function of proteins, and in particular metallo-proteins and proteins in the nucleotide metabolism. We are currently using EXAFS spectroscopy to deduce the detailed structure in the active metal sites in metallo-proteins. However, enzymes in the nucleotide metabolism are generally not metallo-proteins. Some bind magnesium that binds the phosphate groups of the substrate. Furthermore, AlF3 is used to mimic transition states during different reactions - for example hydrolyze of the phosphate groups. With the suggested setup at the beamline, we would be able to reach the magnesium, phosphor and aluminium absorption edges, which would be of outmost importance in the work to clarify reaction mechanisms and reaction paths in the nucleotide metabolism. Research constellation: Pernille Harris and Kenny Sthl, Associat Professor, Department of Chemistry, DTU, Denmark.

Probing microporous and mesoporous materials using argon The pore size, connectivity and adsorption behaviour are central aspects that contribute to the activity of porous catalysts. It is known that the nanoscale space inhibits confined molecules from achieving true long-range order. Since the surface energy between the pore wall and the condensed phase is assumed to influence the systems Gibbs energy there must be changes in thermodynamic properties such as the phase transitions in the confined condensed phases. We propose an XAS experiment on the influence of pressure (0-100 bars) on the local environments about argon absorbed into the nanospaces of microporous and mesoporous materials (three-and twodimensional zeolites and aerogels). Not surprisingly, little (no?) XAS work is reported for this element. With a K-edge energy of 3.2 KeV, this noble gas would be accessible to the proposed soft(er) X-ray beamline. The atomic size and monoatomic nature under ambient conditions makes this element an interesting probe of the varying structure-dependent potentials within the nanopores. Argon has a van der Waals radius of 1.88 and a significant polarizability volume which means that the atoms can access almost all pore sizes. Argon should exhibit a sizeable interaction with the pore walls because of its relatively large dispersion force and the spherical symmetric distribution of its electron cloud which readily adapts to the surroundings e.g. to elliptical symmetry in a regular environment. Argon gas would be compressed up to for example 20 bars which is easily accomplished from a conventional gas cylinder. Indeed, it is expected that EXAFS would be observed at lower pressures in the presence of the materials but not in their absence. Research constellation: Karina Mathisen, David Nicholson, Magnus Rnning, NTNU. The group consists of approximately 5 senior staff members and 10 junior staff members. The main areas of activity are related to inorganic materials and heterogeneous catalysis. There is in-house access to the various types of electron microscopy, x-ray diffraction, Raman- and IR spectroscopy and other methods of characterizing catalysts and materials.

Members of the XAFS steering committee: Professor Ingmar Persson, Department of Chemistry, SLU, Uppsala Professor Ulf Skyllberg, Forest Ecology & Management, SLU, Ume Professor Per Persson, Department of Chemistry, Ume University, Ume Associate Professor Britt-Marie Steenari, Chemical and Biological Engineering, Chalmers, Gothenburg Assistant Professor Sophie Canton, MAX-lab, Lund University, Lund Professor Jan-Dierk Grunwaldt, Technical Chemistry, DTU, Denmark Dr. Anna Puig Molin, Haldor Topsoe A/S, Denmark Dr. Alfons Molenbroek, Haldor Topsoe A/S, Denmark Professor David Nicholson, Department of Chemistry, NTNU, Norway Experts in XAFS beamline design and advisors to the steering committee: Professor Andrew Dent, Diamond Light Source, UK Dr. John Bargar, Stanford Synchrotron Radiation Lightsource, USA

Budget, staffing and time plan Budget proposal for beamline relocation to MAX IV Amount (MSEK) Undulator Front end Optics and experimental hutches and PSS system Infrastructure (fluid, electricity, AC system) Vacuum system Diagnostics including slits and filters KB mirror set up Electronics and controls Control room and lab room equipment -focus end station, table and gas system and sample chamber TOTAL 8 2 2 2 1 1 5 2 1 2 26

Staffing and time plan Time plan 2013 2014 Detailed design

2011 Undulator + FE tenda

2012 Undulator + FE design

2015

Hutches + infrastructure build Undulator + FE production Undulator + FE inst. optics tenda (KB mirrors) optics production Beamline inst.+commisioning

Paperwork

Beamline

External work

Based on time plan we estimate the following personnel requirements during construction and commissioning, assuming that the beamline components will be installed by the manufacturer. Man-years to be financed 2011 2012 2013 1 1 3

Man-years

2014 4

Hard X-ray Environmental XAS Spectroscopy Beamline Spokespersons: Katarina Norn, Ingmar Persson, SLU, Uppsala, Per Persson, Ume University, Ume, Ulf Skyllberg, SLU, Ume, Britt-Marie Steenari and Christian Ekberg, Chalmers, Gteborg, Anna Puig Molina and Alfons Molenbroek, Haldor Topsoe A/S, Denmark, Jan-Dierk Grunwaldt, KIT, Germany and DTU, Denmark, David Nicholson, NTNU, Norway The beamline design at the 3 GeV ring is optimized to deliver high photon flux in the range 4 to 30 keV, making full use of the very low emittance of the 3 GeV storage ring. The beamline is designed to accommodate two experimental stations dedicated for XAFS spectroscopy measurements. At the first experimental station XAFS measurements will be performed with unfocused beam. This possibility is very beneficial for dilute, but homogeneous model systems. An unfocussed beam is also beneficial for samples with heterogeneity at the sub-microscale or less. After that station a set of KB-mirrors will be installed for micro-focusing (enabling -EXAFS and -XANES measurements). The ultimate brilliance of the MAX IV 3 GeV ring and the optical layout of the beamline allows to focus the light in a ~1m2 spot at the -XAFS station. At the beamline X-ray absorption and fluorescence measurements will be standard techniques in combination with microfocus XRF element mapping. The scientific community which will benefit from techniques available at the beamline ranges from environmental, geological and earth sciences to biological and medical research, and material science and catalysis. The design of the experimental stations will accommodate for specially designed sample and gas systems for in situ measurements, as well as cryostats, furnaces and diamond-anvil cell for temperature and pressure control. Additional complementary techniques that will be available at the beamline are Raman and FTIR spectroscopy, UV/Vis and mass spectroscopy and CCD detector for complementary diffraction measurements. Recent development of detectors for XES will be closely followed and the experimental hutch will be built to provide space for XES detection. Main constellations committed to the beamline project: Chemistry, SLU, Uppsala-Ingmar Persson Forest Ecology & Management, SLU, Ume- Ulf Skyllberg Chemistry, Ume University, Ume-Per Persson Chemical and Biological Engineering, Chalmers, Gteborg- Britt-Marie Steenari, Christian Ekberg Chemical and Biochemical Engineering, DTU, Denmark and Chemical Technology, Karlsruhe Institute of Technology (KIT), Germany -Jan-Dierk Grunwaldt Haldor Topsoe A/S, Denmark- Anna Puig Molina and Alfons Molenbroek Chemistry, NTNU, Norway-David Nicholson Dedicated user groups: Lule University of Technology: Jurate Kumpiene, Lale Andreas, Anders Lagerkvist, Evelina Brnnvall Ume University: Per Persson, Erik Bjrn SLU, Ume: Ulf Skyllberg SLU, Uppsala: Ingmar Persson, Daniel Lundberg, Dan Berggren Kleja. Uppsala University: Dimitri Arvanitis, Torbjrn Gustafsson and Kristina Edstrm KTH: Jon Petter Gustafsson, Prosun Bhattacharya and Gunno Renman Stockholm University: Niklas Hedin, Mattias Edn, Lennart Bergstrm and Lars Eriksson Gteborg University: Per-Ola Norrby, Jonny Bjurman, Margareta Edebo Ekroth, Ingalill Nystrm, Anne Hbu and Kristian Andersson Chalmers University of Technology: Magnus Skoglundh, Jan Swenson, Britt-Marie Steenari, Christian Ekberg, Lars-Gunnar Johansson, Jan-Erik Svensson, Lars Erik mand, Gunnar Skanermark, Stefan Allard, Stellan Holgersson, Teodora Retegan and Mark Forman. Lund University: Staffan Hansen, Arne Andersson, Villy Sundstrm, Sophie Canton, Stefan Uhlig, Grigory Smolentsev, Niklas Gador and Pavel Chabera University of Copenhagen: Christian Bender Koch and Hans Christian Bruun Hansen Technical Univeristy of Denmark, Denmark: Kenny Sthl, Pernille Harris, Jan-Dierk Grunwaldt, Karlsruhe Institute of Technology (KIT), Germany NTNU, Norway: David Nicholson, Magnus Rnning, Karina Mathisen, Anders Holmen, Alexey Voronov and Nikolaos Tsakoumis. Manchester University, UK: Nigel Poolton University of Szeged, Hungary: Pal Sipos.

Scientific motivation X-ray absorption spectroscopy (XAS), including a number of techniques as EXAFS (extended X-ray absorption fine structure) and XANES (X-ray absorption near edge structure), plays an exceptional importance in many areas of chemistry and environmental science to determine structure or speciation in non-crystalline samples. EXAFS has been used to determine the structure around the absorbing atom for heavier elements than calcium for more than 30 years, and both theory and data treatment procedures are very well established. Already in the early days its excellent suitability for studying materials in their working environment was exploited. One major challenge is to study low concentration samples, which is a common situation in natural systems. Furthermore, more and more demanding reaction conditions are followed in materials (high temperature, high pressure, corrosive environment) and time-resolved studies are required in the subsecond timescale. One major aim should be to enable XAFS studies at concentrations lower than at any currently running beamline worldwide. Thus, the high photon flux and exceptional beam stability of MAX IV will enable development of a XAFS beamline with unprecedented sensitivity and performance. This includes the challenge to study very small objects or the chemistry extremely close to a surface. We will below give some examples where new scientific borders can be passed by use of the proposed beamline. Fundamental chemistry The knowledge of structures of metal complexes in solution and non-crystalline solid phases is fundamental for the understanding of their chemical and physico-chemical properties. Hydration and hydrolysis of metal ions plays a very important role for e.g. transport and up-take of metal ions in both natural systems, and the active species in industrial applications. The occurrence of metals in the environment is often related to industrial processes and other human activities. As a consequence of the often low concentrations in natural systems, hydrated and hydrolyzed species often are the dominate forms of many metals. An area of increasing importance is to study species and molecular structures of fundamental model systems at low concentration in order to interpret and understand natural systems. There is a trend of replacing lead by bismuth in various products, e.g. ammunition, solders, cosmetics and pharmaceuticals, since bismuth is generally considered to be less toxic than lead. The speciation of bismuth(III) in aqueous systems is well known in concentrated systems, but studies are lacking on dilute systems, and how pH affects the speciation in dilute systems. It is not possible to extrapolate from the structures in the solid state as the nuclearity is normally very concentration dependent, e.g. in [BiOn(OH)12-2n]6+ complexes, n = 4 and 6. Another area where XAS has a unique property is to study structures in the solid state as complement to crystallography, as XAS is lattice independent. A large number of structures of metal complexes, especially such ones with high crystallographic symmetry, have been proven to be incorrect as crystallography gives information of the average. XAS and crystallography are highly complementary techniques, but an area needed to be further developed. The increased use of nanoparticles in consumer products, such as food packing and clothes, for their bactericidal effects, results in potential environmental risk. This kind of very small particles are presumed to have somewhat different structures, especially in the surface which constitutes a large fraction of these particles, but experimental studies are in principle lacking. XAS has for a long time been one of the major tools to study the structures of metal containing active centra in proteins and enzymes. However, there is still a high demand for this kind of studies, and also here higher fluxes, and in some cases also smaller beams, required to study even more dilute systems. Archaeology The present knowledge of speciation and chemical conditions in the Swedish historic warship the Vasa is large parts obtained by synchrotron light. Very detailed information of the sulfur and iron speciation as function of depth has given an in-sight to chemical reaction taken place. The great advantage of using XAS in archaeological material in general is that accurate chemical analyses can be performed without any destruction. There are certainly many areas with e.g. archaeology where XAS techniques can be used to non-destructive analyses of extremely valuable material. Radiochemistry The complexation of actinides in solution and solid phase is an increasingly interesting topic. Detailed spectroscopic studies using e.g. EXAFS have given important insight in the prevalent oxidation state and its coordination chemistry of actinides in both solutions and solid phases. Actinides and especially the light actinides are a very special chemical group in that they are able to assume many different oxidation states both in solution and solid state. XANES is one of the sharp tools that can be used to

obtain information on the oxidation state also at very low concentration, and often the very small amounts available. The speciation of actinides is normally obtained implicitly using potentiometric titration, solvent extraction or ion exchange studies where a model is fitted to the experimental results. The use of EXAFS allows direct study of the coordination chemistry in solution. The interactions of actinides with several natural ligands such as phosphates, silicates and humic substances can be studied as well as interaction with "artificial" but important ligands such as isosaccarinic acid. In addition to these fundamental questions other more applied questions like coordination chemistry in an organic phase will give insight in e.g. how to optimize processes for actinide recovery and separation from spent nuclear waste. Biogeocehmistry and environmental science A revolution in our ability to understand and model Earth surface systems has created a new and rapidly growing research discipline; Molecular Environmental Science (MES). For a rapid development of this research area, XAS techniques play a unique and central role. This branch of science is the acquisition of knowledge at the molecular level of the materials (fluids, minerals, organic matter, biomass, etc) at or near the Earths surfaces, of the chemical and biological processes by which they are dispersed or concentrated, and of the effects on these processes of human activity. Many of these processes have very complex mechanisms that must be understood at a fundamental level in order to develop models for predicting for example the transport of contaminants in aquatic systems or soils. Fundamental knowledge concerning the kinetics and reaction mechanisms of chemical and biochemical reactions that control the transformation of specific contaminants and nutrients and the synergistic and antagonistic reactions among them is also required. XANES and EXAFS spectroscopic methods are well-suited in many cases to provide molecular-level information about these processes, the reaction products resulting from them, and reaction intermediates that control overall reaction rates. Such methods are also needed to understand the complex interactions among biological organisms, natural solids, and contaminant ions and molecules that result in the dissolution of solids, the release of natural contaminants and nutrients, the interaction of contaminant ions with solid surfaces and natural organic matter, and the formation of biominerals and other precipitates that can sequester contaminant/nutrient ions. Many contaminants are present and transported in nature associated with particulate matter where the particle sizes typically are ranging from micro- to nanoscale. The contaminant may be adsorbed to the particle surfaces as surface complexes or surface precipitates, or entrained in pores, or structurally incorporated in the host particle. Knowledge about the detailed molecular speciation, i.e. the molecular structures, compositions, and redox states, of contaminants associated with particles is essential in order to understand and predict their behavior in the environment. Thus techniques are needed for in situ speciation studies, which offer both high sensitivity (due to the often inherently low contaminant concentrations) and high spatial resolution. The application of micro-focused XANES and EXAFS spectroscopies provide means to study both real environmental samples and model systems. One illustrative example of the importance of obtaining molecular information on chemical speciation and its link to biological activity is risk assessment and subsequent possible remediation of mercury contaminated sediments. The critical issue associated to the risk of these sites is to which extent mercury is transformed to the highly toxic and bio-accumulating form of methyl mercury (MeHg). The methylation process is mediated by sulphate and iron reducing bacteria, and their activity is in turn controlled by the availability of energy-rich natural organic matter and the chemical speciation of sulfur and iron. Thus, in order to make a proper risk assessment of these sediments, we need to understand how bacteria interplay with different forms of organic matter, sulfur, iron and mercury, on a molecular level. A first approach to solve this complicated issue is taken by a combination S-XANES, Hg-EXAFS and Fe-XAS in order to link the chemical speciation of S, Hg and Fe to the methylation process. However, only with the photon flux, low emittance and spatial resolution obtained with MAX IV these processes could be quantified at in situ conditions. Catalysis research Catalysis plays a decisive role in all chemical areas. More than 90% of the chemical processes use nowadays catalysts demonstrating its impact on the world economy. In addition, it is considered the key technology in the solution of energy and environment problems. In order to understand processes on catalytic surfaces often model systems are used. Equally important is the study of the real catalyst. Industrial heterogeneous catalysts are complex multicomponent systems, usually consisting of several elements and phases. The state of the catalysts depends intimately on the conditions under which the catalyst operates. The study of the catalyst under reaction conditions is essential to obtain structural

and chemical information on the active state and attain the understanding needed to design better catalysts in a rational way. For these purposes, the EXAFS technique is unique with its high penetration length and elementspecificity. Hence, it becomes possible to study the chemical state of a specific element in a catalyst, whether it is amorphous or acting as a promoter, a poison or a main component. It is a key technique for probing nanoparticulate materials, such as colloidal and heterogeneous metal catalysts. The high brilliance of modern synchrotron radiation x-ray sources facilitates in situ studies which provide direct structure-function relationships with both spatial and time resolution; this is especially effective when applied in combination with complementary techniques such as x-ray diffraction, mass spectrometry, and optical or vibrational spectroscopies. New XAS technique developments in data acquisition and, especially, detection in combination with brighter synchrotron sources promise even more sophisticated structural analysis. X-ray emission spectroscopy (XES) has already shown to be a valuable technique in 3d and 4d transition metal systems to separate the pre-edge features from the K main edge and resolve previously unobserved spectral features with a high sensitivity to the chemical and electronic environment of an element. The multiple pre-edge features and shoulders present in the XANES region become better resolved and easier to separate and analyse with the so called high energy resolution fluorescence detection (HERFD) technique. Insight in reactant adsorption sites and electronics of the metal nanoparticles is thus achievable. The energies of the fluorescence emission transitions are very sensitive to the chemical environment. When different emissions can be resolved and assigned to specific chemical environments, selective XAFS can be performed to probe those specific environments. This allows the characterization of individual components in chemical mixtures. The new MAX IV light source provides an excellent opportunity for probing the elementary processes in catalytic processes.

Technical description From the outset of user operations there is a strong demand for high quality XAS at the MAX IV facility. In order to utilize the advanced qualities of the MAX IV light source and to outperform currently available XAS facilities, the proposed XAS beamline will combine high brilliance generated from the source with versatility of spatial and energy resolution and energy range. XAS applications require a stable, broad energy range, non-coherent, high-flux source. In order to utilize the high flux and low divergence of the source, the beamline is proposed to be constructed at the 3 GeV ring on a 3.8 m long in-vacuum permanent magnet undulator (PMU) with 189 periods and a period length of 20 mm. The beamline is expected to operate in the energy range 4-30 keV, thus in order to utilize the maximum flux generated from the undulator source the 3rd, 5th , 7th, 9th and 11th harmonics need to be used (Fig. 1). The best XAS beamlines have traditionally been constructed on bending magnets or wigglers, which needs to be taken into consideration in the next phase of design process, the detailed technical report. The choice of an undulator source instead of a wiggler requires high demand on the stability of the source. The undulator is required to produce beam for highly stable and reproducible XAS scans up to 1500 eV scanning range.

Fig. 1. Flux of protons in the harmonics of the emitted synchrotron radiation An undulator generates a series of narrow-band harmonics with high flux whose energy can be manipulated by physically adjusting the undulator gap. To its advantage, the total power of an undulator is significantly lower than compared to a wiggler, and the beam divergence is much smaller. The use of narrow band source for XAFS requires that either the gap be scanned synchronously with the monochromator or that the gap be tapered along the length of the undulator so as to broaden its spectrum at the expense of diminished flux (Fig. 2).

Fig. 2. Flux density of tapered (blue) and un-tapered (red) undulator as a function of energy. The magnetic field strength is varied by 10% over a length of 1m.

As it can be seen in fig.2, by varying the magnetic field strength by 10% over a length of 1m, the flux density decreases from 1015-1014 to 1013 (ph/s/mm2/0.1%BW) for 3rd, 5th , 7th and 9th harmonics. But by tapering the undulator the flux density distribution becomes much more even over the energy range, it very much resembles the even flux distribution over a broad energy range generated from a bending magnet or a wiggler. The proposed undulator source, PMU20, will allow for fast gap scanning as well as undulator tapering mode, which will enable for run the monochromator in Quick scan mode. Beamline characteristics Several possible options have been considered for the beamline optics setup to optimize the beam size and divergence, beam stability and convenience of use. This design proposes implementation of two experimental stations, one for XAS measurements and the other one for -focused XAS measurements (see Fig. 3 and Table 1).

Fig. 3. Overall layout of the beamline at the 1.5 GeV ring at the MAX IV facility The beamline design is based on a liquid nitrogen cooled double crystal monochromator (DCM) with in-vacuum interchangeable flat Si(111) and Si(311) crystals and two sets of mirrors. The first optical element is the DCM which is placed 32m from the source. The high total power of 14.8 kW produced by the source gives power density of 94 W/mm2 at the first monochromator crystal at 32m from the source. In order to prevent severe power load on the crystals, cooling with liquid nitrogen is required. After the monochromator, a pair of water cooled flat mirrors for higher order harmonic rejection is installed. One consequence of using crystal monochromator is that higher order reflections are always present. For example, for the Si(111) crystal the second order reflection is forbidden so that the most intense high order harmonics is the (333) reflection at three times the energy. In order to decrease and remove contributions from higher order harmonics two flat mirrors will be used. The mirrors act as low pass energy filter. They have unit reflectivity for X-rays below the critical angle for total external reflection, and the reflectivity falls rapidly above this angle. The critical angle varies with X-ray energy, and the mirror coating, so that the mirror high energy cutoff can be tuned to reject the unwanted harmonic energy. In order for mirrors to operate in full energy range 4-30 keV, they are coated with two stripes, Pt and Pd. The double mirror system removes effectively higher order contribution by keeping the exit beam direction without loosing X-ray flux. There are no focusing optical elements installed prior to the XAS station. Thus, the beam size at sample position on the XAS station at 40m from the source is 1.0x0.9 mm2 (h x v) and flux at 10 keV is 7.8*1014 (ph/s/0.1%BW). After the XAS station slits are used to cut down the beam size to 0.1x0.1 mm2 before the beam reaches the KB mirrors, which are used to focus the beam horizontally and vertically down to 1x1 m2 beam spot at the -XAS station. The -focusing of the beam results in significant decrease of flux at the -XAS station to 3.4*1011 (ph/s/0.1%BW). Experimental stations The design of the experimental stations will accommodate for specially designed sample and gas systems for in situ analyses including flow-through cells, grazing incidence surface measurements, as well as cryostats, furnaces and diamond-anvil cell for temperature and pressure control. Flow-through cells are important for in situ measurements of chemical, environmental and geochemical solution flow experiments, and for catalyst at controlled temperature and gas flow measurements. Flows-through cells are also important for biological and environmental samples where a static solution may suffer radiation damage. Other specially developed in situ sample cells include those for electrochemical and fuel-cell research and high pressure measurement. The highly collimated high brightness beam provided by MAX IV is excellent for surface XAS measurements. Measurements are made in total reflection, using either the reflected beam or

fluorescence. The high flux at this beamline will significantly improve the ability to measure very dilute, sub monolayer surface species. An important mode of data collection will be continuous-scan mode, where the monochromator is kept in continuous motion while measurements are made. Scans in this mode will only take seconds each, allowing for time resolved studies on this time scale. This beamline is dedicated to XAS and -XAS measurements in combination with XRF element mapping. On demand complementary techniques that will be available at the beamline are Raman and FTIR spectroscopy, UV/Vis and mass spectroscopy and CCD detector for complementary diffraction measurements. Also the rapid development of detectors of X-ray emission spectroscopy will be followed and included at the beamline. The equipment at the beamline including sample chamber and detectors will be movable easily between the two experimental stations, so that users have possibility to conduct experiments at both stations during allocated beamtime. Table 1. Source parameters Type Length (m) Period length (mm) No. of periods K value RMS effective vert. source size (m) RMS effective hor. source size (m) RMS effective vert. source div. (rad) RMS effective hor. source div. (rad) Flux density @ 10 keV (ph/sec/0.1%BW) FWHM beam size @ 40 m, h x v (mm2) bulk-XAFS Flux density@ 10 keV @ 40 m (ph/sec/0.1%BW) bulk-XAFS FWHM beam size @ 45 m, h x v (m2) -XAFS Flux density @ 10 keV @ 45 m, (ph/sec/0.1%BW) -XAFS Power density @ 10 keV @ 32 m (W/mm2) DCM Total power (kW) Shielding requirements The high energy of the photons transmitted through the beamline requires that all the components be enclosed to prevent ionizing radiation in the users area. The first two optical elements, the DCM and the mirrors for harmonics rejection could share a single optics hutch. The second hutch should enclose the experimental area which will include the KB mirror system for the -XAFS station.

PMU20 3.790 20 189 2.19073 9.25 49.1 11.5 12.6 1.1 x 1015 1 x 0.9 7.8 x 1014 1x1 3.4 x 1011 94 14.8

Research project proposals from dedicated user groups Transformation of Fe oxides in remediated soil The project aims at studying transformations of metallic Fe (vs Fe oxides) to Fe oxyhidroxides/oxides added to As and metal contaminated soils over time. Iron oxides are particularly effective for arsenic (As) immobilization capable of reducing dissolved As in soil by more than 90%. Poorly crystalline iron oxyhydroxides, such as ferrihydrite, have the largest specific surface area and therefore are the most reactive among Fe oxides. Corrosion of iron grit (Fe0) added to soil produces ferrihydrite, which reacts with dissolved As and reduces its mobility. Iron oxyhydroxides aging results in more crystalline Fe oxide phases such as goethite and hematite, which have lower specific surface area. This can cause a release of sorbed As and increase its leaching. Therefore changes in the relative abundance of Fe phases of various crystallinity can impact long-term As stability in amended soils. Extended X-ray absorption fine structure (EXAFS), X-ray absorption near-edge structure (XANES) and micro X-ray fluorescence (XRF) techniques, in combination with selective dissolutions and leaching tests will be applied to determine oxidation state, speciation, fractionation and local structure of As and Fe in soils remediated by phytostabilisation technique. The application of synchrotron based spectroscopic techniques will help to more accurately assess the risks associated with amendment remediation projects. Research constellation: Jurate Kumpiene, Anders Lagerkvist, Waste Science & Technology, Lule University of Technology (LTU). The unit consists of 5 senior staff members and 5 junior staff members working in cooperation with researchers at the Department of Chemical Engineering and Geosciences, LTU, within the areas of waste characterisation, utilisation, risk assessment, etc. Chemical and mineralogical transformations in ashes during ageing processes Ageing processes like hydration, dissolution, carbonation, oxidation/reduction and precipitation result in changes of the mineral composition of ashes and, hence, their chemical and physical properties. When using ashes as secondary construction materials, e.g. in landfill top covers, such changes can cause either leaching or immobilization of hazardous compounds, as well as they can enhance or deteriorate the mechanical stability of the construction. Hence, it is important to know which secondary mineral phases will form and how the speciation of various chemical compounds changes. Analytical methods we use to detect the chemical and mineralogical changes in aged ashes are: XRD and SEM for identification of well-crystallized mineral phases and morphological analysis of particles. Energy dispersive X-ray analysis (EDS, EDX or EDAX) is planned to be used for the identification of elemental composition of a certain point within the specimen. However, there is a need for a more accurate analytical technique such as extended X-ray absorption fine structure (EXAFS) in order to determine the element speciation and local structure in aged ashes in deeper detail. Scanning Tunneling Microscopy (STM) is of great interest for us, e.g. in order to see the micro changes of the phase boundaries in particle surface or thin sections down at the atomic layer. Research constellation: L. Andreas, E. Brnnvall, S. Diener; Div. of Waste Science & Technology, LTU. The unit consists of 5-8 senior staff members and 4-7 junior staff members. The main areas of activity are related to waste characterization and processes in e.g. waste treatment, soil remediation or landfilling that change material properties and lead to different behavior with regard to biological, chemical and mechanical stability (e.g. leaching/immobilization, gas generation).

