Materials Properties Measurements and Particle Beam Interactions Studies Using Electrostatic Levitation

G Model
MSR-437; No. of Pages 53

Materials Science and Engineering R xxx (2013) xxxxxx
Contents lists available at ScienceDirect
Materials Science and Engineering R

journal homepage: www.elsevier.com/locate/mser
Materials properties measurements and particle beam interactions

studies using electrostatic levitation
Paul-Francois Paradis a,b,*, Takehiko Ishikawa a, Geun-Woo Lee c,g, Dirk Holland-Moritz d,
Jurgen Brillo d, Won-Kyu Rhim e, Junpei T. Okada a,f
a
Japan Aerospace Exploration Agency, Tsukuba Space Center, 2-1-1 Sengen, Tsukuba, Ibaraki 305-8505, Japan
INO, Remote Sensing Group, 2740 Einstein, Quebec, Quebec G1P 4S4, Canada
Korea Research Institute of Standards and Science, 267 Gajeong-ro, Yuseong-gu, Daejeon 305-340, Republic of Korea
d
Institut fur Materialphysik im Weltraum, Deutsches Zentrum fur Luft- und Raumfahrt (DLR), 51170 Koln, Germany
e
California Institute of Technology, Materials Science Department, Mail Stop 138-78, Pasadena, CA 91125, United States
f
Japan Science and Technology Agency, Precursory Research for Embryonic Science and Technology (PRESTO), Kawaguchi, Saitama 332-0012, Japan
g
Department of Science of Measurement, University of Science and Technology, Daejon, 305-333, Republic of Korea
b
c
A R T I C L E I N F O
Article history:
Available online xxx
Keywords:
Electrostatic levitation
Materials processing
Supercooling
Nucleation
Thermophysical properties measurement
Atomic dynamics
A B S T R A C T
Electrostatic levitators have been around for more than 30 years and have become mature tools for the
material science community. Originally developed as positioners for materials and uid science
experiments in space, they saw a myriad of offsprings throughout the world for ground-based research,
not only in space agencies but also in governmental laboratories, in universities and in the industry.
Electrostatic levitators eliminate any physical contact with a container allowing to process and study
corrosive or high temperature materials in their solid or liquid phases. Moreover, heterogeneous
contamination from the container being avoided, it is possible to reach and maintain supercooled and
metastable phases. This, in turns, permits a host of fundamental and applied studies. The nucleation and
solidication phenomena can be scrutinized, the atomic structure and dynamic of liquid and metastable
phases can be probed and the physics of molten drops could be investigated. On a more applied
standpoint, the measure of thermophysical properties and the synthesis of materials with new properties
are also possible with current facilities.
This paper rst describes the principle of electrostatic levitation and retraces the development of
various facilities throughout the world, focusing on the advances made by each research group. The
capabilities of electrostatic levitation for materials processing and synthesis under different
environments are then presented. The paper successively covers in length its contribution for the
measurements of thermophysical properties and for fundamental studies using high energy particle
beams. Finally, the outlook of electrostatic levitators and its attractiveness for space experiments in
materials sciences are discussed.
2013 Elsevier B.V. All rights reserved.
Abbreviations: AC, alternative current; A/D, analog to digital; ADL, aerodynamic levitation; BESL, beam electrostatic levitator; BMG, bulk metallic glass; Caltech, California
Institute of Technology; CCD, charge coupled device; CN, coordination number; CNT, classical nucleation theory; CPMD, Car-Parrinello molecular dynamics; D/A, digital to
analog; DC, direct current; DISRO, distorted icosahedral short-range ordering; DLR, Deutsches Zentrum fur Luft- und Raumfahrt (German Aerospace Center); DSC, differential
scanning calorimetry; DTA, differential thermal analysis; ESCAPES, electrostatic containerless processing system; ELF, electrostatic levitation furnace; ESA, European Space
Agency; ESL, electrostatic levitator; FTIR, Fourier transform infrared; GFA, glass forming ability; HDL, high density metallic liquid; Hi-Lite, High Temperature Levitation
Instruments for Thermophysical Evaluation; HRIS, high resolution inelastic scattering; HRPD, high resolution power diffractometer; HTESL, high temperature electrostatic
levitator; IHI, Ishikawajima Heavy Industries; ISRO, icosahedral short-range ordering; ISS, International Space Station; ITS, International Temperature Scale; JAERI, Japan
Atomic Energy Research Institute; JAXA, Japan Aerospace Exploration Agency; JPL, Jet Propulsion Laboratory; KRISS, Korea Research Institute of Standards and Science; LDL,
low density semimetallic liquid; LLPT, liquid liquid phase transition; MCPD, multi channel photo detector; MLWF, maximally localized Wannier functions; MRO, medium
range order; NASA, National Aeronautics and Space Administration; NASDA, National Space Development Agency; NIMS, National Institute for Materials Science; MSFC,
Marshall Space Flight Center; PID, proportional integral derivative; PSD, position sensing detector; RF, radio-frequency; RMC, reverse Monte-Carlo calculations; SEM,
scanning electron microscope; SRO, short range order; TTT, temperature time transformation; UV, ultraviolet; WU-BESL, Washington University Beam Electrostatic Levitator;
YAG, yttrium aluminum garnet.
* Corresponding author at: INO, Remote Sensing Group, 2740 Einstein, Quebec, Quebec G1P 4S4, Canada.
E-mail address: paul-francois.paradis@ino.ca (P.-F. Paradis).
0927-796X/$ see front matter 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.mser.2013.12.001
Please cite this article in press as: P.-F. Paradis, et al., Mater. Sci. Eng. R (2013), http://dx.doi.org/10.1016/j.mser.2013.12.001
G Model

2
P.-F. Paradis et al. / Materials Science and Engineering R xxx (2013) xxxxxx
Contents
1.
2.
3.
4.
5.
6.
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Electrostatic levitation technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Development and description of facilities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1.
Battelle Institut . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1.1.
National Aeronautics and Space Administration-Jet Propulsion Laboratory .
2.1.2.
2.1.3.
Space Systems Loral/NASA-Marshall Space Flight Center/Washington U . . .
National Space Development Agency/Japan Aerospace Exploration Agency .
2.1.4.
National Institute for Materials Science . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1.5.
German Aerospace Center (DLR) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1.6.
2.1.7.
Korea Research Institute of Standards and Science . . . . . . . . . . . . . . . . . . . .
Northwestern Polytechnical University . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.1.8.
Charging strategy and levitation initiation [6,10] . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.2.
Capacitive charging [6,10] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.2.1.
2.2.2.
Photoelectric emission charging [6,10] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Thermionic emission charging . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.2.3.
Heating . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.3.
Sample rotation control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.4.
2.4.1.
Importance of rotation control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Rotation control methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2.4.2.
Materials processing and synthesis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Crystallization and vitrication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
3.1.
3.2.
Solidication studies. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Nucleation studies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
3.3.
3.4.
Phase diagrams . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Reduced-gravity processing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
3.5.
Materials thermophysical property measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Density and thermal expansion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.1.
Measurement method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.1.1.
Experimental results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.1.2.
Surface tension . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.2.
4.2.1.
4.2.2.
Viscosity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.3.
4.3.1.
4.3.2.
Ratio of heat capacity to emissivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.4.
4.4.1.
4.4.2.
Emissivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.5.
4.5.1.
4.5.2.
Electrical conductivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.6.
4.6.1.
4.6.2.
Vapor pressure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4.7.
4.7.1.
4.7.2.
Short-range structure and atomic dynamics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Hard sphere model . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.1.
Neutron scattering experiments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.2.
Preliminary experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.2.1.
Elastic and quasi-elastic experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.2.2.
Synchrotron scattering experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.3.
Inelastic scattering. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.3.1.
Elastic scattering . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5.3.2.
Conclusions and outlook . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1. Introduction
The processing of materials without any containers, crucibles,
or walls has several advantages [13]. For one, it allows the
processing of corrosive materials or materials whose melting
temperatures are higher than that of the crucible. Handling of high
temperature materials in their solid or liquid phases is thus
achievable. It also eliminates or reduces the temperature gradients
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within the material being processed or studied that are caused by

the thermal conduction of the crucible or walls. Because there is no
physical contact with a container, physico-chemical contamination from the crucible or walls is avoided. This implies that
thermodynamic property determination of the original material
can be obtained. Moreover, heterogeneous contamination from the
container being avoided, this makes possible to reach and maintain
supercooled and metastable phases, leading to vitrication of
G Model

materials or to materials exhibiting new crystalline phases.

Because the material is not in close vicinity with a crucible, access
of a material sample by heating laser beams or more importantly
by various diagnostic tools such as optical imaging or high energy
beams (e.g., neutron, X-ray) is improved. The above mentioned
advantages, in turns, permit a host of fundamental and applied
studies. The atomic structure and dynamic of liquid and
metastable phases can be probed and the physics of molten drops
could be investigated. On a more applied standpoint, the measure
of thermophysical properties and the synthesis of materials
(including vitrication) with new properties are not only possible
but simplied when using electrostatic levitators. These subjects
will be covered in details in the forthcoming sections.
The above mentioned merits and the need to accurately
position a sample subject to g-jitters and external forces during
materials science experiments in reduced gravity triggered a host
of hardware development, all of which have their own merits and
limitations [416]. Electrostatic levitators, as will be described in
details in the next section, are rather complex and costly
instruments, sometimes tricky to operate, that require active
feedback system to handle sample of materials. However, they
have a myriad of merits compared to other levitation schemes,
including the fact that a single instrument can handle conductors
and semi-conductors in addition to insulators under high vacuum
or pressurized conditions. The vacuum conditions provide an ideal
environment to minimize contamination-prone materials such as
metals. Operation under a pressurized atmosphere is attractive
when processing high vapor pressure materials. Changing the gas
composition provides a mean to modify the sample stochiometry
and, therefore, opens the door to the production of materials with
tailored or improved properties (e.g., optical, mechanical, chemical, electrical, magnetic). Also, because an electrostatically
levitated sample is free from any enclosure, it represents an easy
target for various diagnostics detectors and probes (cameras,
position detectors, photomultipliers, lasers, X-rays, etc.). Compared to aerodynamic [12,13,17] or aerostatic levitators [18],
electrostatic levitators provide precise sample position control
(translation as well as rotation), provide more quiescent processing conditions, less temperature gradients, and allow a full access
to the sample by diagnostics probes. Also, when operated under
vacuum, the electrostatically levitated sample experiences fast

radiative cooling. Electrostatic levitators permit the handling of
high temperature liquids and the position stability, as well as the
surface of a liquid sample, is not altered as much as in the case of
acoustic or aero-acoustic levitators [7,11,14]. Compared to
electromagnetic levitators, the electrostatically levitated sample
is not surrounded by coils, which makes some characterization
studies easier [9] and exhibits different internal ow behavior [19].
Furthermore, the sample is not subject to strong convection during
processing and its shape is not deformed. Although optical
levitators are interesting for several investigations, they are
limited to sub-millimeter size objects on the ground [8,20].
Contrary to electromagnetic and optical levitators, levitation and
heating are not coupled in the electrostatic scheme which gives
more control over heating, cooling, and solidication. At last,
although cold crucibles can handle large amounts of material, they
exhibit substantial temperature gradients and strong induced
convection as opposed to electrostatic levitators [21]. A comparative summary of the main characteristics of different levitation
techniques with regards to materials processing and study is
presented in Table 1.
This paper rst devotes a section on the electrostatic levitation
which describes the development of the technique and explains
the underlying physics, in particular sample charging strategies,
sample positioning and rotation control, and sample heating. A
subsequent section is concerned with materials processing, study,
and synthesis. In this section, crystallization and vitrication,
solidication, nucleation, and phase diagrams studies as well as
reduced-gravity processing are successively addressed. The
thermophysical property measurements for density, thermal
expansion, surface tension, viscosity, electrical conductivity, heat
capacity, emissivity, and vapor pressure are covered in depth,
describing the measurement methods and presenting the unique
data taken to this date with electrostatic levitators. The contribution of electrostatic levitation to atomic dynamic studies, namely
with regards to the hard sphere model, neutron scattering
experiments, synchrotron scattering experiments is then discussed in length. The outlook of electrostatic levitation and its
associated diagnostic tools in materials science is addressed before
discussing the reduced gravity experiments planned in orbit.
Table 1
Comparative summary of the characteristics of different levitation techniques with regards to materials processing and study.
Levitation
technique
Processing environment
Material
Access to
sample for
diagnostics
Stability at high
temperature
Comments
Rotation control; levitation and heating

uncoupled; high speed feedback;
complex system; costly; ISS operation
to come soon
Levitation initiation easy; large samples
processed; levitation and heating
coupled; somewhat complex; Sample
deformation; rotation control difcult;
inner ow; used on-board ISS
Used on-based space shuttle;
somewhat complex
Type
Size
High vacuum
Pressurized
atmosphere
Electrostatic
Conductor;
semi-conductor;
insulator
mm-size
Possible
Excellent
Excellent
Electromagnetic
Conductor
cm-size
Possible
Possible but
pressure range
limited by
Paschens rule
Possible
Fair
Good
Acoustic
Conductor;
semi-conductor;
insulator
Conductor;
semi-conductor;
insulator
Conductor;
semi-conductor;
insulator
Conductor;
semi-conductor;
insulator
cm-size
Impossible
Possible
Good
Bad
mm-size
Impossible
Possible
Fair
Good
Simple system; inner ow; used during

parabolic ights
cm-size
Impossible
Possible
Excellent
Good
Used on-based ISS; combustion

experiments; complex system
Atoms to
mm-size
objects
Possible
Possible
Excellent
Excellent
Levitation and heating coupled

Somewhat complex
Aerodynamic
Ultrasonic
Optical
G Model

2. Electrostatic levitation technique

2.1. Development and description of facilities
2.1.1. Battelle Institut
The concept of electrostatic positioning for materials processing
in space dates back from before 1977 when the Eurpoean Space
Agency (ESA) started funding research and development activities
[22]. The rationale of this effort was the exploration of the merits
and limitations of various containerless processing systems which
were compliant with the furnace systems installed on Spacelab.
The conceptual study about electrostatic positioning was performed at the Battelle Institut in Frankfurt and, as a result, a
technology demonstrator was built [4,23,24]. The positioner was
designed for sample processing under vacuum and at temperatures up to 1500 8C. Such temperatures could be reached with a
mirror heating furnace or with an isothermal heating furnace
[4,23]. The electrodes of this electrostatic positioner were
tetrahedrically arranged and the spacing between them was twice
that of the sample diameter which was specied as 1 cm. These
were made out of Pt and had a spherical shape of 8 mm in
diameter. The facility was designed such that the sample was
electrically neutral during the whole experiment.
The positioning forces were caused by the dielectric polarization, p, of the sample in the inhomogeneous electric eld. If the
dielectric constant e of the material is greater than unity, the
polarization becomes
p
e1
:
e1
(1)
The force, F, acting on the sample depends on the electrode

potential, U, and can be expressed in terms of the change of the
capacitance, c, with the sample displacement:
F
1
rc U 2
2
(2)
When voltages of up to 10 kV were applied, the positioning

force was approximately 103104 g. This means that levitation
on the ground was not possible using this scheme. However, the
authors estimated that it should be sufcient for positioning under
the microgravity conditions of Spacelab, where the residual forces
were in the order of 105106 g. On the TEXUS sounding rocket,
the g-level was in the range of 104105 g [5].
The capacitance of each electrode was a function of the distance
of the sample to that specic electrode. This fact was used in order
to sense the sample position. The position control was performed
by a proportional integral derivative (PID) controller and the high
voltage, applied to the electrodes was adjusted such that the
sample position remained stable. To show that the device was
working, it was tested in a setup where a dummy sample, attached
to a short pendulum, was placed inside the electrode system. This

pendulum was suspended on the furnace. The furnace itself and
the positioner were both suspended on a long pendulum which
performed forced oscillations. The sample position was obtained
from the displacement of the long pendulum and it was compared
to the variation of the capacitance recorded simultaneously [4,23].
Ten years later, in 1988, an improved version of this electrostatic
positioner, equipped with CCD cameras for the position sensing,
was own on a sounding rocket mission (TEXUS 19) [5]. During the
rocket launch, one of the cameras was misaligned and made the
sample moved uncontrolled inside the furnace, going into and out
of the focus of the mirror heating system during the experiments.
This resulted in a temperature which was much lower than that
planned and the sample did not fully melt. Rather, it collided with
one of the electrodes and got stuck. As no further funding was
granted, and because the Battelle Institut in Frankfurt was closed
down only a few years later, the project was no longer pursued.
2.1.2. National Aeronautics and Space Administration-Jet Propulsion
Laboratory
2.1.2.1. Early facilities. Systematic and fundamental research and
development was carried out at the National Aeronautics and
Space Administration (NASA)-Jet Propulsion Laboratory (JPL)
spanning two full decades in the 1980s and the 1990s. Groundbased technology demonstrators using several electrode congurations and operational at atmospheric conditions were successfully developed and tested [6]. The earliest version of the
electrostatic levitators or positioners consisted in two concave,
parallel dishes (Fig. 1(a)). It was chosen for the simplicity of its
mechanical design and the required servo control system.
Assuming a pair of horizontal, parallel electrodes, the equation
Mg = (V/d)Q has to be satised in order to levitate an object
between the electrodes, where M is the mass of the object carrying
a charge Q, g is the gravitational acceleration, and V is the voltage
difference between the plate electrodes which are separated by a
distance d. Typical experimental values of these parameters were
Q =4 109 C, M = 0.1 g, d = 1.2 cm, and V = 13 kV. In order to
generate a lateral restoring force, the design used a circular convex
top electrode and a matching concave bottom electrode. The
electrostatic lines of force could therefore be decomposed into
vertically lifting components and horizontally centering components. More importantly, because of Earnshaws theorem regarding the absence of potential well, and therefore the lack of a
stationary position for a charged sample subject to an electrostatic
eld [25], an active control system that varies the potential
difference between the electrodes had to be used to ensure stable
levitation of a charged sample.
To improve 3D position stability, the dish-type positioner was
modied as to generate lateral centering forces for a range of
Fig. 1. Pictorial representation of the electrode conguration of JPL early electrostatic levitators: (a) dish type; (b) ring type; (c) tetrahedral type [6].
G Model

levitators, the position of the levitated object was sampled at a

frequency of 120 Hz and this measurement was used to compute
output values proportional to the controlling electrode voltages
according to a proportionalintegralderivative (PID) servo algorithm [26].
Fig. 2. Block diagram of the main position control components of the JPL early
electrostatic levitators (shown here for the tetrahedral positioner conguration)
[6].
acceleration levels. As in the previous design, active position

control was implemented along the vertical symmetry axis. The socalled ring positioner (see Fig. 1(b)) created a radially symmetric
eld to force a charged object into a two-dimensional potential
well with respect to its movement in a lateral plane thanks to the
addition of two annular electrodes to the dish-type levitator. This
passively centers the object. As shown in Fig. 1(b), the lateral
centering force was produced by maintaining the ring electrodes 2
and 4 at a higher voltage level than their respective central
electrodes 1 and 3 at all times.
To achieve three-dimensional active servo control in view of a
reduced gravity operation, a tetrahedral positioner was designed,
constructed, and tested (Fig. 1(c)). It had four spherical electrodes
in a tetrahedral arrangement and used two charge coupled device
(CCD) cameras to image, along the three axes, the sample being
levitated. Because an active feedback control system was used, the
sample could be positioned anywhere within the levitation space.
This electrode conguration was successful in actively damping
oscillations in all directions.
The gure below illustrates the main components of the control
system used for these levitators: the CCD cameras for imaging the
position of the sample, the camera interface logic to convert the
video signal from the cameras to an integer representing the object
position for each axis, a personal computer to implement the
control algorithm, four digital-to-analog converters to generate
control voltages for four programmable high-voltage units, and a
chamber containing up to four electrodes (Fig. 2).
Diffuse backlighting was used to make the levitated sample to
appear as a dark group of pixels on a bright background on the CCD
cameras. Because of the limited capacity of the computer in the
1980s, camera interface hardware was used to extract the centroid
of the position of the sample from the two CCD camera images to
relieve the control computer of the image processing task. In these
2.1.2.2. High temperature facility. To further the capability of their

electrostatic levitator to support materials science in space, the Jet
Propulsion Laboratory pursued the development of a high
temperature electrostatic levitator (HTESL) operating under
vacuum [10]. Figs. 3 and 4 illustrate schematically the electrostatic
levitation furnace which consisted of a stainless steel chamber that
was typically evacuated to 105 Pa before sample processing
began. The chamber housed a 23 mm diameter sample charged
by electronic emission (charging processes to be discussed in a
later section) which was levitated between two horizontal
electrodes, a slightly concave bottom electrode (25 mm dia.) with
a through hole and a gold at top electrode (25 mm dia.). The
through hole permitted sample handling with a single stainless
steel pedestal that retrieved a specic sample from a 10-sample
capacity carrousel. By applying electric elds ranging from 4 to
20 kV/cm between the disk electrodes, samples of various
elemental metals (e.g., In, Sn, Bi, Pb, Al, Ge, Cu, Ni, Ti, and Zr),
and metallic alloy materials (e.g., InSb, NiZr, glass forming) could
be levitated in vacuum. The top electrode could be gimbaled with a
dedicated mechanism, allowing accurate electrode balancing and
spacing (12 mm between both electrodes). These electrodes were
mainly effective for vertical position sample control. In addition,
four secondary spherical electrodes with applied positive or
negative potentials, distributed around and at the height of the
levitated sample, were used to further control the horizontal
position. Here again, a feedback position control system was
implemented to ensure stable sample positioning. Position sensing
was achieved with a set of orthogonally disposed HeNe lasers and
the associated position detectors. The position information,
obtained by the shadow of the HeNe laser illuminated sample,
was fed to a computer that input updated values of x, y, and z to a
high voltage amplier at a rate of 720 Hz so that a predetermined
position could be maintained.
The upper electrode was surrounded by four coils that were
used as a stator to generate a horizontal and rotating magnetic
eld. The magnetic eld was used for sample rotation control [27].
Sample rotation could also be controlled using photon pressure
[28]. In addition, an AC voltage was superimposed on the levitation
voltage from the top electrode to excite drop oscillations for
surface tension and viscosity experiments [29].
The sample was observed by two CCD cameras (Fig. 4). One
camera offered a general view of both the electrode assembly and
the sample. One high resolution CCD cameras, equipped with a
telephoto objective allowed sample perimeter and surface features
to be analyzed in conjunction with a high intensity white
Fig. 3. Schematic representation of the electrode conguration and active position control hardware used by the JPL high temperature electrostatic levitator (shown in one
plane).
G Model