Molecular speciation of Iron and Manganese in Soils, Sediments and Surface Waters The aims of this project are to develop a method for characterizing the molecular speciation of Fe, and Mn in environmental water samples under in situ like conditions using X-ray absorption fine structure (XAFS) spectroscopy and secondly to use this method in combination with studies on soil and sediment samples to characterize the speciation of Fe and Mn in a boreal catchment. We will use novel adsorbents (nanoparticles) specially designed to adsorb and thereby concentrate Fe and Mn species without inducing any major structural distortions. The adsorbent may then be separated from the water as wet pastes and analyzed by XAFS spectroscopy. In the second phase of this project, this method will be used to study how the Fe and Mn speciation in environmental samples varies with different geochemical parameters (pH, properties of organic carbon and presence of other metals), landscape characteristics (vegetation and soil type), and seasonal changes. Samples from soils, soil solutions, stream and lake waters and sediments from a boreal catchment in northern Sweden will initially be studied. In addition to a fundamental knowledge about Fe and Mn geochemistry, the molecular-level knowledge gained will improve the understanding of the role of Fe and Mn, and indirectly also phosphorus, in the bacterial utilization of terrestrially derived organic matter in stream and lake water and its importance for lake aquatic food webs. Thus, in a broader context this project has implications for the biogeochemistry of carbon. Lead PI: Prof. Per Persson, Dept. Of Chemistry, UmU. The research group consists of 3 senior and 6 junior staff. Focus is on molecular-level studies of processes at mineral, organic, and bacterial surfaces that influence the biogeochemical cycles of elements. The main objective is to provide fundamental understanding of chemical speciation, mechanisms and rates of reactions in the inherently heterogeneous aquatic and terrestrial environments.

Biogeochemistry of trace metals (mercury) in soils and sediments Mercury contamination is a severe environmental problem both at local point sources (industrial sites) and in forested wetland ecosystems. The focus of our research is to identify and quantify factors in control of transformation of inorganic mercury (Hg) to the highly toxic and bioaccumulating form of methylmercury (MeHg) in soils, sediments and waters. We also need to understand processes promoting the mobility and transportation of Hg and MeHg We combine state-of-the art analytical techniques like species-specific isotope dilution, SR spectroscopic, electron microscopic and isotope labeled microbial activity experiments to link the chemical speciation of Hg to net formation of MeHg. SR techniques includes Hg LIII-edge EXAFS, Fe K-edge XAFS and S K-edge XANES experiments conducted at beamlines at NSLS, ESRF, ANKA and MAX-lab. Our fundamental Hg EXAFS studies of the complexation of Hg to natural organic matter have received the highest recognition (Top Science Award by the journal Environmental Science and Technology in 2006). We have also made similar studies of Cu(II), Cd and Zn. We anticipate that an XAFS dedicated beamline at MAX IV will be most useful for further progress in this scientific field. Lead PI: Prof. Ulf Skyllberg, Dept. of Forest Ecology and Management, Swedish University of Agricultural Sciences, Ume and Ass. Prof. Erik Bjrn, Chemistry Department, Ume University. The research group in addition includes 3 PhD students and 2 Post-Docs. The objective is to provide fundamental understanding of chemical speciation, mechanisms and rates of reactions of mainly mercury but also other trace metals in aquatic and terrestrial environments.

Structure of hydrated, hydrolyzed and solvated metal ions and complexes in solution The knowledge of structures of metal complexes in solution and non-crystalline solid phases is fundamental for the understanding of their chemical and physico-chemical properties. Hydration and hydrolysis of metal ions plays a very important role for e.g. transport and up-take of metal ions in both natural systems, and the active species in industrial applications. The detailed coordination chemistry in solution gives in several cases the back-ground to why certain metal ions are catalytically active. The occurrence of metals in the environment is often related to industrial activities, or other human activities. The structures of hydrated metal ions in aqueous solution are accurately determined, but the structures of the hydrolyzed metal ions in aqueous solution are poorly studied, even though they play a very important role in natural systems. The often low concentrations in natural systems causes that the dominating species are in the hydrated and hydrolyzed forms of the metal. An area of increasing importance is to study the speciation, and their structures, of fundamental model systems at low concentration in order to be able to interpret and understand results from studies of natural systems. In this kind of studies synchrotron light based techniques as EXAFS, XANES and XPS are of utmost importance as one aims to study more and more dilute systems. This also means that the demand for high beam flux is steadily increasing. These studies are supported by the Swedish Research Council, and with beam-time from MAX-lab, Stanford Synchrotron Radiation Light-Source SSRL) and the European Synchrotron Radiation Facility (ESRF). Research constellation: Ingmar Persson and Daniel Lundberg, Department of Chemistry, SLU, Uppsala; Magnus Sandstrm and Lars Eriksson, Department of Material and Environmental Chemistry, Stockholm University, Stockholm. Local structure and dynamics at the nano-scale by means of EXAFS The project focuses on the local structure and dynamics of atoms in low symmetry environments, especially in systems exhibiting a high surface to volume ratio. The existence of nano focus possibilities at MAX IV will allow expanding our understanding on out of equilibrium growth phenomena leading to nano structuring in novel materials. Model systems in this area are surfaces and interfaces. We want to explore, using state of the art EXAFS, the correlation of specific material properties with the various moments of the Pair Distribution Function (PDF). Fields of interest are novel low dimensional magnetic materials and magnetic nanostructures relating with the existence of specific magnetic phases. Such phenomena are of technical relevance following the magneto elastic contribution to the total energy. The K edges of the late 3d ferromagnets are of interest in this context. Another emerging field of study is the one of magnetic inclusions in dilute magnetic semiconductor materials. Related fields of study concern the determination of the local crystallographic order on a surface or for an atom in a nanoinclusion, EXAFS operates without the presence of long-range order. Temperature dependent K-edge surface EXAFS is an ideal tool to complement material properties characterized in the home laboratory. With the high brilliance MAX IV storage ring we will be able to highlight the role of the asymmetry of the PDF on novel materials, with applications in the area of magnetism and surface science. We plan to extensively use an improved EXAFS analysis to systematically control systematic errors in the higher PDF cumulant values. A novel, Bayes-Turchin, approach to analyse EXAFS, has been developed within this collaboration, for the in situ determination of small effects in the EXAFS oscillations, integrating the ab initio FEFF code for EXAFS analysis. Research constellation: Dimitri Arvanitis, Physics and Astronomy, Uppsala University; Takehisa Konishi, Chiba University, Japan; Juanjo de Miguel, Universidad Autonoma de Madrid; Iwona Kowalik, IFPAN, Warsaw; Elizabeta Holub-Krappe, Helmholtz Center Berlin, Germany. This constellation combines the groups and expertise of several senior researchers. This collaboration is supported by national funds and funds targeting transnational collaborations, following bilateral agreements between the countries involved.

Lithium batteries during charge and discharge Materials for lithium batteries are often complex both in composition and in structure. Within the ngstrm Advanced Battery Centre we synthesise and characterise new such materials. The lithiation or delithiation of the materials is accompanied with a corresponding redox process in the host. Often there is also a structural change, a phase transition or an amorphization/crystallization. A set of tools is needed to fully reveal the mechanisms of the electrochemical activity. XANES and XAFS are especially useful for us in the study of redox activities in multi substituted transition metal oxides or silicates. The electrochemical activity of silicon, a promising new high capacity anode material for lithium batteries, is coupled to an amorphization of the material. Understanding the structure of the amorphous material is crucial for explaining the observed limitations in the reversibility of the lithiation process in certain composition ranges. For electrode materials with intrinsic non crystalline impurities it is possible to follow the electrochemical response both in the main phase and the impurity with XANES and or XAFS. Research constellation: T. Gustafsson and K. Edstrm, ngstrm Advanced Battery Centre, Uppsala University. The unit consists of approximately 10 senior staff members and 20 junior staff members. The main areas of activity are related to bulk, surfaces, interfaces, and nano-structures of electrochemically active materials. Studies of biomineralized and biomimetic calcium carbonates Synchrotron spectromicroscopy techniques are particularly useful in studying the inherent compositional variations in biominerals. Calcium carbonates are the most abundant biominerals in nature and it is for many reasons important to study them. There are many studies of the X-ray spectroscopical dependencies for the cations and the anions in these solids. These have been very important to the understanding of the local structure of calcium carbonates. Calcium carbonates often form via ionic clusters that fuse into amorphous nanoparticles, which finally transforms into crystalline forms. In addition to X-ray spectroscopy we apply a multipronged approach with using solid-state NMR spectroscopy and AFM and EM to enhance the understanding. We will employ both biomimetic synthetic means and biomineralized system to try to reveal the intricate details in the formation of calcium carbonate at low temperatures, which clearly involves both equilibrium and out-of-equilibrium dependencies. Research constellation: Niklas Hedin, Department of Materials and Environmental Chemistry, Stockholm University. Collaboration with Denis Gebauer (presently at SU); TK Sham, Western Ontarioconcerning evaluation of data. Is a partner of a potential EU (FP7) ITN-network - Mineral Formation in Biology: Disorder Order Transformations. Collaborations with the groups of Mattias Edn and Lennart Bergstrm at Stockholm University.

Speciation of metals and arsenic in soils, aquatic colloids and recycled materials The aim of this research is to obtain direct information on the coordination and oxidation states of metals and arsenic in materials relevant in the field of environmental technology. EXAFS and XANES spectroscopy, as well as microfocus XAFS / XRF element mapping, are used to obtain direct information on the speciation of metals and arsenic in environmental media and to study processes at the solid-solution interface, for example sorption to (hydr)oxides and complexation onto organic matter. Elements in focus at present include iron, vanadium, arsenic, copper, lead, cadmium and chromium. With the proposed XAFS Spectroscopy beamline we will be able to study the speciation of trace metals (such as arsenic, vanadium, cadmium and possibly also bismuth) at environmentally realistic concentrations; this will provide exciting possibilities for us to study the in situ speciation of trace metals with XANES/EXAFS, which currently is difficult at most existing synchrotron light source facilities. XRF element mapping is an important tool when elucidating the phase composition of metals in contaminated soils and sediments. The research combines direct spectroscopic methods with geochemical modelling and other complementary methods (e.g. using SEM, XRPD, CFF, FFF and ecotoxicity tests), and the obtained information is used to optimize remediation methods and improve environmental risk assessment procedures. There is extensive collaboration with a large number of national and international partners. Funding is from research councils (VR, Formas, SIDA) and from industrial sources (SSAB, LKAB). Research constellation: J.P. Gustafsson, P. Bhattacharya, G. Renman, Land and Water Resources Engineering, KTH, D. B. Kleja, Soil and Environment, SLU. The units consist of about 8 senior staff members and about 5-10 PhD students active in this research field. Homogeneous metal catalysis in organic chemistry We are investigating and developing homogeneous metal catalysts for applications in organic synthesis and neighboring disciplines. In many cases, the nature of the active catalyst is unknown. Currently, we are employing a combination of computational techniques and experimental kinetic studies, sometimes supplemented with NMR techniques to elucidate the mechanism and the structure of the active species. We have recently become interested in applying XAFS techniques to furnish critical data about our systems. We're currently working with Fe catalysts, where we need to ascertain both oxidation state and solution structure. Future applications will include both Cu and Pd, and possibly other metals in the first two periods of the transition metals. The new beamline would provide us with new opportunities in our investigations of these metals. Research constellation: Prof. Per-Ola Norrby, Department of Chemistry, University of Gothenburg. Application of XANES and EXAFS in the Cultural Heritage Conservation science X-ray methods such as EDX and XRF have long been used as research tools by material scientists and chemists active in art technological research, conservation of museum objects and historic building materials for characterization of e.g. pigments, mortars and corrosion of bronzes and ancient coins aiming at determination of elemental composition. With the use of XRD it has been possible to more thoroughly characterize and identify crystalline compounds. However, the sample size required for XRD have often made analysis with XRD impossible when precious museum objects are analysed. With the introduction and increased availability of synchrotron radiation in elemental analysis notably XANES and EXAFS it will be possible to extend research to hitherto impossible problems regarding detailed material characterization of ancient metal alloys and also of ancient non-crystalline materials made of glass and enamels on porcelain, ceramics and metal objects and the state of degradation of these materials. In addition, building materials could be characterised in more detail and various degradation and atmospheric corrosion mechanisms could be clarified and understood. Research constellation: Jonny Bjurman, Margareta Edebo Ekroth, Ingalill Nystrm, Anne Hbu, Kristian Andersson, Cultural Heritage Conservation Gteborg University. Synchrotron radiation application research in cooperation with B-M Steenari, Environmental inorganic Chemistry.The main areas of activity are related to investigation of material composition and material degradation processes in cultural objects and building materials.

Reactions of ash forming species in combustion of solid fuels and high temperature corrosion The metal bearing fuel components are exposed to a complicated system that includes drastic temperature changes, reducing and oxidising conditions, the presence of various gases. In addition, mineral additives and combustion bed materials are used in some applications, such as fluidised bed boilers. Thus, a number of transformation reactions are possible for the metal species in the fuel. Knowledge of the chemical forms, i.e. the speciation, of metals in ash of various types is essential for the development of appropriate methods to modify, handle and utilise combustion residues. The research on the chemistry of metals in combustion and in ash has benefitted from results obtained from XAFS measurements made at ESRF and MAX-lab. The speciations of Cd, Cu and Zn has been the primary targets of investigation and we aim to continue investigating the role of different fuel additives, such as kaolin and sewage sludge, on the reactions and binding of these metals and others, such as Pb, Cr and Ni. We also work on treatment methods for ashes and slag, and in those investigations XANES and EXAFS will provide information on oxidation state and speciation of various elements. In addition, in the research on high temperature corrosion processes in combustion facilities and in other energy conversion applications, such as fuel cells, the detailed information about element oxidation state and speciation that can be obtained from XAFS measurements can be a valuable complement to other methods used. Research constellation: B-M. Steenari, C. Ekberg, L-G. Johansson, J-E. Svensson, L-E mand, Environmental Inorganic Chemistry; Industrial Materials Recycling; Competence Centre High Temperature Corrosion and Energy Conversion Chalmers University of Technology. The constellation consists of 8 senior and 10 junior scientists from different departments at Chalmers. The main areas of activity are related to combustion and gasification of solid fuels, such as biomass, coal, waste derived fuels and sewage sludge and include investigations of ash fouling, corrosion as well as ash and slag properties. In addition material issues and corrosion processes in fuel cells are being investigated.

Application of XAFS methods in nuclear chemistry The complexation of actinides in solution and solid phase is an increasingly interesting topic at the moment. Detailed spectroscopic studies using e.g. EXAFS have given important insight in the coordination and oxidation state of actinides in both solutions and solid phases. Actinides and then especially the light actinides are a very special chemical group in that they are able to assume many different oxidations states both in solution and solid state. XANES is one of the sharp tools that can be used to obtain information on the oxidation state. The coordination chemistry in actinide solution is often obtained implicitly using potentiometric titrations, solvent extraction or ion exchange where a model is fitted to the experimental results. The use of EXAFS allows direct study of the coordination chemistry in solution. The interactions of actinides with several natural ligands, such as phosphates, silicates and humic substances, can be studied as well as interaction with "artificial" but important ligands such as isosaccarinic acid. In addition to these fundamental questions other more applied questions like coordination chemistry in an organic phase will give insight in e.g. how to optimise processes for actinide recovery and separation from spent nuclear waste. Research constellation: C. Ekberg, Gunnar Skarnemark, Stefan Allard, Stellan Holgersson, Teodora Retegan, and Mark. Foreman Nuclear Chemistry Chalmers University of Technology. The group consists of the above mentioned seniors which work full or part time and 7 junior scientists working ful time. The main areas of activity are actinide chemistry, solution chemistry, radiation chemistry, nuclear reactor chemistry, production and investigation of super heavy elements and radiopharmaca.

Catalysis research at the Competence Centre for Catalysis at Chalmers The research is focused on catalysis for emission control with a growing share of energy related catalysis. It is executed in three main programs; Reduction of nitrogen oxides in excess oxygen, Oxidation of hydrocarbons and particulates, and Catalytic techniques for sustainable energy systems. The programs are closely related with strong synergies, where the common themes are energy, emissions and catalysis. Of special importance for the successful research in the centre is the strong connection between experimental and theoretical activities, the collaboration between different disciplines and the close involvement in the projects by the member companies. The research on NOx storage catalysis has been particularly successful. Experimental studies in combination with kinetic modelling and electronic structure calculations have enabled breakthroughs in both kinetics descriptions and mechanistic understanding of this concept. Regarding the industrial interface, the attention is manifested by many recent requests for participation in joint research projects within the frame of, e.g., EU, MISTRA, SSF, FFI, as well as in bilateral projects with companies. Of special importance in catalysis research is techniques that enable us to follow catalysts and catalyzed reactions in situ. Research constellation: Magnus Skoglundh, Chalmers. The Competence Centre for Catalysis, KCK, is since 1995 an interdisciplinary research centre within heterogeneous catalysis at Chalmers. The research is focused on catalysis for emission control with a growing share of energy related catalysis. KCK has successfully developed into an internationally well-known research centre with a very broad expertise and is today internationally leading in environmental catalysis. KCK strongly support the proposed beam-line at MAX IV dedicated to in situ XAFS studies. By this unique set-up, including a sophisticated reactant delivery system, we will be able to, simultaneously, follow the catalyzed reaction (changes in gas phase concentrations of reactants and products by mass spectrometry), the surface coverage (evolution of reaction intermediates and speculators on the catalyst by infrared spectroscopy) and the active phase (changes of the structure and oxidation state by XAS) under reaction conditions.

Understanding ion conduction in glasses from experimental and computational techniques We use mainly neutron and x-ray diffraction, EXAFS and dielectric conductivity measurements in combination with reverse Monte Carlo (RMC) modelling and bond-valence calculations to explore the relation between structure and conductivity in fast ion conducting glasses. In this project the proposed beamline at MAX IV will be ideal for carry out the EXAFS measurements, which give us detailed structural information about the local environment of the mobile cations. Thus, with the proposed beamline for EXAFS measurements we will be able to determine whether the mobile cations are mainly coordinating to anions in the added salt or oxygens in the glassy network. Both bond distances and coordination numbers can be estimated with good accuracy. The EXAFS data, with its detailed structural information about the local cationic environment, can thereafter be used as input data in RMC modelling of the microscopic glass structure. The inclusion of EXAFS data in the structural modelling will then improve the reliability of the, for the conductivity, important local structure around the mobile cations. By applying bond-valence calculations on the structural models we are furthermore able to determine the energetically most favorable pathways for the ions, and thereby understand how the ionic conductivity depends on the detailed microscopic structure of the glasses. The knowledge can be used to develop new optimized ionic conductors for future solid state batteries and other electrochemical cells. Research constellation: Mainly J. Swenson Chalmers and S. Adams Singapore University. The project also involves several other senior and junior staff members through different national and international collaborations.

Selective oxidation on metal oxide catalysts The aim of the project is to obtain basic information about complex metal oxide catalysts. Our interest here is to disclose the catalytic functions and the related structures that are required of a catalyst to perform selective oxidation or ammoxidation of a hydrocarbon to the desired product involving several elemental steps. Besides activity measurements, catalyst characterization is a major part of the research. The main techniques used are XRD for determination of the bulk structure, XANES to have information about the coordination and valences of the metals, XPS to obtain information about the surface composition and the oxidation states of the metals, Raman spectroscopy to have structural information about supported oxides, and electron microscopy (SEM, TEM, HRTEM) which gives structural information about individual crystals, defects and amorphous material. Synchrotron techniques (XRD, XANES, EXAFS) are useful for the project especially for in situ studies, giving information about the changes in structure and oxidation states that occur under influence of the catalytic reaction, the temperature and the partial pressures of the reactants. Research constellation: A. Andersson, R. Hggblad, Chemical Engineering, LTH. The unit consists of approximately 4 senior staff members and 4 junior staff members. The main areas of activity are related to heterogeneous catalysis with focus on basic research of candidate catalyst systems for use in important industrial processes. Catalyst characterization is a major activity using a variety of physical techniques including synchrotron radiation aiming at creating a better understanding of the relationship that exists between catalytic performance and catalyst structure including surface structure.

Study of clay minerals using X-ray techniques The KBS-3 concept for a Swedish repository for high-level radioactive waste includes three barriers: copper canister, swelling clay and suitable rock. It is vital that the clay retains its properties over a long period of time. Available clay materials are evaluated under repository-like conditions in the alternative buffer materials experiment (ABM), which was started at the sp Hard Rock Laboratory in 2006. The first of the three ABM parcels, containing 11 different clay materials each, was retrieved in May, 2009. The aim of our project is to study fundamental processes of importance in this context. In order to determine the oxidation state of iron in the swelling clay minerals we use XANES at the FeK-edge from the ABM samples, which have been exposed to reducing conditions in the ground. Determination of the spatial distribution of reduced iron in the clay barriers would be greatly facilitated if mapping techniques using a micrometer-sized x-ray beam could be utilized. Research constellation: Staffan Hansen, Polymer & Materials Chemistry, Lund University; Daniel Svensson, SKB AB, Oskarshamn; Clay Technology AB, Lund.

Structural dynamics with time resolved X-ray spectroscopy It is a long nourished dream among chemists to get both structure and dynamics from the same experiment, i.e. to directly obtain time resolved structures showing the three-dimensional evolution of a molecular system in the course of a chemical or biological reaction. The true molecular timescale, where chemical bonds are broken and formed, charge is transferred between molecules and atoms or ligands are exchanged in the course of a complex reaction, is that of picoseconds and femtoseconds. In order to monitor and follow in real time how such reactions occur we consequently need ultrashort X-ray pulses in the femtosecond and picoseconds time domain. X-ray absorption spectroscopy (XAS) is a powerful probe of local electronic and geometric structure of molecules and materials. XAS does not require crystalline samples, which makes it a powerful tool for study of e.g. biomolecules, solid-state materials and liquid phase samples. Molecular function often emanate from a local structural change, making time resolved XAS an ideal tool for studies of molecular function. Specific areas of research where TR-XAS will be implemented: Photocatalysis with transition metal complexes; chemical reaction dynamics the molecular basis of chemical reactivity breaking and making of chemical bonds; artificial photosynthesis; electron transfer in metal-organic complexes for dye-sensitized solar cells; function of metal ions in natural pigments (melanin). Since molecular structural dynamics occurs on a wide time scale from microseconds to femtoseconds it is essential to have access to both the ultrafast (~100 fs) and somewhat slower (~100 ps) timescales in different experimental facilities. Research constellation: V. Sundstrm, S. Canton, J. Uhlig, G. Smolentsev, N. Gador, P. Chabera, Chemical Physics, Lund University. Approx 30 scientists working on molecular dynamics in chemistry, biology and material science, using ultrafast spectroscopy techniques probing the electromagnetic spectrum from the far infrared (THz) to the X-rays.

Structure and function of biological materials At least 50 % of all proteins are metallo-proteins and their functions are related to redox processes. We are currently using EXAFS to deduce the detailed structure around the active metal sites in metallo-proteins. These sites are generally poorly described from X-ray crystallographic data due to limited resolution and Fourier termination errors at the metal site. Another problem is the tendency to reduction of the metal in the X-ray beam. We are developing a flow-cell that will avoid that problem and which will allow studies under variable redox, pH etc conditions. MAX IV will with -focusing and high intensity be ideal for this kind of studies. Catalysis in ionic liquids We are approaching the end of the fossil fuel era and the chemical industry is looking at alternative, renewable sources for fuels and raw materials. Ionic liquids are effective media for catalysis in the production of bio-fuels and raw materials, and they have become an important part of the catalysis research in our department. When transition metal complexes are involved EXAFS is a very powerful tool for structural characterizations before, under and after the processes. In particular in situ measurements using reaction cells will be crucial for the understanding and development of these processes. Research constellation: Associate professors Kenny Sthl and Pernille Harris. In addition are two Ph.D. students presently engaged in these projects at Department of Chemistry, Technical University of Denmark, Lyngby.

Structure and biogeochemistry of cationic and anionic layer minerals Minerals with layered structures play a central role in defining a number of soil and sediment properties. Classical are ion exchange properties, where the minerals themselves are unchanged due to the reactions. Recently a lot of interest has focused on the dynamics that particularly transition metals exhibit during reactions, and how that in turns changes the properties of the minerals. Because these minerals are part of the soil and sediment turnover of important nutrients and xenobiotics, we must learn the details of these interactions. We plan to use the dedicated beamline at MAX IV for detailed investigations of these reactions and thus compliment our TEM and Mssbauer studies of these minerals. Lead PIs: Ass. Prof. Christian Bender Koch & Professor Hans Christian Bruun Hansen, Department of Basic Sciences and Environment, Faculty of Life Sciences, University of Copenhagen The research group in addition includes 2 PhD students and 2 Post-Docs. The objective is to provide fundamental understanding of structure and reactivity of layered minerals in soils and sediments Structure-activity relationships in heterogeneous catalysis using fast scanning EXAFS and microspectroscopic methods The long-term aim of this project is to develop catalysts for exhaust gas catalysis (selective catalytic reduction and NOx-storage-reduction) and energy related catalysis (e.g. transformation of biomass platform molecules and synthesis gas to higher alcohols). Both at Karlsruhe Institute of Technology (Energy Related Catalysis Research) and at the Technical University of Denmark (Catalysis for Sustainable Energies) strategic research has been devoted to the direction, among which operando spectroscopic studies is of outmost importance to rationally design new and better catalysts. For this both conventional EXAFS studies but also more advanced spectroscopic studies are required, among which time-resolved and microspectroscopic studies are of outmost importance. This is because many structural transformations occur in the millisecond to second timescale, especially ignition and extinction of reactions, oscillatory reactions or reduction/oxidation. In this case QEXAFS is an excellent tool for further investigations. Moreover, selective oxidation reactions of biomass platform molecules and exhaust gas catalysis will require spatially resolved studies. This is due to the fact that the concentration of the substrate molecules and the product concentration will change over the reactor. In order to determine its structure, a microbeam in combination with a Quick-scanning monochromator would be advantageous. Finally, in many cases promoters will significantly improve the catalytic activity, which require a high intensity beam and appropriate fluorescence detectors. In summary we suggest the following equipment installed at a hard X-ray EXAFS beamline infrastructure for catalysis experiments including on-line analysis by gas chromatography, mass spectrometry and infrared spectroscopy implementation of a quick-scanning monochromator for time-resolved measurements (full EXAFS region) option for focussing to a microbeam high intensity using an insertion device and good fluorescence XAS detecting systems, optional RIXS and high energy resolved fluorescence detected XAS combination with complementary techniques would be beneficial (XRD, Raman, Infrared).

Research constellation: Jan-Dierk Grunwaldt has a Chair in Chemical Technology Heterogeneous Catalysis at the Karlsruhe Institute of Technology (KIT, University Campus) and strong collaboration with the Technical University of Denmark (formerly Chair in Catalysis and Chemical Engineering, now adj. professorship). The group consists of several senior staff members. Focus is on catalyst preparation, application in energy-related catalysis and exhaust gas catalysis and in situ spectroscopy. In collaboration with the ANKA synchrotron facility new in situ spectroscopic cells for operando studies in catalysis and sensor technologies are developed that could be preferentially extended to MAX IV to establish complementary studies.

Characterisation of catalytic processes in SCR-deNOx systems Synchrotron based research is a strategic priority at NTNU and access to beamtime is crucial to completing PhD projects within the set timeframe. An example of a project is the structural and electronic characterization of materials used in the selective catalytic reduction of NOx. The removal of NOx is important for air quality and the search for cost effective catalysts is ongoing. Zeolites commonly used in the SCR-deNOx process have problems such as diffusion limitations and coking. Therefore, we have turned our attention to aerogels. The silica aerogels are a class of mesoporous materials with large surface areas and highly interesting surface properties such as hydrophobicity. We have developed a method for incorporating copper into silica xerogels and aerogels. Preliminary in situ XAS studies with limited beamtime reveal that the system is interesting. The aerogel stabilizes copper(I) during treatment with a propene/NO/O2 mixture. Catalytic measurements on copper aerogel show an abrupt increase in deNOx activity after 400C, a conversion greater than those reported for our commonly used copper zeotype systems We propose extending this work to include variants of the system that include a range of pore sizes, copper contents combined also with other elements. This experiment is an example of several that are only possible with the appropriate infrastructure such as that at the SNBL and reflects the increasing sophistication of XAS experiments. Research constellation: Karina Mathisen, David Nicholson, Magnus Rnning, NTNU. The group consists of approximately 5 senior staff members and 10 junior staff members. The main areas of activity are related to inorganic materials and heterogeneous catalysis. There is in-house access to the various types of electron microscopy, x-ray diffraction, Raman- and IR spectroscopy and other methods of characterising catalysts and materials.

Studies of Fischer-Tropsch catalysts at industrial working conditions The aim of this proposal is to study Fischer-Tropsch catalysts by measuring cobalt K-edge XAS (XANES and EXAFS), preferably in combination with XRD and Raman during Fischer-Tropsch (FT) activation and synthesis. The modes of deactivation in FT synthesis catalysts are highly depending on reaction conditions. It is therefore necessary to study the catalysts at industrial working conditions (typically 20 bar, 210C, H2/CO=2) to obtain relevant data. Information from the proposed techniques is highly complementary and provides in combination with simultaneous activity measurements an approach to deconvolute the various deactivation mechanisms. XAS is able to give information about the oxidation states of Co during the reaction whereas XRD gives information about crystallite/particle sizes and hence sintering. The transformation of hcp cobalt into fcc cobalt is a possible explanation for the loss of activity during FT synthesis. Both XRD and XANES are able to distinguish between hcp and fcc cobalt. Also formation of inactive cobalt phases such as cobalt aluminates and carbides are detectable both in XRD and XAS. Raman (in combination with other techniques) is capable of distinguishing between various types of carbon containing deposits. The results from the in situ experiments will be compared with ex situ results obtained on spent catalysts from an industrial pilot plant and supplemented with results from e.g. TEM, chemisorption, SAXS and kinetic studies. Research constellation: M. Rnning, A. Holmen, A. Voronov, N. Tsakoumis. Department of Chemical Engineering, NTNU, Trondheim, Norway. The Catalysis Group at NTNU/SINTEF consists of 12 senior staff members and 30 PhD/postocs. The main area of activity is heterogeneous catalysis, mainly within energy and environmental technology. The group is involved in several EU-funded projects and is part of a national CoE on natural gas conversion (inGAP).

Correlating luminescence processes with the structural and defect properties of wide bandgap optical materials The use of synchrotron radiation offers unique possibilities for probing and understanding the sometimes complex processes that underpin luminescence in wide band-gap materials; this is realised since the local structure of a material (as revealed by x-ray absorption spectroscopy) can be analysed directly through the luminescence emission itself. Of particular importance is the soft x-ray regime, since not only does this encompass many of the most important core-level energies of technologically relevant materials, but the methods are most sensitive/useful in this energy range. To exploit such Optical Detection of XAS (ODXAS), we have an on-going programme of instrumental and technique development, which underpins our research interests in a number of fields. To this end, 3 mobile spectrometers have been constructed (for ODXAS, micro-imaging ODXAS, and correlation of ODXAS with spin-resonance of optically-active defect sites). When deployed at MAX IV, these will open up new research possibilities, in terms of both the high brilliance of the photons, and in exploiting the timed structure of the photon pulses for probing fast luminescence transitions. Research constellation: N.R.J. Poolton and B. Hamilton; Photon Science Institute, Manchester University, UK and A.J.J. Bos, Technical University of Delft, The Netherlands. The collaborative working group consists in total of 7 academic staff together with associated research students. The main areas of activity relates to understanding of the optical processes active in semiconductors and insulators (for use in optical devices, memory storage and persistent luminescence phosphors).

Chemistry of metal ions in strongly alkaline solutions and solids crystallizing from them The project is aimed at characterizing the structure and reactions of various metal ions present in strongly alkaline aqueous solutions, both in the liquid state and in the solids crystallizing from these liquids. Several metal ions are known to be sparingly soluble in these systems, but they are suspected to form highly soluble ternary complexes containing bi- and trivalent metal ions and certain complexing agents. These solution species could be the key e.g. to understand the mechanism of the action of alkaline earth metal ions in the so-called causticization process of industrial process liquors, or the formation of layered double hydroxides, recently proven to form even under these harsh caustic conditions. Characterization of these solution species as well as the solid crystals obtained from the liquors is of obvious importance both from industrial and academic perspective. X-ray absorption spectroscopy is the most suitable technique to reveal the local structure of these metal ions (e.g., Al(III), Ca(II), etc.) in these compounds (in particular for those forming in solutions). The use of XAS makes possible to obtain a detailed picture of these systems, when it is used in combination with other complementary experimental means. We already have some experience with the EXAFS facility at MAX-lab (beamline 811) for studying the local structure of Fe(III) in alkaline solutions and in the solid state. It would be extremely useful for our research group to have opportunity to perform further XAS experiments and we would certainly take the opportunity for using this facility in our project. Research constellation: P. Sipos, I. Plink, University of Szeged, Hungary. The research group is part of the Chemistry Division (48 senior staff members) within the Faculty of Science and Informatics and consists of 2 senior staff members, 2 PhD students and several undergraduate students. The main areas of activity are concerned with solution equilibria and structure, nanostructures and catalysis. The group has in-house access to multinuclear NMR, FT-IR, FT-Raman, various microscopies and powder X-ray diffraction. Inter-departmental collaborations provide access to further facilities, such as solution X-ray diffraction and Mssbauer spectroscopy.

Main constellations committed to the beamline project Spokes persons and members of the XAFS steering committee: Professor Ingmar Persson, Department of Chemistry, SLU, Uppsala Professor Ulf Skyllberg, Forest Ecology & Management, SLU, Ume Professor Per Persson, Department of Chemistry, Ume University, Ume Associate Professor Britt-Marie Steenari Chemical and Biological Engineering, Chalmers, Gothenburg Professor Christian Ekberg, Chemical and Biological Engineering, Chalmers, Gothenburg Professor Jan-Dierk Grunwaldt, Technical Chemistry, DTU, Denmark Dr. Anna Puig Molin, Haldor Topsoe A/S, Denmark Dr. Alfons Molenbroek, Haldor Topsoe A/S, Denmark Professor David Nicholson, Department of Chemistry, NTNU, Norway Experts in XAFS beamline design and advisors to the steering committee: Professor Andrew Dent, Diamond Light Source, UK Dr. John Bargar, Stanford Synchrotron Radiation Lightsource, USA

Budget, staffing and time plan Budget proposal Undulator Front end Optics and experimental hutches and PSS system Infrastructure (fluid, electricity, AC system) Vacuum system Diagnostics including slits and filters Double crystal monochromator KB Mirror set up Electronics and controls Control room and lab room equipment Two end stations, chambers, sample mounts, gas system, tables Detectors for XAFS measurements Raman Spectrometer UV/Vis Masspectrometer CCD Detector for XRD measurements TOTAL Staffing and time plan 2011 Undulator + FE tenda 2012 Undulator + FE design Hutches + infrastructure build Undulator + FE production Undulator + FE inst. Beamline + optics tenda Beamline + optics production Beamline + optics inst. Commissioning beamline External work Time plan 2013 2014 Detailed design 2015 2016 Amount (MSEK) 12 5 5 5 2 4 4 3.2 5 2 3 4 2 1 1.5 2 60.7

Paperwork

Based on time plan we estimate the following personnel requirements during construction and commissioning, assuming that the beamline components will be installed by the manufacturer.

Man-years

2011 1

Man-years to be financed 2012 2013 2 4

2014 4

2015 4

The Materials Science Beamline Spokespersons: Peter Lazor, Uppsala Univ., Ingmar Persson, SLU, Uppsala, Sven Lidin, Lund Univ., Edvin Lundgren, Lund Univ., Jens Birch, Linkping Univ,. Magnus Odn, Linkping Univ., Stefan Carlson, MAX-lab It is proposed to construct a world-class Materials Science beamline operating at energies up to 100 keV. The exceptional flux and smooth energy distribution from a super-conducting wiggler source at the 3GeV ring at MAX IV will be used for state-of-the-art X-ray diffraction experiments (XRD) and X-ray absorption spectroscopy (XAS). The beamline will to a large extent be complementary to the proposed Swedish beamline at Petra III, Hamburg and the high energy range is also complementary with scientific research performed at neutron sources. Close beamline collaboration with the European Spallation Source (ESS), Lund, is thus anticipated. The beamline will also complement the proposed undulator beamlines at MAX IV that cannot effectively access energies above 30 keV. The main experimental techniques covered by the proposed beamline are: XRD and XAS studies requiring high X-ray penetration through thick widows or samples In-situ, high-resolution powder diffraction High-energy XAS, K-edges above 30 keV (e.g. lanthanides, 36 - 86 keV) X-ray fluorescence spectroscopy on dilute concentrations of heavy-metals Grazing incidence XRD and XAS Three-dimensional X-ray diffraction (3DXRD)

Time-resolved experiments (ms range) for the study of dynamical processes at real operating conditions will be at the core of beamline operation. Of particular interest are studies at non-ambient conditions such as high-pressure or high or low-temperature studies, where the environmental chambers have to be penetrated. The materials engineering community will need access to highenergy photons to penetrate bulk engineering components found in the automotive and aeronautical industry. Stress and strain relationships and penetrating imaging of bulk materials is of large interest to commercial users. An integration of other analytical techniques such as Raman spectroscopy will be made to offer complimentary information simultaneously with the X-ray measurements. This beamline will therefore be an outstanding tool for many Materials Science research topics. Main constellations committed to the beamline project: Department of Earth sciences, Uppsala University Department of Chemical and Biological Engineering, Chalmers University of Technology Division of Synchrotron Radiation Research, Lund University Department of Chemistry, SLU, Uppsala Division of Polymer and Materials Chemistry, Lund University Department of Physics, Ume University Department of Physics, Biology and Chemistry, Linkping University Division of Surface and Corrosion Science, Royal Institute of Technology Competence Center for Catalysis, Chalmers University of Technology Division of Chemical Engineering, Lund University SKB AB, Oskarshamn, Clay Technology AB, Lund Department of Materials and Environmental Chemistry, Stockholm University Division of Combustion Physics, Lund University Materials Science and Engineering, Royal Institute of Technology Department of Chemistry, Technical University of Denmark Institute of Physics PAS, Warsaw, Poland Dept. of Materials Chemistry, Adam Mickiewicz University, Poland

Scientific motivation Research at photon energies above 30 keV is important in Materials Sciences and gives the opportunity to perform unique experiments that are not possible at other beamlines at MAX IV. The penetration depth for important construction materials such as copper metal at 100 keV (see Table 1.) is sufficient to perform in situ experiments in many commercial and industrial process chambers. This also has profound advantages in experiments on e.g. buried thin-film interfaces and on samples contained in reaction cells with thick windows, such as diamond-anvil cells and other hightemperature/pressure devices. Experimental difficulties such as absorption, extinction and multiple scattering effects, often complicating data analysis at lower energies, can in most cases be neglected at higher energies. For liquid and amorphous samples, the possibility to reach high momentum transfers in the range of q = 30 - 50 -1 is crucial for a successful data analysis. The high q range is also necessary in high-resolution electron density studies when investigating bonding in e.g. transition metal complexes. Table 1. One absorption length (1/element) at different energies for important construction metals. Al 30 keV 100 keV 3.4 mm 21.8 mm Fe 0.16 mm 3.7 mm Cu 0.1 mm 2.5 mm

New materials: There are many important applications for high energy X-ray experiments on novel materials, such as thermoelectric materials which can transport heat or directly convert heat to electrical power. The most frequently used thermoelectric material is Bi2Te3. An important use of the beamline would be for in-situ high-energy XAS studies (Te K edge is at 31 keV), as well as careful crystallographic investigations up to high q values to study complex structural modulations. Hard cutting tools are important for industry, and there is an intense research for new ceramics and composite materials. To improve the hardness of cutting tools, e.g. tungsten carbide grains are often bound by a binder phase, consisting of e.g. Co and Ta. The tools can also be hardened by spray- or dip-coating with hard carbides. High-energy XAS and XRD can be used to study in detail the bonding of binder phases to WC, and the microstructural changes in the cutting tools during machining can be studied in situ at operating conditions. Nanostructured metal has attracted much interest both from applied and fundamental aspects stemming much from the changes in mechanical and magnetic properties. New routes to e.g. W, Ni, Co and Cu and alloys or heterometallic mixtures of them have been developed. Applications may be found in porous electrodes and catalysts, thin film magnetic sensors, chemically and wear resistant and ductile coatings. The mechanisms and control of the heating process are obtained through detailed studies on the phase-development from the viscous liquid to the final metals and their sintering on further heating. An important development in the synthesis of new silicon nitride based phases, such as amorphous La4,8Si5,2O5,6N8,0, has made it possible to make silicate glass with an exceptional refractive index. In-situ XAS measurements of the La K edge (39 keV) is a possible route to study the La bonding in the material. Time resolved studies can be made to study the effects of quenching from high temperature conditions. Energy research: For research on solar cells, batteries and fuel cells, it is important to follow processes (phase changes, ion mobility, electronic system changes...) in situ and in real time. Timeresolved studies using both XAS and XRD are very powerful techniques to investigate the properties of suitable materials for these applications. With the high-energy X-rays and surface sensitive techniques, inner part of batteries or thin-film membranes can be probed. The development of new electrolytes for Grtzel-type solar cells is important for optimization of solar cell performance. One type of solar cells uses a dye on an electrode that captures sun light by exciting its electronic system. Timeresolved in-situ studies can play an important role in the optimization of dye, electrode materials and inorganic electrolytes. High-pressure and high-temperature studies: The MAX IV facility would give the opportunity to build a beamline dedicated to the study of materials exposed to extreme conditions typical of the earths interior. The importance of such a beamline is given by the need for experimental data on structural

parameters for compounds at high pressures and temperatures. Fundamental research in physics, geophysics, and chemistry, as well as the development of solid state theory would benefit from this beamline. High pressure research is experiencing a series of technical and scientific breakthroughs. The discovery of novel physics, super-hard and wide band-gap materials as well as reaching deeper understanding of planetary interiors, deep-ocean biology and other extreme environments are some of the contributions of "extreme conditions" research.

X-rays X-ray

Fig. 1. Principle of (a) the diamond anvil cell and (b) the Paris Edinburgh large-volume press. New technologically important materials may be explored, and due to the possibility of using large volume presses, as well as diamond anvil cells, recovery strategies of significant amounts of material can be determined (Fig. 1). In-situ time-resolved experiments at extreme conditions could be applied to research areas like studies of catalysts, hydrothermal synthesis and corrosion. These are areas that are likely to have a large impact on chemical and technological industries. The optimal "extreme conditions" beamline should be capable of producing a highly focused, high-intensity photon beam, at energies up to 100 keV for experiments using large volume presses. To minimize attenuation of the X-ray beam by parts of the high-pressure/high-temperature sample holders, energies above 20 keV are necessary. High-energy X-ray absorption spectroscopy (XAS) is a growing research field that is not offered at many facilities around the world. The reason for this has been the difficulty of treating the increased core-hole lifetime broadening of the energy resolution at higher energies. The rare-earth elements are of common interest to both materials research (optoelectronics) and geochemistry, at trace concentrations. Routine XAS work has been limited to the L edges (at 5.5 to 11.3 keV), but these often overlap and interfere (there being 48 L edges in that span). In contrast, the 16 K edges of these elements are nicely resolved over the span of 38 to 65 keV (Fig. 2.). In environmental sciences, research on combustion in fluidised beds and the specification of metals in combustion residues, as well as studies of leaching of ash components require structural analysis of heavy metals in trace amounts (ppm levels). Another way of measuring the high energy K edges is by collecting the partial fluorescence yield (PFY) from the sharp 3p-1s transitions. This will be explored at the beamline by using a highresolution crystal analyser detector system in Rowland geometry.

Fig. 2. Normalized K-edge X-ray absorption spectra of lanthanide(III) ions in aqueous solution. (a) Before, and (b) after deconvolution of the core-hole width.

X-ray fluorescence (XRF): In research fields such as forensic sciences and cultural heritage studies it is often crucial that the sample is unchanged after the experiments. XRF spectroscopy is a nondestructive technique that, by using energies up to 130 keV, can measure heavy-metal concentrations in the ppm range and below for e.g. uranium. Spatial mapping of heavy-metal contaminants in the sample can be performed using a micron sized X-ray beam. X-ray powder diffraction including pair-distribution function studies: Phase identification, crystal structure determination and kinetic studies are some of the very many applications of the X-ray powder diffraction technique. It is one of the most over-subscribed techniques at synchrotron sources and is one of the cornerstones of any Materials Science dedicated beamline. The pair distribution function (PDF) analysis method is a powerful tool for the study of glasses, liquids and amorphous materials, as well as crystalline or partly crystalline materials, yielding crucial information about atomic-scale structures of nanosized materials and glassy conductors. The PDF method, which involves the direct model free Fourier transformation of X-ray powder diffraction data, gives the probability of finding any two atoms at a given interatomic distance. To obtain reliable results from the PDF analysis it is necessary to measure to high q values using high energy X-rays. Thin films, interfaces and multilayers: Grazing incidence surface X-ray scattering provides direct access to the structure of artificially and self-ordered two-dimensional inorganic, organic, biological and composite systems with characteristic length scales from a few tenths of a nanometers to several micrometers. Control of growth stresses is important for functional thin films. In situ depositon and grazing incidence X-ray diffraction may be used to tailor the stress-gradient throughout a thin film, thus enabling growth of stress-free or intentionally highly-stressed thin films and multilayers. This is important for the understanding of the physical origin of observed stress-generating phenomena during growth or annealing of individual layers in a multilayer structure. By using high energies, buried surfaces under thick layers (Fig. 3) can (a) (b) be effectively accessed and measured. X-ray Silicon nanowires can be used for Electrolyte X-ray electrical detection of bio molecules. This is because the conductance of a tiny Electrode nanowire is very sensitive to surface charges. Thus, the nanowire surface is Fig. 3. (a) High energies allow the penetration of thick functionalized with receptor molecules electrolyte layers for reflectivity and diffraction studies that bind specifically to a certain bio of the buried surface. (b) Sideways transmissionmolecule. The nanowires can be studied reflection scheme to enhance the signal from the using grazing incidence diffraction and bottom layer. 3D reciprocal-space mapping. Strain properties in materials: A number of properties of materials including fatigue, fracture and component performance are governed by the magnitude of strain fields around inclusions, voids and cracks. By the use of high-energy X-rays (high q-range), the full strain tensor can be derived directly from the diffraction signal of materials. Electron charge density studies: A number of important biological processes such as electron transfer and oxygen storage are known to involve polynuclear transition metal complexes with oxy-bridged metal cores. Charge density distributions is used to understand the chemical bonding and nuclear dynamics of molecular systems at a quantitative level. To determine the electron density around atoms, single-crystal X-ray data has to be collected to high q values at high photon energies. X-ray magnetic circular dichroism: A diamond phase retarder can be used to convert the hard X-rays from linear to circular polarization at energies below 30 keV. A development of phase retarders in the high energy range up to 100 keV is of great interest for in situ studies of magnetic materials. This would allow the X-ray magnetic circular dicroism techniques to be used on samples in thick-walled sample chambers. Three-dimensional X-ray diffraction: Non-destructive methods providing comprehensive threedimensional information on the structure and dynamics of polycrystals on the scale of the the grains, subgrains, particles or domains are of great industrial importance. 3DXRD mapping [1] is a unique technique to study deformed micro-structures and direct in situ observation of new orientations of bulk

Poulsen, Three-dimensional X-ray diffraction microscopy, mapping polycrystals and their dynamics, Springer, Berlin (2004)

nuclei in transformations. The position, morphology, phase, and crystallographic orientation can be derived for hundreds of elements simultaneously and their elastic strains can be determined. Furthermore, the dynamics of the individual elements can be monitored during typical processes such as deformation or annealing. A similar technique that will be pursued is X-ray diffraction contrast tomography, DCT [2], which combines absorption tomography and 3DXRD.

Fig. 4. 3D reconstruction of crystal grain distribution in annealed aluminium alloy.

Ludwig et al. J. Appl. Crystallogr. 41, 302 (2008)

Beamline description The beamline is based on a super-conducting multi-pole wiggler photon source (Table 2) that emits high-energy radiation with flux densities above 1014 photons/s/mrad2/0.1%bw at 120 keV. The angular acceptance of the beamline will be 1 x 0.1 mrad2 (horizontal x vertical). To relieve the optics from the substantial heat-load created by the wiggler photon flux, most of the low energy photons (below 20 keV) will be filtered out. Fig. 5 shows flux curves for the super-conducting wiggler with a 0.1 x 1 mrad2 aperture and 5.7 mm diamond filter. To achieve beamline operation from "day one", a simple optical scheme will be adopted. Further more complex optics will be added only after successful and stable operation of the basic setup. Efforts can then also be more effectively directed towards detector systems for high energies, which are likely to go through a fast and important developing phase during the coming few years. Heat-load management: The super-conducting wiggler emits a total power of 74 kW, and an initial finite-element analysis indicate that a 0.2 mm thick diamond filter, brazed to a water-cooled molybdenum holder, would reach a temperature of 10000 K when struck by the beam. By using the rather narrow aperture of 1 x 0.1 mrad2 (dictated by the storage ring design) before the filter, the temperature is still 2000 K. Finally, by tilting the filter to a 2 degrees grazing angle toward the beam (increasing also the effective thickness to 5.7 mm), the temperature drops to 340 K. The power after the filter becomes ~4 kW, which may still be too high for the cooled crystal optics, even though thin crystals in transmission mode is less sensitive to the heat load. This concept is only a preliminary design and further calculations have to be performed. Successful operation using such powerful beams has been shown at other synchrotron sources (e.g. rotating disk filters at ESRF and SLS) and a close contact and monitoring of their designs is crucial. Optical design: To obtain a beam-delivery system that is as simple and stable as possible. this beamline will adopt a similar optical concept as ID01, APS [3], and ID11, ESRF [4]. It is based on a high heat-load double crystal monochromator operated in Laue-transmission mode (LDCM). This monochromator will be either liquid-nitrogen, or water cooled, and operated under UHV conditions. Table 2. Beamline specifications Source SCW46 1969.48 mm total length 46 mm period length 42 periods K = 15.6, B = 3.6 T Ec = 21.7 keV Total power = 72 kW Energy range 30 - 120 keV (0.1 - 0.4 ) Energy resolution LDCM: Si(111): 2 10-3 (E/E) BDCM: Si(111): 2 10-4 Si(311): 5 10-5 Beamline accept. 1 x 0.1 mrad2 (h x v) Flux on first optics3 x 1014 @ 20 keV, Phot/s/0.1%bw 1 x 1013 @ 120 keV Beam size on XRD: 5x5 m2 to 40x4 mm2 sample (h x v) XAS: 0.5x3 mm2 to 30x3 mm2 Flux on sample ~ 1013 @ 20 keV (unfocused) Phot/s/0.1%bw ~ 1012 @ 120 keV (unfocused)

1e+16

Flux (ph/sec/0.1%bw)

(a) (b) (c)

1e+15

1e+14

1e+13 10 20 30 40 50 60 70 80 90 100 110 120

Energy (keV)

Fig. 5. Flux curves 25 m from the sopurce for (a) the SCW, (b) with 0.1 x 1 mrad2 aperture, and (c) with aperture plus 5.7 mm of diamond filter.

For stability reasons and to obtain maximum flux throughput by horizontally concentrating the wiggler beam, an operation in the horizontal plane is anticipated. The LDCM has an energy resolution sufficient for most XRD and XRF experiments (E/E ~ 10-3). Due to the larger band pass, an order of magnitude higher monochromatic flux is gained compared to the standard Bragg-reflection monochromators.

3 4

Shastri, J. Synchrotron Rad. 11, 150 (2004) Baruzzo et al. Medsi/Pan America SRI 2008

Included in the design of the LDCM, the development of a stable energy scanning mode is of high importance. If a true scanning mode can be implemented, crystal properties can be selected so that a much narrower band pass is achieved. In such case, the LDCM can be used also for XAS experiments.

40 m

35 m

30 m

25 m Frontend

XRD

CRL

XAS

Bragg DCM

LaueDCM

Beam cond.