6
Fig. 4. Schematic representation of the JPL high temperature electrostatic levitator.
background light [30]. In addition, a detector was equipped with an

interference lter (HeNe emission line) and a monochromator slit
to determine the oscillating amplitude of a sample from its HeNe
laser backlit shadow [29]. A similar sensor was used for sample
rotation rate measurement by detecting the reected HeNe laser
beam from its surface [27]. Recently, Rustan et al. [31] claimed to
have improved the positional stability of the levitated samples by
replacing the HeNe lasers by high-power, quasi-monochromatic
LEDs. According to their data, the drift in the sample vertical
position is reduced by at least one order in magnitude.
Sample heating was achieved up to 1000 8C by a 1 kW xenon arc
lamp and an associated reector. At this temperature the xenon arc
lamp was gradually switched to a 100 W YAG laser [32] to reach
higher temperatures. A pyrometer which operated at a wavelength
of 4 mm was used to avoid any interference by the xenon arc lamp
radiation. When only the YAG laser was used, a single (750 nm) or
three color pyrometer was used.
Besides sample positioning and fundamental development in
areas of rotation and oscillation control, several non-contact tools
for the thermophysical property determination was achieved by
the JPL group over the years. The overall work opened several
unique research opportunities in property measurements (density
[30], the ratio of isobaric heat capacity to hemispherical total
emissivity [33], surface tension, viscosity [29]), solidication
studies [34], and in drop dynamics [35]. In year 2000, the facility
was moved from JPL to the department of materials sciences at the
California Institute of Technology.
This facility was much inuential in the development or
construction of several electrostatic levitators in the United States
(e.g., Loral/MSFC/U Washington; Iowa U) as well as elsewhere in
the world (e.g., NASDA/JAXA, DLR, KRISS). In the following
paragraphs, emphasis is given to the main contributions and the
signicant differences between these facilities and the original JPL
facility [10] with regards to their impact in materials science.
2.1.3. Space Systems Loral/NASA-Marshall Space Flight Center/
Washington U
An off-spring of the JPL developed levitator is the electrostatic
containerless processing system (ESCAPES) [15,36]. This
facility, built by Space Systems Loral, incorporates several
design improvements over the prior, JPL electrostatic levitation
technology. The levitator was upgraded with a circle type design

for side electrodes and a more digitalized control program
compared to the original JPL design. In this facility, heating and
charging sources were separated by using a heating laser and a
deuterium arc lamp, so that the runaway discharging effect could
be avoided, and therefore could improve the position control of a
sample. Also, both the heating and charging light sources being
narrow spectral bands, this allowed the use of optical pyrometry
and other diagnostics at all times throughout processing. This
facility has been upgraded with several diagnostic tools by the
NASA Marshall Space Flight Center to make possible the
investigation of thermophysical properties, phase equilibria,
metastable phase formation, supercooling and nucleation,
timetemperature-transformation diagrams and other aspects
of materials processing [37,38].
The ESL system in Marshall Space Flight Center was modied
(called Beam ESL) in a joint effort with a team at Washington
University in St-Louis, for in situ structural studies of several types
of materials by high energy synchrotron X-ray scattering at the
Advanced Photon Source at Argonne National Laboratory [39].
Incident X-ray beam energies were available in the range from 30
to 130 keV. For X-ray input, a Be window port was used in the ESL
chamber. The maximum wave vector q range was extended up to
14 A1 with this facility. This beam line facility allowed the in situ
determination of the atomic structures of equilibrium solid and
liquid phases, supercooled liquids and time-resolved studies of
solidsolid and liquidsolid phase transformations. Furthermore,
the same team recently developed a modular electrostatic levitator
(called WU-BESL) for easy setting up and operation into a
synchrotron X-ray beam line scattering facility [40]. This modular
facility was optimized for diffraction studies of high-temperature
liquids at high-energy synchrotron beam lines. In this version, the
positioning and alignment for X-ray beam line can be controlled
with micrometer accuracy, which can give better signal and
uniform intensity.
2.1.4. National Space Development Agency/Japan Aerospace
Exploration Agency
2.1.4.1. Sounding rocket facility. To take advantage of containerless
processing and of the microgravity environment offered by the
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Fig. 5. Schematic representation of the NASDA electrostatic levitation dedicated to the sounding rocket TR-1A [16].
Reprinted with permission from S. Yoda et al., J. Japan Soc. Microg. Appl. 17, 7686. Copyright 2000, Japan Society of Microgravity Application.
Japanese Experiment Module of the International Space Station

(ISS), the National Space Development Agency of Japan (NASDA)
(became part of the Japan Aerospace Exploration Agency (JAXA) on
October 1st, 2003) started in the 1990s the development of
electrostatic levitation furnaces [16,41,42]. The rst facility was
developed by Mitsubishi Electric Corporation for testing on-board
a sounding rocket (TR-IA) and consisted in a stainless steel
chamber under a control atmosphere that contained an automatic
sample-exchange mechanism and a set of electrodes (Fig. 5) [16].
In this facility, the sample was heated by four diode lasers
(810 nm), and each laser power could be controlled independently,
which enabled both uniform and non-uniform heating. The sample
was observed with a thermal imaging system and with a video
camera and its temperature was measured with a pyrometer
(1.55 mm). During the free-fall part of the sounding rocket ight, a
spherical BiFeO3 specimen with a diameter of 5 mm was laser
heated and solidied in an oxygen and nitrogen mixture
atmosphere [43].
2.1.4.2. Ambient pressure facility. Although the NASDA preliminary
tests of an electrostatic levitation furnace (ELF) on-board a
sounding rocket showed promising results [43], further groundbased work was deemed necessary before such a facility could be
fully operational on the ISS. Therefore, post-ight efforts were
specically aimed to optimize the sample positioning and control
(stability, rotation, oscillation, etc.) and to implement laser-based
heating methods for use on-orbit. Parallel efforts were also
directed to devise new processing methods and to improve
various non-contact material diagnostic techniques to make the
electrostatic levitation furnace a true research facility to support
several elds in materials science on the ground. Early goals
targeted the measurements of thermophysical properties such as
density, heat capacity, emissivity, surface tension, viscosity,
electrical resistivity, and thermal conductivity of high temperature
materials in their solid, liquid, or deeply supercooled phases.
Another rationale was to have a facility with which new and better
quality materials with tailored or unusual magnetic and dielectric
properties could be developed. The study of metastable phases
formation and nucleation phenomena was also a motivation.
A rst-generation ground-based facility was thus developed
starting from 1999 [4446] for use with pure metals, metallic
alloys, semiconductors, and dielectrics under vacuum or pressurized atmospheres. This facility used an electrode conguration and
a feedback control system reminiscent of the JPL design. Early

hardware and software development work and testing was done
with this facility.
2.1.4.3. Vacuum facility. Although the contemporary electrostatic
levitator furnaces such as those developed by Rhim et al. at JPL and
its offspring built by Space Systems Loral [6,10,15] had numerous
qualities, they also had a number of limitations that were
addressed by NASDA/JAXA with a dedicated vacuum facility
[47]. For one, the early designs used a carousel below the bottom
electrode for sample handling. This worked ne for hard samples
with diameters larger than 1.5 mm but jamming problems arose
for smaller samples or for soft materials. In addition, a single
pedestal being used, a risk of contamination was possible if
samples of different materials were processed. Fig. 6 shows, among
other things, the sample handling mechanism designed for the
JAXA vacuum electrostatic levitator. It consisted of a single sliding
cartridge containing ten individual molybdenum or tungsten rods.
Not only did this circumvented any cross-talk contamination
problems between distinct samples but permitted the handling of
Fig. 6. Schematic representation of the JAXA vacuum electrostatic levitator

illustrating the sample handling cartridge system, the catcher, the electrode layout,
and the induction coils to control sample rotation.
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8
very soft or porous materials. Addressing this issue was an

important step forward to allow for easier and faster processing
(no need for sample pre-cleaning before the experiment) and more
accurate surface tension and viscosity measurements. Furthermore, sub-millimeter samples could also be easily handled using
this system thus avoiding any jamming problems. A conical catcher
helped to retrieve unsuccessfully levitated samples.
The parallel disk electrodes design together with the four
surrounding spherical electrodes reported early in the development of electrostatic levitators [10] provided sufcient lateral
stability for many materials (Sn, Zr, Si, etc.). However, the
horizontal restoring forces supplied by this scheme were not
strong enough when dealing with evaporative materials such as Ti,
Mo, and W. Sample instability problems were especially acute
when large laser power was used to reach the extreme
temperatures required to study highly refractory materials. To
improve the horizontal position control of such material samples, a
at, top electrode smaller (10 mm dia.) than the bottom concave
electrode (25 mm dia.) was used (Fig. 7). The conical electrical eld
distribution resulting from this arrangement provided a horizontal
eld component and thus a natural restoring force toward the
center diminishing the hurdle of processing very refractory metals
[48,49]. This, together with four spherical electrodes brought to the
height of a levitated sample, offered improved 3-D sample
stability, even for high vapor pressure materials. In this facility,
the bottom electrode was made out of tungsten to withstand the
severe temperatures induced by the combined 700 W of laser
heating.
The position feedback control system relied on a PID scheme,
identical to the original JPL design [10] and was implemented by
two sets of orthogonally disposed HeNe laser and position
sensors. However, the feedback loop could be chosen (over a range
of 240720 Hz) depending on the application to ensure that the
sample was maintained in a xed position and that the feedback
frequency had a minimal effect on the molten sample dynamic
itself [50].
Contrary to its JPL predecessor, the coils were located near the
bottom electrode. Not only did this facilitated the handling of the
top electrode for maintenance but this arrangement avoided the
risk of electrical breakdown between the electrode on which the
high voltage was applied and the coils, therefore ensuring that
levitation of a sample was not prematurely terminated. An
important contribution of this facility resides in the implementation of a technique to shorten signicantly the launch initiation
and the total processing times from several hours in some cases to
a mere few seconds with the technique introduced later in Section
2.2.
Sample heating was performed using the radiation coming from
computer controlled CO2 (10.6 ym) and Nd:YAG lasers (1.064 mm).
To avoid the destabilizing effect of photon and evaporative
anisotropic induced forces observed when a single beam is used
Fig. 7. Laser beams conguration in JAXA vacuum facility to heat a levitated sample.
[51] and to maintain good sample position stability, a attened

tetrahedral laser heating conguration was implemented (Fig. 7)
[48]. Specically, three focused beams (50 W each) of CO2 lasers
(10.6 mm emission) in a same plane, separated by 1208, hit the
specimen. In addition, the focused beam of a 500 W Nd:YAG laser
(1.064 mm) (equipped with a 090% power attenuator) heated the
sample from the top. Heating with the most powerful laser along
the vertical was the best conguration as the strongest eld and
the fastest feedback were also along this axis. Besides the
exceptional 3D sample position stability it provided, this multibeam heating conguration helped to control sample rotation and
improved temperature homogeneity.
The JAXA vacuum facility was equipped with several cameras
not only to help handling of samples, adjust the laser beams, and
monitor the levitation of the sample but also to record images of
the shape, texture, and melting, solidication behavior during
processing (Fig. 8). As in the original JPL facility, detectors were
used to measure the sample rotation rate and the amplitude of
deliberately induced oscillations. The radiance temperature of the
sample was measured over a 12503800 K range using two
automatic pyrometers (operating at 0.90 mm and 0.96 mm) with
respective acquisition rates of 10 and 120 Hz. Calibration to the
true temperature was performed using the known melting
temperature of the material with Plancks law using a custommade software.
2.1.4.4. Pressurized facility. The previously developed electrostatic
levitators could levitate isothermal solids and liquids in ambient
conditions and various metallic solids and molten materials in
vacuum, including metallic glasses [52]. However, they were not
suitable to levitate and melt several types of oxide materials for
several reasons. The vacuum or low pressure environment in
which they operated was detrimental for materials with high
vapor pressure. In addition, when processing some of these
materials (e.g., CaAl2O4) the absence of a gaseous environment
altered the original stochiometry and a pressurized atmosphere
was required. More importantly, these facilities, as they were, had
no appropriate means of sufciently charging the levitated sample
as to bring it into a molten state. Hence, containerless processing of
these molten materials was not feasible.
The usual mode of initiating electrostatic levitation, relying on
capacitive surface charging of a sample resting on a pedestal was
not sufcient to allow levitation of most oxide materials. Attempts
of charging through photo-electric effect by irradiating a focused
ultra-violet laser beam on a sample was not successful either. The
heating of a sample resting on the pedestal until it reached a
temperature at which thermionic emission dominated charging
mechanisms showed evidence of electrical charge accumulation
[53]. However, this technique was plagued with stickiness
problems, especially for materials with low melting temperature
and made levitation initiation difcult if not impossible. To avoid a
physical contact between the sample and the pedestal the idea was
to use an aerodynamic diffuser. The diffuser allowed sample
levitation with a satisfactory stability prior to launch into the
electrostatic levitation mode. The diffuser, designed along the
results of Refs. [12,13,54], consisted of a converging-diverging
nozzle with a 608 diverging angle and a 1 mm diameter throat. This
angle was selected as the best compromise between a narrow
potential energy well width and a minimum diffuser wall-tosphere distance. The ow rate was kept as low as possible to
minimize the potential energy well depth in which the sample was
trapped. This conguration thus exerted on the sample a weak
force that minimized the electrostatic forces needed to extract it
when it accumulated sufcient charges. In addition, this type of
diffuser provided lateral restoring forces, allowing acceptable
sample stability. By aerodynamically levitating the sample, it was
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Fig. 8. Pictorial representation of the main system components (view from the top) of the JAXA vacuum electrostatic levitator.
possible to increase the sample charge to a level suitable for

electrostatic levitation while avoiding any contamination. Although the exact charging mechanisms are still unknown,
thermionic emission seemed the dominant one since the
temperature at which surface charges were sufcient for launch
was around 1500 K [55]. Surface ionization of the surrounding
molecules could also have contributed to charging.
The facility, depicted schematically in Fig. 9, consisted of a
stainless steel chamber, designed to safely withstand a 500 kPa
pressure of air, nitrogen, or oxygen [56]. The pressurized condition
is an advantage in electrostatic levitation since it permits to apply a
higher eld between the electrodes before electrical breakdown

occurs, hence permitting levitation of heavier samples. The
electrostatic levitator part of this facility was based on a design
by Rhim et al. [10] and the positioning hardware and software
system was identical to that of the JAXA vacuum facility. Fig. 10
illustrates the interior arrangement of the chamber that housed the
parallel disk electrodes. The top electrode rested on a xy
positioning translation stage to ease alignment. This electrode
had a hole which permitted gravity assisted sample loading from a
18-specimens capacity carrousel, that allowed the handling of
porous, soft, non-spherical, and sub-millimeter samples. A conical
Fig. 9. Pictorial representation of the main system components (view from the top) of the JAXA pressurized electrostatic levitator.
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10
and error, which prepare and complement synchrotron X-ray

experiments. This small apparatus also provides the advantage of
portability that makes it well suited for experiment at the SPring-8
synchrotron radiation facility. A duplicate of this facility was
constructed at Tokyo University for diffraction and Compton
scattering studies at SPring-8 [61]. An even smaller facility was
developed for atomic dynamic studies with the BL35XU beam line
at SPring-8 [59,60].
Fig. 10. Schematic representation of the JAXA pressurized electrostatic levitator

illustrating the sample handling carrousel, the receiving and retrieving cones, the
electrode layout, and the aerodynamic levitator used to electrically charge the
sample prior to launch into electrostatic levitation mode.
catcher helped to retrieve unsuccessfully levitated samples. The

bottom electrode (electrically grounded) had a central hole
housing a pedestal. This pedestal performed dual tasks: it helped
to retrieve and position the sample before launch and, having the
shape of an aerodynamic diffuser, it allowed, as described before,
charging without the sample sticking to a pedestal.
The sample was heated using an unfocused CO2 laser whose
power was controlled by a computer. Heating the sample from the
above offered several advantages among which: it ensured a
symmetric heating, important to optimize the stability of an
aerodynamically levitated sample; it minimized natural convection; and it allowed continuous sample heating throughout all
phases of processing, from launch to levitation. Laser heating
allowed quick sample cooling (radiative and conductive) by simply
turning off the laser power. Again, temperature data were recorded
with optical pyrometers. A low resolution camera offered a general
view of both the electrode assembly and the sample and a high
resolution camera imaged more closely the sample to detect any
changes occurring in its shape or on its surface. By using these
instrument and procedures, several oxides (e.g., Nd-CaAl2O4,
CaAl2O4, Y3Al5O12, BiFeO3, BaTiO3, CaF2, BaB2O4-Na2O, BaTi2O5)
could be heated, melted, supercooled, and solidied without any
charge loss problems, allowing thermophysical property measurements and solidication studies. Very recently, JAXA build a brand
new pressurized facility based on the design of this levitator. This
new chamber can safely withstand a pressure of 1 MPa.
2.1.4.5. Beam line facilities. Concomitantly to the vacuum and
pressurized facilities used for materials processing and thermophysical properties determination, JAXA designed a vacuum
facility specically aimed for atomic dynamic studies and
structural characterization of materials in prolonged liquid or
supercooled phases by neutron scattering [57,58]. This facility is
described later in Section 5.2.1. Moreover, a compact electrostatic
levitator was also developed for the structural analysis of hightemperature liquids by X-ray diffraction methods [59,60]. Again,
the overall layout was very similar to the pressurized facility.
However, all the hardware necessary for the sample positioning
control and for sample observation was located on the top of the
chamber to avoid that high energy diagnostic beam impinged upon
the hardware. Therefore, tiny mirrors were used within the
chamber to redirect the laser beam used for feedback control and
the sample image toward the observation camera. This levitator
can be set up on a two axis diffractometer with a laboratory X-ray
source, which is very convenient in performing structural
measurements of high-temperature liquids. In particular, since
the laboratory X-ray source allows a great amount of user time,
preliminary or challenging experiments can be performed by trial
2.1.4.6. ISS facility. After a few decades of ground-based research

and development and parabolic ight testing, JAXA has initiated,
will the help of IHI Aerospace, the development, design, and
construction of an electrostatic levitation furnace dedicated to the
materials science in reduced gravity [62,63]. The facility will most
likely be launched by a H-IIB rocket on-board the HTV Konotori
spacecraft in 2015. The facility (Fig. 11) will be housed in the
Japanese experimental module Kibo of the International Space
Station (ISS).
The main components of this facility are similar to the groundbased levitators, comprising of a processing chamber, a levitator, a
position feedback control system, heating lasers, a cartridge
holding samples, and thermophysical diagnostic tools (e.g.,
cameras, photodetectors, pyrometers). The major differences
between this levitator and the previous ones are the number
and layout of the electrodes and the presence of a mechanism to
handle (set and retrieve) a sample under reduced gravity
conditions. Fig. 12 shows the electrode conguration in which
each of the six electrodes is located in the middle of each face of a
cube. This conguration was simpler to implement with software
and positioning control compared to a tetrahedral conguration
and exhibited great efciency in maintaining a sample subject to
forces along the three axes. This facility is mainly aimed to the
processing of oxide materials, thermophysical property measurement, and fundamental nucleation, solidication, and vitrication
studies. A photograph of the breadboard model is shown in Fig. 13.
The basic requirements are listed in Table 2.
2.1.5. National Institute for Materials Science
The National Institute for Materials Science (NIMS), located in
Tsukuba, Ibaraki, Japan, developed a vacuum electrostatic levitation furnace for containerless solidication studies [6466]. In this
system, there are three electrodes: one top electrode and two
Fig. 11. Illustration of the processing chamber (left) and of the sample cartridge
(right) [62].
Reprinted with permission from N. Sugi et al., J. Jpn. Soc. Microg. Appl. 23, 2025.
Copyright 2006, Japan Society of Microgravity Application.
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Table 2
Specications of the JAXA ISS electrostatic levitation furnace [62,63].
Item
Requirement
Sample diameter
Position stability
Atmosphere
25 mm
100 mm
Ar/N2 up to 2 atm
Low pressure (103 Torr) through
waste gas line
4 diode lasers (970 nm) (200 W total)
Pyrometry
1 for density measurement and
1 for general view
Density by image analysis
Surface tension and viscosity
by oscillation drop method
>10,000 frame per second
Heating
Temperature measurement
Camera
Thermophysical property
measurement
High speed camera
Fig. 12. Electrode conguration of the breadboard model for JAXA ISS electrostatic
levitation furnace [62].
2.1.6. German Aerospace Center (DLR)

The Institute of Materials Physics in Space at the German
Aerospace Center (DLR) in Cologne started the development of
electrostatic levitation facilities in the late 1990s. Currently, two
stationary electrostatic levitators are operated in the institute. A
schematic sketch of the facilities is depicted in the gure below.
The electrically charged sample (S) is levitated by the electrostatic
eld of two vertically arranged electrodes. Two pairs of additional
side electrodes are used to control the horizontal position of the

samples. The electrode system (ES) is installed within an ultra-high
vacuum (UHV) chamber (V) that can be evacuated down to a
pressure of 108 mbar by use of a turbo molecular pump. The
chamber is equipped with several viewports allowing various
kinds of in situ diagnostics (e.g., temperature measurement, video
imaging) (Fig. 14).
Reminiscent of the JPL design, the specimen is illuminated by
two crossed expanded beams of red lasers (PL) to determine the
sample position. The shadow of the sample in the two laser beams
is monitored by two-dimensional position sensitive Si-photodetectors (PSDs). The sample position signals from the PSDs are the
input for a closed-loop sample position control algorithm [67],
which controls the high voltages supplied to the electrodes on a
millisecond timescale. To generate the main levitation force, a
high-voltage amplier with a maximum output voltage of 20 kV is
used to drive the two vertical electrodes. For the horizontal
position control, each channel of a four-unit 3 kV bipolar highvoltage ampliers powers one of the four horizontal electrodes.
Each of the perpendicular pairs of horizontal electrodes is operated
with equal voltage but with opposite polarity.
For heating the specimen, two 25 W infrared ber-coupled diode
laser (IR) emitting at a 810 nm wavelength are employed. The
sample temperature is measured with a pyrometer (P). For
outgassing the samples prior to levitation, the facilities are equipped
with a sample pre-heating device. This consists of a tungsten or
Fig. 13. Photograph of the breadboard model for JAXA ISS electrostatic levitation
furnace [62].
Fig. 14. Schematic representation of the DLR stationary levitators. Sample: S;

electrode system: ES; infrared heating lasers: IR; positioning lasers: PL; position
sensitive detectors: PSD; UV lamp with focusing mirror optics: UV; UHV chamber:
V; pyrometer: P.
concentric electrodes located at the bottom, reminiscent of the JPL

earlier design [6]. By appropriately setting the voltage between the
electrodes (20 kV), a potential well is created enabling a sample
(up to 5 mm in diameter, 0.1 g mass) to levitate. To initiate
levitation, a sample is placed on the bottom electrode and is rst
capacitively charged and then launched by applying a potential
difference to the three electrodes. After the sample is levitated,
electrical charge is maintained by irradiating ultraviolet light onto
the sample. The position of the sample is controlled through a
feedback system running at 1000 Hz. Sample heating is achieved
by two Nd-YAG lasers having respective power of 150 W and
250 W under an ultimate vacuum of 106 Pa.
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12
ceramic rod that can be moved through a hole in the center of the
bottom electrode, thus raising the solid sample to a position at which
it can be illuminated and heated by the heating lasers.
To compensate the charge losses during heating of the sample
before charging by thermionic emission becomes efcient at
elevated temperatures, the specimen is illuminated by the
ultraviolet light of a deuterium lamp. This helps the specimen
to gain charge by means of the photoelectric effect.
The stationary electrostatic levitators at DLR are utilized to
study the supercooling behavior of various melts of metals and
semiconductors [68], to measure the thermophysical properties of
the melts such as density and viscosity [69], and to investigate the
crystal growth behavior during non-equilibrium solidication of
supercooled melts [70,71]. The design of electrostatic levitators
described above is also the basis of DLRs mobile ESL which is used
for some of the scattering experiments that are described in
Section 5. Moreover, the sample position control technology
developed at DLR constitutes the heart of Washington Universitys
WU-BESL [40] and of a facility at Iowa State University [31].
2.1.7. Korea Research Institute of Standards and Science
In the view of standards in metrology, levitation techniques are
attractive. Up to date, the denition of the International
Temperature Scale (ITS) was based on a series of metal xed
points from which freezing temperatures are dened as closer to
their thermodynamic temperatures as is possible. To obtain the
metal xed points, a crucible that contains molten metals is
needed. However, the crucible can be a source of impurities, and
react with the molten metals causing contamination. Thus, the
crucible can affect the measurement of the xed point temperatures. Moreover, mechanical stress after repeated melting and
freezing processes can causes the breakage of even graphite
crucibles [72]. Although the metal-carbon eutectics may be
accepted as a clever way to circumvent the contamination of
metals and breakage of the container, this method cannot avoid the
reaction with the container wall. Furthermore, a temperature
gradient between a heat source and the sample, and a time lag of
the freezing temperature recovery after supercooling hinders
accurate measurement. Therefore, it is highly desired that the
sample should be isolated from the container so that thermal
radiation from the samples alone could be studied.
Levitation techniques, in particular, electrostatic levitation
operating under high vacuum, can provide the desired solution.
The containerless environment given by the ESL allows controlling
the amount of supercooling of the molten sample by adjusting the
power of heating lasers. Unlike the contact method using a
crucible, the ESL technique offers a clear physical meaning of
supercooling, recalescence, and plateau which subsequently
accompany the release of latent heat of crystallization, and are
useful information to determine the standard temperature. In
addition, in a metrology standards view point, the secondary
thermophysical properties of molten material liquids at high
temperature are doubtful. Therefore more reliable thermophysical
properties (e.g., heat capacity, density, viscosity, surface tension,
emissivity, thermal conductivity, and fusion enthalpy) of molten
liquids can be obtained using ESL compared to other levitation
techniques. A vacuum ESL does not have any contamination from
the presence of gas, neither the convection induced either by an
induced current or a gas ow. The shape of the molten sample
being very close to that of a sphere, no complex analysis of the
measured quantities is necessary. For these specic reasons, the
Korea Research Institute of Standards and Science (KRISS) decided
to develop an electrostatic levitator, called Hi-Lite (High Temperature Levitation Instruments for Thermophysical Evaluation), for
the measurement of thermophysical properties for standards as
well as materials science at high temperatures.
Fig. 15. Schematic diagram of the electrostatic levitator in KRISS.
The facility built by KRISS is schematically described in Fig. 15.

This system is based on early developed models [10,15,47]
consisting in ve main parts, a vacuum chamber, electrodes and
high voltage ampliers, position and rotation control hardware,
charging and heating systems, and diagnostic tools for physical
properties measurement. Since the details of these ESL are
described in previous sections, emphasis is given here to the
particularities of the system.
The vacuum chamber, including the electrode system, is placed
on top of an optical table equipped with a vibration isolation device
and is operated under a typically 107 Torr vacuum using a turbo
pump. For levitating a sample (Fig. 16), x, y, and z positions are
initially determined by two position sensitive detectors and two
HeNe lasers (632 nm), located orthogonally to each other
(Fig. 14). The laser beams enter to the PSD located at opposite
sides. Once a set-position for the sample is decided, a high voltage
is applied to the top electrode using a high voltage amplier. In
addition, two pairs of electrodes are distributed around the bottom
electrode, to adjust the lateral positions of the levitating sample
with two high voltage ampliers. When the sample approaches the
set-position, the voltage applied to the top electrode is adjusted to
keep the sample at the set-position with a PID feedback control
(2 ms time interval). In this levitator, various shapes of electrodes
(disk, convex rod, and cylinder) are used depending on experiments. The basic shape used in KRISS is a convex rod (16 mm
diameter) for the top electrode, and a concave disk (30 mm
diameter) for the bottom electrode. The rotation control is identical
to that developed at JPL [27].
2.1.8. Northwestern Polytechnical University
Recently, a team at Northwestern Polytechnical University in
Xian, China developed an electrostatic levitator with a single-axis
feedback control system to achieve levitation of various types of
materials such as metals, inorganic materials, and polymers [73].
Fig. 16. A metallic sphere levitated at KRISS.
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13
The levitated sample is said to display satisfactory levitation

stability in both the vertical and the horizontal directions thanks to
the constraining force produced by spherical electrodes.
2.2. Charging strategy and levitation initiation [6,10]
Sample charging is a critical part of electrostatic positioning.
The amount of charge on the sample surface determines the
positioning force on the sample from a given electrostatic eld. In
order for the electrostatic positioning technique to be employed,
the physical processes that allow charges to accumulate on the
sample had to be identied. Three charging methods that are
relevant during different phases of processing have been
employed: capacitive, photoelectric and thermionic charging.
2.2.1. Capacitive charging [6,10]
Capacitive charging is employed for sample launching and
levitation at the beginning of each experiment prior to the use of the
other charging mechanisms. In capacitive charging, surface charge
on the sample increases as the top-electrode potential increases
until electrical contact with the bottom electrode is broken and the
sample is levitated. In order to make the charge polarity consistent
with that induced by the other charging methods, a positive charge is
induced by applying negative voltages on the top electrode. The
initial sample charge will remain unchanged only in the absence of
any discharging ions which may be produced by the sample and the
surrounding electrodes under strong UV irradiation. When several
charging mechanisms are acting simultaneously, sample charging
becomes a dynamic process.
2.2.2. Photoelectric emission charging [6,10]
Photoelectric charging induced by an appropriate UV source
will maintain a sufcient charge even in the presence of
neutralizing ions. Photoelectric emission arises from electron
excitation by radiation, usually within a depth that the radiation
can penetrate. Emission of a photoelectrically excited electron can
occur only if it possesses sufcient energy to reach the surface and
overcome the work function. The magnitude of sample charging
depends on the photoelectric yield, which is the number of emitted
electrons per absorbed photon. For most metals, emission is more
effective in the UV range (less than 400 nm). At photon energies of
several eV above threshold, the photoelectric yield from metals is
of the order of 104 electrons per photon. At photon energies 5
20 eV above threshold (corresponding to wavelengths in the
vacuum UV region), the yield increases to a maximum of about 0.1
electrons per photon which is attributed to emissions from the
bulk material deep inside the surface layer. Since maintaining a
high positive charge on the sample is the objective, it is desirable to
encourage high electron emission by the sample while discouraging electron emission by the electrodes. This explains why the
electrode material is chosen so that it has a higher work function
that the sample material.
2.2.3. Thermionic emission charging
The time required to bring samples of some materials into the
liquid state, for which characterization is intended, can take
several hours due to electrical charge loss occurring upon heating if
photoelectric effect charging alone is used [10,15]. To alleviate this
problem, NASDA/JAXA devised a procedure in which a sample,
resting on the pedestal, was heated with laser beams at the
temperature at which thermionic emission occurs (1500 K) [53].
The rate of thermal electron emission from a heated solid follows
the RichardsonDushman equation [74]:

f
Jf; T AT 2 exp
;
KT
where A 120 A=cm K2
(3)
Fig. 17. Laser beams conguration in the JAXA vacuum facility for sample levitation
initiation by thermionic effect and during levitation.
where k is the Boltzmann constant, T is the absolute temperature of

the material, and f is the effective work function. Although the
above equation represents a theoretical value and real materials
usually have lower values, J is a rapidly increasing function of
temperature and thermionic emission is the dominant charging
mechanism when the sample temperature exceeds 1500 K, even in
the presence of various discharging electrons and ions. To initiate
levitation, the sample, sitting on a pedestal was heated while
monitoring its temperature with the pyrometers. The sample was
heated with one beam (CO2 laser) whereas the two remaining
beams (CO2 lasers) converged at the location at which the sample
was going to be positioned after the launch (Fig. 17a). Once the
sample reached a temperature close to 1500 K, at which the
thermionic emission was sufcient to charge the sample, a high
voltage (about 24 kV) was applied between the two electrodes,
and the feedback control software was activated. A few seconds
later, the sample was launched into its normal levitation position.
The preheating laser beam was then redirected with a mirror on
the sample to ensure position stability and to increase the
temperature (Fig. 17b).
This method may result in contamination for some samples, in
particular for materials which melting temperature is close to that
at which thermionic emission occurs since the method implies
partial melting of the sample placed on the bottom electrode.
Therefore, if maximum supercooling of the liquid is sought, and to
guaranty homogeneous nucleation process, UV charging method is
preferable.
2.3. Heating
In the original JPL facility [10], sample heating was achieved
with a 1 kW UV-rich high pressure xenon arc lamp. The radiation
produced by the bulb was roughly collimated into a 5 cm
diameter beam by a parabolic reector at the back of the bulb
housing. The beam was then focused by a 7.5 cm focal length fused
quartz lens into a small spot in order to maximize the light ux on
the sample and to minimize shining UV light onto the electrode
that would generate photoelectrons competing against sample
charging. An iris in front of the xenon lamp was computer driven to
control the power delivered to the sample.
One hurdle with the use of a single radiation source, such as a
xenon arc lamp, is called the runaway discharging effect [15].
The intensities of the heating radiation and the charging radiation
are coupled because they come from the same source. As described
by Rulison et al. [15], adsorbed surface impurities evaporate as
cations as the sample is heated. Therefore, the sample requires
continuous recharging through ultraviolet radiation. In the single
source design, the only way to increase the intensity of the
ultraviolet radiation is to increase the arc lamp power, which
increases the rate of heating, causing a further loss of charge.
Because of this effect, some materials become very difcult if not
G Model

14
impossible to levitate and melt. To alleviate this problem, the

facility built by Space Systems Loral comprised a YAG laser source
in addition to a deuterium arc lamp [15]. The intensities of light
from those two sources were independently controllable and
runaway discharging could be avoided, enabling the study of a
wider range of materials. Another difculty that was dealt with
was the fact that a xenon arc lamp had a broadband spectral
emission. This implied that both the visible and infrared
wavelength regimes were ooded, thus, making optical diagnostics difcult. Measurements of emissivity and temperature could
only be done when the xenon lamp was off, that is, when the
sample was cooling. Again, the use of narrow and separate spectral
band light sources for charging and heating by the ESCAPES system
solved this issue [15].
As was previously seen, the use of laser for heating is
advantageous for several reasons. However, special care should
be taken to avoid the destabilizing effect of photon and evaporative
anisotropic induced forces [51] as to maintain good sample position
stability, especially when processing is done under vacuum.
Processing of such materials as Ti with a single laser beam led to
position instabilities so large as to terminate levitation. Therefore,
while observing the constraint of the chamber layout, multi-beam
heating conguration was implemented to the JAXA vacuum facility.
This conguration consisted in a attened tetrahedral laser heating
conguration [51]. Three focused beams (50 W each) of CO2 lasers
(10.6 mm emission) in a same plane, separated by 1208, hit the
specimen. In addition, the focused beam of a 500 W Nd:YAG laser
(1.064 mm) heated the sample from the top. Heating with the most
powerful laser along the vertical was the best conguration as the
strongest eld and the fastest feedback were also along this axis.
Besides the exceptional 3D sample position stability, this multibeam heating conguration helped to control sample rotation and
improved temperature homogeneity.
A true tetrahedral laser heating conguration was later
implemented by Caltech on the HTESL to enhance temperature
uniformity [75,76]. A thorough investigation of temperature
uniformity of an electrostatically levitated spherical sample was
carried out at Caltech for several beams heating conguration [76].
Not surprisingly, this theoretical and experimental study concluded that there was an enhanced temperature uniformity for samples
heated with four diffuse laser beams arranged in a tetrahedral
geometry. Specically, an enhancement factor of 50 in the
temperature uniformity was observed for a tetrahedral geometry
over a single focused beam. This improvement in temperature
uniformity substantially reduces Marangoni and gravity driven
convection and might even enable atomic diffusion measurements
in the supercooled liquid states of some materials [76]. Scientists at
KRISS also make the spot size of the heating laser larger than 1 mm,
but smaller than the sample size to optimize homogeneous
heating.
2.4. Sample rotation control
2.4.1. Importance of rotation control
In addition to sample position stability requirements, rotation
control capability is a must for a contactless processing facility
[27,28,76,77]. Sample rotation control is required during containerless materials processing to ensure accurate pyrometry readings,
to improve thermophysical property measurements (e.g., density,
surface tension, viscosity), and to ease the study of atomic
structure and dynamics by scattering of high energy particles.
Sample rotation is preferable during material processing since it
allows better sample temperature homogeneity, if the rotation axis
is perpendicular with that of the incoming heat. Rotation control is
also an advantage for fundamental studies (e.g., isotope separation
study, drop dynamics) or when synthesizing materials. It impacts
segregation of different density materials, facilitates the mixing of

liquids, eases ning in glass forming systems, and could eventually
be used to produce hollow spheres with optical applications.
Control of the rotation helps a sample to maintain a spherical
shape, or a sample deformed through centrifugal force to recover a
spherical shape. This in turn simplies the data analysis when
performing density or vapor pressure measurements from digitized images or when determining surface tension and viscosity
with the drop oscillation technique. In addition, control of rotation
can be utilized to measure the surface tension of highly viscous
materials for which the oscillation drop technique cannot be
employed [78]. However, sample deformation, induced instability,
induced sedimentation by centrifugal force, and non-hydrodynamically quiet drop conditions, to name but a few, could occur
due to excessive rotation. Even a low rotation rate could induce
non-negligible acceleration a as indicated by:
2
a 2p f r
(4)
where f is the rotation frequency and r the sample radius. From this
relationship, the radial acceleration normalized with the gravitational acceleration (g-level) at sea level as a function of rotation
frequency for samples of different diameters can be found. It
indicates that millimeter-size samples with a rotation rate as low
as 1 Hz would experience g-levels well over those of the
International Space Station [79]. Therefore the advantages of
microgravity environment would be completely spoiled. Experimental results presented by Professor R.K. Wunderlich (Ulm
University) at a seminar sponsored by the Japan Space Forum in
Tokyo, Japan, in 2002 dramatically showed that under certain
circumstances, electromagnetically levitated samples can be
deformed due to rotation occurring in microgravity. The reasons
of sample rotation, on the ground as well as in microgravity, are
multiple and depend on the levitation and heating schemes. In the
present case, a possible source of rotation is the slight misalignments of the heating laser beams. Therefore, the use of a rotation
control device is necessary not only for ground-based experimental work but also to take full advantage of the reduced gravity
conditions offered by an orbital platform such as the ISS.
2.4.2. Rotation control methods
Different approaches can be used to control rotation of levitated
samples. Their application depends on the processed material
(electrical conductor, insulator), the rapidity of desired implementation, the accuracy, and the processing environment (high
vacuum, pressurized atmosphere, rareed gas, etc.). Four schemes,
namely the rotating magnetic eld, the linear and angular photon
momentum transfer, and the ultrasonic pressure, are shortly
reviewed and discussed next.
2.4.2.1. Rotating magnetic eld. For electrical conductors, the use of
rotating magnetic elds is very attractive. Following earlier work
[27], four coils are used as a stator to generate a horizontal and
rotating magnetic eld (Fig. 17). Each of the coils is wound on a
glass spool with an insulated copper wire. The glass is used to
electrically insulate the spools from the proximity of the high
voltage electrode. A soft iron core is inserted in the spool to
increase the magnetic eld [27]. In JAXA vacuum facility, the coils
surrounded the lower electrode [80] to ease maintenance and to
lower the risk of arcing between the high voltage top electrode and
the coils. Plates of MacorTM further prevented any arcing and
protected the coil assembly from contact with an unsuccessfully
processed molten sample (Fig. 18).
The principle of this technique relies on that of the asynchronous induction motor, where a stator generates the magnetic eld
and where the rotor is the sample. If an ac voltage V at frequency vv
G Model