Fig. 6. A tentative beamline layout showing the major optics and experiment stations. DCM = double-crystal monochromator, CRL = compound-refractive lens. After the successful installation and operation of the LDCM, a spectroscopic grade double-crystal monochromator operated in Bragg mode (BDCM) that can achieve the required energy resolution (E/E ~ 10-4) is installed before the XAS station. This monochromator will use the monochromatic beam from the LDCM. Both monochromators will be synchronized by ardware encoder outputs (capability in e.g. DeltaTau controllers) for fast and precise operation. Due to the high energy, the design of the BDCM is greatly simplified by the possibility to operate it in air or He atmosphere, without any special crystal cooling. By choosing different crystal planes in both monochromators, e.g. Si(111) for LDCM and Si(311) for BDCM, higher order harmonic content can effectively be excluded. Space in the optical hutch will be saved for future upgrades (e.g. multilayer mirrors or collimating CRL's), or user supplied optical equipment. XAS experiment station: The first experimental station is dedicated to X-ray absorption spectroscopy and will be equipped with ion chambers for transmission mode experiments. For X-ray fluorescence spectroscopy on dilute metal concentrations, a multi-element energy-dispersive Ge detector is anticipated. To utilise the sharpening effect of XAS data by measuring the partial fluorescence yield (PFY), a high-resolution detector based on an analyzer crystal setup will be available (Fig. 7). This is an upgrade that will be included in the design but will be made only after stable operation of the XAS station. A large area detector will be used for simultaneous X-ray diffraction detection. The sample stage should be equipped with vertical and horizontal translations, as well as roll, yaw and pitch rotations for the sample. It should be able to move a weight of at least 100 kg with high precision. A vacuum compatible sample chamber with integrated heating elements, liquid He/N2 cryostat, and gas-flow system with mass spectrometer will be the standard setup. The gas-flow system will be developed in collaboration with Haldor Topsoe A/S and the Swiss-Norwegian Beamline, ESRF.

Fig. 7. A bent-crystal spectrometer based on the Rowland circle geometry at BM30b/FAME, ESRF [Hazemann et al. J. Synchrotron Rad. 16, 283 (2009)].

XRD experiment station: The XAS and XRD hutches will be separated by a wall and beam stop so that measurements can be performed in the XAS experiment hutch while users install equipment in the XRD hutch. A heavy-load multipurpose diffractometer (Fig. 8) compatible with heavy UHVchambers, furnaces, cryostats, high-pressure cells, magnets, etc. will be installed in the XRD hutch. It would be possible to use the Newport diffractometer currently used at beamline I811, MAX-lab for this purpose. This diffractometer will most likely be competitive even at year 2015, provided that the control electronics is upgraded. Powder diffraction experiments can be performed on the diffractometer in two ways. 1) A position sensitive detector covering 90 - 120 degrees in 2 for time-resolved studies. 2) An analyzer crystal detector system for ultra-high resolution measurements. For high-resolution single-crystal diffraction and 3DXRD experiments, a low sphere-of-confusion goniometer system can either be built as a separate diffractometer, or if it is compact enough, be mounted Fig. 8. Newport heavy-load multidirectly on the hexapod of the heavy-load diffractometer. purpose diffractometer Large and fast area detectors are anticipated for an efficient collection of X-ray diffraction and scattering data. The usual CCD and hybrid pixel detectors based on silicon are not efficient at higher energies and the best options today are probably detectors used in homeland security applications, such as the Pixium flat-panel detectors [Daniels and Drakopoulos, J. Synchrotron Rad. 16, 463 (2009) ]. Collaboration on new developments for high energy area detectors will be made with SCINT-X, KTH for structured scintillator techniques, and Christer Frjdh, Mid Sweden Univ. for MEDIPIX developments. A position-sensitive detector for high-resolution timeresolved powder diffraction is anticipated. For this purpose there is an interesting development by Peter Siddons, NSLS, in Ge strip detector techniques. As a complimentary technique, Raman spectroscopy has proven to be very useful [Boccaleri, J. Appl. Cryst. 40, 684 (2007)] and a system that is adapted to both experiment stations will be available. The Raman system can also be used for off-line advanced high-pressure research using diamond anvil cells, or naturally also for general Raman measurements. Sample environment: The beamline will provide many different sample environments specially adapted to be mounted on the XRD diffractometer and on the XAS sample stage. Linkam and Anton-Paar high-temperature furnaces (1500 -2000 K) Furnace chamber with gas system for catalysis research (1200 K) Liquid He/N2 cryostat (4.2 K), Oxford cryostream (30 K) Diamond anvil cells (3 available from beamline I811, 100 GPa pressures) Paris-Edinburgh large-volume press (1 mm3 sample, 20 GPa, 1100 K) UHV-compatible sample chamber with load-lock system UHV to ambient pressure reactor chamber for surface catalysis (available from beamline I811)

Ancillary equipment: Redundancy in terms of more expensive equipment, such as detectors, will most likely be organized through a MAX IV pool of instruments. A large stock of spare parts and other equipment will be available at the beamline: Vacuum: Pumps, tubing, gaskets and fittings, gauges and controllers Electrical: Connections, fuses, power supplies Electronic: Current amplifiers, signal and data cables, connectors, multimeter and oscilloscope Alignment: Laser levels, auto level, theodolite and auto collimator system Ruby fluorescence system for pressure calibration An extensive set of tools

Control room and lab: One hutch for beamline control will be built. It will be divided into two sections for the XAS and XRD experiments, so that XAS experiments can progress when XRD users are performing installation and pre-alignment (using lasers). A small lab for temporary sample storage when transferring samples from the MAX IV preparation labs, and simple sample preparation will be available. The equipment will include desk space, optical microscope and tools.

Project descriptions Ordering in intermetallics The research in my group is focused on ordering in intermetallics. This area is of fundamental interest, representing an area of chemistry where bonding and valence are still incompletely understood, but also an area where there are a lot of interesting applications such as thermoelectrics, magnetocalorics and hydrogen storage materials. All aspects of intermetallic research depend on structural data, and structural elucidations are often complex and demanding. The use of synchrotron radiation is an indispensible tool in this research. The proposed beamline that will allow studies at short wavelengths will allow us to study a range of problems inaccessible to laboratory X-ray sources, and I strongly endorse the construction. Sven Lidin, Inorganic Chemistry, Stockholm and Lund University. Materials at extreme conditions of deep planetary interiors On behalf of the high-pressure mineralogy group at the Department of Earth Sciences, studying properties of materials at extreme conditions of deep planetary interiors, I wish to express our great interest and strong support for constructing the Materials Science Beamline at the new Swedish synchrotron radiation facility MAX IV. The anticipated experimental techniques, as well as the projected energy range, beam spot size, and other characteristics will make this beamline an ideal tool for high pressure, laser-heated diamond anvil cell experiments aiming at answering the most relevant questions concerning the evolution and dynamics of the Earth and other planetary bodies. Our research group is prepared to commit the time and other resources in order to assist the development of this beamline, which will represent a major research tool not just for a high-pressure research but for a broad geoscience community as well. Peter Lazor, Physical Geochemistry, Uppsala University. Carbon-based nanostructured materials at high pressures I am very happy to see plans for a Materials Science Beamline at MAX IV ring. During the last few years I have taken part in a number of projects involving high pressure diffraction work at three different beamlines (ID09A, ID27 and BM01) at the ESRF, Grenoble, and I have made several trips to the ESRF. Having access to a facility for high pressure structural work within Sweden would be an advantage from many points of view, in particular regarding travel time and ease of transport. At such a facility we would be interested in carrying out high pressure structural studies in Diamond Anvil Cells (DACs), primarily at room temperature but, if possible, also at both low (LN2) and high temperatures. The Department already has several DACs suitable for this particular type of work, and at would be very convenient to use the same procedure as at the ESRF, bringing pre-mounted samples in DACs already under pressure to the new beamline for diffraction work. Materials of particular interest during the last few years have been carbon-based nanostructured materials (fullerenes, nanotubes, "peapods") and complex hydrides, but many other materials may be of interest when the beamline becomes available Bertil Sundqvist, Dept. of Physics, Ume Univ.

Kinetic studies of solid-state transformations in wear protection layers Nanostructured materials' intention is to use the Material Science beamline at MAX IV for the following puroses: (1) Kinetic studies of solid state transformations of transition metal nitride/carbides/oxides synthesized by various physical vapor deposition techniques. These systems can be grown in a metastable state which upon exposure to a combination of temperature and pressure evolve a microstructure with favorable properties for example for wear protection of cutting tools. Basic phenomena of this spinodal decomposition such as diffusion barriers and chemical alloying will be studied. (2) 3D microscopy will be used to further the understanding of the micromechanical behavior of polycrystalline aggregates by evaluating the individual behavior of single grains in terms of elastic and plastic deformation. The group aims at doing basic research inspired by applications an we collaborate closely with companies such as SECO Tools, Sanvik Tooling, Element Six, Ionbond Sweden, Uddeholm, SKF etc. through large programs such as SSF-Materials Science program"MultiFilms", VINN Excellence center "FunMat", and VR-Linneus Grant "LiLi". Prof. Magnus Odn, Nanostructured Materials, Linkping Univ. Anodizing process of Al, and in situ catalytic investigation through quartz gas reaction tubes We propose to perform two different types of experiments at the Materials Science Beamline at MAX IV. In the first experimental setup, a new in situ electrochemical cell will be developed in which a high energy micro focused beam will penetrate one side of the cell and illuminate the functional interface of interest in the electrolyte, providing structural information of the interface on the atomic scale. Two material systems of interest can immediately be identified: a) A metal surface such as Al under anodizing conditions exploring the growth of a protective Al oxide/hydroxide depending on the composition of the original Al surface and the composition of the electrolyte. Such investigations could lead to an increased understanding of the anodizing process and the development of improved metal and in particular Al products, which is of significant interest to Swedish industry. b) In situ studies of functional interfaces in fuel cells under working conditions for the future development of more efficient fuel cells. In the second setup, we propose to develop a new in situ reaction cell for catalytic investigations. In this setup, an ordinary quartz based reaction tube containing the real catalyst material and flowing gases will be placed in the beam. The beam will penetrate the quarts glass as well as the catalytic material as the catalyst is "at work" converting gases into useful products or harmless substances. The cell will be scanned perpendicular to the beam, thereby providing a two dimensional cross section of the catalyst. At the same time, the gas is analyzed along the gas tube. In this way, we hope to obtain structural information of a real catalyst under working conditions, with the aim of developing new and better future catalysts. Such investigations are of significant interest of a number of industries in the Scandinavian region. Edvin Lundgren, Johan Gustafson, Synchrotron Radiation Research, Lund Univ.; Christofer Leygraf, Surface and Corrosion Science, KTH.; Magnus Skoglundh, Competence Center for Catalysis, CTH. Pressure induced transformations in polymers Concerning a new Materials Science Beamline at MAX-lab, we would be very interested to use such in our studies of pressure induced transformations under extreme conditions, especially if such studies can be done at both low and elevated temperatures. We presently use high pressure, in situ, Raman and dielectric spectroscopy and thermal properties measurements under high pressure to induce and study changes in materials of fundamental and technical importance. Besides phase transitions, the investigations include studies of pressure induced amorphization and reversing transformations under extreme conditions. We also study pressure induced irreversible transformations, which yield new states that can be recovered under normal pressure conditions, and currently one project concerns cross-linking of polymers with and without nano-fillers. The Materials Science Beamline would be used to augment these studies to get key information about structural changes, in situ, under high pressure. Ove Andersson, Dept of Physics, Ume Univ

High-Energy X-ray Absorption Spectroscopy: A New Tool for Structural Investigations of Lanthanoids The X-ray absorption spectra of aqueous solutions of hydrated lanthanoid(III) ions above their K edges have been measured in the energy range 38 (La) to 65 (Lu) keV. It is shown that the large widths of the core hole states do not appreciably reduce the potential structural information on the high-energy K edge EXAFS data. Experimental results show that an accurate determination of the structural parameters of the hydrated lanthanoid(III) ions can be obtained from the analysis of the K edge absorption spectra. The available k-range of the K edge spectra is much wider compared to that of the L3 edge, which are affected by the presence of very severe double-electron excitations, especially for the lighter lanthanoid(III) complexes. A comparative K and L3 edge EXAFS data analysis of nonahydrated crystalline neodymium(III) trifluoromethanesulfonate shows a clear advantage of the K edge analysis over the conventionally performed L3 absorption edge studies for structural investigations of lanthanoid(III) compounds and third row transition metal compounds. This is due both to the smaller influence of the double-electron excitations and to the wider k-range available. It has been found that from the analysis of a single EXAFS spectrum it is not possible to unambiguously determine the first shell coordination number, if the sample is not highly symmetric. However, the distance trend obtained from the analysis of the K edge data could be promising in elucidating the geometrical changes of the hydration structure throughout the lanthanoid series. Ingmar Persson and Daniel Lundberg, Department of Chemistry, SLU, Uppsala; Paola DAngelo, Department of Chemistry, University of Rome La Sapienza, Rome, Italy; Adriano Filipponi, Department of Physics, University dell Aquila Via Vetoio, LAquila, Italy. Selective oxidation on metal oxide catalysts The aim of the project is to obtain basic information about complex metal oxide catalysts. Our interest here is to disclose the catalytic functions and the related structures that are required of a catalyst to perform selective oxidation or ammoxidation of a hydrocarbon to the desired product involving several elemental steps. Besides activity measurements, catalyst characterization is a major part of the research. The main techniques used are XRD for determination of the bulk structure, XANES to have information about the coordination and valences of the metals, XPS to obtain information about the surface composition and the oxidation states of the metals, Raman spectroscopy to have structural information about supported oxides, and electron microscopy (SEM, TEM, HRTEM) which gives structural information about individual crystals, defects and amorphous material. Synchrotron techniques (XRD, XANES, EXAFS) are useful for the project especially for in-situ studies, giving information about the changes in structure and oxidation states that occur under influence of the catalytic reaction, the temperature and the partial pressures of the reactants. A. Andersson, R. Hggblad, Chemical Engineering, LTH. Study of clay minerals using X-ray techniques The KBS-3 concept for a Swedish repository for high-level radioactive waste includes three barriers: copper canister, swelling clay and suitable rock. It is vital that the clay retains its properties over a long period of time. Available clay materials are evaluated under repository-like conditions in the alternative buffer materials experiment (ABM), which was started at the sp Hard Rock Laboratory in 2006. The first of the three ABM parcels, containing 11 different clay materials each, was retrieved in May, 2009. The aim of our project is to study fundamental processes of importance in this context. In order to determine the oxidation state of iron in the swelling clay minerals we use XANES. We also investigate the swelling kinetics of the layer silicates with powder X-ray diffraction. If penetrating highenergy X-rays could be utilized for the diffraction experiments, robust sample holders in metal could be used. The samples could then be studied under conditions, which are more similar to those in a real repository. Staffan Hansen, Polymer & Materials Chemistry, Lund University; Daniel Svensson, SKB AB, Oskarshamn; Clay Technology AB, Lund.

Materials synthesis at extreme conditions The long-term goal of this project is to advance high pressure materials synthesis to a much broader applicability in terms of chemical reactions than what has been previously possible. The key is the enlargement of reaction volumes to approach 0.5 cm3 while maintaining accessible pressures up to at least 7 GPa. This represents a unique pressure-volume capability in academic settings and gives prospect to add pressure as a variable to solid-liquid reactions, such as flux and hydrothermal reactions, and solid-molecular fluid reactions with in situ generated H2, O2, N2, NH3, F2, etc. Emerging possibilities are access to hydrides, oxides, nitrides, and fluorides with unusual electronic structures and oxidation states and the exploitation of solvents in high-dense supercritical states as reaction environments. The materials science beamline at MAX IV will allow for in-situ diffraction and spectroscopy experiments on samples/reaction mixtures at various temperatures and pressures by using (resistive heated) diamond anvil cells (DACs). This gives the unique possibility to map reaction conditions that subsequently can be transferred to a large-volume synthesis experiment. Ulrich Hussermann, Department of Materials and Environmental Chemistry, Stockholm University. In situ catalysis investigations Catalysis plays a decisive role in all chemical areas and thus in the world economy. Understanding technological issues like reactor packing and oil and gas flow dynamics in catalytic reactors are essential in order to improve reactor design and efficiency. In order to get through the stainless steel walls of industrial reactors high energy X-ray beams with high flux are required. The extreme high energies achievable in the high energy beamline proposed at MAX IV open up new possibilities. In situ tomography can for instance be used to image the catalyst bed and put in evidence film effects in real reactors under steady reaction conditions. Catalyst bed reduction, start up and shut down procedures used at industrial plants can be reproduced in real reactors while followed by in situ XRD. The new knowledge can be decisive to optimize these procedures. Anna Puig Molina, Characterization R&D, Haldor Topse A/S Structural changes in materials induced by pressure, temperature or electric fields A main part of the work at the division of Inorganic and Structural Chemistry at the Department of Materials and Environmental Chemistry (formerly FOOS Chemistry) at Stockholm University concerns structural characterisation of materials, using techniques that include diffraction, EM and solid state NMR. The vast range of materials presently studied includes mesoporous crystals, nano-structured materials, soft/bio-materials, zeolites, transition metal oxides, hydrides, intermetallics, ceramics, semiconductors, catalysts and minerals. Although our in-door capabilities are good, experiments at synchrotrons and neutron facilities are frequently needed. The availability of a 30-100 keV X-ray beam line at MAX IV would provide us the considerable advantage of close-by access to XAS/XRD experiments of all the techniques quoted in the information pdf file e.g. time-resolved studies, data for pair-distribution functions, extreme conditions research. For our present or near-future planned research the possibility of recording XRD data for samples in vessels and/or under pressure is in particular attractive, as it could provide a means to study e.g. crystallization mechanisms for zeolites, structural changes in materials induced by pressure/temperature/electric field, or pressure/temperature induced amorphisation. The development of the beam line is thus expected to significantly benefit our research. Xiaodong Zou, Department of Materials and Environmental Chemistry, Stockholm University Application of hard X-ray imaging techniques to combustion systems and devices. Very hard X-ray will be used to image inside complex multiphase and heterogeneous flow and reaction systems of interest for combustion. The studies include gas-phase, spray and biomass combustion. The techniques will be directed towards applications to real world combustion systems and devices. The experiments will give fundamentally new input for the developments of combined chemistry- and flow dynamics models to make significant progress in combustion/energy conversion Science and Technology. These techniques will be very important for industrial partners Frederik Ossler, Division of Combustion Physics, Physics Department, Lund University

Time-resolved growth of individual bulk nano-sized tungsten carbide grains in polycrystalline cemented carbides The long-term aim of this project is to further develop the three-dimensional X-ray diffraction technique to be able to investigate submicron grains with full three-dimensional crystallographic and morphological information of bulk grains in polycrystalline materials. The model material that will be used for this purpose is cemented carbides, which means that WC grains are embedded in a Co matrix. This material has an extremely fine grain size and is therefore ideal as a model material to push the boundaries of the technique. In addition to the experimental methodology aim it will also be the purpose of this project to increase the understanding of grain growth in cemented carbides and grain growth in general. This will be achieved by in-situ sintering studies of grain growth at high temperatures. A. Borgenstam, P. Hedstrm and J. gren, Materials Science and Engineering, KTH. Nano-structured materials New functional materials are in many cases depending on their nano-structure, for example grain size and/or defects, or being amorphous. Wide angle scattering experiments (WAXS) offers a way of structural characterization of these materials by means of PDF-modelling. However, to be effective data have to be collected to very high Q-values. The Materials Science Beamline will offer such a possibility by its large energy range. One group of materials of interest is expanded austenites, high level nitrogen or carbon stainless steels, another is bulk metallic glasses. In addition, for both types of materials EXAFS studies of heavier elements (>Zr) will be very important for characterization of the local structures. In situ measurements to capture fatigue mechanisms both in bulk and locally will be a challenging but realistic possibility for this beamline. Associate professor Kenny Sthl, Department of Chemistry, Technical University of Denmark Structural properties of modern materials at ambient and high pressure Our groups are using high pressure diffraction as a tool in studies of modern materials since end of 1990s, with research focused on phase transitions and elastic properties of semiconductors and oxides. For this purpose, using high-energy X-ray beams has the important advantage of access to a large number of diffraction peaks. Consequently the information on the structure at the Materials Science Beamline will be much more detailed as compared to more classical beamlines offering X-ray energies of the order of 10 or 20 keV. For the purpose of high-pressure studies of inorganic materials, suitable pressure cells (diamond anvil cells and or a Paris-Edinburgh type cell) should be available. The materials of interest for our groups include mainly semiconducting and magnetic materials (nitrides, chalcogenides and multicomponent oxides). The planned studies involve these materials at the nanometric scale. For this direction, the opportunity, at ambient pressure, for using the Pair Distribution Function method is very attractive. This technique is developing rapidly and the limitation of necessary condition of using very high energies will be satisfied at MAXIV competing with only a few synchrotrons in the world. Wojciech Paszkowicz, Institute of Physics PAS, Warsaw, Poland, and Pawel Piszora, A. Mickiewicz University, Poznan, Poland

Beamline project organization The overall scientific responsibility of the beamline is shared among the "dedicated user groups", listed below. The design and construction of the beamline will be supervised by the "beamline advisory committee", listed below. Procurement, installation and operation of the beamline will be performed by an assigned group of MAX-lab staff in collaboration with the manufacturer of the equipment. The beamline project will be arranged after a project management template made for MAX-lab by the consultants PlanB. This company has implemented a common protocol for project management at MAX-lab. Dedicated user groups: Dept. of Earth Sciences, Uppsala University - Geophysics, Extreme conditions research - Peter Lazor Environmental Inorganic Chemistry, Chalmers Univ. - Fuel cell electrolyte materials - Sten Eriksson Synchrotron Radiation Research, Lund University - Buried interfaces - Edvin Lundgren Synchrotron Radiation Research, Lund University - Surface catalysis - Johan Gustafson Dept. of Chemistry, SLU, Uppsala - High-energy XAFS - Ingmar Persson Inorganic Chemistry, Stochkholm and Lund Univ. - High energy X-ray diffraction - Sven Lidin Dept. of Physics, Ume University - Nanocarbon compounds, high pressure - Bertil Sundqvist Dept. of Physics, Ume University - Pressure induzed transformations - Ove Andersson Nanostructured Materials, Linkping University - Hard surface layers - Magnus Odn IFM, Linkping University - Thin film and multilayers - Jens Birch Surface and Corrosion Science, Royal Institute of Technology - Corrosion science - Christofer Leygraf Chemical and Biological Engineering, Chalmers Univ. - Environmental catalysis - Magnus Skoglundh Chemical Engineering, Lund University - Catalysis - Arne Andersson Polymer & Materials Chemistry, Lund University - Clay minerals - Staffan Hansen SKB AB, Oskarshamn, Clay Technology AB, Lund - Clay minerals - Daniel Svensson, Materials and Environmental Chemistry, Stockholm University - High pressure - Ulrich Hussermann Materials and Environmental Chemistry, Stockholm University - Structural chemistry - Xiadong Zu Division of Combustion Physics, Lund University - Combustion systems - Frederik Ossler Materials Science and Engineering, KTH - Hard materials - A. Borgenstam, P. Hedstrm, J. gren Department of Chemistry, Technical University of Denmark - Nanostructured materials - Kenny Sthl Institute of Physics PAS, Warsaw, Poland - High pressure - Wojciech Paszkowicz Dept. of Materials Chemistry, Adam Mickiewicz University, Poland - High pressure - Pawel Piszora

Beamline advisory committee Peter Lazor, Dept. of Earth Sciences, Uppsala University Edvin Lundgren, Synchrotron Radiation Research, Lund University Ingmar Persson, SLU, Uppsala Sten Eriksson, Chalmers Univerity of Technology Jens Birch, IFM, Linkping University Robert Feidenhans'l, KU, Denmark Anna Puig Molina, Haldor Topsoe, Denmark Poul Norby, Ris DTU, Denmark David Nicholson, NTNU, Norway Ragnvald Mathiesen, NTNU, Norway Michael Drakopoulus, Diamond Light Source, UK Guoyin Shen, Advanced Photon Source, USA ke Kvick, MAX-lab, Lund, University Yngve Cerenius, MAX-lab, Lund University Carsten Gundlach, MAX-lab, Lund University Katarina Norn, MAX-lab, Lund University Stefan Carlson, MAX-lab, Lund University

Budget, staff and time plan Budget proposal Description Super-conducting wiggler, 2 m Frontend components Optical & experiment hutches incl. Personal Safety System Optics Laue-DCM Bragg-DCM Compound refractive lenses Diagnostics incl. slits End stations XAS station XRD station Sample environment Infrastructure Electronics, control, computing Vacuum system Misc. incl. fluids, liq.N2 & air condition Other Control room and lab 2 Total: 65 Time plan and staff Table 3: Time plan 2011 2012
Beamline design Tenders beamline & wiggler, delivery Design of XAS and XRD endstations Calls for tender of XAS and XRD endstation Beamline construction XAS and XRD endstation construction Commissioning beamline Commissioning XAS and XRD endstations Operation

Price (MSEK) 10 5 10 3 1 1 4 4 10 3 5 2 5

2013

2014

2015

Based on Table 3 we estimate the following personnel requirements during construction and commissioning Table 4: Man-years 2011 Man-years 1 2012 2 2013 3.5 2014 3.5 2015 2.5

The Imaging and Tomography Beamline Spokespersons: Yngve Cerenius, MAX-lab, Crister Ceberg, Medical Radiation Physics, Lund University, Robert Corkery, Institute of Surface Chemistry, Stockholm, Birger Schmitz, Dept. of Earth & Ecosystem Sciences, Lund University, Sergey Peredkov, BESSY, Germany 3D imaging using synchrotron X-ray microtomography allows unprecedented, non-destructive access to the structure, chemical composition and dynamics inside naturally occurring, technological and culturally historical materials well beyond what is currently available in Sweden. A microtomography beamline at MAX IV will significantly boost research in 3D imaging of samples as diverse as meteorites and fossils for studying the evolution of the solar system and the emergence and evolution of life on Earth; to biological tissue, medical devices, foods, and pharmaceuticals for studying health, disease and treatment; to metals, alloys, insulation materials, combustible materials for understanding phase transformations in steel and alloys, energy efficiency and energy conversion; to cultural heritage items. This wiggler beamline on the 3 GeV ring will enable research at the forefront of non-destructive materials probing. The beamline design and flexible end station set-up make a large range of investigations possible where imaging in 2 or 3 dimensions at synchrotrons has shown its usefulness. These applications include: Materials science (e.g. pores, cracks, precipitations, grain structures, small components, phase transitions and morphological transitions) Biology and geology (e.g. plants, insects, stones, fossils) Medicine (e.g. imaging of implants, structures of bones or soft tissues including application like micro-localization of toxic elements or tumor-targeting molecules) Cultural Heritage (old wood; stone and rock in sculptures, architectural materials, rune stones, glassware, oil paintings, frescos, ceramic vases etc; metal objects coins, swords, jewellery etc; historically significant books, documents and papers; objects from burial mounds and other archaeologically significant materials) The beamline is based on a superconducting wiggler providing competitive photon flux levels in the energy range up to 100 keV and relatively large irradiated areas. The number of optical components should be kept to a minimum to ensure best possible beam quality but the design will ensure monochromatic as well as a white beam option for high flux application (e.g. for fast in situ experiments). The high degree of coherence of the X-ray beam at the MAX IV facility will be utilized for phase contrast imaging. The design of the beamline and end station will permit a large range of imaging methods in 2 and 3 dimensions. High resolution absorption microtomography and phase contrast enhanced microtomography is expected to be standard experimental techniques at the beamline. In addition it is essential to also obtain chemical information from the sample. This will be achieved by scanning the energy over an absorption edge for a specific element and observe the absorption variations (XANES) and fluorescence (XRF) mapping. The proposal also contains setting up a commercial microtomography set-up including a conventional X-ray source at the present MAX-lab to build up a user community and the needed in-house knowledge about the technique. At MAX IV this equipment will be a part of the new imaging laboratory where it can be used for pre-characterization of samples Main constellations committed to the beamline project: Medical Radiation Physics, Lund University Institute of Surface Chemistry, Stockholm Dept. of Earth & Ecosystem Sciences, Lund University Dept. of Information Technology and Media, Mid Sweden University Dedicated user groups: Physical Metallurgy, KTH, Stockholm Johan gren Materials Engineering, Lund University - Srinivasan Iyengar Swedish University of Natural Science, Stockholm Stefan Bengtson & Else-Marie Friis Dept. of Physics, NTNU, Trondheim, Norway - Ragnvald Mathiesen Div. of Combustion Physics, Lund University - Frederik Ossler