15
To show the capability of this method to control rotation, tests

were performed with a 2.1 mm diameter Zr sample (30.5 mg) [77].
The sample was rst heated, melted, and solidied to ensure
correct pyrometer setting. The sample was melted once more and
then brought to a xed temperature (1950 K). Once this was
achieved, the rotating magnetic eld technique (eld frequency
400 Hz, current > 0.3 A) was applied to bring the sample back to its
non-rotating state. As is shown in the photographs of Fig. 20, about
only 17 min were necessary to reach bifurcation state when the
sample shape changed to that of a tri-axial ellipsoidal (123 Hz)
from a non-rotating state (0 Hz). Successful control of sample
rotation was also achieved for several other metallic samples (e.g.,
Sn, liquid Si, Zr, V, Nb, Mo, Hf, Re, W) (Fig. 21).
Fig. 18. Side view of the rotation coils as implemented on the JPL high temperature
electrostatic levitator. A charged conducting sample can be rotated around the
vertical direction when a rotating eld is applied in the same direction [27].
is applied to a stator having a resistance RST and an inductance LST,

the torque t; experienced by the sample (the rotor in this case) is:
tM
vv V 2
R2ST
2 2
v LST
!
1
RSP

1v
vv
2.4.2.2. Linear photon momentum transfer [28]. The rotating

magnetic eld technique is very efcient for rotation control of
electrical conductors but an alternative method is required for
insulators or relatively poor electrical conductors. For a nonspherical sample, torque can be imparted whatever is the electrical
conductivity of the material by the momentum transfer from
reected or absorbed incoming photons at the surface of a sample.
If the sample is spherical, however, only materials that are opaque
to the incoming radiation of a light source could experience
rotation through linear momentum transfer by photon absorption.
As was explained in length elsewhere for a spherical sample
levitated in vacuum [28], if the photons of a laser source incident to
the sample surface are absorbed, the torque tL imparted to the
sample can be written as:
(5)
tL
4pr 2 LeT s SB T 4
c
(6)
where RSP and v are respectively the resistance and the rotation
frequency of the sample.
To generate the magnetic eld, a signal generator sent two
sinusoidal signals with a p/2 phase difference. Each of these signals
was amplied and sent to a control box that allowed the choice
between horizontal and vertical elds. The box also permitted to
select a clockwise or anti-clockwise eld rotation (Fig. 19).
As was experimentally determined [27], the applied torque
necessary to spin a 2.38 mm diameter sample at 200 Hz is around
2 1011 N m when the rotation frequency of the applied
magnetic eld is 400 Hz and the coil current is 0.2 A.
Accurate measurement of sample rotation frequency is important for accurate determination of torque induced to the levitated
sample. To measure the sample rotation frequency, the reection
of a low power (10 mW) HeNe laser beam impinging onto the
sample surface was detected by a silicon photodetector. The output
voltage of the detector was amplied and digitized to get a Fourier
power spectrum using a LabVIEWTM software package. Such a
power spectrum showed peaks at all harmonics of the sample
rotation frequency. In addition, the stroboscopic effects generated
by the television monitor helped to visually determine the
frequency at 30 Hz intervals.
Fig. 19. Block diagram of the electronic components that generate appropriate
electric currents to the coils to produce the desired magnetic eld necessary for
sample rotation [27].
Fig. 20. Photographs showing, from the side, a Zr sample being subject to a rotating
magnetic eld, from a static state up to bifurcation [77].
Reprinted with permission from P.-F. Paradis et al., J. Japan Soc. Microg. Appl. 20,
218225. Copyright 2003, Japan Society of Microgravity Application.
G Model

16
with the electrostatic facilities around the world on millimetersize samples would require time scales too long that would hinder
practical applications. Detailed calculations for electrostatic
levitation applications are presented in the literature [77].
2.4.2.3. Ultrasonic pressure. As was shown by Trinh [83], the
rotation of acoustically levitated sample under a pressurized
atmosphere is possible. The origin of the torque, as evidenced by
ow visualization, appears to be linked with steady acoustic
streaming ows induced by high intensity sound waves [84]. This
was made possible through small horizontal translation adjustments made either to a reector or a transducer relative to their
axially symmetric position. Although no relationship was given
between power and sample size, the rotation rate could be
controlled by varying the ultrasonic level while keeping the
reector and transducer displacement from symmetrical in a xed
position.
3. Materials processing and synthesis
3.1. Crystallization and vitrication
Fig. 21. Photographs showing, from the side, a Zr sample being subject to a linear
photon momentum transfer, from a static state all the way to bifurcation [77].
Reprinted with permission from P.-F. Paradis et al., J. Japan Soc. Microg. Appl. 20,
218225. Copyright 2003, Japan Society of Microgravity Application.
where r is the radius of the sample, L is the moment arm, eT is the

emissivity of the material, sSB is the StefanBoltzmann constant, T
is the sample temperature, and c is the speed of light. Although this
technique has been applied for now only for samples levitated in
high vacuum, it could in principle be applied for samples levitated
in pressurized environment as long as the generated torque
overcomes the drag torque. The main drawback of this technique is
the dependence of the torque on the incident number of photons
and hence on the power of the light source. That is, the material
shall be able to withstand the energy input from the light source.
To show the capability of this technique for rotation control,
specic tests were performed with a 2.1 mm diameter Zr sample
(30.5 mg) [77]. The sample was rst heated, melted, and solidied
to ensure correct pyrometer setting. The sample was melted once
more and then brought to 1950 K. Two of the three laser beams
were centered on the sample whereas the third beam was offset as
to yield a ca. 0.5 mm moment arm to induce rotation. Fig. 20 shows
a series of photographs taken in time from a non-rotation state
(t = 0 min) up to the bifurcation state (t = 46 min). Again, this
method of sample rotation control was successfully used for a
variety of metallic samples (e.g., Sn, liquid Si, Zr, V, Nb, Mo, Hf, Re,
W).
If rareed gas dynamics conditions were to prevail, radiometric
forces could also produce some torque by absorption followed by
local heating of the molecules surrounding the sample [81].
However, these conditions are difcult to meet with an electrostatic levitator due to the problem of electrical breakdown.
As was suggested by Poynting [82], transport and transfer of
angular momentum by a circularly polarized wave is possible.
However, the level of torque generated by lasers currently used
Both crystallization and vitrication are sensitively affected by

impurities (i.e., heterogeneous nucleation sites). Since electrostatic
levitation provides containerless environment with minimized
heterogeneous nucleation sites, phase transformations can be well
studied without contamination or other surface effects. Moreover,
because supercooled liquids can be easily obtained using ESL, a
direct study of the crystallization and the vitrication from
supercooled liquids can be undertaken, which cannot be achieved
with conventional contact methods. This allows understanding the
detailed phase transformation paths and helping in the discovery
of new metastable phases.
Pioneering crystallization experiments with electrostatic levitators were carried out by Rhim and Chung [85] that grew
lysozyme protein crystals. The containerless method provided
simple and clean growth environment. The simplicity came from
the fact that freely oating liquid drops adopted a spherical shape
due to the intrinsic surface tension and thus exposed the drop to
isotropic thermal transfer and vapor diffusion elds. A spherical
drop also yielded accurate determination of its size which in turn
related to the protein concentration level. This together with the
lack of physical contact with container walls, which could have
induced uncontrollable nucleation, eased the overall control of
protein saturation level [85].
In a high temperature investigation involving ESL, Lee and et al.
reported for the rst time that an icosahedral quasicrystal (iphase) could directly form from supercooled liquids on as-casted
TiZrNi alloy system [86]. The detailed crystallization paths of the
liquids were revealed by ESL experiments [87,88]. That is, the
supercooled liquid TiZrNi alloys with 21 at.% Ni show a two-step
recalescence event with 29 at.% Ti 45 at.% upon crystallization
(Fig. 22). The rst recalescence is the signal originating from the iphase formation, and the second one comes from the C14 Laves
phase. Both phases were identied by synchrotron X-ray diffraction study during each recalescence event (Fig. 23) [87]. This was a
very important observation which veries Franks hypothesis [89],
that is, icosahedral short range order (ISRO) as the local order of
liquid metals. This aspect will be discussed in details in Section 5.
The two-step recalescence often disappeared and showed just a
one-step recalescence event if the supercooling deepened (Fig. 24)
[90]. In other words, only the i-phase on TiZrNi alloys forms
from the supercooled liquids, but no C14 Laves phase. Since the
deep supercooling gives more volume fraction of the i-phase
during the recalescence, the latent heat may not be enough to
stimulate the nucleation of the C14 Laves phase. One interesting
G Model

17
Fig. 24. Temperature as a function of time for the free cooling of liquid
Ti39.5Zr39.5Ni21 in ESL. Double recalescence on small supercooling (a), and single
recalescence for i-phase from deeply supercooled liquid (b) [90].
Reprinted with permission from G.W. Lee et al., J. Acta Mater. 59, 49644973.
Copyright 2011, Elsevier.
Fig. 22. Two-step recalescence for alloys containing 21 at.% Ni and different Ti to Zr
ratio [87]. The formation of the i-phase occurs in (b)(d).
Reprinted with permission from G.W. Lee et al., Phys. Rev. B 72, 174107. Copyright
2005, American Physical Society.
Fig. 23. (a) Cooling curves for an electrostatically levitated Ti39.5Zr39.5Ni21 droplet
(2.5 mm diameter) as a function of temperature showing two recalescence events
(indicated by arrows). (b) X-ray diffraction patterns for the supercooled liquid
Ti39.5Zr39.5Ni21 at 1029 K, during the 1st recalescence to the i-phase, and during the
2nd recalescence to the C14 Laves phase [88].
Reprinted with permission from K.F. Kelton et al., Phys. Rev. Lett. 90, 195504.
Copyright 2003, American Physical Society.
fact from this result is the critical cooling rate for the formation of
the i-phase. As the supercooled liquid drops onto a Cu rod in the
ESL, the critical cooling rate of the i-phase formation for TiZrNi
alloys was estimated to be less than 100 K/s (Fig. 25) [90]. This
value is much smaller than that of other metastable quasicrystal
formation (>500 K/s) [91].
The critical cooling rate is particularly important in bulk
metallic glass (BMG) study, since it is a key parameter to determine
glass forming ability (GFA). For the determination of the critical
cooling rate, a temperature-time transformation (TTT) diagram
should be constructed. The construction of a TTT diagram is very
hard to achieve in conventional contact methods since it requires
that the supercooled liquid should be maintained at certain
temperatures. ESL has been used for the construction of such
diagrams for obtaining the critical cooling rates of BMG [9294].
For instance, Fig. 26 shows the TTT diagram for Pd40Cu30Ni10P20.
PdCuNiP, ZrTiNiCuBe (Vit 1), and ZrNbCuNiAl
exhibited critical cooling rates of 0.33 K/s [92], 2 K/s [93], and
1.5 K/s [94], respectively.
ESL raised a question for the GFA of BMG. In the conventional
contact methods, it is expected that the larger size BMG should
Fig. 25. Cooling curves of Ti37Zr42Ni21 after quenching from 758 8C onto a Cu rod.
The cooling rates for each region are shown [90].
Reprinted with permission from G.W. Lee et al., J Acta Mater. 59, 49644973.
G Model

18
Temperature (K)
2500
Tm
2000
1500
1000
Time (s)
Fig. 28. Typical cooling curve for an Y3Al5O12 sample (12.61 mg) (120 Hz sampling
rate) [98].
Fig. 26. Timetemperature-transformation (TTT) diagram for Pd40Cu30Ni10P20

(PCNP). The solid line describes a numerical t [92].
Reprinted with permission from J.F. Lofer et al., Appl. Phys. Lett. 77, 681683.
Copyright 2000, AIP Publishing LLC.
have the lower critical cooling rate. However, cooling experiments

with ESL revealed that this is not always true. It was reported that
the size of Zr62Cu20Ni8Al10 BMG increases with a small addition of
Ti. Therefore the slower cooling rate is expected on Zr57Ti5Cu20Ni8Al10. However, the cooling rate was similar with both BMGs.
Interestingly, the electrostatically levitated liquid with no Ti
(Zr62Cu20Ni8Al10) became glassy, whereas the melt with Ti
additions (Zr57Ti5Cu20Ni8Al10) showed crystallization (Fig. 27)
[95]. This reversed result was explained with surface crystallization induced by the container. That is, the liquid with no Ti might
be more affected by surface crystallization from the container on
as-casting. Therefore, small addition of Ti could depress the surface
crystallization. This reects the advantage of containerless
environment, since the container plays a role in heterogeneous
nucleation sites as well as a heat sink for thermal conduction.
Accordingly, the GFA of BMG is the result of the competition
between thermal conductivity and heterogeneous nucleation (or
surface crystallization) by a container.
In the oxide arena, vitrication of several aluminate and
silicate materials was achieved with electrostatic levitation.
Crystalline samples of 50%CaO50%Al2O3 [56,96], <1% mol Nd2O3
50%CaO50%Al2O3 [97], and Y3Al5O12 [98] compositions (2 mm

diameter) could be electrostatically levitated with JAXA pressurized
facility. The samples exhibited excellent position stability when
applying a 7.5 kV voltage between the electrodes. From the surface
changes (from spheroid to sphere) and pyrometer readings, the
samples were fully melted when irradiated with a laser power of less
than 50 W. The samples were heated to a temperature in excess of
2350 K. A representative temperature prole for an Y3Al5O12 sample
depicting an average radiative and conductive cooling rate of
245 K/s and subsequent vitrication from the supercooled state is
shown in Fig. 28. The absence of a recalescence peak indicates
sample vitrication. The recovered glass samples were smooth,
transparent, and spherical. Bubbles that were sometimes seen when
rst heating the solid polycrystalline sample could not be observed
by optical microscopy after vitrication. This suggests that ning
occurred through gas dissolution or by bubbles bursting at the
surface of the levitated drop.
Similar experiments were conducted in vacuum at the NASA
Marshall Space Flight Center. Glasses of Li2O2SiO2 (LS), and Ptdoped Li2O2SiO2 (0.001 wt%) (Pt-LS) compositions were melted,
cooled and reheated at controlled rates with an electrostatic
levitator furnace [99]. The experiments were carried out with
spherical, 2.53 mm diameter, glass samples. The measured critical
cooling rates leading to glass formation, for the processed LS and PtLS glasses, were 14 2 8C/min and 130 5 8C/min, respectively. The
same compositions processed with a crucible yielded to critical cooling
rates of 62 3 8C/min and 162 5 8C/min, respectively. The activation
energy for crystallization for the LS glass processed by levitation was
higher than that for an identical composition processed in a container.
From this, the authors of this study [99] suggested that the glass
forming ability for a containerless melt increases signicantly
compared to an identical melt in contact with a container. The absence
of heterogeneous nuclei coming from the walls of a container and
imbedded in the melts held in containers would explain the increased
glass forming tendency of the containerless melts.
3.2. Solidication studies
Fig. 27. Free radiation cooling curves for levitated (a) Zr57Ti5Cu20Ni8Al10 and (b)
Zr62Cu20Ni8Al10 alloys from the liquid to the solid phases. (b) Does not show a
recalescence, signaling glass formation, while (a) shows a recalescence near 790 K,
indicating crystallization [95].
Reprinted with permission from T.H. Kim et al., Appl. Phys. Lett. 87, 251924.
Several metals and semiconductors have been successfully

levitated, melted, cooled, supercooled, and solidied using vacuum
facilities around the world (e.g., [47,100]). The Mo sample
processed with electrostatic levitator showed a thermal dendritic
structure throughout the entire surface uniformly without any
apparent grain boundaries implying heterogeneous nucleation
must have been suppressed due to the containerless condition
[101]. The back reection Laue pattern also revealed the
homogeneity of the processed sample.
Spherical Nb single crystals could also be grown via containerless electrostatic levitation [102,103]. The processed samples
remained spherical without any macroscopic shape change by
solidication exhibiting a uniform dendritic surface morphology.
Crystallographic {1 1 1} planes exposed in equilateral triangular
G Model

shapes on the surface by preferential macroetching and spotty

back-reection Laue patterns conrmed the single crystal nature
of the processed samples [102,103]. No hysteresis in magnetization between zero eld and eld cooling also implies a clean
defect-free condition of the spherical Nb single crystals.
Fig. 29 is illustrated some representative thermal histories of
millimeter-size samples processed with the vacuum JAXA facility.
The solidication of a number of metallic alloys was also
investigated [107]. For example, utilizing the containerless
electrostatic levitation facility at NASA/MSFC, materials scientists
were able to supercool the Ni59Nb41 (atomic) alloy by 210 K which
was 1608 farther than the results of previous ight experiments
[108]. Supercoolings were clustered around 200 K during the
repeated meltingsolidication cycles on a single sample. Prior to
this work, a metastable liquid separation had been presumed to
limit the supercooling of this alloy. However, microstructural
observations have revealed that supercooling was limited by
crystal nucleation. Electrostatic levitators have also been specically used for the measurements of solidication kinetics, in
particular the growth velocity and the lifetime of metastable
phases [36]. Studies have been carried out for nucleation occurring
spontaneously and for nucleation intentionally induced with a dart
for metallic alloys [109,110] and silicon [111].
Besides elemental and alloyed metals, several compounds such
as bulk metallic glasses [52], 76%BaB2O424%Na2O [112], BaB2O4
[112], YIG [112], some slags [113], CaF2 [114], BiFeO3 [115], BaTiO3
[115], Al2O3 [116,117], and Nd2Fe14B [118] have been successfully
levitated, melted, cooled, supercooled, and solidied using either
pressurized or vacuum facilities.
The containerless solidication behavior of 2 mm diameter
Nd2Fe14B samples was studied at different cooling rates and the
effects of supercooling depth on the microstructure and magnetization were investigated [118]. For the sample solidied at the
lower supercooling level, the developed dendritic residual Fe and
Nd rich phases were found in the microstructure. For the sample
solidied with the highest supercooling level, the developed
dendritic Fe was suppressed and a ne microstructure was
obtained (average grain size of Nd2Fe14B: 24 mm). Furthermore,
the sample that experienced the deeper supercooling had a higher
magnetization than that of the sample processed with a lesser

degree of supercooling [118].
The solidication of barium titanate (BaTiO3) from deep
supercooled phases at different cooling rates was carried out with
the pressurized levitation furnace [115]. The material resulting
from containerless solidication was transparent and consisted of
micrometer-size particles and a single crystal phase exhibiting a
giant dielectric constant over 100,000 and weak temperature
dependence over the 300100 K range [119124].
3.3. Nucleation studies
Nucleation is a stochastic uctuation phenomenon of atoms or
molecules from which a new phase forms from a parent phase. For
the crystallization, atoms should be aggregated and form nuclei in
the supercooled liquid. If the energy of the nuclei overcome an
energy barrier (i.e., nucleation barrier), the nuclei become stable
and continuously grow. Here, the nucleation barrier is governed
two parameters; one is the crystal-liquid interfacial free energy
and the other is the volume Gibbs free energy. The nucleation
barrier is given as follows,
DG n
16p
s3
;
3 dm=v2
Is
6n 2=3 kB TNA
phTl
jdmj
6pkB Tn
1=2

DG n
exp
kB T
(8)
(b) 2800
2300
Tm
2200
2100
2000
1900
1800
2600
Tm
2400
- allotropic transition
2200
2000
1800
1600
1700
0 1 2 3 4 5 6 7 8 9 10111213
Time (s)
(c) 4000
Time (s)
(d) 4000
3500
Temprature (K)
Temperature (K)
(7)
where s, dm, and v are the interfacial free energy, the Gibbs free
energy difference between the initial and nal phases per atom, and
the average atomic volume v. The direct measurement of the
interfacial free energy is very difcult, since the interface is too small
to measure and because it is composed of only a few atomic layers.
Whenever a container is used to conne a liquid, the container
provides heterogeneous nucleation sites that the liquid cannot
deeply cool down. This complicates the analysis to obtain the
interfacial free energy using the classical homogeneous nucleation
theory (CNT). Electrostatic levitation can resolve the difculties,
since it provides a containerless environment. According to the CNT,
the homogeneous steady state nucleation rate is given by
Temperature (K)
Temperature (K)
(a) 2400
19
Tm
3000
2500
2000
Tm
3500
3000
2500
2000
1500
1500
4
6
Time (s)
10
Time (s)
Fig. 29. Thermal history of selected millimeter-size samples processed with JAXA vacuum levitation furnace: (a) Rh (Tm = 2236 K; 185 K/s average cooling rate, 184 K
supercooling) [104]; (b) Hf (Tm = 2504 K; 710 K/s average cooling rate, 285 K supercooling; ab allotropic transition) [105]; (c) Re (Tm = 3441 K; 1100 K/s average cooling
rate, 915 K supercooling) [106]; (d) W (Tm = 3695 K; 1820 K/s average cooling rate, 500 K supercooling) [48].
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20
Table 3
Interfacial free energies, a = s/DHf, work for critical cluster formation, and critical radius r* for the three phases (i, Laves, and b).
Phases
i-phase (Ti39.5Zr39.5Ni21)
C14 Laves (Ti40Zr30Ni30)
Solid solution phase (Ti49Zr49Ni2)
s (J/m2)
0.062 0.002
0.095 0.006
0.077 0.002
aLS
W*/kBTr
0.324 0.009
0.375 0.017
0.59 0.013
58.28 0.15
60.68 0.29
61.21 0.40
where h, l, n*, kB, NA and DG n are the viscosity, the average atomic
jump distance, the number of atoms in the critical nucleus, the
Boltzmanns constant, and the Avogadro number, respectively. For
the initiation of the crystallization from a supercooled liquid, at
least one critical size nucleus should form. This requires that the
number of the critical nuclei in the supercooled liquid with a given
liquid volume V, nucleation rate Is, and time tr, should be greater
than one, as follows [125]:
Is T r V t r
1
(9)
If all other thermophysical parameters in Eqs. (7)(9) can be

obtained, then the interfacial energy in Eq. (7) can be determined,
satisfying Eq. (9). Using this method, the interfacial free energy on
TiZrNi alloys showed a lower value for the i-phase than for
crystalline phases (Table 3) [86,87]. This appeared in the supercooling ability of the liquid alloy. Fig. 30 shows large supercooling
for the simple crystalline phase (bcc) whereas small supercooling
occurs for the i-phase) [87].
The physical meaning of the interfacial free energy or supercooling ability can be understood by Turnbulls coefcient a which
is given by
!
DScon fig bulk DScon fig inter face
s
N
a
i
(10)
DS f
DH f N
where Ni is the number of atoms in the interface, N is the number of
atoms in the crystal plane, DScong (bulk) is the congurational
entropy of the bulk system, DScong (interface) is the congurational
entropy of the interface, and DSf is the fusion entropy per atom.
Eq. (10) explains the similarity of local orders of liquids and
crystals. In other word, small interfacial free energy means similar
local orders of liquids and crystals, expecting smaller a. Indeed, a
smaller a, 0.324, was reported for the i-phase compared to those
for polytetrahedral and simple crystal, being 0.375 and 0.59
respectively, for TiZrNi alloys when using ESL [86,87], since the
local order on elemental liquids and alloy liquids was icosahedral
Fig. 30. Reduced supercooling for TiZrNi liquids as a function of Ni concentration

([Ti/Zr] = 1); the solid lines are a guide to the eye [87].
r* (A) (at Tr)
17.23 0.32
14.38 0.57
19.56 0.13
Used parameters
r (g/cm3)
Cp (J/mol-K)
DHf (kJ/mol)
5.712
5.448
5.884
44.24 1.54
42.45 3.78
33.57 1.65
8.48 0.40
11.2 0.42
6.12 0.13
(Table 2) [87,126129]. This is consistent with Holland-Moritzs

report using EML that the calculated a values were 0.34 for the i
phase, and 0.39 and 0.43 for the complex crystal phases l-Al13Fe4
and m-Al5Fe2, respectively [130]. According to Eq. (3-3-1), the
nucleation barrier should be smaller for the i-phase than that for
the polytetrahedral phase (C14 Laves phase) [86]. In Fig. 31, the iphase shows a lower nucleation barrier and a smaller critical
radius of the nucleus (r* = 2s/(dm/v)) compared to those of the
other two crystalline phases [87]. The smaller nucleation barrier or
interfacial free energy explained why the i-phase formed directly
from liquid rather than the stable C14 Laves phase [86,87].
The interfacial free energy can be changed by small additions
resulting in the congurational change. The small additions enforce
or undermine the stability of the SRO in liquid, affecting supercooling. Recently, small additions of Cu, Ag, Au, Pt, Pb, and Si on the
formation and stabilization of TiZrNi icosahedral quasicrystals (iphase) were studied. Among these elements, only the small addition
of Ag (24 at. %) signicantly improved the stability and formability
of the i-phase with small supercooling and long plateau of i-phase
formation, but without C14 Laves phase (Fig. 32) [131]. This was
explained that the proper atomic size ratio of Ag and Zr removed the
space frustration of the icosahedral clusters, and enhanced ISRO and
extended icosahedral short range order (ISRO) in the liquid, i.e.,
medium range order (MRO), thus reducing the interfacial free
energy. Hence, the i-phase in TiZrNiAg liquid alloy should easily
nucleate with smaller supercooling.
Fig. 31. (a) Calculated work for critical cluster formation and (b) critical radius for
nucleation of the three phases using Turnbulls driving free energy expression
(dm = DHf DT/Tm) [87].
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21
Since the heterogeneous nucleation sites were minimized using

ESL operated under high vacuum, the low interfacial free energy on
the quasicrystal alloys raised an important question about the
classical nucleation theory. That is, whether a clear distinction
between homogeneous and heterogeneous nucleation is possible,
or not [87]. This has yet to be claried.
As suggested by Skripov [132] a statistical approach is able to
provide further insight into the mechanism of crystal nucleation
from supercooled melts. When assuming that nucleation processes
are described by Poisson statistics, under non isothermal conditions (cooling rate dT/dt 6 0) the probability for nucleation in a
sample of volume V within the temperature interval between T and
T + dT is given by:
!
Z T S
VIS T
VI T
:exp
dT
v1; T dT dT
(11)
jdT=dtj
T I dT=dt
The analysis of the probability distribution function of
experimentally observed supercooling values allows to determine
the pre-exponential factor KV as well as the activation energy DG*
in the steady state nucleation rate function (Eq. (8)) [132]. By
means of a slightly modied statistical approach, Morton et al.
[133,134] investigated the nucleation and supercooling behavior
of Zr samples of different purity levels processed with an
electrostatic levitator at Space Systems Loral. These studies reveal
that the average supercooling, the pre-exponential factor, KV, and
the activation energy for nucleation, DG*, increase with increasing
purity of the samples. In a later work at DLR [68] even larger levels
of supercooling were reached for liquid Zr by electrostatic
levitation (Fig. 33). Interestingly, the observed supercoolings
Fig. 33. Probability distribution functions of supercoolings measured in 100

experiment cycles for pure Zr by electrostatic (right) and electromagnetic levitation
(left) [68]. The solid lines correspond to the probability distribution functions as
computed according to Eq. (11).
exceed the hypercooling limit (DThyp = DHf/DCp). When using

the electromagnetic levitation technique, signicantly lower
supercoolings were achieved (Fig. 33). The better supercoolability
achieved with the electrostatic levitator may be explained by the
cleaner environmental conditions during processing under vacuum in the ESL as compared to processing under He atmosphere in
the EML. The statistical analysis of the probability distribution
functions of the 100 measured supercoolings (Fig. 33) gives a preexponential factor as high as KV 1042 m3 s1 for the ESL
processing and a smaller value of KV 1025 m3 s1 for the EML
processing. While the former value of the pre-exponential factors
indicates that the measured maximum supercoolings obtained in
the ESL approaches the limit of supercoolability as given by the
onset of homogeneous nucleation, the EML value is indicative of a
heterogeneous nucleation mechanism [135]. The determined
value of the activation energy DG* = 75 kBT for the ESL experiments
corresponds to a Turnbull coefcient of a
0.61 that is close to the
prediction from the negentropic model by Spaepen [91] for a bcc
structure of abcc = 0.7.
3.4. Phase diagrams
Fig. 32. Timetemperature curves of Ti37Zr42Ni21 (a) and (Ti37Zr42Ni21)96Ag4 (b)

liquids [131].
Reprinted with permission from G.W. Lee et al., J. Alloy. Comp. 537, 171174.
Electrostatic levitation is a useful tool to build phase diagrams.

In general, the construction of phase diagram by annealing and
other thermal experiments such as differential thermal analysis
(DTA) or differential scanning calorimetry (DSC) is time consuming. In addition, contamination and/or reactivity of materials at
high temperature limit the phase diagram construction to low
temperatures. In this viewpoint, ESL provides quick and easy
measurements of solidus and liquidus temperatures for high
melting temperature materials and offers detailed phase transformation paths. Also, the microstructure of a material formed upon
cooling in ESL results solely from a pure sample, with no
contribution from container wall.
High temperature high vacuum electrostatic levitation was
used to determine the complete timetemperature-transformation (TTT) diagram of the Zr41.2Ti13.8Cu12.5Ni10.0Be22.5 bulk metallic
glass forming alloy in the supercooled liquid state [52]. This was
the rst report of experimental data on the crystallization kinetics
of a metallic system covering the entire temperature range of the
supercooled melt down to the glass transition temperature. The
measured TTT diagram exhibited the expected C shape. Existing
models that assume polymorphic crystallization cannot satisfactorily explain the experimentally obtained TTT diagram. This
originates from the complex crystallization mechanisms that occur
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22
Fig. 34. Temperature-time cooling curves for ESL-processed TiZrNi alloy liquids
for low Ni concentrations that nucleate b(Ti/Zr) as the primary crystallizing phase
[87].
in this bulk glass forming system, involving large composition

uctuations prior to crystallization as well as phase separation in
the supercooled liquid state below 800 K.
Another phase diagram study was carried out with ESL for Ti
ZrNi alloys. For example, Fig. 34 shows the sequent crystallization
on TiZrNi alloys on cooling: liquid ! b solid solution
phase ! C14 Laves phase. In this case, phase transformation
temperatures are determined on heating and cooling. If either the
solidus or the liquidus temperature is known, the other temperature can be determined by assuming the same emissivity
of the sample. The rst recalescence temperature for the phase
transformation decreases with Ni concentration, which reects a

lowering in liquidus temperature. A small plateau at near 750 8C in
Fig. 34(b) indicates the formation of a new phase (C14 Laves) as the
concentration of Ni increases [87].
The microstructure obtained by scanning electron microscope
(SEM) clearly shows that the C14 Laves phase is formed upon
cooling (Fig. 35(c)) [87,136]. From the ESL cooling curves and in
situ X-ray diffraction study on cooling in ESL, the primary and
secondary phases were determined [87]. All phases on TiZrNi
alloys that were determined by ESL, X-ray, SEM, DTA, and DSC are
shown in the pseudo-ternary phase diagram of Fig. 36 [87,90].
Recently the combination of the ESL technique with in situ
diffraction of synchrotron radiation has been utilized for the
assessment of the phase diagram of binary GdZr alloys at high
temperatures [137]. For example, Fig. 37 shows X-ray diffractograms of Gd35Zr65 at different temperatures between 1273 K and
1973 K that provided direct information on the phase equilibria.
Noteworthy is also the shift of the positions of the rst diffuse
maximum from the liquid phase and of the (1 1 0) reection of bcc
Zr(Gd) within the semi-solid regime. While the effect of thermal
expansion is negligible, these shifts are dominated by the
temperature dependence of the compositions of the liquid and
of the Zr(Gd) solid solution. Hence, analysis of the peak positions as
a function of temperature allows mapping of the solidus and the
liquidus line in the GdZr phase diagram [137].
3.5. Reduced-gravity processing
Originally developed for materials science in Earth orbit by
space agencies, a number of experiments were carried out to test
the hardware using aircraft or sounding rockets ying parabolic
trajectories that offered reduced gravity conditions. The rst of
such demonstration was made by JPL to show the capability of
electrostatic forces to position a large (1 cm diameter) liquid drop
in reduced gravity, that otherwise could not be realized on the
ground unless the surface tension of the liquid was extremely high
Fig. 35. (a) X-ray diffraction for low Ni concentrations showing a-solid solution (&) and C14 Laves phase (O). (b) SEM microstructures of Ti49Zr49Ni2. (c) C14 Laves phase
forms on Ti47.5Zr47.5Ni5, which corresponds to the small plateau near 750 8C in Fig. 33 (b) [87].
Reprinted with permission from G.W. Lee et al., Phys. Rev. B 72, 174107. Copyright 2005, American Physical Society.
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Fig. 36. Pseudo-binary phase diagram of TiZrNi alloys with equal ratio of Ti and
Zr. Maximum supercooling temperatures (+) are given from [87,90].
2005, American Physical Society; Reprinted with permission from G.W. Lee et al., J
Acta Mater. 59, 49644973. Copyright 2011, Elsevier.
23
One of the obvious advantages offered by a reduced gravity

environment is that the mass of the object can be substantially
increased since all the control voltage can be used to compensate
small g perturbations instead of levitating against the large
constant g force. Assuming a maximum acceleration perturbation
of 3 102 g within the KC-135, the maximum mass which the
electrostatic positioner could theoretically handle was approximately 5 g. Rhim et al. [6] reported that 3 g objects could be
successfully positioned during the KC-135 experiments. This
maximum limit could easily be extended to over 500 g if the
residual acceleration is signicantly reduced (e.g., 104 g).
The European Space Agency [4,23] also devised an experiment
to test an electrostatic positioning system by containerlessly
processing a Li-silicate glass sample. The crystallization and
demixing of such a glass composition is strongly inuenced by
the heterogeneous nucleation occurring at the crucible wall. It was
hoped that melting, supercooling, and resolidication under
containerless conditions would yield a glass with a better
homogeneity. A 8 mm diameter glass sample with a 24 mass%
Fig. 37. X-ray diffractograms of Gd35Zr65 at different temperatures. The positions of

the reections from the crystalline phases are marked by different symbols. The
dashed line indicates the position of the main diffuse maximum from the Gd(Zr)
liquid [137].
[6]. Experiments were carried out with a tetrahedral electrode

conguration using water as test material. The reduced gravity
environment was provided by the NASA KC-135 aircraft that ew a
series of parabolic arcs, each of which yielded approximately 25 s
of low gravity environment (102 g).
As soon as the zero-g portion of the parabola started, a known
amount of liquid was injected through a nozzle until a drop was
fully formed at its tip (Fig. 38). During this period, the drop was
gently pulled toward the top electrodes by applying +7 kV on each
of the top three electrodes while the bottom electrode and the
nozzle were at ground potential. This prevented the drop from
falling away from or breaking connection with the nozzle due to
small acceleration perturbations. Then, the electrode voltage was
suddenly increased to nearly +20 kV and the drop was fully
charged. Simultaneously, the nozzle was quickly retracted by a
solenoid. The increased repulsion and retraction of the nozzle
broke the charged drop free. The drop then moved toward into its
pre-set position under control of the servo system. Drops
composed of a liquid shell surrounding a gas core were also
successfully deployed and positioned during these experiments.
The sequence can be seen in the gure below.
Fig. 38. Pictures taken from a video camera taken during a successful zero-gravity
launching of a compound drop using the JPL tetrahedral positioner. It shows one of
the rst successful positioning of a compound liquid drop in reduced gravity. (a) A
dyed water drop with an air core is attached to the nozzle and resting on a velvet
pad, ready to be launched. (b) It is repelled from the nozzle with the application of
voltage under servo control. (c) The neck is being broken showing a Taylor cone. (d)
The compound drop is in the air and being held at the pre-set position [6].
Reprinted with permission from W.-K. Rhim et al., Rev. Sci. Instrum. 56, 307317.
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24
Li2O76 mass% SiO2 composition was doped with 0.1 m% of Co(II)oxide to increase its optical absorptivity [5,24]. The sample was
preheated to the transformation temperature prior to the launch.
Once in microgravity, it was released by a sample handling
mechanism and maintained in the focus of a heating mirror by the
electrostatic positioning system. By applying high voltages (from
3.5 to 5 kV) between the electrodes, the uncharged, polarized glass
sample was supposed be positioned. However, a misalignment of
one of the CCD camera used for position control occurred during
the launch. As a result, the electrodes were thus wrongly activated
and no proper positioning was achieved. The sample moved
irregularly between the electrodes and, therefore, being not always
in the mirror focus, it reached a temperature of only 500700 8C,
instead of the target 1150 8C, before it stuck to one of the
electrodes. The nuclei did not dissolve and phase separation
occurred. As shown in Fig. 39, the initially transparent blue sample
turned to blue opaque.
Containerless solidication of BiFeO3 has been carried out by
NASDA (JAXA) in microgravity with an electrostatic levitation
furnace on board a sounding rocket (TR-IA) [16]. The aim of this
experiment was to study the solidication behavior of oxide
insulator material in microgravity. A spherical BiFeO3 specimen
with a diameter of 5 mm was laser heated and solidied in an
oxygen and nitrogen mixture atmosphere. The microstructure
resulting from solidication in the levitation furnace was
compared with that obtained from solidication in a 10 m drop
tube and in crucibles [43]. In the crucible experiments, the
segregation of the primary Fe2O3 phase could not be suppressed,
even if the cooling speed increased to 5000 K/s. However it did
suppress in a 0.3 mm diameter droplet solidied in the drop tube
experiment. This suggests that containerless processing effectively
promoted the supercooling of the BiFeO3 phase although the
positioning system did not work as expected, therefore inducing
thermal gradient in the sample as it moved with respect to the
heating laser beams (Fig. 40). In the microgravity experiment,
although a homogeneous BiFeO3 phase was not observed in the
5 mm spherical specimen, an anomalous ne cellular microstructure appeared due to deep supercooling. In addition, the phase
transitions of BiFeO3 were measured by DTA from room
temperature to 1523 K and its liquidus temperature was estimated
to be 1423 K.
Following extensive ground-based research and development
in terms of position control system and thermophysical property
measurements, additional testing was carried out in reduced
gravity by JAXA with a dedicated facility [62]. Experiments were
done aboard the Mitsubishi MU-300 aircraft. During the parabolic
ight, stable positioning, laser heating and melting, cooling,
supercooling, and solidication of a Zr sample could be successfully completed.
Fig. 39. Photographs of the sample before (a) and after (b) processing in reduced
gravity.
Fig. 40. Laser power and temperature proles measured by pyrometry (a) and video
images illustrating the uctuating position of the sample during heating and
cooling while in reduced gravity (b) [16].
Reprinted with permission from S. Yoda et al., J. Japan Soc. Microg. Appl. 17, 7686.
4. Materials thermophysical property measurements