YKI, The Institute for Surface Chemistry, Stockholm - Daniel Kalnin Dept. of Earth and Ecosystems Sciences, Lund University - Birger Schmitz Dept. of Medical Radiation Physics, Lund University - Sven-Erik Strand, Crister Ceberg Dept. of Oncology, Ume University - Elisabeth Kjelln Dept. of Biomedical Radiation Sciences, Uppsala University - Bo Stenerlw Dept. of Radiation Physics, Linkping University - Eva Lund Dept. of Medical Physics, Karolinska University Hospital - Albert Siegbahn Dept. of Oncology, Lund University - Jan Tennvall Dept. of Pathology, Lund University - Elisabet Englund Dept. of Radiation Physics Malm, Lund University - Sren Mattsson Dept. of Radiation Physics Malm, Lund University - Anders Tingberg Dept. of Historical Osteology, Lund University - Torbjrn Ahlstrm Radiation Physics, Surgery, and Pathology, University of Gothenburg - Eva Forsell-Aronsson

Imaging and Tomography The use of high brilliance and partial coherent synchrotron light for radiography and tomography allows rapid imaging with different contrast modes and resolutions down to sub-microns. This type of non destructive material probing is of high interest for a very wide range of applications and it will be possible to image samples as diverse as meteorites and fossils for studying the evolution of the solar system and the emergence and evolution of life on Earth; to biological tissue, medical devices, foods, and pharmaceuticals for studying health, disease and treatment; to metals, alloys, insulation materials, combustible materials for understanding phase transformations in steel and alloys, energy efficiency and energy conversion; to cultural heritage items such as wood from the Vasa ship (Fors, 2008) and Viking boats, stone from rune stones and objects from burial mounds for studying the conservation of Swedens national treasures. The user groups will typically have scientists otherwise unfamiliar with general synchrotron applications. For these users a microtomography beamline may be the entrance door also to other beamlines. This is an attempt to summarize the possibilities within three distinct disciplines: Materials Science, Earth Science and Medical Research reflecting the interest among the main constellations behind this proposal. Materials Science Imaging the interior structure of technologically significant materials in a non destructive way allows both understanding of the structure as a function of the process or synthesis variables and also acts as input data for modeling where a 2D model is inadequate. Perhaps the most important classes of technological materials that can benefit from structure oriented 3D microtomography are heterogeneous materials, in order to characterize the spatial distribution of distinct physical/chemical components, including free space. Amongst the important subclasses of heterogeneous materials are composites, porous materials and multigranular, multiphase materials. Therefore the class of heterogeneous materials represents the vast majority of materials that are being developed today. Homogeneous monophase crystalline materials, glasses and soft materials such as liquid crystals, gels and amorphous metals form another very important subset that can be imaged for defects, cracks, fractures and unwanted heterogeneities. 3D tomography therefore is widely applicable to the full range of today's advanced materials design and will be a key and indispensible characterization tool necessary for Swedish research and technology to be internationally competitive, both academically and industrially. Microtomography allows unprecedented 3D imaging of the microstructure of materials of industrial interest. This is of great interest for a number of different classes of materials. Below is a nonexhaustive list classified to illustrate the diversity of materials that could benefit from microtomographic imaging and chemical mapping: Materials with high porosity: Polymeric foams & ceramics Organic materials (bones, tendons, skin) Materials for agro-food (cornflakes, ice cream, chocolate pralines) Geological materials (clays) and civil engineering (soil, concrete, rocks) Entangled materials (glass wool, paper) Pharmaceuticals 3D structure of pills and tablets and capsules Composite materials: Multiphase ceramics Metallic multiphase materials/alloys Reinforced composites (polymer /paper / ceramic, metal / ceramic) Metallic materials: Steel, aluminium, brass, alloys of zirconium The possibility to utilize the high brilliance of MAX IV also gives the opportunity to do fast time resolved measurements enabling the study of phase transformations like solidification processes which could improve the understanding of optimal component production or solid phase transformation

in steel and other construction materials which is important. For the latter type of materials the penetration power of a synchrotron beam is essential. The X-ray beams produced at third generation synchrotron sources like MAX IV exhibit a high degree of coherence. This allows recording phase contrast images by varying the sample to detector distance. The great advantage with this type of imaging is the increased sensitivity for light materials (e.g. polymers) or for composites made up of materials with similar densities, like the common Al-Si alloy. Earth Sciences Three dimensional studies of geological samples by microtomography have seen a rapid expansion during the past few years, and it is becoming an increasingly important standard application in the earth sciences. Basically it will replace the classical tedious techniques of slicing and polishing geological samples in order to reconstruct structures of the sample interior. Almost all sub-disciplines in the earth sciences, including paleontology, meteoritics, soil studies, igneous petrology, mineralogy and sedimentology will benefit substantially from the new technique.

Fig 1 An embryo of an early cnidarian, about 540 million years old, from the Kuonamka River in the northern Siberia. The tomograms reveal eight tentacles studded with stinging capsules, never before seen in a fossil. As regards applications in the earth sciences, for example Ebel and Rivers (2007) recently presented a review in Meteoritics & Planetary Science of the potential use of 3D synchrotron microtomography studies of extraterrestrial materials. They could record the 3D density structures of bulk meteorites (0.5-3.0 cm3) at resolutions of 10-17 m/voxel edge, and of individual chondrules and calciumaluminium inclusions (CAI's) at resolutions as fine as 1.2 m/voxel edge. They showed that there is also a large potential in locating and quantifying different types of inclusions in millimeter sized extraterrestrial meteorites and to study the internal structure of microscopic (0.1-1 mm) minerals. In one experiment, Ebel and Rivers dispersed 200 microscopic spherules from lunar soils on glueimpregnated cellophane paper. By microtomography they could search for rare olivine phenocryst with possible glass inclusions. Paleontology is a field where microtomography can be expected to play a particularly important role in the coming decades. Swedish paleontologists, e.g. Stefan Bengtson and Else-Marie Friis, have been world-leaders in finding new, extraordinary applications of microtomography. Some of these studies are already classical, for example, in the study led by Bengtson of 600 million years old fossilized embryos. 3D microtomography could provide new important insights in the embryology during the initial emergence of the metazoans, i.e. the "animal kingdom" (Donoghue et al. 2006). Phase contrast X-ray tomography was used by Friis et al. (2006) to link fossil Cretaceous seeds to important groups of extinct Mesozoic seed-plants with cycad-like leaves and flower-like reproductive structures. These findings represent crucial insights into the evolution of plants. Three dimensional microimaging is likely to soon become an essential component of every earthscientist's toolkit, especially as instruments and facilities emerge that are optimized for increasingly sophisticated geological applications. In addition by performing X-ray fluorescence tomography the chemical composition of the fossils could be studied directly. Being able to analyze the elemental composition of the specimens non-invasively in three dimensions would mean a significant new step in understanding both the original composition and the taphonomic history of fossils.

Biomedical Applications Synchrotron radiation offers many exciting opportunities for biomedical applications in imaging, radiobiology and experimental radiotherapy. For absorption-contrast imaging, the high flux of the radiation makes it possible to use only a narrow energy-interval, optimised for the specific imaging situation. This reduces the effect of beam-hardening and scattered radiation, and results in improved image contrast. It also reduces the dose to the investigated object, since the beam does not include radiation at energy levels not contributing to image contrast. This is particularly important for imaging of living animals. While absorption-contrast imaging is extremely well suited for element-specific imaging, for instance by using the K-edge subtraction technique, there is in biological and clinical studies also often a need to differentiate between different kinds of soft tissue. With phase-contrast imaging, the soft tissue contrast is increased dramatically, as compared to the absorption-contrast technique, and biologically relevant structural and density variations are very much enhanced. At the same time, the radiation dose can be further reduced. Furthermore, the very small source size and large distances allow for an extremely good spatial resolution. With X-ray microscopy, both using absorption and phase contrast, objects can be imaged with a sub-micrometer resolution, allowing, for instance, probing the elemental distributions within a single cell. The most striking feature of synchrotron radiation imaging, as compared for instance with electron microscopy, is the possibility for micro-tomography with a spatial resolution of a few micrometres. This makes it possible to do morphological characterisation and element-specific imaging in 3D of tissue samples as well as living animals, and opens up for countless possibilities in biomedical and pre-clinical research. High energy synchrotron radiation also offers specific possibilities for experimental radiotherapy. Microbeam radiotherapy and photo-activation therapy have been found particularly promising. Microbeam radiotherapy uses highly collimated arrays of microplanar X-rays, with extremely high dose rate and very small divergence. In the separation between the microbeams, there is no primary irradiation. The existing data suggest that this technique is much better tolerated by normal tissue, than conventional broad beams. Photo-activation therapy is based on the selective accumulation of a drug containing heavy atoms into the tumor cells. Monochromatic synchrotron radiation in an optimized energy interval is then used to produce non-repairable, lethal damage to the tumor cells via photo-interactions with the high-Z atoms. A unique, and extremely interesting possibility for radiobiological research with synchrotron radiation, lies in the prospect of combining these radiation and imaging capabilities. It is well known that radiation effects depend on typical in vivo characteristics, such as vasculature and various immunological factors. Thus, there are important advantages to study radiobiological events using intra-vital microscopy. With a synchrotron based intra-vital microscope one would be able to combine the ability for irradiation with very high precision with the specific imaging capabilities reviewed above, directly in the living animal. Most synchrotron radiation facilities today have biomedical programs. Many of them even have dedicated beamlines, and biomedical imaging is often regarded as one of the core activities. The possibility of a Swedish biomedical program at MAX IV has attracted an intense nation-wide interest. We foresee that this is a growing activity and this beamline will give an excellent opportunity to realize many of the proposed projects and found a base for a dedicated biomedical beamline in a later stage. Research projects have been proposed in all the different areas mentioned above. Imaging applications include morphological characterization of tissue, micro-localization of toxic elements and tumor-targeting molecules in vivo, as well as real-time monitoring and quantification of tumor cell biological events. There are also proposals for radiobiological and therapeutic applications, as well as for the development of novel dosimetric methods suited for synchrotron radiation beams. As most of these biomedical applications are pre-clinical, it should be mentioned that there will be a future need for a nearby laboratory for housing and handling of research animals. Some applications will potentially also have great clinical and public value, and it should be considered to prepare for a future possibility for human subjects to be able to access the beamline area (preferably in a patient-friendly milieu). Finally, as similar requirements will be put on the future ESS facility, coordination of these issues is essential.

Yvonne Fors. Sulfur-Related Conservation Concerns for Marine Archaeological Wood. The Origin, Speciation and Distribution of Accumulated Sulfur with Some Remedies for the Vasa. PhD Thesis, Stockholm University 2008 Carlson, W. D., 2006. Three-dimensional imaging of earth and planetary materials. Earth and Planetary Science Letters 249: 133147. Cauzid, J., Philippot, P., Somogyi, A., Mnez, B., Simionovici, A., and Bleuet, P., 2006. Standardless quantification of single fluid inclusions using synchrotron radiation induced X-ray fluorescence. Chemical Geology 227: 165183. Donoghue, P.C.J., Bengtson, S., Dong, X.-p., Gostling, N., J., Huldtgren, T., Cunningham, J.A., Yin, C., Yue, Z., Peng, F. & Stampanoni, M. 2006. Synchrotron X-ray tomographic microscopy of fossil embryos. Nature 442: 680683. Ebel, D. S. & Rivers, M. L., 2007. Meteorite 3-D synchrotron microtomography: Methods and applications. Meteoritics & Planetary Science 42: 16271646. Friis, E.M., Crane, P., Raunsgaard Pedersen, K., Bengtson, S., Donoghue P.C.J., Grimm, G.W. and Stampanoni M. 2006. Phase-contrast X-ray microtomography links Cretaceous seeds with Gnetales and Bennettitales. Nature 450: 549-553. P Sourtti and W Thomlinson: Medical applications of synchrotron radiation. Phys. Med. Biol. 48:R1R35, 2003. Z Bencokova, J Balosso and N Foray: Radiobiological features of the anti-cancer strategies involving synchrotron x-rays. J. Synchrotron Rad. 15:74-85, 2008.

Beamline Description Beamline Summary Energy range Photon Source Optics 10 100 keV Super-conducting wiggler Monochromator: Internally cooled liq N2 DCM with Si(111), Si(311) & Si(511) crystals White beam option Optional set of compound refractive lenses after the monochromator for microfocus applications. 40 * 4 mm Standard mode: < 1 micrometer Using a compound refractive lens as X-ray magnifier: 200 nm (achievable at < 30 keV) Fast absorption and phase contrast imaging in 2 or 3 dimensions (radiography and tomography) plus chemical information by XRF and XANES.

Maximum field of view Maximum resolution Experimental Techniques

Source and Front end The beamline will be situated on a superconducting wiggler (Table 1) providing sufficient flux at energies up to 100 keV (Fig. 2). High X-ray photon energies are needed both for sample penetration of e.g. steel based samples but also for covering the K edges of contrast agents such as Gd (50 keV), I (55 keV), Pt (84 keV) or toxins like Hg (83 keV) or Pb (88 keV) Wiggler (super conducting) 2 12 33 3.5 19.6 20.9 75 67

Length [m] Magnetic Gap [mm] No of periods Peak Field [T] K value Critical Energy [keV] Total Power [kW] On Axis Power Density [kW/mrad2]

Table 1 Parameters on the superconducting wiggler (scw46ID)

Fig 2 Angular flux density a function of energy

The maximum aperture (defined by the design of the storage ring) is 1 mrad horizontal and 0.1 mrad in the vertical direction. The storage ring vacuum is separated from the beamline with a high quality diamond window (thickness 200 microns) with negligible coherence degradation. In addition an assembly of motorized removable attenuators will be used for spectral filtering when operating the beamline in white beam mode. Optics Hutch In order to guarantee the best possible beam quality in terms of stability and homogeneity the number of optical elements should be kept to a minimum. Besides white beam slits and diagnostics the main optical component is an internally liquid nitrogen cooled monochromator placed at 23 m from the source. In order to cover the complete spectral range this DCM must be equipped with Si(111), Si(311) and Si(511) crystals. The beamline will be operated in monochromatic or white beam mode depending on the application. White beam: Monochomatic beam: Experimental Hutch The standard sample position will be at 40 meters from the source providing a maximum field of view of 40*4 mm2. A shielded evacuated beampipe between the optics and experimental hutch provides a cost effective solution to achieve a large field of view. The flexible end station will permit a wide range of different samples and experimental techniques. A six axes high precision stage will provide the needed degrees of freedom for sample orientation. While an air bearing rotation stage will provide the scanning possibilities needed. The stage will be followed by a detector mounted on a motorized stage that allows optimizing the distance from sample to detector for absorption or phase contrast imaging. For high resolution applications sets of exchangeable compound refractive X-ray optics will be used both as incident beam condensers and post-sample objective lenses. There are different schemes for placing and combining these lenses to provide resolutions down to about 200 nm. At present this high resolution mode is feasible at energies below 30 keV. However, progress in CR lens research and manufacturing gives us a hope to extend the energy region to higher energies. For many of the described applications it is essential to also obtain chemical information from the sample. This could be achieved scanning the energy over an absorption edge for a specific element and observe the absorption variations (XANES). Fluorescence mapping will be done in combination with a micro beam option. By inserting sets of CR lenses after the monochromator a (< 10 m) micro beam can be formed, however, at the price of reduced flux on the sample. Detectors Different types of detectors will be needed depending on the application. A high resolution, fast readout, low-noise detector consisting of a scintillator in combination with an optical microscope and a CCD camera, such as the FreLoN or SensiCams would be the preferred choice for high resolution micro tomography. An energy discriminating area detector such as the Medipix3 in combination with white beam would be of interest for biomedical applications such as imaging with contrast agents. Finally a detector with read out speeds up 10 kHz would be required for time resolved experiments such as fluid dynamics or crack propagations. The CMOS camera could provide the needed read out performance but it should be noted that this is for large field of view/ low spatial resolution studies. In this type of flexible set-up the foreseen standard techniques would be absorption and phase contrast micro tomography, with the possibility to also obtain chemical information for elements with absorption edges all the way up to 100 keV. This combination will not be achievable at any other suggested beamline at MAX IV. It can also be noted that the combination of white (high energy) beam and near-field phase contrast is a powerful imaging technique also for organic samples since one can take advantage of the MAX IV coherent properties to form adequate near-field fringes and low absorbed radiation doses. Time resolved tomography (ultra fast, few s/tomogram) Fast high resolution radiography K-edge tomography, XRF & XANES imaging

Microtomography at MAX II The proposal also contains a commercial micro tomography set-up with a conventional X-ray source at the present MAX-lab to build up a user community and the in-house knowledge about the technique. At MAX IV this set-up will be a part of the new imaging laboratory where it can be used for precharacterization of samples, help in alignment and as second X-ray source for dual-energy imaging.

In situ three-dimensional imaging of engineering materials (Imaging/Tomography) Imaging using high energy X-rays is the only available technique to study different bulk phenomena in situ with high spatial resolution and high time resolution. The long term aim of this project is to explore this technique to solve different scientific questions and here one example is given. Bainite and martensite are common microstructures in ultra high strength steels and it is of practical importance to control these transformations during processing and reliable models are extremely valuable. For the modeling it is needed to have detailed knowledge regarding the mechanisms, which, especially for the bainitic transformation, has been debated for a very long time. New information would be gained by comparing the formation of bainite and martensite formed in the same steel at almost the same temperature using high energy X-ray tomography. The growth rate of martensite is very high, 1000 m/s has been reported, and the microstructures formed are very fine, nanoscale, why high energy Xrays are needed. Research constellation: A. Borgenstam, P. Hedstrm and J. gren, Materials Science and Engineering, KTH. The unit consists of 6 senior staff members and 7 junior staff members. The Division of Physical Metallurgy at Materials Science and Engineering at KTH is world-leading in the modeling of thermodynamics and kinetics in phase transformations. Although the main emphasis is on new theoretical predictive tools, experimental measurements and microstructure characterization play essential roles.

In situ sintering of porous metal powder compacts - Characterization of changes in pore structure and grain morphology using the tomographic method The long-term aim of this project is to characterize the progress of sintering in bulk metal powder compacts and develop a 3-D model for the same which would be useful in optimizing the production of near net shape powder metallurgical components. In this context, it is necessary to understand the structural changes and densification mechanisms in metal powder compacts as they are heated to and held at the appropriate sintering temperatures. In situ studies on sintering based on surface observations using an Environmental Scanning Electron Microscope, are being carried out at LTH (Materials Engineering Lab). But, changes in the bulk of the sample can only be studied by tomographic methods. The proposed project envisages kinetic studies on sintering in small metal/alloy powder compacts in the temperature interval 25 to 1200 C, in a protective gas environment (mildly reducing). Expected results from the studies include data on the size, shape and distribution of pores and particles in the bulk of the sample as a function of time and temperature and elucidation of the various stages of sintering. Research constellation: S. Iyengar, Materials Engineering and Colleagues from the Mechanical Engineering faculty, LTH. The unit consists of approximately 10 senior staff members and 15 junior staff members. The main areas of activity are related to mathematical modelling of various phenomena and experimental studies on materials characterization (using ESEM), thermodynamics and kinetics of materials and processes at elevated temperatures.

Synchrotron-based X-ray tomographic microscopy (srXTM) of fossil organisms (4 projects) The beginnings of multicellularity During most of its 4 billion years of existence, Earth's biosphere was almost exclusively microbial. Size increase through multicellularity has, however, been a constant theme through a large part of this history. We are investigating the origins of multicellularity by studying uniquely well preserved 2.11.6 billion year old microbial communities that include various forms of colonial organization and multicellularity. The majority of these appear to represent cyanobacteria, but there are also forms present that suggest other types of prokaryotes, as well as what may be some of the earliest eukaryotes known. In order to work out aspects such as cell diameter, length, and volume, as well as cell differentiation, cell junctions, and colony structure, we need complete three-dimensional information of the fossil microfabrics. Such information we are now obtaining through srXTM. The embryology of the earliest animals Fossilized embryos from the earliest period of animal diversification, a little more than half a billion years ago, were discovered in the late 1990s. With the aid of srXTM, we are now able to uncover the fossilization mechanisms that preserved the embryo fossils and to determine the developmental processes that were involved in shaping the major groups of animals. Subcellular structures are frequently preserved; these are often near the limit of resolution of currently available srXTM setups. The earliest presumed animal embryos are nearly 600 million years old, but our srXTM-generated data show that these particular forms have a mitosis pattern that is more similar to that of certain protists than of multicellular animals. Indubitable animal embryos occur some tens of millions of years later, and these give crucial information about the early evolution of various animal phyla, such as cnidarians. The origins and evolution of animal skeletons Biomineralized skeletons appear in diversity in the fossil record from about 550 million years ago. With the help of srXTM we obtain information about their often complex internal structure, which is used to reconstruct their mode of biomineralization and skeletal growth. As a further bonus, we can build up a virtual library of microfossil specimens that may serve as a web-based type collection for taxonomic use. This procedure circumvents the problem of loans and restudy of fragile and irreplaceable specimens. The early evolution of flowering plants The origin and rise to dominance of flowering plants (angiosperms) has been a topic of intensive debate for more than hundred years. Discoveries of well-preserved angiosperm flowers and other reproductive structures from 12065 million year old strata have yielded direct information about the first 50 million years of angiosperm evolution. The first substantial finding of Cretaceous flowers was from the Late Cretaceous of southern Sweden, but similar floras with charcoalified flowers have subsequently been discovered in other parts of the world. Recent application of synchrotron radiation X-ray microtomography has greatly improved the quality and quantity of information retrievable from the fossils. The scans reveal astonishingly fine details at the cellular level. For the tiny flowers, a submicrometer resolution is a prerequisite for a detailed systematic assessment. Many of the floral organs are typically in the size range of 100500 m, pollen grains are 630 m in diameter, and critical details of the pollen wall are at nanometer scale. The discovery of the fossil flowers and other mesofossils from the Cretaceous has greatly influenced current discussions on angiosperm origin and diversification. Divergence time of angiosperm lineages and molecular substitution in various lineages can be analyzed, with fossils used as calibration points and for mapping character evolution in extant lineages. Research constellation: Stefan Bengtson and Else Marie Friis, Swedish Museum of Natural History, Stockholm

Solidification of metals and alloys Solidification processing dictates the initial microstructure formation in metals and alloys and is most often decisive to the final product properties. Prevalent growth processes are complex realisations of non-linear transport dynamics (mass and heat diffusion, convection, capillarity and attachment) in systems far away from equilibrium, where the anisotropic solid-liquid interface constitutes a so called free-value boundary. Over the last couple of decades, fundamental understanding of solidification modelling has advanced rapidly due to computer modelling at time and length scales from the atomistic to the full scale of castings. At the most decisive time- and length scales (diffusion, convection and capillarity) in situ high resolution X-ray imaging techniques (2 and 3D) have evolved to become the most important tools for model validation and for securing proper assessment for processes characteristics. Research group: Ragnvald Mathiesen, Physics, NTNU, Lars Arnberg, Mat. Techn., NTNU, Arne Dahle, U Qeensland, Australia. Ragnvald Mathiesen and Lars Anrberg have been among the groups to pioneer the use of synchrotron radiation imagning in solidification science. At present the NTNU partners participate in two FP7 projects on solidification, plus a variety of other intl. (ESA), bilateral and national projects on solidification. The NTNU solidification group comprises 10 PhDs and 4 Post Docs. Application of hard X-ray imaging techniques to combustion systems and devices Very hard X-rays will be used to image inside complex multiphase and heterogeneous flow and reaction systems of interest for combustion. The studies include gas-phase, spray and biomass combustion. The techniques will be directed towards applications to real world combustion systems and devices. The experiments will give fundamentally new input for the developments of combined chemistry and flow dynamics models to make significant progress in combustion/energy conversion Science and Technology. These techniques will be very important for industrial partners. Research constellation: Frederik Ossler, Combustion Physics, Physics Department, Lund University. This constellation combines the groups and expertise of 25 researchers (50% senior scientists) with access to combustion labs and facilities, lasers and combustion devices. The constellation is also part of a EU funded network for combustion/Energy Research 3D microstructure analysis of semisolid multi component Food and Delivery matrices The aim of this project is to increase knowledge concerning 3D microstructure as a function of storage stability and influence of production of high quality confectionary products and pharmaceutical delivery matrices. The development of new ways to approach semisolid multi component solid dispersions is going along with instrumental development. The state of the art knowledge of the production thereof includes different tempering and processing steps such as prilling. Good processing prevents phase separation as well as surface segregation and crack formation needed for controlled delivery systems. Those phenomena can be monitored on a surface phenomenologically. However invasive measurements which involve physical contact have shown to influence the microstructure. A temperature controlled sample holder as well as non destructive microtomographic measurements have already been tested at synchrotron and lab bench installations where resolution of flux is missing. The resolution required for confectionary products is in the range of 10 microns. Additional analysis will be carried out on the surface using AFM, ESEM and profilometry techniques to complement the 3D microstructure from a surface point of view for increased resolution since delivery is based on both bulk and surface properties. Dr. Daniel Kalnin, Dr. Robert Corkery, YKI, The Institute for Surface Chemistry, Stockholm, Sweden ; Vincent Faivre, UMR 8612, University Paris Sud, Chtenay-Malabry, France. This combination of three senior researchers in the field of porous material for delivery, lipid and pharmaceutical delivery matrices combines two groups and expertise of three senior researchers. YKI is also part of a European project involved in improving the quality of semisolid food systems ProPraline.