The knowledge of thermophysical properties and their temperature dependence is essential to improve industrial processes, to
support modeling efforts when designing new materials, and to
validate theoretical and empirical models in material sciences. In
particular, in discussing the nature and behavior of liquids, density
is a vital quantity. From a practical standpoint, density data
provide essential information for mass balance calculations in
rening operations and thermal natural convection phenomena in
furnaces, and help in compound design [138]. From a fundamental
point of view, knowledge of volume changes at the melting point is
of critical importance to understand solidication processes.
Moreover, the density of a liquid is needed in the description of
the radial distribution function from which other basic properties
such as surface tension and viscosity can be derived. Knowledge of
the surface tension is useful to optimize such processes as bubble
migration, rening, casting, and welding and provide fundamental
information for surface physics. The viscosity, or the resistance of a
liquid to sheer forces, is of great interest in both the theory and
technology of liquid behavior [138]. From a theoretical aspect,
viscosity is an indirect measure of the friction among atoms and
helps to evaluate diffusion, a basic property of liquids. From an
application perspective, viscosity plays an important role to
elucidate quantitatively problems in uid ow phenomena (e.g.,
rise of bubbles and inclusions in melts, casting) as well as those
related to the kinetics of reactions in industrial production [139].
Knowledge of viscosity is equally important to understand glass
formation [140], bers drawing [141], hypertension [142], and the
evolution of planetary cores [143]. Several elds of materials
science require knowledge of diffusion because it limits the rate of
G Model

heterogeneous reactions between reactants and because it also

limits impacts the distribution of solute elements during
solidication [138]. The measurements of specic heat of a liquid
allow determining other thermodynamic parameters such
as the enthalpy, entropy, and the Gibbs free energy [33,138].
Moreover, when measured in the supercooled region, these
quantities carry special implications for the studies of solidication
processes and for the selection of metastable phases of interest
[144,145].
Information of the emissivity of a material surface is a basic
prerequisite for both for accurate non-contact temperature
measurement and for heat transfer calculations, in particular for
estimating radiative power [138]. The emissivity is a thermophysical property difcult to handle because it depends on the
nature of a material, the temperature and roughness of its surface
as well as wavelength and angle. Electrical conductivity plays an
important role in materials processing operations such as rening,
electromagnetic stirring for melt cleanliness and microstructural
control, and the obvious need to evaluate the efciency of a
material to conduct electricity [138]. Electrical conductivity is an
important quantity that can be related to or electrical resistivity
and thermal conductivity. From a fundamental aspect, a measure
of the electrical conductivity provides an indication of the freely
moving electrons within a material. Vapor pressure is of
importance as it is intimately linked with the cohesive or binding
energy in a material [138]. Moreover, the temperature dependence
of the vapor pressure is of theoretical importance since the latent
heat, and hence the binding energy of the lattice can be obtained.
Besides it fundamental utility for thermodynamic calculation and
in understanding the atomic dynamic in the uppermost layers of a
material, vapor pressure data are necessary to improve such
industrial processes as pyrometallurgical production, rening, or
vapor deposition [79,138] and when designing materials for high
temperature applications.
Measuring the properties of materials in their solid phase at
temperatures near their melting point or in their liquid phase is
challenging with traditional methods using crucibles [138]. The
crucible is a source of contamination especially if the material
under investigation is corrosive, whether because of its chemical
characteristics or because of its melting point relative to that of
the crucible. In the case of highly refractory materials (e.g., W,
Re, Os), access to a suitable crucible if difcult. Contamination of
the sample under investigation leads to values of properties that
could be far from the true ones, especially surface tension, and
hinders the access to deep supercooled phases. Moreover, the
contact with a crucible generates thermal gradient and modify
the shape of a sample material due to surface tension forces
between the crucible and the molten sample. Departure from a
simple shape of the sample, like that of a sphere, adds challenges
to the whole data analysis. These reasons explain, for example,
why the density and surface tension data are so scarce and
mainly limited to the melting point and why no viscosity data
appear in the literature for elemental metals with melting point
above 2500 K.
The advent of electrostatic levitation and the development of
the associated non-contact diagnostics techniques over the last
three decades circumvented the above mentioned difculties
and allowed an accurate and quick determination of the
thermophysical properties of several materials, in particular
refractory metals, metallic alloys, and oxides, in their solid,
liquid, and supercooled phases over large temperature intervals.
In this section are presented the measurement methods and a
summary of the thermophysical property measurements taken
so far with electrostatic facilities (density, surface tension,
viscosity, self-diffusion, ratio of heat capacity over emissivity,
emissivity, electrical conductivity, and vapor pressure).
25
4.1. Density and thermal expansion

4.1.1. Measurement method
The measurement of the density of liquid drops in electrostatic
levitation has been originally reported by Chung et al. [30] who
have adapted a method previously developed by El Mehairy et al.
for electromagnetic levitation [146]. Once an electrostatically
levitated sample is melted, it takes a spherical shape due to surface
tension and the distribution of surface charge. The sample is
illuminated from behind with an intense spectrally broad light
source and the video images from a high resolution black and
white camera equipped with a telephoto objective are recorded
throughout the experiments [30]. Alternatively, the droplet can be
illuminated from the rear by an intense light source such that of a
cold-light source or a collimated laser [147151,77]. This gave a
close look at the sample, allowing sample perimeter and surface
features to be analyzed (Fig. 41).
The image of a non-rotating sample was then digitalized and
the sample area was readily obtained. Assuming that the sample
was axi-symmetric, the volume was found from this area, and,
because its mass was known, the density could be found by
dividing the mass by the volume. For this imaging method to allow
accurate density determination for a variety of materials (e.g., from
Sn to W), excellent illumination contrast has to be maintained
during all phases of processing [53], for a sample in its liquid phase
well above its melting temperature or for a sample at room
temperature. A spectrally broad light (white) source works well for
a large range of materials (e.g., Sn, Ti). However, when a sample
attains very high temperatures during an experiment (2000 K),
careful selection of the lamp was paramount to make sure that the
background lighting efciency did not change when the sample
cooled and solidied. A simple spectral analysis was performed to
optimize the contrast between the sample and the background
light over the whole temperature range over which data are
gathered. A temperature span of 15003500 K was selected as it
covered temperatures in excess of the melting points of all
refractory metals, including tungsten. In this analysis, the spectral
response of the camera and the spectral characteristics of both the
sample emission and those of the lighting source were considered.
Assuming that the sample behaved like a blackbody, the Wien
wavelength at 3500 K was found to be 827 nm whereas it dropped
to 2898 nm when the sample cooled to 1500 K. A quick analysis
shows that the blackbody radiation from the sample does not vary
much with temperature in the blue-ultraviolet range, especially
around 450 nm. Hence the spectral output of a UV lamp was well
suited for imaging a sample experiencing temperatures from
1500 K to 3500 K. For experiments involving refractory materials, a
high-pass lter at 450 nm was used in conjunction with a UV lamp.
Moreover, the response of a typical CCD camera was still very good
in that spectral range. By using this experimental arrangement, the
spectral characteristics of the sample, as seen by the camera, were
Fig. 41. Schematic of DLR optical setup for the measurement of the density with an
electrostatic levitator.
G Model

26
rather constant over a large span of temperature. Alignment,

collimation, and intensity of the UV lamp were also carefully
chosen not to induce any electron avalanche from the electrodes
from which levitation problems could otherwise arise.
The images are saved on the computer and after the
experiment, the video images are digitalized and the sample
radius is extracted from each image. Different procedures and
consistent fail proof algorithms have been suggested for recognition of the edge of the drop to derive accurate volume
determination [30,147,148]. Edge points are t with the spherical
harmonic functions through 6th order Legendre polynomials and
the volume is found following optimization of the Legendre
polynomials [30,147]. Because the edge detection also identies
the laser specular reections (e.g., position sensing lasers) seen on
the images, an improved procedure has recently been suggested by
DLR [147]. This step involves recursive tting of the edge curve by a
model function.
The images are then matched with the temperature data of the
sample. To avoid the ill-effect of evaporation or to speed up the
data measurements, the heat source is then blocked with
mechanical shutters allowing the sample to cool. Since the mass
of the sample is known and because its volume is calculated from
the digitization procedure, density can be found as a function of
temperature by simply dividing the mass by the volume. The
recorded images are calibrated by levitating a steel sphere with a

precisely known radius [151] under identical conditions.
This technique is applied for samples levitated under vacuum as
well as under pressurized conditions. In these measurements, the
uncertainty is typically estimated to be less than 2% from the
resolution of the video grabbing capability and from the
uncertainty in mass measurement [53]. Optical microscopy and
electron probe microanalysis are generally performed after the
experiments to ensure that voids or oxide or nitride layers were not
present on the surface or in the bulk of the solidied samples.
4.1.2. Experimental results
The density of several materials (metals, semiconductors,
insulators) could be measured over very wide temperature ranges,
in their solid state and also in their liquid state, well above the
melting temperature as well as much below the melting
temperature, in their supercooled state. Several of these measurements constitute the rsts to be reported that cover a large
temperature span in the liquid phase and that included a large
temperature incursion into the supercooled region. Representative
results for liquid and supercooled Si [77], W [48], Ir [152], and
BaTiO3 [115] are presented in Fig. 42.
Fig. 42 highlights the capability of the levitation scheme to offer
measurements over very wide temperature ranges. Also, it is
Fig. 42. Typical measurements for the density obtained with electrostatic levitation coupled with an imaging technique: (a) Si [77].
Reprinted with permission from P.-F. Paradis et al., J. Japan Soc. Microg. Appl. 20, 218225. Copyright 2003, Japan Society of Microgravity Application; (b) W [48]: (c) Ir [152];
and (d) BaTiO3 [115].
G Model

Table 4
Some measured density data of molten metals and semiconductors.
Element
Tm (K)
Ce
La
Pr
Nd
Au
Gd
Tb
Si
Ni
Y
Pd
Ti
1072
1191
1204
1294
1337
1586
1629
1683
1728
1796
1828
1941
Pt
Zr
2041
2128
V
Rh
B
Hf
Ru
Ir
2183
2237
2360
2504
2607
2719
Nb
Mo
Ta
2750
2896
3290
Os
Re
3306
3441
3695
Density r
Reference
r(Tm)
(103 kg/m3)
dr/dT
(kg/m3 K1)
6.41
6.00
6.50
6.59
17.4
7.41
7.84
2.55
7.89
4.15
10.66
4.21
4.17
19.2
6.34
6.21
5.46
10.82
2.17
11.82
10.75
19.87
19.5
7.73
9.11
14.75
15.0
19.10
18.65
18.4
16.43
0.83
0.39
0.51
0.57
1.44
0.46
0.47
0.65
0.21
0.77
0.51
0.22
0.96
0.15
0.27
0.49
0.76
0.25
0.55
0.56
0.71
0.85
0.39
0.60
0.85
0.41
1.16
0.79
0.91
1.08
27
Table 5
Measured density data of molten oxide materials [97,98,115,116].
Composition
Tm (K)
Density r
3
[156]
[157]
[157]
[157]
[158]
[159]
[160]
[77,153]
[161]
[162]
[163]
[164]
[165]
[166,167]
[32]
[168]
[169]
[104]
[170]
[105]
[171]
[171]
[152]
[172]
[173]
[171]
[106]
[175]
[106]
[174]
[48,176,177]
important to point out that the entire data taking process is carried
out over a very short period (a few seconds). Not only does this
ensure that the impact of evaporation is minimized, but this also
permits several data to be acquired in a single day, thus giving the
opportunity to validate reproducibility. Except for the quadratic
behavior exhibited by Si (agrees with [153]), the linear dependence
with temperature of the metals compares well with the theoretical
works of Reynolds [154] and Steinberg [155]. Most of the data
measured so far with electrostatic levitation combined with the
imaging technique are summarized in Table 4 [32,48,104
106,77,153,156177].
At the melting point, the values agrees generally very well with
those with those measured by other techniques (e.g., drop weight
technique in vacuum, the isobaric expansion method, the pendent
drop method, the sessile drop method, and, in some case,
aerodynamic or electromagnetic levitation coupled with imaging)
when respective experimental uncertainties are taken into
account. The discrepancy observed between the results (values
at the melting temperature as well as temperature coefcients)
obtained with electrostatic levitation and other techniques could
be attributed to the difference in processing techniques and the
extent to which evaporation losses have been considered. The
containerless approach in high vacuum offered by electrostatic
levitation, isolated the samples from container walls and gases,
whereas the other methods often implies possible chemical
reactions between the highly reactive molten materials and a
crucible, a support, or residual gases. This can alter the nal density
values. Other possible sources of error could arise from the imaging
technique, in particular the focusing of the sample, the digitization
of the image, and the measurements of sample mass. Material
purity, oxygen solubility in the samples, gasication, surface
oxidation or nitridation and level of vacuum could also, to some
extent, explain the discrepancies. Temperature measurements too
BiFeO3
Nd-CA
BaTiO3
YAG
Al2O3
1363
1878
1893
2240
2327
Reference
3
r(Tm) (10 kg/m )
dr/dT (kg/m K)
6.74
2.83
4.04
4.08
2.93
1.31
0.21
0.34
0.29
0.12
[115]
[97]
[115]
[98]
[116]
are subject to errors. However, emissivity data are scarce,

especially for refractory metals above their melting temperature,
and, to our knowledge, have not been reported for supercooled
materials. The interested reader is invited to consult the cited
literature for a full presentation of the data of each material, for the
complete comparison with the data, when available, obtained with
conventional methods.
Other than simple elements, the specic volume or density of
metallic alloys (e.g., [178,179]), quasi-crystals [180], bulk metallic
glasses [181,182], clathrate [183], and slags [113] have been
measured. Table 5 presents the density and temperature coefcient for some molten oxides.
A substantial emphasis was also given on binary ZrNi liquid
alloys and data of their molar volume have been reported by
Ohsaka et al. [184]. In their work, four different alloy compositions
have been studied: Ni50Zr50, Ni36Zr64, Ni33.33Zr66.66, and Ni24Zr76.
As a function of temperature T, the molar volume V(T) is
represented by the following a linear law,
VT V L 1 aT T m
(12)
where a is the thermal expansion coefcient and VL is the molar

volume at liquidus temperature TL. The results for the molar
volume and the density are summarized in the Table 6.
The experiments performed in DLR with both electrostatic and
electromagnetic levitation could conrm the data for Ni50Zr50,
Ni36Zr36, and Ni24Zr76. Among these, only the results for Ni36Zr36
have been published up to now [69]. A comparison with the data of
Ohsaka is given in table 6 and is illustrated in Fig. 43. The numerical
deviation between different runs as well as from the data of Ohsaka
is less than 0.2%, which lies within the respective experimental
uncertainties (Fig. 43).
Fig. 43. Density of liquid Zr64Ni36 versus temperature measured by DLR using
electrostatic levitation [69,150]. The solid and hollow symbols, respectively,
correspond to two different runs with individually prepared samples. For
comparison, the measurement of Ohsaka is shown by the dashed line [179].
G Model

28
Table 6
Parameters for the molar volume and density of liquid ZrNi binary alloys measured using the electrostatic levitation technique.
Alloy
TL (K)
VL (cm3/mol)
a (105/K)
r(TL) (g/cm3)
dr/dT (104 g/cm3/K)
Reference
Ni50Zr50
Ni36Zr64
Ni36Zr64
Ni33.33Zr66.66
Ni24Zr76
1533
1283
1283
1393
1233
10.49
11.53
11.56
9.64
12.01
5.58
5.18
5.42
4.39
5.51
7.15
6.90
6.88
8.34
6.95
3.99
3.57
3.73
3.66
3.83
[184]
[184]
[69]
[184]
[184]
In Table 6, the molar volume of Ni33.33Zr66.66 [184] is

signicantly lower than those of Ni36Zr64 and Ni24Zr76, although
its composition is in between. Normally, only small changes of the
density occur with a variation of the composition [185]. The
authors conclude that this unusual behavior could be a sign of an
extraordinary chemical short-range order in the liquid at this
composition. They support their conclusion by the fact that, in the
solid, Ni33.33Zr66.66 corresponds to an intermetallic phase.
4.2. Surface tension
The surface tension of an electrostatically levitated specimen of
material was determined by the oscillation drop technique [29], a
method in which the frequency of the oscillation of a molten
sample about its equilibrium shape was measured [186]. This
method was attractive as it allowed measurements not only for the
liquid state above the melting temperature but also for the
metastable state of supercooled melts. To measure the surface
tension using this method, a sample was rst heated, melted, and
brought to a selected temperature, while closely ensuring excellent
Fig. 44. Schematic description of the electrode conguration by which a drop

oscillation can be induced.
position stability, low sample rotation, and sample sphericity. In

case the shape of a droplet was not spherical (due to excessive
rotation), a counter torque was applied either with a magnetic eld
or by appropriately steering the beams of the heating lasers to
restore the spherical shape.
To excite the drop oscillations, an AC voltage amplier was
inserted between the bottom electrode and the electric ground
as schematically shown in Fig. 44 for the JPL HTESL. As usual, the
top electrode was connected to a high voltage amplier for
levitation control. The electrode assembly, being axially symmetric, could effectively excite even modes in which the n = 2
mode was the lowest mode. The oscillating amplitude of a drop
was detected using the drop-amplitude detection system shown
in Fig. 45. The levitated drop was back lit by a collimated laser
beam to create a drop shadow on a circular photodetector. The
drop shadow was masked from the detector except for a narrow
monochromator slit so that the detected signal was sensitive to
the oscillating drop amplitude. A narrow band interference lter
at the illumination laser wavelength was placed in front of the
detector to reject stray light. When dealing with a volatile
sample material, the sample has to be weighted before and after
the experiment, and the actual sample mass at the time of data
taking can be closely estimated using the thermal history during
the experiment and the temperature dependence of the vapor
pressure of the material.
In a typical experiment, a P2(cos u)-mode drop oscillation was
induced to the sample by superimposing a small sinusoidal electric
eld on the levitation eld. The transient signal which followed the
termination of the excitation eld was detected and analyzed using
software. A typical signal of the decay of the oscillation is shown in
Fig. 46. This was done many times for a given temperature and
repeated for several temperatures. Using the characteristic
oscillation frequency vc of this signal, which was calculated by
a fast Fourier transform and then corrected for non-uniform
surface charge distribution [187], the surface tension s could be
found from the following equation [188,189],
v2c
8s
ro3 r
"
1
Q2
64p2 ro3 seo
!#
1 Fs ; q; e
Fig. 45. Schematic description of the detection system used for measuring the amplitude of deformation of a levitated sample.
(13)
G Model
Amplitude (arbitrary units)
29
6000
4000
2000
0
-2000
0.2
0.4
0.6
0.8
-4000
-6000
Time (s)
Fig. 46. Typical transient oscillation of a levitated metallic drop.
where
Fs ; q; e
243:31s 2 63:14q2 s 1:54q4 e2

176s 3 120q2 s 2 27s q4 2q6
(14)
and ro is the radius of the sample when it assumed a spherical

shape, r is the liquid density, Q is the drop charge, eo is the
permittivity of vacuum, and q and e are dened by
q2
Q2
16p2 ro3 eo
(15)
and
e2 E2 r o eo
(16)
respectively, with E being the applied electric eld. From Eq. (13), it
can be noticed that the surface tension depends on the sample
radius and density. For density, the data obtained with the imaging
technique (see Section 4.1.1) is substituted in Eq. (13). Also, to
ensure that the measured properties were not distorted by sample
evaporation, the radius variation was monitored in real time using
the imaging technique instead of relying solely on a measurement
of the mass of the sample before and after the experiment.
During the experiments, the video images from a highresolution camera were recorded (Fig. 47). After the experiment,
each value of the radius at each oscillation was obtained by image
analysis. This procedure eliminated the measurement error due to
sample evaporation. Moreover, the aspect ratio of the sample (ratio
between the horizontal and vertical radii) was also calculated to
evaluate the experimental error induced by sample rotation.
While measuring surface tension, the liquid sample was
intentionally rotated to suppress the excitation of oscillation
modes other than the P2 (cos u)-mode. On the other hand, the
characteristic oscillation frequency vc and the decay time t were
dependent on the rotation rate of the liquid sample V, by the
following equations [188,189]:
Dvc 19 V
21 vc
vc
2
"
2 #
1
1
2 V
1
3 vc
t Dt t
(17)
(18)
where Dvc and Dt are deviations of the characteristic oscillation

frequency and decay time due to the rotation, respectively.
Unfortunately, rotation rate measurements used for the solid
sample were not applicable for the liquid sample because of its
shiny surface and sphericity. Instead, the rotation rates of the
liquid sample were estimated by monitoring the aspect ratio of the
sample. Theoretical predictions of the liquid drop shape of rotating
Fig. 47. Typical transient oscillation of a levitated metallic drop.
drops have been advanced to a high degree of accuracy by Brown

and Scriven [190], and Rhim and Ishikawa [78] have conrmed that
the liquid drops which are levitated and rotated in electrostatic
levitators followed the predictions. Based on the predictions,
relations between the aspect ratios of rotating liquid drops and
rotation rates can be expressed by

2
Rhorizontal
V
V
1 1:476 102
1:2532
Rvertical
vc
vc
3
4
V
V
1:7877
3:7385
:
vc
vc
(19)
Using Eqs. (16)(18), relations between the aspect ratio and
Dvc or Dt can be estimated. According to Rhim et al. [78], if the

aspect ratio of a rotating sample is less than 1.02, the reduced
sample rotation rate (V/vc) is less than 0.13 and effects of the
sample rotation to both the characteristic oscillation frequency
and the decay time should be no greater than 1.5%. During
experiments, it is therefore preferable to monitor the aspect ratio
of a levitated sample so that it does not exceed 1.02. The
uncertainty of the measurements with this technique was
estimated to be better than 5% from the response of the oscillation
detector and from the density measurements.
Instead of using the drop oscillation, the surface tension can be
measured by monitoring the shape evolution of rotating drops
G Model

30
(b)
2320
2300
2280
2260
2240
2220
2200
2400
Tm
2500
2600
2700
2800
Surface Tension (mN/m)
(a) 2340
2700
2600
2500
2400
2300
Tm
2200
3300 3400 3500 3600 3700 3800
2800
Temperature (K)
(d)
3000
2800
2600
2400
2200
Tm
2000
3200 3300 3400 3500 3600 3700
Temperature (K)
(c)
Temperature (K)
750
700
650
600
Tm
550
2100 2200 2300 2400 2500 2600
Temperature (K)
Fig. 48. Typical measurements for the surface tension obtained with electrostatic levitation: (a) Ru [170]; (b) W [48]: (c) Os [175]; and (d) Al2O3 [117].
[190]. The validity of this surface tension measurement technique,

originally proposed by Elleman et al. [191] was experimentally
veried by Rhim et al. [78]. This technique offers an alternative
technique for those liquids where the drop oscillation technique
cannot be used. As a demonstration, the technique was applied to a
glass-forming alloy (Zr41.2Ti13.8 Cu12.5Ni10.0Be22.5) and its surface
tension was measured down to the lower temperature where the
drop oscillation technique could not be applied due to its high
viscosity.
The surface tension could be measured over large temperature
ranges, well above the melting temperature and down into the
supercooled region. As depicted in Fig. 48 for several materials (Ru
[170], W [48,176,177], Os [175], and Al2O3 [117]), the surface
tension exhibited a linear behavior as a function of temperature.
A non-exhaustive list of the surface tension data measured over
the years is presented in Table 7 [32,48,49,100,104,105,152,156,
157,159,160,165,166,170,175177,194199]. At the melting
point, the values obtained by electrostatic levitation show
remarkable agreement with most published values when respective experimental uncertainties are considered [192] and the
temperature coefcients compare generally well with those
calculated by Allen [193].
The discrepancy observed between the results (values at the
melting temperature as well as temperature coefcients) obtained
with electrostatic levitation and other techniques could be
explained by the fact that the containerless approach in high
vacuum offered by electrostatic levitation, isolated the samples
from container walls and gases, whereas the other methods often
implies possible chemical reactions between the highly reactive
molten materials and a crucible, a support, or residual gases. This
can contaminate the sample and drastically impact the surface
tension. Other possible sources of error or contamination could
arise from the material purity, oxygen solubility in the samples,
gasication, surface oxidation or nitridation, and level of vacuum.
Again, temperature measurements are also subject to errors.
Detailed data presentation and analysis could be found in the cited
literature.
It is interesting to note that by using the density data at the

2=3
2=3
melting point, the T m =Vm factor (Vm being the quotient of the
molar mass over density) could be calculated and, together with
the surface tension values at the melting point, shows excellent
agreement with the empirical relation proposed by Reynolds et al.
Table 7
Measured surface tension data of metals and semiconductors.
Element
Tm (K)
Surface tension g
g(Tm)
Ce
La
Pr
Nd
Gd
Tb
1072
1191
1204
1294
1586
1629
Y
Ti
1796
1941
Pt
Zr
2041
2128
V
Rh
2183
2237
B
Hf
2360
2504
Ru
2607
Ir
Nb
2719
2750
Mo
Ta
Os
Re
W
2896
3290
3306
3441
3695
Reference
(103 N m1)
dg/dT
(103 N m1 K1)
751
752
777
754
822
893
866
804
1557
1555
1800
1459
1500
1935
1940
1925
1060
1614
1612
2256
2269
2241
1937
1967
2290
2154
2480
2710
2477
0.07
0.056
0.052
0.095
0.097
0.096
0.11
0.05
0.16
0.18
0.14
0.244
0.11
0.27
0.30
0.28
0.067
0.10
0.11
0.24
0.27
0.16
0.20
0.17
0.26
0.21
0.34
0.23
0.31
[156]
[157]
[157]
[157]
[159]
[160]
[100]
[162]
[194]
[195]
[165,166]
[32]
[194]
[196]
[104]
[195]
[197]
[105]
[195]
[170]
[195]
[152]
[194]
[195]
[198]
[199]
[170]
[49]
[48,176,177]
G Model

31
Table 8
Measured surface tension data of oxides [117,195].
Composition
Tm (K)
Surface tension g
g(Tm) (10
Al2O3
BaTiO3
2327
1893
3
Nm
640
349
4.3. Viscosity
The viscosity was determined by the drop oscillation method by
measuring the decay time of the surface oscillation of the levitated
sample [29]. In this method, a sample was molten and brought to a
selected temperature. During the sample heating, electric currents
were applied to four coils to rotate the sample about the vertical
axis at a rate of around 5 Hz. The liquid sample was intentionally
rotated to suppress the excitation of oscillation modes other than
the P2cos(u)-mode. This amount of sample rotation stabilized the
rotation axis and helped eliminate the measurement error due to
the random rotation of the sample. The rotating magnetic eld was
removed before viscosity measurements were carried out. Then, a
P2cos(u)-mode of drop oscillation was induced in the sample by
superimposing a small sinusoidal electric eld on the levitation
eld. An oscillation detection system, illustrated in Fig. 45,
measured the uctuation of the vertical diameter of the molten
sample with a 4096 Hz sampling frequency. The transient signal
that followed the termination of the excitation eld was already
shown in Fig. 46.
This signal was analyzed using an in-house written LabVIEWTM
program, and the characteristic oscillation frequency vc and decay
time t were obtained. This was done many times for a given
temperature and repeated for several temperatures. Using the decay
time t given by the signal, the viscosity h can be found by [201]
rro2
5t
Reference
)
dg/dT (10
0.082
0.03
[154]. From all the data for the refractory materials, it seems
remarkable that other than their very high melting temperatures,
the magnitude of their properties or the behavior of their
temperature dependence are not signicantly different from those
of lower melting point materials, even when compared with
mercury at 300 K.
The surface tension of some molten oxide materials is
presented in Table 8 together with the temperature coefcient.
1
3
Nm
1
1
)
[117]
[200]
Sometimes, it suppresses the sample oscillation whereas sometimes it promotes the oscillation. This introduces a large
experimental uncertainty in the decay time, and the measured
viscosity values contain large experimental errors. In order to
minimize this effect, it is important to select the sample size and
the position control parameters so that the control frequency does
not overlap with the characteristic oscillation frequencies of the
sample. In early measurements, the position control frequency
range was DC to 360 Hz (720 Hz sampling rate) which overlapped
the sample oscillation frequency (150300 Hz) and introduced
large experimental uncertainties. In recent experiments, the
position control frequency range was reduced from DC to
120 Hz (240 Hz sampling rate). Another improvement was
recently made with regard to oxidization of the sample. It was
noticed during the viscosity measurements of rare earth metals
that the sample surface tended to be oxidized near the melting
temperature which resulted in erroneous data. In order to monitor
the oxygen partial pressure, a quadruple mass spectrometer was
attached to the chamber and conrmed that the oxygen partial
pressure was no larger than 2 106 Pa [50,202]. Also, the surface
of the levitated sample was monitored by a camera to conrm that
the surface was clean and that no sample oxidization occurred.
Samples of several elements (titanium, nickel, zirconium,
niobium, ruthenium, rhodium, hafnium, iridium, platinum, and
terbium) were weighed and melted into spheroids using an arc
melting furnace. The samples were weighed again and samples of
proper size were selected so that the characteristic oscillation
frequencies were above 160 Hz. The purities of the samples, their
mass and the frequency ranges of their characteristic oscillations
are shown in Table 9.
(20)
where ro is the radius of the sample when a spherical shape is

assumed and r is the liquid density. Similarly, using the
characteristic oscillation frequency vc given by the same signal,
the surface tension g could be found from the following equation
[29]:
v2c 8grro3
(21)
The viscosity measurements with the oscillating drop technique assume that the levitated droplet is free from any external
forces. However, in order to levitate a sample against gravity, a
strong electric eld is applied. Moreover, since a high speed
feedback position control is applied, viscosity measurements with
electrostatic levitators are conducted under strong electric elds
with DC and AC components.
The effect of this position control force on the viscosity
measurements was studied and is summarized in Fig. 49 [50,202].
When the frequency range of the sample position control overlaps
with the characteristic oscillation frequency of the molten sample,
the sample positioning force interacts with the sample oscillation.
Fig. 49. Conceptual drawing showing how to avoid the effect of sample positioning
force in the viscosity measurement using the oscillating drop method: (a) relation
between position control frequency and sample oscillation frequency from DC to
360 Hz frequency range, (b) relation between position control frequency and
sample oscillation frequency from DC to 240 Hz [202].
G Model

32
Table 9
Purity, size and typical characteristic oscillation frequencies of the samples
[50,202].
Material
Purity (%)
Sample size (mg)
Characteristic oscillation
frequency (Hz)
Ti
Ni
Zr
Nb
Ru
Rh
Hf
Ir
Pt
Tb
99.9
99.997
99.5
99.9
99.9
99.9
97
99.9
99.98
99.9
1322
3037
3442
2627
3032
3638
3639
2830
3031, 5354
2325
245355
195220
166187
246250
245258
202213
183192
253262
224228, 165166
167174
Another technique was proposed by Ohsaka et al. [203] that

could determine the viscosity of highly viscous liquids, particularly, supercooled liquids that exist at temperatures below their
freezing points. The technique involves levitation of a liquid drop
using an ultrasonic standing wave, and elongation of the drop by
rotating it beyond the point of bifurcation. The elongated drop is
then allowed to come back to its original shape by surface tension
driven relaxation. The time-dependent shape parameters of the
relaxing drop is related to the viscosity through a relaxation model.
This technique has not been used so far with electrostatic levitators
but does show promise.
Similarly, it is worth noting that a method for determining the
creep of materials at high temperatures has been developed and
implemented with the electrostatic levitator at NASA-MSFC [204].
The method was successfully used at temperatures up to 2600 K. It
exploits the change of mechanical stress within a rotating sphere
to determine the stress dependence of the creep rate in a single test
instead of the several tests necessary with conventional techniques
[36].
The viscosity could be measured over large ranges of
temperatures, well above the melting temperature and down into
(b) 15
Viscosity (mPa.s)
Viscosity (mPa.s)
(a) 10
the supercooled region. Representative data for several materials

(Gb [160], W [205], Mo [198], and B [197]) obtained with
electrostatic levitators combined with the oscillating drop
technique are depicted in Fig. 50. The temperature dependence
of the viscosity exhibited an Arrhenius behavior for all measured
metals.
Prior to investigations with electrostatic levitators, the viscosity
data were extremely scarce, sometimes inexistent, and besides Zr,
were limited to the melting point. The ESL data nonetheless
compare well with the scarce data appearing in the literature when
experimental uncertainties are considered. Furthermore, even
when no data are available for comparison with conventional
techniques (e.g., for elements with melting temperatures above
2500 K) the ESL data at Tm generally agree well with the values
calculated by Andrade [206].
As far as the temperature dependence of viscosity is concerned,
one of the biggest concerns on the measurements with containerless processing is the solubility of residual gases (oxygen or
nitrogen). The presence of residual oxygen and nitrogen is virtually
unavoidable in the chamber and the high solubility tendency of
some refractory metals could alter the data. Another concern is the
effect of positioning force to the viscosity measurement. Even
though the levitation procedures were improved to minimize the
effect [197,198] the levitated sample cannot be free from the
external forces under terrestrial conditions. A non-exhaustive list
of the viscosity data measured over the years for several materials
is presented in Table 10 [32,49,104,152,156,157,159,160,166
168,171,172,175,193199,205]. At the melting point, the values
obtained by electrostatic levitation agree with most published
values when respective experimental uncertainties are considered
[192,193].
The viscosity of some molten oxide materials is presented in
Table 11 [117,200] together with the Arrhenius tting coefcients.
Measurements of viscosity and is also required when investigating the dynamics in Zr-based bulk metallic glass forming
systems. However, the use of classical methods, such as the
oscillating cup method [207,208], is a real challenge to measure the
viscosity of chemically reactive liquid metals or alloys at high
temperature. Containerless techniques circumvent this issue and
electromagnetic levitation is a prominent method but is plagued
6
4
2
12
Tm
6
3
Tm
0
3300 3400 3500 3600 3700 3800
Temprature (K)
0
1550 1600 1650 1700 1750 1800 1850
Temperature (K)
9
7
5
3
Tm
1
2600 2700 2800 2900 3000 3100
Temperature (K)
Viscosity (mPa.s)
(d) 7
(c)
Viscosity (mPa.s)
6
5
4
3
2
1
0
2300
Tm
2400
2500
Temperature (K)
2600
Fig. 50. Typical measurements for the viscosity obtained with electrostatic levitation: (a) Gb [159]; (b) W [205]; (c) Mo [198]; and (d) B [197].
G Model

33
Table 10
Measured viscosity data of metals and semiconductors.
Element
Viscosity h
Tm (K)
h(Tm) (10
Ce
La
Pr
Nd
Gd
Tb
1072
1191
1204
1294
1586
1629
Y
Ti
1796
1941
Pt
2041
Zr
2128
V
Rh
2183
2237
B
Hf
2360
2504
Ru
2607
Ir
2719
Nb
2750
Mo
Ta
Os
Re
W
2896
3290
3306
3441
3695
a
b
3
Reference
Pa s)
3.31
2.75
2.82
5.07
4.9
5.3
12.0
3.6
3.3
4.4
7.1
4.82
4.7
4.7
4.83
4.3
4.9
2.9
2.8
7.1
5.2
5.0
6.1
6.0
7.0
5.0
4.5
5.6
8.6
4.2
7.9
6.9
Note
h = h0exp(E/RT)
h0 (103 Pa s)
E (103 J/mol)
0.012
0.381
1.38
0.43
1.7
1.399
0.583
0.00287
0.61
0.033
1.72
0.25
0.37
0.76
50.5
19.6
7.14
26.5
14
18.2
41
106.5
27.0
76.6
22.8
49.9
44.8
31.8
1.23
1.31
0.09
[156]
[157]
[157]
[157]
[159]
[193]
[160]
[162]
[193]
[171]
[193]
[166,167]
[193]
[168]
[32]
[194]
[193]
[104]
[197]
[195]
[105]
[195]
[171]
[195]
[152,172]
[195]
[172]
[198]
[199]
[175]
[49]
[205]
22.7
24.7
64.3
0.84
0.50
0.47
0.60
0.59
1.85
1.05
0.55
0.27
0.004
0.0017
0.08
0.11
44.4
48.7
51.2
49.8
52.2
30.0
35.5
48.9
73.0
213
220
133
128
a
a
a
a
b
a
Improved procedure.
It can hardly t the Arrhenius function.
Table 11
Measured viscosity data of oxides.
Composition
Tm (K)
Viscosity h
Reference
h(Tm) (mPa s)
Al2O3
BiTiO3
2327
1893
h = h0exp(E/RT)
30
15
with strong turbulent ows that are induced inside the molten
drop and hinder viscosity measurements on the ground [209,210].
It is therefore obvious that it is a strong advantage of electrostatic
levitation that containerless viscosity measurements are possible
within certain limits [150]. Viscosity data on binary ZrNi alloys
have been published by Ohsaka et al. [184]. Their results can be
represented by an Arrhenius equation with activation energy for
viscous ow E and a pre-exponential factor h1. They are
summarized in the following table (Table 12).
As described in Section 4.3.1, a high resolution-high speed
camera is used in DLR for determination of the time dependent
radius signal Rz(t) after the P2cos(u) mode has been excited. The
camera has a resolution of 480 500 pixels and records images
with a frame rate of 2000 Hz [150]. The use of a high-speed camera
allows to collect 1020 data points per oscillation and to determine
the vertical radius Rz(t) with a precision of better than 1%. For an
entire viscosity measurement, the duration of an experimental run
is roughly 15 min. An example of a measured R(t) curve is shown in
Fig. 51 for a liquid Zr64Ni36 sample at 1182 K. As shown by Becker
h0 (mPa s)
E (kJ/mol)
3.2
0.53
43.2
53.5
[117]
[200]
[211], Lambs law is only fullled when the dissipation of energy

due to the excitation of the vortex ow in the bulk can be
neglected. This is the case if the oscillation amplitude is smaller
than 10% of the radius at rest.
Fig. 52 shows the results for the viscosity as function of
temperature. Values were obtained in the broad temperature
range of 10501750 K. Large supercoolings of up to 230 K were
achieved. At liquidus temperature, TL, the viscosity is 11.5 mPa s. It
reaches a value of approximately 130 mPa s for T 1100 K which
is large compared to most non-glassforming metallic alloys [212].
Table 12
Arrhenius constants for the viscosities of liquid binary ZrNi alloys [184].
Alloy
TL (K)
h (mPa s)
E (kJ/mol)
Ni50Zr50
Ni36Zr64
Ni33.33Zr66.66
Ni24Zr76
1533
1283
1393
1233
0.105
0.0028
0.065
0.0025
63.0
95.8
67.0
90.7
G Model

34
Fig. 51. Measured vertical radius as function of time (symbols) for a liquid Zr64Ni36
sample at 1182 K. The dots represent the experimental data and the solid line
represents a t of a damped sine curve [69].
each sample mass within the above mentioned 5% scatter.