3D microstructure analysis of thermal insulation material The aim of this project is to increase knowledge concerning 3D microstructure of thermal insulation materials as a function of storage stability and influence of production parameters and various binders and fillers. The development of new thermal insulation materials requires a knowledge of the thermal and mechanical properties in relationship to the product structure. Using 3D microtomographic data the microstructure and distribution of various chemically distinct components can be studied to see how production parameters effect the final structure of the material. This is important for optimizing the performance of the product as the function is dependent on the structure. The 3D data will then also be useful for testing in computer simulations and for comparing against experimental performance data, also for optimization of the thermal insulation properties. From YKIs perspective, we are interested in increasing performance through understanding the spatial distribution of important surfaces and interfaces throughout these composite materials. Dr. Robert Corkery, YKI, The Institute for Surface Chemistry, Stockholm, Sweden

Silicate inclusions in sediment-dispersed extraterrestrial spinel grains Recently we have discovered how to reconstruct the variations in the flux and types of meteorites reaching Earth throughout the last 3.5 billion years. It was generally assumed that meteorites which fell on the sea floor in a distant past have completely decomposed due to weathering. However, one spinel-group mineral, chromite, which represents 0.25% of the mass of the original meteorite, is extremely resistant to weathering, and also to different types of acid-treatment in the lab. By aciddissolving large samples of sediment of different ages it is possible to separate remains of the meteorites that fell on the ancient sea floors (Schmitz et al., 2003). The relict chromite grains also contain small inclusions of the original silicate matrix of the meteorites (Alwmark & Schmitz 2009). In this project meteoritic chromite grains (= 100-250 m) from sediments of different ages will be searched by 3-D microtomography for silicate inclusions (= 2-20 m). Inclusions only exist in some of the chromite grains, and compared to our present polishing approach microtomography will dramatically increase the efficiency with which inclusions can be found. The inclusions will be analyzed for chemical composition and cosmic ray tracks, revealing unique knowledge about the history of the solar system. The first knowledge about the three-dimensional distribution, shape and size of inclusions in spinels from meteorites of different groups and types will be produced. Research constellation: Birger Schmitz, Dept. of Earth and Ecosystem Sciences, Lund University Biological effects of Auger electrons in photo-activation therapy It is hypothesised that photo-activation therapy relies on the effect of the short-ranged Auger electrons following photo-reactions in high-Z contrast agents. Although promising results have been demonstrated with PAT using Iomerone (iodine) as contrast agent, even better results have been obtained by using cis-platinum as contrast agent. It was suggested that this large effect was due to DNA-damage from radiation-induced Auger electron emissions from internalized cis-platinum. Another agent with a well documented intracellular uptake is thallium. Radioactive thallium (201Tl) has earlier been used by our group for experimental treatment of rat glioma, whereas a high therapeutic effect was demonstrated. This was believed to be due to an intracellular uptake of thallium via the Na-K-ATPase pump activity, possibly even into the cell nucleus, leading to the emission of numerous low energy Auger electrons in the very close vicinity to the chromosomes and the DNA. Thus, intracellular drug uptake seems to be essential for the success of PAT. The purpose of this project is to further investigate the role of Auger electrons in photo-activation therapy. Research constellation: Sven-Erik Strand, Crister Ceberg, Bo-Anders Jnsson, Department of Medical Radiation Physics, Lund University; Bo-Baldetorp, Department of Oncology, Lund University; Leif Salford, Department of Neurosurgery, Lund University

The abscopal effect in microbeam and grid radiotherapy Conventional radiation therapy often fails because of the risk of damage to the surrounding normal tissue. Microbeam radiation therapy (MRT) may have the possibility to overcome this limitation. It has been shown that synchrotron MRT is tolerated much better by normal tissue as compared to conventional broad beams. Furthermore, it has been demonstrated in an intracranial rat tumor model, that MRT has the potential to eradicate the tumor at doses well tolerated by the normal brain. However, the mechanisms of MRT and grid radiotherapy are not yet fully understood. It has been suggested, that the radiation dose applied during the MRT therapy is high enough to initiate the production of cytokines involved in the bystander response, leading to a systemic release of tumoricidal factors such as cytokines, which may cause an abscopal tumor regression response with increased apoptosis. Our purpose is to further investigate the role of bystander and abscopal effects in MRT and grid radiotherapy. This may have important clinical implications, also in gamma knife therapy, intensity-modulated radiation therapy and stereotactic body radiation therapy. Research constellation: Crister Ceberg, Bertil Persson, Department of Medical Radiation Physics, Lund University; Leif Salford, Henrietta Nittby, Department of Neurosurgery, Lund University; Bengt Widegren, Department of Cell and Organism Biology, Lund University

Monitoring and quantification of tumour-cell biological events using intra-vital microscopy The biological effects of radiation have been extensively studied in cellular cultures as well as in animal models. The end points in animal experiments are often tumor growth or survival time, or factors that can be measured in samples excised from the sacrificed animal. In cell cultures, biological effects can be quantified in more detail, for instance by measuring oxidative stress or by studying cellto-cell signaling pathways. However, cell cultures lack many of the important characteristics of the milieu in the tissue of a living animal, such as for instance the vascular and immunological systems. Since both the vasculature and various immunological factors have been shown to be of great importance for radiation effects, there are important advantages to study radiobiological events in vivo using intra-vital microscopy. By using a synchrotron based intra-vital microscope one would be able to extend these possibilities to also study morphological changes following radiation. More important, by using the synchrotron also to irradiate the subject, it would give a unique and outstanding possibility to monitor tumor-cell biological effects on a microscopic scale in living animals. Research constellation: Elisabeth Kjelln, Dept. of Oncology, Ume University; Partners: Dept.of Medical Radiation Physics, Lund University; Dept. of Oncology Lund University The Auger effect in molecular targeting therapy Auger electron emitters have the potential to improve tumor therapy. Characteristic for the biological Auger effect is that the cell killing ability is much higher than expected from the delivered radiation dose. However, very little is known about the critical DNA lesions which are induced by the Auger electron cascade. In the proposed project we aim to study a number of issues that are relevant for targeting therapy using photoactivation of Auger electrons. Since the release of the Auger cascade by the synchrotron radiation can be controlled in time and space, we will be able to study basic radiation action mechanisms which may be critical for the survival of an irradiated cell. In the proposed project we will expose mammalian cells (rodent wt cells and/or human tumor cells) to DNA- or cell-targeting agents with incorporated stable nuclides (e.g. In, I, Pt) before activation by synchrotron radiation. The project includes studies on: 1) Radiation chemistry, direct vs. indirect action, 2) DNA damage clustering, 3) DNA damage and chromatin structure, 4) DNA repair. Research constellation: Bo Stenerlw, Unit of Biomedical Radiation Sciences, Rudbeck Laboratory, Uppsala University. The group has 20 years experience of cellular and molecular radiation biology, especially on effects of ions beams and radionuclides. Partners: Medical Radiation Physics, Lund University

Investigations on EPR dosimetry using intense, soft X-ray synchrotron radiation Sensitive EPR dosimeters based on lithium formate are suitable for dose determinations at low energy photon irradiations. The dosimeters are however slightly LET, Linear Energy Transfer, dependent shown in experiments with irradiations from conventional X-ray tubes with well known spectra and with conversion factors from air kerma to absorbed dose in water deduced from Monte Carlo calculations. We suggest that more accurate determinations of the LET dependence should be possible with an intense, monochromatic synchrotron beam. This knowledge is necessary for accurate dose determinations for cell irradiations or brachytherapy dose plan verifications with photons in the energy range 20-120 keV. Furthermore, EPR imaging is a new emerging tool for imaging of dose distributions. We propose that important information about fundamental radiation damage processes such as radical distributions and LET dependence of radical formation could be gained using high resolution EPR imaging of small phantoms irradiated with intense pencil beams from the synchrotron. EPR imaging using potassium dithionate as phantom material provides high spatial resolution in dose mapping and may also be used to give information about local LET. Research constellation: Eva Lund, Dept. of Radiation Physics, Linkping University Enhancing the effect of radiotherapy by using a dose enhancing or synergistic agent This is a project with the aim of determining the possibility of certain drugs to penetrate the cancer cells and to attach to DNA and thereby destroying the parenchymal cells reproductive integrity. Various techniques should be used for this work, such as fluorescence-based computed microtomography and X-ray or neutron diffraction. We hope to be able to perform these experiments in parallel both at MAX IV and at ESS. Research constellation: Albert Siegbahn, Dept. of Medical Physics, Karolinska University Hospital; Dept. of Oncology-Pathology, Karolinska Institute Radiation biology non-target and dose-rate effects in microbeams Radiotherapy (RT) remains one of the main curative and palliative methods for treating cancer. Despite fast progress in such new techniques as intensity modulated radiotherapy, proton and heavy ion therapy, and the gamma knife, the curative results need to be improved. This is especially true in the field of paediatric therapy, where the patient has a long life expectancy and where it is particularly important to avoid side effects to healthy tissue. In this respect a promising new RT method appears to be the microbeam radiation therapy (MRT). MRT uses highly collimated, quasi-parallel arrays of microplanar X-ray beams produced by synchrotron sources. The main features of MRT are an extremely high dose rate and very small beam divergence. Thus, very high doses can be delivered to sharply defined targets, while the surrounding, healthy tissue is spared. The existing data suggest that MRT therapy is indeed very well tolerated by the healthy tissue. The high precision of dose delivery in MRT also makes it possible to use it for photon activation therapy (PAT) which is based on irradiating a tumour loaded with a chemotherapeutic drug that is activated by radiation. Before MRT can be applied in the clinic, it has to be studied in greater detail. Research is needed both in fields of dosimetry and biology. Given the lack of single dose point, what dosimetric model should be applied? Do irradiated cells exert a bystander effect on the surrounding, non-hit cells? How do different tissues react to high dose-rate microbeam radiation? These important questions can only be answered in synchrotron facilities equipped with a beam-line dedicated for biomedical research. In view of the above, I was very happy to learn of the plans to construct such a beamline in the future MAX IV facility in Lund. I would like to express my deepest support for this enterprise and the interest to participate in biomedical research that this beamline will enable. Research constellation: Andrzej Wojcik, Centre for Radiation Protection Research, Dept. of Genetics, Microbiology and Toxicology, Stockholm University.

Micro-localisation of tumor targeting molecules The aim of this project is to develop clinically feasible tumour targeted therapies by the use of shortrange high-efficiency radionuclides. One example is the alpha-emission from 211At, conjugated to tumour-binding ligands for application in disseminated sub-clinical residual cancers. Before clinical applications of any new radiation therapy modality, however, careful dosimetric investigations need to be carried out. In radionuclide therapy, this requires detailed knowledge of the distribution of the radiopharmaca in question. In the case of short-ranged radionuclides, such as 211At, however, noninvasive measurements of the 3D-distribution in cells and tissue are not trivial. This could be achieved by using micro-computed tomography with synchrotron-generated high-energy x-rays. With this technique, it could even be possible to perform 3D localisation of the relevant nuclides in living animals. This would become an excellent tool in the development of new tumour-targeting radionuclide conjugates, and it would also make an extremely important contribution to the interpretation and understanding of the results from pre-clinical trials with radionuclides. Research constellation: Jan Tennvall, Dept. of Oncology, Lund University; Sven-Erik Strand, Dept. of Medical Radiation Physics, Lund University; Ragnar Hultborn, Section for Oncology, Radiation Physics, Radiology and Urology, The Sahlgrenska Academy, University of Gothenburg

Three-dimensional morphological characterization of tissue: Beyond histology In the human brain, the neuropathology group in Lund takes particular interest in the subtle and not sharply delineated alterations in subcortical structures, i.e. the myelin and the white matter. Changes in this compartment are often caused by ischemia and hypoxia - and clearcut strokes are only a minor part of a huge spectrum of pathologies which may undermine the neurons in the cortex. This area, with hypoxic-ischemic damage, plus acute, not yet delineated strokes, may be a good target for therapeutic intervention - if pathology is identified at an early, amenable stage. Such identification provides a possible therapeutic window, but requires a close correlative work of multimodal tissue analysis, in which detailed histopathological workup represents one part. It has been demonstrated that synchrotron-based microtomography can give much superior results (as compared to conventional histology) considering the possibility to quantitatively analyse the structure of the tissue without destroying the specimen. This is relevant for questions with respect to pathological processes, and offers a very promising tool for the non-destructive three-dimensional structural analyses under physiological and pathophysiological conditions. Research constellation: Elisabet Englund, Dept. of Pathology, Lund University

Syncrotron radiation based X-ray fluorescence analysis Research groups at Lund University (Medical Radiation Physics, Malm and Environmental and Occupational Medicine, Lund) have pioneered the development and application of methods for in vivo analysis of heavy metals in the human body. Methods for analysis of lead in the human skeleton (fingerbone), cadmium in kidneys and liver and mercury in kidneys have been developed and have been frequently used for analysis of contamination in various groups of occupationally exposed persons and of members of the public. In relation to such studies there is a large interest to get information about the microscopic distribution of the elements in various organs and tissues (kidneys, liver, skeleton). For the direct detection of biologically relevant metals in single cells and of their speciation, XRF offers a number of advantages compared to other microprobe techniques. It combines high spatial resolution and high sensitivity. The aim of the project is to develop methods for cellular chemical element imaging, and direct speciation analysis, using synchrotron radiation X-ray micro- and nanoanalysis. The recent improvements in focusing optics for keV X-rays allow application to chemical element analyzis in subcellular compartments. Synchrotron radiation X-ray fluorescence provides chemical element imaging with less than 100 nm spatial resolution. Moreover, synchrotron radiation offers the unique capability of spatially resolved chemical speciation using micro X-ray absorption spectroscopy. The potential of these methods in biomedical investigations will be investigated within the fields of cellular toxicology, and pharmacology, bio-metals and metal-based nanoparticles. For lead, dental enamel has been considered an ideal material for reconstruction of the exposure histories, because heavy metals incorporated into the enamel are encapsulated as they are chronologically absorbed during the subjects growth. Therefore, this ability of the enamel will be utilized by in situ analysis of the enamel lead content with SRXRF. The microscopic distributions of Cd and Hg in human and rat kidneys will also be studied. The methods will increase the abilities to reconstruct human environmental exposures to heavy metals and link the exposures to various toxic effects. Research constellation: Sren Mattsson, Dept. of Radiation Physics Malm, Lund University, Jimmy Brjesson, Dept. of Diagnostic Radiology, Halmstad Hospital 3D mammography with synchrotron radiation Phase-contrast with synchrotron radiation has a potential to improve sensitivity and specificity in breast cancer detection and classification. The added information that can be gained from the phasecontrast images can help the breast radiologists in their task beyond what can be done purely based on the normal attenuation images. The technique can also be used for three dimensional imaging. These characteristics make synchrotron radiation an interesting field for breast imaging research. Research constellation: Anders Tingberg, Dept. of Radiation Physics Malm, Lund University

Micro-tomographic imaging in historical osteology Synchrotron radiation techniques advances archaeology and its sub-disciplines in several ways. Detailed knowledge regarding the material and chemical properties of artefacts, ecofacts, and works of art, provides information crucial to the conservation of the cultural heritage. Furthermore, the in depth knowledge of the material provides possibilities to research the provenance of the raw materials, manufacturing procedures, pigments used, etc. Our project focus on biological tissues from archaeological contexts, particularly bone. Several questions are addressed. Paleopathology is a discipline that studies diseases in past populations, specifically diseases that leaves osseous traces. The application of 2D and 3D microtomography to pathological specimens with known diagnosis would enhance our ability to diagnose accurately with respect to archaeological specimens. We are also interested in describing the life-history of humans and animals based on incrementally growing tissues, such as secondary dentine of the teeth. We want to use microtomography to describe the growth of these tissues, and, combined with stable isotopes, map the history of an individuals life. Lastly, we focus on the natural degradation of bone. A database with bone specimens from different geological contexts and ages are subjected to microtomography and will elucidate the nature of bone diagenesis and ultimately, the breakdown and disintegration of bone. Research constellation: Torbjrn Ahlstrm, Mats Roslund, Dept. of Historical Osteology University Lund

Optimisation of radiation therapy by enhanced dosimetric models and basal radiobiological knowledge The long-term aim of this project is to optimise radiation and radionuclide therapy of cancer, using better knowledge of radiation dosimetry and biological effects of radiation. Toxicity in normal tissues is the limiting factor for radiation and radionuclide therapy of tumours. In many applications, bone marrow is the critical organ, but for recently introduced radiopharmaceuticals the kidneys, thyroid, liver, intestines, and the lungs might be important. There is a clear need to determine the effects of radiation on normal tissues and also the tolerance doses. Synchrotron micro-computed tomography for biological tissue characterization could be essential both for development of morphological models of these normal tissues together with the tumour, to be included in dosimetric models, and for evaluation of morphological effects of irradiation. Furthermore, studies of the cellular and molecular effects on both tumour and normal tissues after precision irradiation using a synchrotron microbeam would further facilitate optimization of radiation therapy. Research constellation: E. Forssell-Aronsson, H Ahlman, O Nilsson, Radiation Physics, Surgery, and Pathology, University of Gothenburg. The unit consists of approximately 10 senior staff members and 10 junior staff members. This constellation combines the groups and expertise of three senior researchers. The main areas of activity are related to radiation therapy, dosimetry, radiation biology, tumour biology, tumour pathology and surgery. The competence in the group contains theoretical considerations, experimental studies and clinical applications.

Phase-contrast stereoscopic X-ray imaging (PSXI) The project is aimed at determine the feasibility of a phase-contrast stereoscopic X-ray imaging (PSXI) method for medical purposes. We intend to use the well-known propagation-based (in-line), phase-contrast imaging technique during our imaging experiments. We will compare with images obtained with conventional attenuation-based stereoscopic imaging methods as well as with some single-projection, phase-contrast X-ray images. System parameters of interest in clinical applications such as dose-level and appropriate X-ray photon energies to achieve optimized stereoscopic images will be explored experimentally. Research constellation: Albert Siegbahn, Dept. of Medical Physics, Karolinska University Hospital; Dept. of Oncology-Pathology, Karolinska Institute

Main constellations involved in the project Department of Medical Radiation, Lund University Contact persons: Crister Ceberg & Bo-Anders Jnsson Primary interest: Usage of synchrotron radiation in medical imaging and therapy Department of Information Technology and Media, Mid Sweden University Contact person: Christer Frjdh Primary interest: Detector development Department of Earth and Ecosystem Sciences, Lund University Contact person: Birger Schmitz Primary interest: Microtomography Institute for Surface Chemistry Contact person: Roger Corkery Primary interest: Usage of imaging and tomography methods in materials science Advisory group Marco Stampanoni, Beamline Scientist, TOMCAT Beamline, Swiss Light Source, Paul Sherrer Institut, Switzerland Astrid Haibel, Beamline Scientist, Micro- and nano-tomography beamline, GKSS Outstation at DESY Hamburg, Germany Alberto Bravin, Beamline Scientist, Medical Imaging Beamline, ESRF, France Avraham Dilmanian, NSLS, Brookhaven Medical Department, US Ragnvald Mathisen, Dept. of Physics, Norwegian University of Science and Technology, Trondheim, Norway

Budget, Staffing and Time Plan Budget

Table 2 : Budget Description Superconducting Wiggler Frontend Optical & Experimental Hutches incl. Personal Safety System Optics Monochromator Focusing Optics (several sets of refractive lenses, Be, C, Si & Ni)) Beam Diagnostics incl. Slits Endstation Detectors (incl CCD (Frelon type), Energy discriminating area detector and ultrafast CMOS) A six axes high precision stage Sample Environment Optical table and detector translator Infrastructure Electronics, controls & computing Vacuum Misc. incl. AC, fluids & liq. Nitrogen Others Control room + sample prep lab. Total Amount (MSEK) 10 5 10 6 5 4 12 4 1 1 6 2 5 2 73

Time Plan
2011 Table 3: Time plan 2012 2013 2014 2015 Beamline design Purchase Procedure FE & wiggler design Installation of hutches and infrastructure Production of bl components Installation of beamline components Installation front end & wiggler Commissioning front end & wiggler Commissioning beamline Commissioning data collection & analysis Operation

Paperwork

Beamline

External work

End stations

Note that it could be decided that the wiggler also could be designed and developed at MAX-lab. Staffing Based on Table 3 we estimate the following personnel requirements during construction and commissioning. Out of these the committed user constellations will contribute with in total two manyear over the total construction period.
2011 1 Table 4: Man-years during construction 2012 2013 1 3 2014 4 2015 4

Man-years

In operation, this beamline will require three beamline scientists, one of which being primarily focused on the medical user community. The extensive amounts of collected data and its treatment will require one beamline computer engineer. In addition a technician that could be shared with another beamline would be needed. In total: 4.5 persons.

A short-pulse facility for time-resolved X-ray science at MAX IV Spokesperson: Jrgen Larsson, Physics Department, Lund University In the scientific evaluation of MAX IV by the Swedish Research Council (VR 20:2006) the ultrafast capabilities made possible from the LINAC design was identified as one of the two important unique features of the MAX IV project together with the high brilliance of the storage ring. The ultrafast beamline has been considered as the first beamline at MAX IV to become operational. This is because it utilizes the MAX IV Linear Accelerator (LINAC) as an electron source. The storage rings will be completed more than one year after the LINAC. The urgency for a funding decision is high since the time plan assumes a positive financing decision before the fall 2010. The time plan also relies on the start of the building of the LINAC tunnel around the same time. The ultrafast beamline will facilitate studies of the structure and dynamics of materials. Such studies are of fundamental importance for key scientific problems directly related to programming materials using light, enabling new storage media and new manufacturing techniques; for obtaining sustainable energy by mimicking photo-synthesis; and for gleaning insight into chemical and biological functional dynamics. Due to the emergence of X-ray sources with high peak brilliance, the field of picosecond Xray diffraction has developed rapidly over the last few years. The key technology behind future breakthroughs in this area is the generation and detection of very short and very intense X-ray pulses with femtosecond duration. The femtosecond X-ray beamline at the MAX IV short-pulse facility (SPF) will have pulse lengths on the time scale of atomic vibrations (100 fs) at wavelengths matching interatomic distances (). Swedish scientists have a prominent international profile in developing and utilizing ultrafast X-ray techniques. With strong national activities it is anticipated that we will maintain this position. The facility will be of great interest not only for the Scandinavian research community. It will be an internationally leading facility for X-ray pump-probe experiments. We aim to create a unique experimental infrastructure: The Ultrafast hard X-ray beamline at the short-pulse facility at MAX IV Synergies Coordinating Scandinavian research in ultrafast X-ray science. A strong national base infrastructure will allow for sufficient Scandinavian access to short-pulse Xray sources.

Possible scientific breakthroughs Understanding of light driven charge-transfer in artificial photosynthesis for the photocatalytic production of fuel. New characterization of transport properties in nanostructures. New tools for materials synthesis - Transforming materials with light. Direct observation and exploitation of coherent reaction dynamics in solution and within proteins.

Budget 75,000 kSEK

1. Scientific Motivation 1.1 Vision There is something in common between charge-transfer reactions in artificial photosynthesis, structural changes in ferroelectric memories and organic electronics, magnetic moment reversal, photo-induced chemical reactions, transport of energy in nanostructures and the initial steps governing the function of proteins. The common feature is that the processes occur in less than one picosecond. There is a scientific need to understand these processes on a fundamental level. So far the main tool for the study of ultrafast dynamics has been femtosecond spectroscopy. The importance of the field and time-domain was recognized when Ahmed Zewail was awarded the Nobel prize in chemistry 1999. For molecules consisting of few atoms, the structural dynamics can be deduced from the timeresolved spectra. For more complicated molecular systems, for nanostructures and solids X-ray methods can reveal the structural dynamics. It has been recognized since the discovery of X-rays that they are a superior tool for structural determinations. Within the last few years, novel X-ray techniques have been developed allowing direct probes of small atomic motions on ultrafast timescales, using direct ultrafast structural methods. Studies of structural dynamics has so far been hampered by a lack of sufficiently bright sources. We aim to exploit the MAX IV LINAC to develop an infrastructure for ultrafast pulsed X-ray science. This will enable us to study for the first time fundamental processes in photo-chemistry, photo-physics, material science, chemistry and biology. The core members consisting of Swedish groups and international groups who contribute resources to the project will use this infrastructure to study key scientific problems including: Photocatalysis and charge transfer process in artificial photosynthesis for light driven production of fuel (Villy Sundstrm, Lund) Functions of metal ions in natural pigments (Villy Sundstrm, Lund) Studying phonon propagation in nanostructures (Jrgen Larsson, Lund) Ultrafast investigations of ferroelectric materials (Jrgen Larsson, Lund) Visualizing chemical reaction dynamics (Jan Davidsson. Uppsala) Ferromagnetic and multiferroic materials (Olof Karis, Uppsala) Laser melting of ice (Carl Caleman, Uppsala) Deterministic protein motion (Richard Neutze, Gteborg) Diffractive optics for short-pulse X-rays (Ulrich Vogt, KTH, Stockholm) Modelling of ultrafast X-ray science (Hans berg, Theoretical Chemistry, KTH, Stockholm) Dynamic Structures in Organic Semiconductors (Martin Meedom Nielsen, Copenhagen) Investigation of transient liquids by diffuse scattering (Klaus Sokolowski-Tinten, Duisburg) Collective effects in photo-induced phase transitions (Eric Collet, Rennes)

1.2. Overview of Scientific Field Through developments in laser technology over the last decades, studies of dynamic phenomena on a femtosecond time scale have been made possible. In chemistry and biology, fundamental processes such as bond breaking, bond isomerization, and charge separation have been extensively investigated using ultrafast laser spectroscopy. It is, however, not possible to obtain structural information from these measurements without a complete knowledge of the potential energy surfaces involved, and this limitation rapidly becomes insurmountable as the complexity of the system of study increases. The study of phase transitions in solids through laser optical spectroscopy is even more indirect since it is the electronic properties of the material, rather than the positions of its atoms within its lattice, which is probed. A prominent example is efficient ruthenium based substances which are black. This mean that they absorb efficiently, but unfortunately also that information is not available from spectroscopy with visible light. When X-rays are used as a probe, information about the molecular structure can be deduced directly from X-ray diffraction. This is the way static structure determination of crystalline materials as well as large molecules has been performed since the discovery of X-ray radiation. However, the field of time-resolved X-ray diffraction has been source driven, when nearly all groundbreaking studies have been preceded by improvements of sources, ultrafast detectors and X-ray optics. Over the last years optical pump/X-ray probe experiments were mainly applied in order to study structural reorganization, phonon physics and dissociation processes in both the liquid and the solid

phase [1-19]. A number of groundbreaking papers have been published. Since the discovery of X-rays, the average brilliance of X-ray sources has been increasing by more than 3 orders of magnitude every 10 years. Each new generation of machines has brought up new applications without making established methods less valuable. Time-resolved X-ray studies require instruments with intense and very short X-ray pulses. A quantum leap was taken when the SASE-FEL (Self-Amplified Spontaneous Emission Free Electron Laser) at SLAC, achieved lasing in April 2009. In the fall 2010, the first hard-ray pump-probe experiments will be carried out. The proposed infrastructure complements the LCLS. The ability to create a wide spectrum from a wiggler is unique to the MAX IV SPF and facilitates time-resolved EXAFS. Also for time-resolved scattering experiments MAX IV will be world leading. Pump-probe experiments on solids and many nano-structured materials can be done at the 4-5 orders of magnitude lower flux at the MAX IV SPF compared to LCLS. The LCLS is over-subscribed by a factor of 10 and the MAX IV SPF is 4 orders of magnitude more powerful than the best ultrafast X-ray source in operation today. A precursor to LCLS was the Short-Pulse Photon Source (SPPS). The SPPS project had a large Swedish participation. It demonstrated that a source producing 2 orders of magnitudes lower flux than the MAX IV SPF could revolutionize ultrafast structural dynamics. Among the scientific highlights was the development of the electro-optic sampling technique for bunch characterization [1], groundbreaking studies on non-thermal melting [6, 7, 10], lattice dynamics in Bi [3], scattering from liquids [12]. Since LCLS occupies the same physical space, SPPS was closed in 2006. 1.3 The impact of the MAX IV SPF The LINAC based X-ray Short-Pulse Facility (SPF) at MAX IV proposed here, will be a unique international facility. Time-resolved X-ray science is a field which currently is limited by X-ray flux. So far two types of X-ray sources have been dominating. On one hand laboratory laser-produced plasma X-ray sources have a short pulse duration, strongly fluctuating intensity, low flux and are radiating in 2 steradian solid angle. Beamlines at electron storage rings (such as D611 at MAX II) using a femtosecond laser synchronized to the storage ring with ultra-fast streak cameras can yield sub-ps time resolution, but the X-ray flux per unit time is limited. The LCLS will become operational in 2009, but the amount of beamtime for pump-probe experiments can be expected to be around 500 hours per year starting late 2010. This means that 10 teams can have 2 days of beamtime each over a year. Clearly this is insufficient and the MAX IV LINAC which will be operational in 2013 will be in high demand. The flux from the MAX IV SPF is lower than at an X-ray free electron laser, but sufficient for a range of experiments spanning over several disciplines. Condensed Matter Physics Upon femtosecond laser excitation, strong changes of the effective potential energy surfaces, which determine the equilibrium structure of a solid, can be induced. This may lead to atomic rearrangement even on a sub-picosecond time-scale. A very exciting example is the sub-picosecond solid-liquid phase transition induced by femtosecond laser irradiation in covalently bonded semiconductors. This process is often called non-thermal melting since the transition takes place on a time scale much shorter than the time required for transfer of energy from the excited electrons to the thermal motion of the lattice. The high flux at the MAX IV SPF will allow for studies of photo-induced phase transitions in solid matter by diffuse scattering. The ultra-fast macroscopic switching of materials in solid state opens new avenues for the manipulation of matter with light and it will present a high potential for new keys in industrial innovation. Indeed, information storage in materials is based up to now on switching kinetics governed by slow thermal activated nucleation-growth processes above the nanosecond time scale. Switching in a macroscopic or nanostructured material triggered by coherent molecular and domain wall motions would signify a technological breakthrough. Especially, in relation with the investigated molecular materials, there is a large demand in optical information processing (ultra-fast writing and/or erasing) and optical devices for telecommunication applications (large spectral photo-induced changes). In addition, the (dis)appearance of magnetic species controlled by light (as in spin transition systems) supplies a new channel for information storage. This is coming up in molecular materials by virtue of photo-induced co-operative and coherent change in molecular identity, such as its charge state and/or spin state. In addition light pulse driven coherent reversal of domain orientations (ferroelectric or other ones) appears possible with the control of the interplay between the number of excited molecules and the amplitude of the related soft mode.

X-ray Optics and Damage Although the number of photons emitted by the SPF will be several orders of magnitude below XFEL radiation, in a focused SPF beam equal intensities can be reached. Therefore the SPF will be a unique tool for investigations on diffractive optics since the focused beam is still much larger than the structures in the zone plate optics. Photo-Biology The key reaction steps in many proteins and other biological systems are simple chemical reactions like bond dissociation reactions, bond isomerization events, and electron transfer reactions, all of which induce conformational changes in the surrounding protein. In solution these reactions and the coupled solvent response frequently occur on the sub-picosecond to picosecond timescale. In a protein environment, for which billions of years of evolution has optimized the structure for maximum reaction efficiency, the primary photo-chemical events and the ensuing initial response of the protein can be even faster. Photosynthetic reaction centers, the work-horse of biophysics, and rhodopsins, which harvest the energy and information content of light, provide exciting examples of such optimized reactions. Today, various forms of indirect ultrafast optical spectroscopy are the only means to study most elementary steps of biomolecular function. The MAX IV SPF and time resolved diffraction experiments will allow revolutionary new experiments and unique structural insights into the function of enzymes and photoreceptors on a time scale where their remarkable selectivity and efficiency is achieved. Chemistry It is a long nourished dream among chemists to get both structure and dynamics from the same experiment, i.e. to directly obtain time resolved structures showing the three dimensional evolution of a molecular system in the course of a chemical reaction. There are in principle two routes available to achieve this, time resolved X-ray or electron diffraction and time resolved X-ray spectroscopy. The true molecular timescale, where chemical bonds are broken and formed, charge is transferred between molecules and atoms or ligands are exchanged in the course of a complex reaction, is that of picoseconds and femtoseconds. In order to monitor and follow in real time how such reactions occur we consequently need ultrashort femtosecond X-ray pulses. Ultrashort (~100 fs) X-ray pulse free electron lasers are becoming available at a few large scale facilities worldwide, but the monochromatic X-ray radiation makes them less useful for time resolved X-ray spectroscopy. White light ultrafast Xray sources as proposed for the MAX IV SPF on the other hand can provide the ultimate source for time-resolved X-ray absorption spectroscopy. The intense radiation from the undulator enables even more direct structural investigations of smaller molecules with Wide-angle X-ray scattering. Modelling of Ultrafast X-ray Science High X-ray field pulses offer unique opportunities to study the dynamics of complex transient phenomena in materials. Ultrashort X-ray pulses constitute the fastest probes available for tracing transitions between different quantum states with atomic spatial resolution. They allow measuring time intervals on a femtosecond time scale and provide access to background physical, chemical, and biological processes on a microscopic temporal and spatial scale. As experimental opportunities goes into new realms, it is of the highest importance to involve leading groups in modeling on an early stage so that the methodology for ab initio calculations and simulations match the new capabilities. In the reference list we find 19 groundbreaking, recent publications in Science, Nature and Physical Review Letters involving scientists in the core team. (italic - Swedish teams) 1. 2. 3. 4. 5. 6. 7. 8. 9. Cavalieri, AL, et al. (Including J. Larsson and K. Sokolowski-Tinten)(2005), PRL 94, 114801 K. Sokolowski-Tinten et al., (2003), Nature 422, 287 D.M. Fritz et al (Including: K. Sokolowski-Tinten). (2007), Science 315, 633 K. Sokolowski-Tinten, et al. (2001) PRL 87, 225701 E. Collet et al. (2003) Science 300, 612 AM Lindenberg, J. Larsson, K. Sokolowski-Tinten, K. Gaffney et al. (2005) Science 308, 392 K.J. Gaffney, A.M. Lindenberg, J. Larsson, K. Sokolowski-Tinten et al. (2005) PRL 95, 125701 MBL Cointe, MH Lemee-Cailleau, H Cailleau, E Elkaim, E. Collet (2006) PRL 96, 205503 H. Enquist, H. Navirian, TN. Hansen, AM. Lindenberg, P. Sondhauss, JS. Wark, J. Larsson (2007) PRL 98 225502

10.P. Hillyard et al. (including J. Larsson, K. Sokolowski-Tinten) (2007) PRL 98, 125501 11.S.P. Hau-Riege et al. (including K. Sokolowski-Tinten) (2007) PRL 98, 145502 12.A.M. Lindenberg et al. (including J. Larsson, K. Sokolowski-Tinten) (2008) PRL 100, 135502 13. R. Neutze, R.Wouts, S.Techert, J.Davidsson et al. (2001), PRL 87, 195508 14. J. Davidsson et al., (2005), PRL 94, 245503 15.P. Sondhauss, J. Larsson, M. Harbst, G.A. Naylor et al. (2005), PRL 94, 125509 16.R. Neutze, R. Wouts, D. van der Spoel, E. Weckert, J. Hajdu, (2000), Nature 406, 752 17.L. Gmez-Consarnau, .... R. Neutze, C. Pedrs-Ali, J. Pinhassi (2007) Nature 445, 210. 18.A. Royant, K. Edman, T. Ursby, E. Pebay-Peyroula, E. M. Landau & R. Neutze (2000) Nature 406, 645. 19.K. Edman, P. Nollert, A. Royant,.... J.Hajdu, R. Neutze & E.M. Landau (1999) Nature 401, 822

2. Short description of the MAX IV Short Pulse Facility The beamline at the MAX IV SPF (Short-Pulse Facility) is designed to provide 100 fs bursts of X-rays enabling the real-time study of atomic motion. The X-ray source is coupled to a synchronized femtosecond laser. This enables the study of photo-induced process in samples ranging from single crystals to small molecules in a solvent. The SPF takes advantage of the injector which can support short electron pulses.

Fig. 1. Overview of the SPF hall and the hard X-ray beamline

Energy (wavelength) range 1.8 -20 keV (0.6 6.5 ) Photon source In-vacuum undulator Double crystal monochromator with Si(111) InSb(111) crystals. Monochromator Multi-layer mirrors Photons per pulse 1% BW >1107 below 12 keV Repetition rate 100 Hz Harmonic content <10-3 Si E/E210-4 (2.5-20 keV) Bandwidth InSb E/E410-4 (1.8-20 keV) ML E/E=0.01 (1.8-20 keV) Monochomator throughput >70% crystal >50% ML @ 5 keV Optics Unfocused/ micro focus Polarization Linear Pulse duration <100 fs Synchronization <1 ps 0.2 x 0.22mm2 unfocused Spot size on sample 2 x 2 m microfocus Ultrafast laser (3 mJ) 4-circle goniometer Equipment CCD detector Pilatus detector

1.8 -30 keV (0.4 6.5 ) Wiggler Same as undulator mono White-light option >1106 below 20 keV 100 Hz <10-3 Si E/E210-4 (2.5-30eV) InSb E/E410-4(1.8-30 keV) ML E/E=0.01 (1.8-30eV) >70% crystal >50% ML Gold coated Si mirror Linear <100 fs <1 ps 0.05 x 0.5 mm2 Ultrafast laser (3 mJ) Bolometric detector Dispersive EXAFS

Table 1. Key parameters for the hard X-ray beamline at the MAX IV SPF

Timing and synchronisation By adding a second electron gun, the injector for the MAX IV ring will be modified in order to provide short electron pulses during the periods in between top-up pulses for the electron storage rings. It will be equipped with a laser-driven high brightness electron gun. The gun design from FERMI, Frascati, Rome, will be used in a collaborative effort with the Frascati team. Bunch compression will be done in two double achromats with positive R56. Sextupoles will be used together with the achromats to linearize the second order effects from both acceleration and the compression itself. This will produce clean pulses with a time duration of less than 100 fs FWHM. To monitor the laser synchronization to the X-rays, Electro-Optical Sampling (EOS) will be implemented in order to time-stamp each shot (postsynchronization) User controlled synchronization in the hutch is also needed. This includes diagnostic with different degrees of complexity and temporal resolution. User requested key numbers for the time-structure are: Time duration: 100 fs Jitter: <1 ps (the final aim is 30 fs) (Post-) synchronisation: 30 fs Contrast: 99% of pulse energy in 1 ps

It is consistent with the machine parameters provided that the bunch charge is kept below 0.1 nC. Higher bunch charges can be obtained at the cost of contrast and pulse duration. Feasibility and risk: Laser-synchronization < 1 ps is commercially available. EOS requires local R&D but has been used at the MAX-lab FEL test facility. The FERMI gun has been tested at the FEL test facility at MAX-lab. The user demands for a coherent emitter are quite relaxed. The emittance requirement is many orders of magnitude lower than for a free electron laser, whereas beam divergence and source size are secondary for the MAX IV SPF. At LCLS <5 fs pulses have been obtained by reducing the bunch current. Pump lasers The pump lasers are commercially available. The main laser for the photocathode as well as for the user area are cryo-cooled KHz Ti:Sap amplifiers (1kHz, 10 mJ@800 nm). The appeal of this solution is amplitude stability due to the fact that CW pump lasers for amplifiers can be used. This is important for non-linear conversion schemes. OPAs + mixing with 0.2-10 m wavelength range together with THz generation will cover the needs of the physics and chemistry community. The LINAC can operate at 1 kHz at lower energies. The facility should also make provisions to include a 100 Hz 100 mJ/pulse amplifier. Feasibility and risk: None - lasers are commercially available from several companies. Insertion devices The needs of the ultrafast X-ray community requires two insertion devices which fit in the 20 m long straight section in the SPF beamline. An undulator providing the highest number of photons per pulse should be used for diffraction experiments. Superconducting undulators has not reached the degree of maturity needed in order to incorporate such a device in the first stage. The flux gain from a cryogenically cooled undulator is not sufficiently large to warrant the extra cost. We will install an invacuum undulator. The experience from ESRF is that 15 keV is an ideal photon energy for liquid scattering, 2-5 keV is a useful range for surface materials science. The undulator period will be 20 mm and a length of 10 m is a good trade-off between cost and performance. The requirements for the wiggler are relatively low. A 2-3 m standard wiggler with 60 mm period and K-value=9 can be used in order to give a white spectrum for dispersive EXAFS. Feasibility and risk: None - insertion devices are commercially available from several companies. Optics The undulator radiation has a divergence of less than 20 rad. The beam will still be less than 0.5 mm at the user end station. Offset mirrors for harmonic suppression will be needed, in addition we will use Be lenses and zone-plates for micro- and nano-focusing of the undulator radiation. For the wiggler radiation, a mirror is needed. Gold-coated Si with an incidence angle of 0.25 degrees will fulfill specifications.

For monochromatization, several options are needed. A set of three on the fly inter changeable monochromators will be installed (Si 111), (InSb 111) and (Multilayer optics). An in-house built monochromator based on the design from beamline D611, MAX II, is proposed, but we will also investigate commercial alternatives. User needs determine the monochromator flexibility: Multi-layer mirrors are required to obtain maximum flux for WAXS experiments such as those proposed by Neutze and Davidsson. InSb crystals allow for tuning down to 1.8 keV enabling studies if nanowires, whereas Si crystals are the standard in crystallography due to high quality and narrow bandwidth. Feasibility and risk: The focusing optics for the wiggler beamline is commercially available as is monochromator optics and refractive lenses. Microfocussing with zone-plates is an R&D project together with the Royal Institute of Technology, KTH (Uli Vogt). Wavelength range The beamlines will be separated from the accelerator vacuum by a beryllium window. The useful wavelength range will be 1.8-20 keV for the undulator and 1.8-30 keV for the wiggler. Sample environment The user needs are diverse and a single sample environment is insufficient to cover a broad user base. A set-up which could handle vacuum, liquids, atomic and molecular physics, liquid-helium temperatures etc would be extremely complex and not user friendly. The way to address this will be coupled to the management of the project. We will provide a beamline with a 4-C diffractometer for experiments in air allowing for sample cooling with a cryo-stream. The laboratory thus supplies the basic sample environment above and that the users are given the possibility to build their own set-ups which are interchangable. A dispersive EXAFS set-up will be developed. The facility will need to supply four types of detectors. 1. Diodes 2. CCD-based detectors for high-flux experiments on crystalline materials 3. Pilatus (or similar) detector which is a photon counting detector which removes thermal noise and can analyze photon energies thereby reducing the effect of Compton scattering in diffuse scattering experiments. 4. A very recent development is a bolometric detector which can be used to measure the energy of X-ray photons with a few eV resolution. This enables EXAFS measurement without gratings or monochromators. Feasibility and risk: The bolometric detector is only available from one company. Villy Sundstrms group is currently verifying performance of the first system delivered for X-ray spectroscopy. Other detectors are available from more than one vendor. Background to the specifications given above The user needs and thereby the specification has been determined at a workshop, in connection with the MAX-lab users meeting in November 2007 and in subsequent iterations of the specifications. The world leading international experts were chairing the sessions regarding each part of the instrumentation and accelerator parameters. The session include: Timing, Insertion devices, Optics, Lasers and User end stations. 87 participants were present and additional input has come from scientists who have requested to be on the mailing list. The notes and conclusions from the meeting have been sent out to all participants and other scientists requesting information. The final document detailing with the specification was written in 2008. Similar international infrastructures No incoherent hard X-ray emitters are currently in operation. Very hard X-ray spontaneous emitters are considered for the X-FEL project at DESY 2015-16. LCLS will launch the first hard X-ray freeelectron laser beamline for pump-probe experiments in late 2010. The beamtime will be approximately 500 hours per year for pump-probe measurements, which will enable 5 groups 4 days of beamtime for pump probe experiments. Swedish scientists can apply for this beamtime in international competition. X-FEL will be operational in 2015. Competition will be equally hard. The Japanese hard X-ray FEL project is also ongoing, but it is unclear what the external user policy will be. The MAX IV SPF is the best ultrafast EXAFS source compared to all operational and planned sources world-wide. It is also

the brightest European source for time-resolved X-ray diffraction until the European X-FEL becomes operational in 2015. The short message is that the international research community is starving for an infrastructure such as the MAX IV SPF. Possible future upgrades to keep the facility competitive Provisions for future upgrades are already made in the original design. Such upgrades include: 1. 2. 3. 4. 5. 6. 7. Circular polarization with second undulator Emittance slicing for few fs pulses Ability to extract THz radiation for direct excitation of phonons Ability to extract visible radiation for perfectly synchronized optical pumping Flexible user interface allowing for continuous upgrades of user stations Modular building design allows for many separate beamlines to be built Free electron laser in stage 2 of MAX IV

Free-electron laser in stage 2 of MAX IV New initiatives for medium size FELs are taken by, among others, Paul Scherrer Institut (Villigen, Switzerland) and at the Italian institutes ELETTRA and Frascati. A scheme which is explored is seeding where the amplification process is defined by an initial well defined light beam and harmonic generation (the seed laser wavelength is multiplied). Recently the concept of seeding was demonstrated at 53 nm at MAX-lab (S. Werin). The MAX IV LINAC will enable building a free electron laser as the MAX IV project evolves into a mature phase.

Ultrafast Structural dynamics with time resolved X-ray spectroscopy It is a long nourished dream among chemists to get both structure and dynamics from the same experiment, i.e. to directly obtain time resolved structures showing the three-dimensional evolution of a molecular system in the course of a chemical or biological reaction. The true molecular timescale, where chemical bonds are broken and formed, charge is transferred between molecules and atoms or ligands are exchanged in the course of a complex reaction, is that of picoseconds and femtoseconds. In order to monitor and follow in real time how such reactions occur we consequently need ultrashort X-ray pulses in the femtosecond and picoseconds time domain. Molecular function often emanate from a local structural change, making time resolved X-ray spectroscopy an ideal tool for studies of molecular function. The most elementary molecular dynamics occurs on the femtosecond time scale, making this the ultimate for understanding molecular change and function. As an example, we have successfully studied several metal-organic complexes of great interest for photocatalysis, artificial photosynthesis and dye sensitized solar cells, using ~100 ps X-ray pulses. From these studies it is clear that there are e.g. functional electron transfers, spin cross-over reactions and associated structural changes happening on the sub-ps to few ps time scale. A SPF delivering ~100 fs tunable hard X-ray pulses would be invaluable for studies of such elementary reactions. Research constellation: V. Sundstrm, S. Canton, J. Uhlig, G. Smolentsev, N. Gador, P. Chabera, Chemical Physics, Lund University. Ultrafast THz spectroscopy in material and biological sciences Energetic electrons are the workhorses of many processes in nature as well as materials with widely different functions. Just a few examples are: photosynthesis, solar cells, catalytic processes, enzymes, cell respiration, a multitude of chemical redox processes. Transport of charges and charge mobility is a very important process for the function of these materials and phenomena. Charge transport can traditionally be studied by electrical methods, but they have at least two severe limitations the need of contacts that can severely influence the measurement, and the low time resolution that precludes molecular time scale studies. Ultrafast far infrared (THz) spectroscopy offers a powerful tool for contact free molecular timescale (sub-ps) electrical measurements. The THz frequency range of the electromagnetic spectrum in addition corresponds to that of very low frequency vibrations of for instance biomolecules and may be related to their biological functions. We are presently using laser generated sub-ps THz pulses to probe ultrafast charge carrier dynamics in organic and inorganic semiconductors for novel solar cells. Ultrashort THz pulses from the SPF of MAX IV would offer a much wider spectrum and higher intensity, implying that spectral properties, and thus characteristics, of studied phenomena can be much better understood, the THz pulses can be used for excitation of e.g. vibrational motion in biomolecules and strongly absorbing samples can be studied. The present project aims at studying charge carrier mobility in nanostructured organic, inorganic and hybrid organic/inorganic materials for solar cells and lighting applications. Research constellation: V. Sundstrm, A. Yartsev, S. Canton, C. Ponseca, D. Vitanage. Chemical Physics, Lund University. H. Nemec, P. Kuzel, Czech Acad. Sci., Prague. Time-resolved X-ray diffraction studies of nano-systems Nano-wires have been proposed as electrical interconnects in different nano-scale devices. In many cases electrical conductivity is desirable whereas thermal conductivity is not. Time-resolved X-ray diffraction We have pioneered dynamic measurements of phonon propagation. This class of experiments will enable investigations of propagation of phonons thorough an ensemble of nanowires. This will be done by exciting the nanowires on the substrate side and subsequently probe them on the vacuum side. Propagation cut-offs can be measured as function of the shape and diameter of the nanowires. The ultrafast beamline at MAX IV allows for probing of single nano-wires. Through collaboration with the Nanometer Structure Consortium in Lund, we have access to nanowires of IIIV materials such as InAs and InSb. Research constellation: J. Larsson, Maher Harb, Clemens von Korff-Schmising, Andrius Jurgilaitis, Ralf Nuske, Department of Physics Lund University, Klaus Sokolowski-Tinten Universitt DuisburgEssen, Germany.

Ultrafast investigations of ferroelectrics Ferroelectrics are materials that exhibit a reverse in intrinsic polarization under the influence of an applied electric field. Furthermore, above some critical temperature ferroelectrics undergo a ferroelectric-to-paraelectric phase transition, in which they completely lose their intrinsic polarization. These unique properties along with recent advances in the fabrication of ferroelectric nanostructures have led to an increased interest in the technological applications of ferroelectricity. For example, some of the many existing applications that exploit ferroelectricity include ultrafast switching, dynamic random access memory (DRAM), and high power microwave devices We have recently shown that it is possible to switch the polarisation in KDP (from one ferroelectric structure to the other) via strain pulses which are generated via the piezo-electric effect.. We have also in collaboration with A. Lindenberg at Stanford University worked with switching of domain structures in perovskites using optical and THz (sub-mm wave) radiation. Potentially groundbreaking studies will be used by using THz excitation of the ferroelectric. THz radiation can be made resonant with the soft optical phonon mode and the field strength can be sufficiently strong to exceed the coercive field in the device that are simultaneously resonant with the soft optical phonon model. Research constellation: J. Larsson, Maher Harb, Clemens von Korff-Schmising, Andrius Jurgilaitis, Ralf Nuske, Department of Physics Lund University, Eric Collet (Professor), Maciej Lorenc (researcher), Herve Cailleau (Professor), Marylise Buron (Professor), Marina Servol (Assistant Professor). Universit Rennes 1, France Transient structure of laser-generated disordered states investigated by ultrafast diffuse X-ray scattering We propose to apply time-resolved diffuse X-ray scattering using laser-pump - X-ray probe techniques to investigate the structure and dynamics of liquid-like states of materials after short-pulse laserinduced disordering. In particular, we would like to answer the question how the structure of the disordered state depends on the excitation strength, the disordering pathway and the type of material, and how the structure evolves over time. Thin foils of solid materials will be irradiated by femtosecond optical laser pulses. Subsequent to the laser-induced disordering the scattering of a time-delayed hard X-ray pulse will be observed in normal-incidence transmission geometry. Measurements of the diffuse scattering pattern as a function of the pump-probe time delay yield the transient changes of the structure factor from which the pair-correlation function will be derived. The proposed experiments are taking advantage of the inertial confinement of the excited samples during the first few picoseconds and will provide information on the structural properties of disordered states of materials under extreme conditions of electronic excitation, temperature and pressure. They can only be performed using multi-keV X-ray pulses with sufficient intensity and the required ultrashort pulse duration. Research constellation: Klaus Sokolowski-Tinten, U. Shymanovich, Universitt Duisburg-Essen, Germany, J. Larsson, M. Harb, C. von Korff-Schmising, A. Jurgilaitis, R- Nuske, Lund University Visualizing photo-chemical dynamics in solution through ultrafast X-ray scattering Real time observations of the rearrangement of atoms and molecules in elementary chemical processes represent a challenge in modern science. The possibility of fully understanding the function of an important system and ultimately be able to control it, motivates detailed studies of fundamental chemical dynamics. Time-resolved wide-angle X-ray scattering (WAXS) offers a method of directly probing structural dynamics in a disorder phase. Our first proof-of-principle pico-second experiment could be reported for iodine in solution 2001 and some years later we demonstrated the capability of the method by determining the structure of a transient isomer in a more complex photochemical reaction in the liquid phase. More recently, we demonstrated that time-resolved WAXS has sufficient sensitivity to also enable solvent dependent structural perturbations of transient chemical species to be accurately resolved, i.e. even modest structural rearrangements become discernable using timeresolved WAXS. Numerous fundamental dynamical processes in chemistry occur on time scales significantly faster than the 100 ps X-ray snapshots available at synchrotron sources. While considerable shorter X-ray pulses are now available from laser plasma sources, these sources produce a divergent X-ray beam and do not have sufficient brilliance for WAXS experiments. Free electron lasers (FEL), or subpicosecond photon synchrotron sources, on the other hand, are very suitable. With sub-fs X-ray pulses time-resolved diffraction should be able to accurately quantify branching ratios and visualize

transient structural changes as well as cage dynamics in solution in real time. The scientific gain from such studies will be significant and of very high fundamental importance. Research constellation: J. Davidsson, M. Marcellini, A. Nasedkin, B. Zeitz, Uppsala University Dynamic Structures in Organic Semiconductors: Charge generation Organic electronics provides a link between electronic function, as we know it from computers or silicon based solar cells, and molecular or polymeric materials as they are ultimately found in biology. At the same time, the fundamental understanding of the interplay between molecular organization in the materials and the mobility of charge carriers is still very incomplete, and this is generally viewed as the bottleneck for widening the field of applications of organic electronics. Key challenges in this problem can directly be addressed via time resolved X-ray scattering. One key challenge is charge generation. Electronic excitations within a molecular crystal lattice - the exciton - are either ultimately emitted or trapped by impurities like lattice defects or chemical reactions within the crystal. The capture by an association between an excited monomer and a ground state monomer leads to formation of an excimer (excited dimer). Ultrafast time resolved structural studies is the only way to elucidate the detailed interplay between molecular structure and the ability of organic materials to generate mobile charges and excitons, and thus provide the guideline for a rational design of the next generation organic semiconductors of fundamental importance and high scientific impact to the photochemistry community. Research constellation: Martin Meedom Nielsen, Kristoffer Haldrup, Henrik Lemke, Kasper Skov Kjr, Jakob Petersen, Niels Bohr Inst, University of Copenhagen, Klaus Bechgaard, Deptartment of Chemistry, University of Copenhagen, Klaus B. Mller, Niels Engholm Henriksen, Department of Chemistry, Danish Technical University Organic Semiconductors: Charge and exciton transport It is a major challenge to understand charge and exciton transport in organic semiconductors: Transport is influenced by the strong electron-phonon couplings in molecular materials. The energy released by the relaxations described in 1) is released into phonons and intra molecular vibrations. In e.g. liquid crystalline materials, excitation may also lead to structural phase transitions. Hence, the structure in which the charges move depend upon changes in the geometry of the molecules themselves combined with changes in the crystal lattice due phase transitions, phonons or thermal relaxations, which in turn influence the ability of the molecular arrangement to transport charge. By directly mapping the phonon response of materials to excitation, time resolved structural studies will provide key insights into the functioning of electro-optic active organic materials Research constellation: M.M. Nielsen, K. Haldrup, H. Lemke, K. Skov Kjr, J. Petersen, K. Bechgaard, Univ. of Copenhagen, K. B. Mller, Ni. E. Henriksen, Danish Technical University Nano-focusing of ultrafast X-ray sources Free electron lasers (FELs) emitting in the hard x-ray regime around 0.1 nm wavelength are upcoming ultrafast and ultrahigh brilliance sources at few places worldwide. One of the major challenges is how to focus the hard X-ray laser beam with a typical diameter in the mm range down to spot sizes in the range of 100 nm or less as required by many application experiments. One possibility is the use of diffractive zone plate optics, i.e., circular gratings with decreasing grating constant, which is the topic of a research and development project between the Biomedical and X-ray Physics group, KTH Stockholm, and the European XFEL in Hamburg. The work is recognized as an in-kind contribution to the construction of the European XFEL and funded by the Swedish Research Council. Despite the obvious benefits of zone plate optics the major question presently unknown is for how long a zone plate can withstand the high-intensity FEL beam. This question has been under discussion for some time now and experimental experience is limited to zone plates placed in a direct, unfocused extremeultraviolet FEL beam. For this type of experiments the MAX IV facility can play a very important role since beamtime at XFEL sources is extremely limited. Although the number of photons emitted by the SPF will be several orders of magnitude below XFEL radiation, in a focused SPF beam equal intensities can be reached. Therefore the SPF will be a unique tool for investigations on diffractive optics since the focused beam is still much larger than the structures in the zone plate optics Research constellation Ulrich Vogt, Anders Holmberg, Hans Hertz, Biomedical and X-Ray Physics, Department of Applied Physics, KTH, Stockholm

Deterministic Protein Motions: Time-resolved wide angle X-ray scattering studies of retinal proteins Retinal proteins such as bacteriorhodopsin, sensory rhodopsin and visual rhodopsin are integral membrane proteins that harvest both the energy and information content of light to create chemical energy essential for the cell, and to provide information on the environment through photo-taxis and vision. We have recently developed a radical new approach to study the timeresolved structural biology of membrane proteins using time-resolved wide angle X-ray scattering. This work was performed at the dedicated time-resolved station of the European Synchrotron Radiation Facility and enabled us to visualize the entire history of protein conformational changes in light-driven retinal proteins from a time-scale of nanoseconds to milliseconds. Our vision is to exploit the unique properties of the proposed short-pulse facility of MAX IV to push this method into the femtosecond domain, where the fundamental light-driven reactions occur. All of these membrane proteins contain a buried retinal molecules which photo-isomerizes on a time-scale of a hundred femtoseconds, and this initiates a structural cascade that propagates through structural changes into energy-transduction processes or a light-sensitive signal. It is a fascinating and fundamental question in biology how these membrane proteins achieve their remarkable photon efficiency (the great majority of retinal isomerization events are productive) and selectivity (the retinal isomerization occurs only around one specific bond). These remarkable chemical properties are achieved by careful guidance of the reaction pathway by the protein during the first picoseconds of the reaction. Thus the initial response of these integral membrane proteins to the earthquake of a buried retinal isomerization event is fundamental to photo-biology, and the short-pulse facility provides a unique opportunity to follow these events with time. This work also links to our development of the method of time-resolved wide angle X-ray scattering applied to small photo-chemicals in solution, in collaboration with Jan Davidsson. Research constellation: Richard Neutze, Gergeley Katona, Sebastian Westenhoff, Department of Chemistry, Biochemistry & Biophysics, University of Gothenburg. Deterministic Protein Motions: Time-resolved Laue-diffraction studies of Photo-synthetic reaction centers A problem of central importance to biology is energy harvesting and charge separation reactions in photosynthetic reaction centers. These integral membrane protein complexes harvest photons so as to transport electrons across an energy transducing biological membrane, lightdriven reactions that are responsible for 90 % of the primary energy input into the earths biosphere. Ultrafast spectroscopy studies have suggested that protein conformational changes play an important role in the initial charge separation process, which occurs on a time-scale of femtoseconds to picoseconds. It is crucial to determine the nature of the interchromophore and surrounding protein displacements that are coupled to the initial reaction pathway and dynamically stabilizes the charge separation reaction. We have recently succeeded with time-resolved Lauediffraction studies of a photosynthetic reaction center at the dedicated time resolved beamline of the European Synchrotron Radiation Facility. This work is the first example where time-resolved Laue diffraction has successfully visualized structural changes in an integral membrane protein complex. Our structural results have enabled a lightinduced movement of a single tyrosine residue (TyrL162) towards the photoactivated special pair of chlorophylls (the primary electron donor) to be captured. These findings shed new light on the role of this key conserved residue in stabilizing the charge separation reactions. These recent successes using timeresolved Lauediffraction lay the basis for our planned experiments on photosynthetic reaction centers with fs temporal resolution at the proposed short-pulse facility at MAX IV. Direct visualization of ultrafast rearrangements that occur on the subpicosecond timescale will provide fundamental new insight into the mechanism of energy input into the biosphere, and may have implications regarding the design of artificial photosynthesis for future energy production needs. Similar ultra-fast time-resolved Laue diffraction studies are foreseen to be performed at the short pulse facility of MAX IV on myoglobin: carbon monoxide complexes in collaboration with Ilme Schlichting and Dwayne Miller, both of whom are based in Germany. Research constellation: Richard Neutze, Gergeley Katona, Sebastian Westenhoff, Department of Chemistry, Biochemistry & Biophysics, University of Gothenburg.

Photoinduced phase transitions and Molecular dynamics Precursor phenomena Ultra-fast crystallography goal is to solve structures obtained after femtosecond photo-switching of materials. The first purpose is not only to know the unit cell transformations but also the atomic rearrangements occurring after the phase transformation. Study of forbidden reflections behavior or time-dependent Bragg intensity due to coherent phonons is part of the method which could lead to the knowledge of the photo-switching process and to obtain precise intensity measurements in order to obtain the electron density in the excited state, to study the line shape of the induced Bragg reflections and the diffuse scattering associated to the transformation The investigation of the photoinduced transition has demonstrated cooperative interactions between molecules strong enough to drive a selforganized structural relaxation in the photo-induced state. But it immediately raised a question about the mechanism at the origin of cooperative effects observed in quasi one-dimensional system. This opens a new way for observing the precursor phenomena of the macroscopic switching and the project at MAX IV opens new possibilities Research constellation: Eric Collet, Maciej Lorenc, Herve Cailleau, Marylise Buron, Marina Servol, Universit Rennes 1, France Coherent molecular response The physics of low-dimensional molecular solids investigated at thermal equilibrium opens very interesting possibilities. Indeed, such materials are interesting candidates for light driven ordering, melting or insulating to metal transition. In these systems, a femtosecond laser pulse induces a metallic state from the insulating phase through an ultrafast process, the duration of which was around 1 ps. The magnitude of the cooperative effects is also noteworthy, as one photon can transform up to 1000 molecules. Yet, only X-ray diffraction experiments can reveal structural reorganization, which points again to the great challenge of today: To follow in real time, and on the atomic scale, elementary transformations of matter Research constellation: Eric Collet, Maciej Lorenc, Herve Cailleau, Marylise Buron, Marina Servol, Universit Rennes 1, France Ultrafast structural studies of phase transitions in water Recent spectroscopy experiments as well as computer simulations have described the thermal melting of ice induced by an infrared laser pulse. Here it was shown that melting can happen within a few picoseconds. Since the water density is higher than ice, a void will be formed within the ice-latticebordering melting-nucleation sites. In the mentioned computer simulations melting of ice are shown to be accompanied by a tendency to contract. This means that the attractive forces are stronger than the kinetic pressure. In summary, the melting of ice is very different from melting of other solids, and this has prompted us to propose experiments aimed at direct structural investigations of the process. In contrast to spectroscopy experiments, diffraction experiments are intended to give direct structural evidence of ice-melting. From the scattering images a detailed picture of the melting process can be recovered, which opens up a wide range of possibilities to study the transition between crystalline and liquid water. Being one of the key elements in life as we know it, the physics of water is naturally of large interest. The exact process of the melting of ice is not known, and there is much to learn from performing the right type of experiments, and combine them with theoretical models. It should be noted that in the case of ice melting by infrared pulses the absorption depth is comparable to the wavelength of the radiation (about 3000 nm). Hence, either surface melting can be studied or, when a special very thin container is used, bulk melting is accessible. The proposed ultrafast hard X-ray beamline at the short-pulse facility at MAX IV will be an excellent facility to perform time resolved pump-probe experiments to reveal the physics of phase transitions in water, It will provide X-ray pulses shorter than 100 fs, pump laser in the right wave length regime both for inducing non thermal and thermal melting as well as means for synchronizing the two sources down to a necessary time resolution. Research constellation: C. Caleman, CFEL, DESY, Germany, D. van der Spoel, N. Timneanu, J. Andreasson, Dept. of Cell and Molecular Biology, Uppsala University

Complete structural determination through extended edge fine structure measurements (Theory development) With the modern synchrotron light sources the prospects for ``Anisotropic EXAFS measured in the Raman mode''will be fulfilled. This means that polarization-dependent extended X-ray absorption fine structure will show angular information on randomly oriented molecules and amorphous systems. The physical background of such a possibility is based on a polarization-frequency selection of a partially oriented subensemble from the chaotically oriented molecules and on backscattering of the photoelectrons on the surrounding atoms. This method was suggested in our publication. Some preliminary studies of EXAFS measured in the Raman mode have also been carried out. The experimental condition for this novel technique was suggested in our group, and it holds the promise for complete structural determination and an opportunity to define local geometric conformation with wide ramifications in chemistry and biology, for instance, structural determination of organometallic centers in enzymes. Our plan is here to carry out simulations of the process to predict or aid the data analysis of such experiments, first on some prototype systems, and then on "real" structures; the manganese complex in the Photosynthesis II system serves as one example. Research constellation: Faris Gelmukhanov, Zilvinas Rinkeviciu, Viktor Kimberg, Sergey Gavriluk, Yuping Sun, Jicai Liu, Theoretical Chemistry, KTH, Stockholm Pump-probes with synchrotron sources and optical lasers (mainly theory development) High X-ray field pulses offer unique opportunities to study the dynamics of complex transient phenomena in materials. Ultrashort X-ray pulses constitute the fastest probes available for tracing transitions between different quantum states with atomic spatial resolution. They allow measuring time intervals on a femtosecond time scale and provide access to background physical, chemical, and biological processes on a microscopic temporal and spatial scale. High X-ray field pulses can be used in combination with pump by lasers where delayed probe pulses permit taking snapshots of molecular or condensed-matter dynamics after excitation by a pump pulse. The precise synchronization of the strong optical and X-ray pulses allows for producing an exact timing signal between the X-ray and the optical laser. X-ray pump probe spectroscopy can be divided in two qualitatively different schemes. In the first, the pump low frequency field is applied between the ground and low energy excited states (vibrational or electronic excitation), while the driving field is applied between core excited state in the second scheme. The timing between driving and probe pulses allows to obtain superhigh spectral resolution using the revival phenomenon, and the X-ray pulse allows to study the nuclear dynamics induced by the IR driving pulse. We intend to study, theoretically and experimentally, chemical and biophysical problems with disordered samples using laser assisted X-ray scattering. The idea here is that the polarized laser radiation easily can create oriented molecules with valence shell vacancies (Fig.6, I). This opens up the i:th level for resonant X-ray absorption, and for orientational selection of the optically excited molecules. This scheme has the further advantage that the 1s-i transition is well separated from the main body of X-ray photoabsorption resonances. Research constellation: Faris Gelmukhanov, Zilvinas Rinkeviciu Viktor Kimberg, Sergey Gavriluk, Yuping Sun, Jicai Liu , Theoretical Chemistry, KTH, Stockholm Time-resolved X-ray spectroscopy of nano-particles and clusters Clusters and nano-particles form a very interesting state of matter in between individual atoms and molecules on the one hand and condensed matter (crystals, liquids, glasses) on the other. Their properties often vary greatly and (often) unexpectedly with the addition or subtraction of just a single atom or molecule. Furthermore, they play an important role in catalysis and in many industrial, technological and biological processes such as combustion, semiconductor manufacturing and photosynthesis. They also offer great promise when it comes to molecular engineering in which new materials are created that are specifically adapted to a certain task. We propose to use the Short Pulse Facility (SPF) to study the structure and the dynamics of clusters and nano-particles. The experimental determination of the structure of a particular cluster is a nontrivial task. Theoretical calculations indicate that often several energetically close-lying isomers are possible. Optical, UV/VIS spectroscopy is rarely helpful to discriminate between them, either because the cluster in question simply does not absorb in the UV/VIS region of the electromagnetic spectrum (in particular for small clusters of light elements), or because the absorption/emission spectrum does not vary much between the different isomers.

Research constellation: Peter van der Meulen, Peter Saln, Stockholm University Common development of tools for diagnostics and experimental stations Your proposed project is in line with our plan to build a free electron X-ray laser "SwissFEL" at Paul Scherrer Institute. For these projects we would very much support an exchange of staff and the common development of tools for the diagnostics and the experimental stations. Our strength in the field of ultrafast X-ray physics stems in part from the current activities in femtosecond slicing at the Swiss Light Source (FEMTO), the experience with X-ray detectors (single photon counting and integrating) and the use of pulsed X-rays for resonant diffraction and imaging. The scope and schedule of your project is particularly appealing to us, since SwissFEL will initially concentrate on hard X-rays (> 3 keV) and provide soft X-rays only in a second stage (> 2016). Thus we have a interest in collaborating with you on the use of soft X-rays and contributing to the commissioning of the necessary facilities. Research Constellation: Friso van der Veen, Christoph Quitmann, Rafael Abela, Paul-Scherrer Institute, Switzerland, Jrgen Larsson, Lund University Multiferroic materials Multiferroic and magnetoelectric materials in particular, i.e. compounds where magnetism and ferroelectricity coexist and are coupled, represent one of the frontier research topics in condensed matter physics today. This fact is emphasized by the large volume of publications (more than 100 annually since 2005) with a number of high profile publications in Science and Nature. Due to the possible coupling of two highly relevant functionalities (magnetism and ferroelectricity), these materials have the potential to revolutionize future digital storage and sensor technologies. Hence, the goal of this sub-project is the development of an understanding the relevant properties of these complex materials, both in bulk, in thin films and in nanostructures. Major attention will be devoted to the interplay between ferroelectricity and electronic degrees of freedom in magnets, i.e. on those cases, where spin-, orbital-, or charge-ordering can be the driving force for a spontaneous ferroelectric polarization to develop. A very important and fundamental question in multiferroics is how the timescales for the ferroic properties are connected. Though absolutely key to the usefulness of multiferroics the linking between e.g. ferroelectric and ferromagnetic switching on short timescales are unexplored to date. At first it might seem plausible that the magneto-electric coupling would imply that electric and magnetic switching would occur on the same timescales. On the other hand electric polarization involves displacement of nuclei and thus involves timescales relevant for phonon excitations in the solid while magnetic switching can in principle occur on timescales as short as few picoseconds, thus suggesting that the relevant timescales could differ by orders of magnitude. To unravel this relationship is thus of fundamental importance for the understanding of magneto-electric coupling and multiferroicity in general. In the first stages of experiments the SPF at the MAX IV linac we envision to correlate dynamic structural data obtained using time-resolved X-ray diffraction with magnetic data obtained using time resolved optical techniques such as time resolved magneto-optical Kerr effect. Research constellation: Olof Karis, Uppsala University, Clemens von Korff-Schmising, Lund University

Description of the main constellation(s) involved in the beamline project Lund Laser Center Prof. Jrgen Larsson has been a co-team leader for the LCLS and has been involved in all aspects of instrument design including technical design, building design and budget. He has been involved in all aspects of building up the SPPS beamline at Stanford and D611 at MAX-lab ranging from planning to assembly. He runs a university group and with currently 6 members who will participate in the design, building and commissioning of the beamline. He has together with the accelerator physics group at MAX-lab made the conceptual design of the MAX IV SPF beamline with input from other user groups. He will manage the beamline project at a level of at least 30% time. Henrik Enquist is a former PhD student of Jrgen Larsson now employed full time at MAX-lab to work on the design of the beamline. Prof. Villy Sundstrm has a European Research Council Advanced Investigator grant aimed at structural dynamics of photo-activated chemical reactions. He group in total consists of 30 researchers and 5 people are directly working with X-ray techniques. He will contribute people over the grant period towards achieving time-resolved X-ray spectroscopy at the beamline. Uppsala University Prof. Jan Davidsson is an expert in time-resolved wide-angle X-ray scattering. Davidsson's group will contribute to building and commissioning such a set-up. Gteborg University Prof. Richard Neutze is an expert in time-resolved photo-biology. His group will help in commissioning of the beamline. Royal Institute of Technology, Stockholm Docent Uli Vogt is an expert in refractive and zone plate optics for X-rays. He will work with microfocussing in order to test short-pulse X-ray damage to diffractive optics. Prof. Hans gren has a large activity in X-ray spectroscopy and science. We see a great advantage in involving this group which is well known for finding novel approaches in order to model frontiers of experimental X-ray science. MAX-lab The accelerator physics group is headed by Prof. Mikael Eriksson. Doc. Sverker Werin, Dr Sara Thorin and Dr. Filip Lindau will be important to integrate the accelerator and the beamline. International members of core team Paul-Scherrer Institute, Swiss Light Source (Switzerland), Friso van der Veen (Div. Head Synchrotron Radiation & Nanotechnology Christoph Quitman (Lab head Synchrotron Radiation-Condensed Matter), Director , Rafael Abela, SwissFEL project leaderPhotonics) Center for Molecular Movies (Copenhagen, Denmark), Martin Meedom Nielsen Universitt Duisburg-Essen (Duisburg, Germany), Klaus Sokolowski-Tinten Universit Rennes 1 (Rennes, France), Eric Collet. Cooperation with other infrastructures The MAX IV SPF will be a part of the MAX IV project and will operate within this framework. In addition it will be a facility within the European free-electron laser network EUROFEL. This will involve joint RTD, policy making, exchange of personnel. Currently the European EUROFEL consortium is in a planning stage in the European funded project IRUVX-PP. The member teams of the consortium are from DESY (Germany), BESSY (Germany) Elettra (Italy), SPARX (Italy) MAX-lab (Sweden), NLS (UK) and PSI-XFEL (Switzerland). Currently two other teams are prospective members; Arc-en-ciel (France), and POL-FEL (Poland) Independent of this, PSI management and researchers are supporting the MAX IV SPF and are enthusiastic about staff exchange and joint R&D on user end stations.

Budget, staffing and time plan Time plan The time-plan assumes building start and financing decision summer 2010. Delays of either will delay the project start. Delays in the MAX IV Linac project will influence the beamline project MAX IV project, Beamline project (major components) Building start Q3 2010 Linac installation Q1 2012 SPF hall finished Q2 2012 X-ray optics delivery Q4 2012 Electron beam to SPF Q4 2012 Beamline alignement Q1 2013 Beamline characterization Q2 2013 Commissioning experiments Q3 2013 Key issue: Insertion device delivery time 15-18 months, Procurement 6 months. Demand specification 2-3 months. Lead time from funding decision to order 23-27 months. Funding decision needed Sept 2010 to hold time plan. The insertion devices are needed first and they have the longest lead time. Staffing for expertise, build-up and commissioning: Current Staffing: Henrik Enquist employed as the first beamline scientist. Jrgen Larsson will work 30% for MAX-lab on the project. Contributions from Core teams: EXAFS set-up: Chemical Physics, Lund University, contribute 2 people Single crystal X-ray diffraction set-up: MAX-lab 1 person, Uni-Duisburg 1 person, Rennes 2 persons, Atomic Physics, Lund, 1 person, Copenhagen 1 person total 6 people. WAXS set-up: Uppsala University, Gteborg University and Atomic Physics, Lund University 3 people jointly. Additional staffing requested: We are requesting support for one coordinator each for the WAXS, ESAFS and Diffraction user station. They have responsibilities for detailed technical specifications, procurement and for coordinating the efforts of the contributed staff from the core teams. The support for one manager per set-up over 5 years 2011-2015 gives a total of 15 person-years. Capital equipment Important infra-structures for the accelerator will be developed for the MAX IV injector, but additional components are needed to create a short electron bunch, which is not a requirement for injecting the MAX IV ring, but crucial for the short-pulse facility. Such components are for example a laser driven electron gun (including a dedicated laser) and bunch compression elements, emittance slicing, and diagnostics. We now intend to develop a full-fledged beamline, including all instrumentation, for the MAX IV. The instrumentation needed includes: Laser gun including laser In-vacuum undulator, 7-8 m Bunch compressing magnetic chicane Wiggler Radiation shielding and vacuum components Monochromator and sample chamber High-power laser Wavelength conversion of laser via optical parametric generation Laser beam transport and laser safety, including pulse shaping 7 MSEK 20 MSEK 4 MSEK 2 MSEK 3 MSEK 5 MSEK 4 MSEK 2 MSEK 2 MSEK Milestone First X-ray light Q4 2012 Milestone Milestone Insertion device installation Q3 2012 Laser installation-Q4.-2012

Motion control and optical tables Pilatus detector Other detectors and beam diagnostics Bolometric detector for EXAFS Dispersive EXAFS set-up Total infrastructure cost Staff Total User operation

2 MSEK 5 MSEK 5 MSEK 3 MSEK 1 MSEK 65 MSEK 10,000 kSEK 15 person-years 75,000 kSEK

The purpose of the facility is to make it available to the general scientific community. Beamtime at the infrastructure will be allocated in accordance with the principles at MAX-lab. A Program Review Committee will evaluate applications and beamtime will be allocated according to the rating. At the current time we will use the same reviewers which are evaluating the other proposals for MAX-lab, but it may be necessary to strengthen the expertise in time-resolved structural measurements with one or two new members. 25% of the time needs to be allocated for maintenance and local R&D in order to attract the best possible beamline scientists and engineers. It should be considered if in an initial phase (-2015), the teams building up the different instruments needs to be guaranteed time up to 25%. A peer review system for this allocation should also be implemented User support in the operational phase In order to have adequate user support MAX IV will hire (1) A part time (30%) beamline scientist with overall coordination of activities at the beamline (2) A full time X-ray beamline manager (3) A full-time laser manager.

Appendix- Members of core scientific team Febr. 23, 2010 Chemical Physics, Lund University & Lund Laser Center Research constellation: V. Sundstrm, S. Canton, J. Uhlig, G. Smolentsev, N. Gador, P. Chabera, Approx 30 scientists working on molecular dynamics in chemistry, biology and material science, using ultrafast spectroscopy techniques probing the electromagnetic spectrum from the far infrared (THz) to the X-rays. Atomic Physics Division, Lund University & Lund Laser Center Jrgen Larsson, Ralf Nuske, Andrius Jurgilaitis, Clemens von Korff-Schmising, Maher Harb MAX-lab & Lund Laser Center Sverker Werin, Sara Thorin, Henrik Enquist Dept. of Photochemistry and Molecular Science, Uppsala University J. Davidsson, M. Marcellini, A. Nasedkin, B. Zeitz Dept. of Cell and Molecular biology, Uppsala University C. Caleman (CFEL, DESY, Germany), D. van der Spoel, N. Timneanu, J. Andreasson Department of Chemistry, Biochemistry & Biophysics Gteborgs Universitet Richard Neutze, Gergeley Katona, Sebastian Westenhoff Department of Theoretical Chemistry at KTH, Stockholm Theoretical -Xray Science Faris Gelmukhanov, Zilvinas Rinkeviciu, Viktor Kimberg, Sergey Gavriluk Yuping Sun, Jicai Liu "Computational X-ray spectroscopy" Yi Luo, Cang-Kui Wang, Carlos Araujo, Zgenyu Li, A. Laestadius, Weijei Hua, Qiong Fu "Method and program development in computational X-ray spectroscopy" Hans gren, Kersti Hermansson, Olav Vahtras, Mathieu Linares, Arul Murugan, Staffan Hellstrm, Salam Mohammed, Li Xin, Qiong Zhang Biomedical and X-Ray Physics, Department of Applied Physics, KTH Stockholm Ulrich Vogt, Anders Holmberg, Hans Hertz Universitt Duisburg-Essen Klaus Sokolowski-Tinten, U. Shymanovich Universitt Duisburg-Essen, Germany Universit Rennes 1 Eric Collet, Maciej Lorenc, Herve Cailleau, Marylise Buron, Marina Servol Copenhagen University & Center for Molecular Movies M.M. Nielsen, K.Haldrup, H. Lemke, K. Skov Kjr, J. Petersen, K. Bechgaard Danish Technical University & Center for Molecular Movies K. B. Mller, N. E. Henriksen