Systematic errors, due to non-linear droplet oscillations can,
therefore, be excluded.
In Ref. [69], a comparison with the Ni-self diffusion data
obtained from quasielastic neutron scattering experiments (see
Section 5.2.2) has been performed to validate the StokesEinstein
relation [213]. It is a striking observation that when tting both the
viscosity and the Ni self-diffusion datasets with a VogelFulcher
Tamman (VFT) law, the same value for the activation energy is
yielded, but with an opposite sign. This means, that the product of
the D and h as function of temperature is constant. This is in strong
disagreement with the StokesEinstein relation according to
which it should be proportional to kBT (Fig. 53). Such a behavior
has meanwhile been observed in other systems as well. The
clarication of the specic reasons for is subject of current research
[214].
In conclusion, the use of electrostatic levitation allows to
precisely measuring data over a broad temperature range and the
quality and range of the obtained experimental data allow
establishing a new relation between viscosity and the selfdiffusion in the case of Zr64Ni36.
4.4. Ratio of heat capacity to emissivity
For T > TL, h assumes values between 11.5 mPa s and 8 mPa s. In
Fig. 52, the data are shown together with the viscosities reported
by Ohsaka et al. [184]. For T < TL, there is an agreement within 5%.
For T > TL, however, the two curves signicantly deviate from each
other. This deviation increases with an increase of temperature. At
1500 K, the viscosity reported by [184] is about 30% smaller. To
exclude the possibility that this discrepancy could be caused by a
systematic error in the data, due to some non-linear effect in the
surface oscillation, the experiment was performed in DLR with ve
samples having masses of 20.8 mg, 27.0 mg, 38.2 mg, 41.0 mg, and
86.2 mg [69].
Such a non-linear effect could originate, for instance, from an
excitation of ow vortices in the bulk of the droplet when the
oscillation amplitude is too large [206]. Or, as described in Section
4.3.1, from an interference of the surface oscillation by the
positioning controller [50] which would also lead to an apparently
increased viscosity. In case that such a non-linear effect existed in
the droplet oscillation, the use of samples with different masses
would result in apparently different values of the viscosity. As
illustrated in Fig. 51, however, the same curve, h(T), is obtained for
where m is the sample mass, M is the molar mass, Cp is the constant

pressure molar heat capacity, eT is the hemispherical total
emissivity, A is the sample area, s is the StefanBoltzmann
constant, and T and Tamb are, respectively, the sample and ambient
temperatures. This allows determining the quotient of constant
pressure heat capacity over hemispherical total emissivity (Cp/eT)
of a material sample electrostatically levitated. The radiance
temperature was measured by the pyrometers and was calibrated
to true temperature using the known melting temperature of the
Fig. 52. Viscosity of liquid Ni36Zr64 versus temperature. Solid symbols represent
data measured by Brillo et al. [69] and the open symbols are data from Ohsaka et al.
[184]. The dashed line is an Arrhenius-t and the solid line is a VogelFulcher
Tamman (VFT) t.
Fig. 53. Product of Ni self-diffusion coefcient and the viscosity versus temperature
(symbols) [69]. The solid line is a linear t with zero slope and the dashed line shows
the StokesEinstein (SE) relation.

Since the electrostatic scheme does not input any heat, a high
temperature sample experienced pure radiative cooling when the
heating sources (laser beams or discharge lamps) are blocked and
the resulting energy equation governing the cooling process
reduces to [33]:

mC p dT
4
eT As T 4 Tamb
(22)
dt
M
G Model

35
Table 13
Measured ratio of constant pressure heat capacity over hemispherical total emissivity for some metals.
Metal
Tm (K)
Cp/eT(Tm) (J/mol K)
d(Cp/eT(Tm))/dT (mJ/mol K/K)
Reference
Ti
Zr
1941
2128
3.21
V
Rh
Hf
Ru
Ir
Nb
Mo
2183
2237
2504
2607
2719
2750
2896
45.5
132.28
139.4
150.4
184.0
133.1
179.3
159.5
134.4
159.8
[164]
[32]
[168]
[169]
[104]
[105]
[171]
[171]
[172]
[173]
8.49
8.0
3.15
5.5
5.28
sample. Calibration to true temperature was performed using

custom-made software. After the sample started to cool, both the
image and the cooling curve data could be used to measure the
ratio of constant pressure heat capacity and hemispherical total
emissivity. The recorded video images were digitized and matched
to the cooling curve and the area was extracted from each image.
The ratio of constant pressure heat capacity and hemispherical
total emissivity could be determined from Eq. (21) since all
parameters were known, and since the area was found from the
images and dT/dt from the cooling curve.
The ratio of constant pressure heat capacity over hemispherical
total emissivity of several materials (metals, semiconductors,
insulators) could be measured over very wide temperature ranges,
in their solid state and also in their liquid state, well above the
melting temperature as well as much below the melting
temperature, in their supercooled state (Table 13). Representative
results for liquid and supercooled Ru [170] and for solid, liquid, and
supercooled Nb [172] are presented in Fig. 54.
In addition, the latent heat of fusion can be determined by
adding the enthalpy contributions of the supercooled liquid to that
of the isothermal region following recalescence. The entropy of
fusion DS could then be found using the value of the enthalpy of
fusion DH and the relationship DS = DH/DTm.
The method presented here has the merit of providing the ratio
of constant pressure heat capacity over hemispherical total
emissivity over very large temperature range. However, limitations occur because the knowledge of either the isobaric heat
capacity or the hemispherical total emissivity is needed to obtain
the other thermodynamic parameter. The direct measurement of
these quantities is very challenging and explains why the data are
so scarce. Techniques to directly measure the hemispherical total
emissivity are currently being developed and are introduced
below.
(b) 250
(J/mol.K)
190
180
200
Solid
150
Liquid
170
160
150
2100

The emissivity measurement concept consists in measuring the
spectral intensity of the emission coming from a levitated sample
and to compare it with that from blackbody. From this, the spectral
emissivity can be calculated. This technique is widely used and was
combined with other containerless method including cold crucible
[215] and electromagnetic levitation [216]. Fig. 55 illustrates the
emissivity measurement system developed at JAXA [217,218]. The
system consisted of a multi-channel photo detector spectrophotometer (MCPD), which covered the wavelengths ranging from
700 nm to 1000 nm, a Fourier transform infrared (FTIR) spectrometer that covered from 1.1 to 6 mm, and a blackbody furnace. A
similar system has also been reported elsewhere [219] for use with
the NASA-MSFC electrostatic levitator.
Since the electrostatically levitated sample was smaller than
those of electromagnetic or cold crucible, the intensity of light from
the sample was also smaller. In order to get a good signal to noise
ratio, the measurement system had to be as simple as possible to
eliminate the error source. Therefore, it was decided to put the FTIR
spectrometer on a round table, so that it can observe the light
source (levitated sample or blackbody) without any mirrors. A
camera with a telephoto lens was used with the FTIR spectrometer
to check the sample position to ensure a correct optical alignment.
As for the spectrophotometer, a glass ber was used to guide the
light to the spectrometer. Bafes were inserted in the chamber to
eliminate the unnecessary reection. CaF2 windows were used to
maximize the transmission over the observation wavelength.
Two detectors were used for the FTIR spectrometer. An
extended InGaAs detector covered the 1.12.6 mm spectral band
while a HgZnCdTe detector covered the 3.36 mm range. Experiments were performed sequentially with each detector. The
measurement range of the spectrophotometer (7001000 nm) was
determined to avoid the effects of light sources other than the
Cp
Cp
(J/mol.K)
(a) 200
4.5. Emissivity
2300
2500
2700
Temperature (K)
100
Tm
Tm
2900
50
1600
2000
2400
2800
3200
Temperature (K)
Fig. 54. Ratio of constant pressure heat capacity over hemispherical total emissivity for: (a) liquid and supercooled Ru [170] and (b) for solid, liquid, and supercooled Nb [172].
G Model

36
spectral emissivity over all wavelengths such as:

R
eT
Fig. 55. Spectral emissivity measurement system combined with an electrostatic

levitator [217]: setup conguration during levitation experiment, calibration of the
FTIR spectrometer and calibration of the MCPD spectrophotometer.
sample, such that the position sensing lasers (532 nm and 645 nm)
and the UV light (385 nm).
After the levitation experiment, the FTIR spectrometer and the
spectrophotometer were oriented toward the blackbody furnace
for calibration (Fig. 55). The blackbody furnace was equipped with
a simulated chamber wall with an observation window. A pinhole
was set in front of the blackbody to mimic a levitated sample. The
temperatures of the blackbody were changed from 1473 K to
1773 K with 50 K interval to get the radiation intensity of
blackbody as a function of temperature. The translation functions
from spectrometer signals to the radiation intensity of light were
calculated using the calibration data obtained with the blackbody.
Then, the data of levitation experiment were converted to the
radiation intensity of the sample Is.
The emissivity is the ratio of the energy radiated by a particular
material to the energy radiated by a blackbody at the same
temperature. The radiation intensity from a blackbody IB depends on
wavelength l, temperature T, and Is depends on l, T, and direction of
radiation, u The directional spectral emissivity is dened as [220]
el; u; T
Is l; u; T
IB l; T
eRlIB l; Tdl

IB l; Tdl
R l2
l1
elIB l; Tdl
R l2
l1 IB l; Tdl
R l2
l IS l; Tdl
R l1
2
l1 I B l; Tdl
(25)

Fig. 56 shows the measured spectral hemispherical emissivity
of molten zirconium at its melting temperature [217], together
with the reported data by other researchers [221225]. While our
data covered a wide wavelength range, previous works covered
mainly the visible to the near-infrared region. Our data around the
visible wavelength were around 1419% higher than those
obtained by Cezairlyan et al. by the pulse heating method with
a six-color pyrometer [222] and 3040% higher than those
reported by Krishnan et al. using an ellipsometer in conjunction
with electromagnetic levitation [223]. However, all three data
showed a negative dependence on wavelength, while Hiernaut
et al. [225] reported that the spectral emissivity of zirconium was
independent of the wavelength. No reference data could be found
for wavelengths higher than 1 mm.
Fig. 57 is shown the radiation intensity of molten zirconium at
the melting temperature [217]. It can be noticed that the radiation
intensity reaches a maximum at around 1.4 mm and that the
Fig. 56. Spectral hemispherical emissivity of molten zirconium at its melting

temperature [217].
(23)
where u is the polar angle measured from the normal to the surface
of a sample. The radiation intensity from a blackbody IB is given by
Plancks law of radiation as follows [215]:
IB
2C 1
l5 expC 2 =lT 1
(24)
where C1 and C2 are Plancks rst and second constants,

respectively, 5.96 1017 W m2 sr1 and 1.44 102 mK. Integration of Eq. (21) over all direction gives hemispherical spectral
emissivity. The merit of electrostatic levitation is that the levitated
molten sample is spherical which yields isotropic radiation.
Therefore, the measured spectral emissivity from the spherical
sample is homogeneous at any direction, which means that the
measured emissivity with the electrostatic levitator should equal
to the hemispherical spectral emissivity. The hemispherical total
emissivity eT can be calculated by integrating the hemispherical
Fig. 57. Spectral hemispherical emissivity of molten zirconium at its melting

temperature [217].
G Model

37
This equation shows that when the AC current I1 is kept

constant, the induced torque is inversely proportional to the
resistance of the rotor (sample). Electrical resistivity rel can be
calculated by comparing the torque at certain rotating frequency
(which means vs = constant), with that of a reference material
(whose electrical resistivity is rel,ref) at the same rotating frequency
by the following equation
rel
t re f rel;re f
t
(29)
The torque applied on the levitated sample of mass M, density r,

and radius r can be calculated as:
2
5
t Mr2
Fig. 58. Total hemispherical emissivity for molten zirconium as a function of

temperature [217].
radiation intensities for wavelengths less than 700 nm and for

wavelengths higher than 6 mm were negligibly small, which
conrmed that the selection of wavelength interval (from 700 nm
to 6 mm) was reasonable.
The eT data are shown in Fig. 58 together with the literature data
[33,226]. All the data were obtained using electrostatic levitators.
Rulison et al. [33] calculated eT and Cp by borrowing the value of heat
of fusion [227], while Sung et al. [33,226] used Cp from JANAF [228].
The data obtained with the new technique agree well with the
literature data and eT exhibited a slightly positive temperature
dependence.
4.6. Electrical conductivity
The measurement technique of the electrical resistivity applied
to the electrostatic levitator utilizes the principle of the
asynchronous induction motor by introducing a rotating magnetic
eld to the levitated sample [229]. As explained in Section 2, the
lower electrode was surrounded by four coils that generated a
rotating magnetic eld [230]. Four sinusoidal signals (400 Hz)
whose phases were shifted by 908 were fed to these coils to
generate a rotating magnetic eld with vertical axis. Those phases
could be controllable so that the sample spin direction could be
selected, clockwise (CW) or counter clockwise (CCW).
The basic principle of the sample rotation mechanism is
essentially the same as that of the asynchronous induction motor.
The four-coil assembly works as the stator while the levitated
sample acts as the rotor (Fig. 19).
According to the principle of the induction motor, if an AC current
I1 at frequency vs is applied to a stator, the torque t experienced by
the rotor (having its own resistance R2 and inductance L2, which is
rotating at instantaneous frequency v), is given by
!
sR2
2
t I1 2 2 2
(26)
R2 s L2
dv 8p 5 dv
rr
dt
15
dt
(30)
Eq. (29) implicitly assumes that the sample size and the
distance between the sample and coils are kept constant. However,
it is impossible to make the sample sizes exactly the same as that of
a reference sample. The relations between the sample size and
induced torque could be derived from the work by Braunbek [231].
According to his calculation, the torque t induced on a spherical
sample (radius r, electrical resistivity rel) by a rotating magnetic
eld (intensity H, rotation rate vs) can be calculated from:
t/
p 1
vs r5 H2
4 rel
(31)
which indicates that the induced torque is proportional to r5. With

Eqs. (29) and (30), the sample radius r can be eliminated and the
electrical resistivity can be calculated by the following simple
equation:
dv C vs H2
dt
rrel
(32)
where C is a constant. Eq. (31) indicates that the angular

acceleration of the sample is related to its density and electrical
resistivity. Since vs and H can be easily kept constant, electrical
resistivity can be calculated with a reference sample by:
rre f dv=dtre f
rel
rel;re f
rdv=dt
(33)
Recently, Rustan et al. [31] developed a new non-contact

technique for measuring the electrical resistivity and magnetic
susceptibility of electrostatically levitated high temperature
liquids and solids. Their method combines a tunnel diode oscillator
with an electrostatic levitation furnace to perform noncontact
measurements on millimeter-size spherical samples. The circuit of
the oscillator was inductively coupled to the sample, and changes
in the electrical resistivity and magnetic susceptibility of the
sample could be found by measuring the oscillator frequency as a
function of sample temperature. The validity of their technique
was demonstrated by performing measurements on solid spheres
of pure zirconium and low-carbon steel. Although absolute values
of the resistivity were not determined, the temperature dependence of the resistivity of Zr was measured over the 6401770 K
range and agreed well with literature data. For the low-carbon
steel sample, the ferromagnetic-paramagnetic transition was
clearly observable [31].
where
s
vs v
vs
If s2 L22 is negligibly small, Eq. (25) can be rewritten as:

1
v
t I12
1
R2
vs
(27)
(28)

As a rst step, the electrical resistivity of solid zirconium at high
temperature was measured. Since the sample was heated by lasers,
photon pressure could, depending upon the laser beams alignment, induced a torque to the sample in addition to that generated
by the rotating magnetic eld. To take this effect into account,
frequency measurements were conducted twice, once with a CW
G Model

Fig. 59. Electrical resistivity of Zr as a function of temperature measured with

electrostatic levitation. Data available from the literature are superimposed for
comparison [229].
rotating magnetic eld, and once with a CCW rotating magnetic

eld. Because the direction of the torque induced by the photon
pressure is constant, its effect could be estimated by checking the
difference between the dv/dt in the CW direction and that in the
CCW direction. Fig. 59 illustrates the measured electrical resistivity
as a function of temperature [229]. Data available from the
literature were superimposed on the same gure for comparison.
Generally, our data showed very good agreements with literature
values.
4.7. Vapor pressure
The measurement of the vapor pressure of materials at
temperatures below their melting point does not generally pose
any particular difculties when the modied Knudsen or Langmuir
methods are used. However, the necessity of a chemically inert
container clearly emerges as the temperature of investigation is
above the melting temperature [232]. Reaction of the molten
sample with the crucible leads to melt contamination that changes
the evaporation dynamic and thus alters the measurements of the
vapor pressure with respect to temperature. Moreover, the
crucible is often source of impurities that induce heterogeneous
nucleation in the melt and that hinder the measurement on
supercooled materials. An additional difculty met by conventional techniques is in minimizing temperature gradients in a
sample [232]. For these reasons, it is difcult and sometimes
impossible to apply these techniques to refractory materials,
especially for measurements in their liquid or supercooled phases.
For example, Carpenter et al. [233] reported that the Knudsen
method could not be applied for titanium at high temperature
(Tm = 1943 K [78]), since a non-reactive crucible could not be
found.
Because of its capability to handle and maintain reactive and
high vapor pressure material in their liquid and supercooled
phases, electrostatic levitation furnace was attractive to measure
the vapor pressure [234]. The direct approach of measuring the
sample mass before and after processing (from which the number
of atoms evaporated per unit time could be known) was considered
but was not adopted for two reasons. Although a sample could be
levitated and brought to the liquid state in few minutes, the
temperature prole during the launch initiation sequence was
rather complex and not accurately known since the pyrometer was
adjusted for sample levitation height. Furthermore, this technique
would not cover accurately several temperature ranges in a single
processing.
Rather, it was decided to measure the vapor pressure using the
imaging technique described in an earlier section [53]. Once, a
stably levitated sample was brought to a selected temperature,

images were taken during a certain interval (e.g., 1535 min,
depending on temperature). The radius of the sample was then
extracted from the digitized images and, from the knowledge of the
elapsed time between the start and the end of the experiment, the
sample area variation in time could be accurately measured. This
procedure was repeated for a few temperatures covering not only
high temperature solid conditions but also the supercooled and
liquid phases. The window of the pyrometer was carefully
inspected and thoroughly cleaned between each experimental
run to ensure correct temperature readings.
Since the sample evaporated isotropically, the situation was
similar to that of the effusion Knudsen method, assuming that the
effective area of effusion was the surface of the sample at a given
time. Hence, the vapor pressure Vp (Pa) could be obtained using the
Knudsens equation [235,236]:
V p T 1:013 105
am2pRT 1=2
tA
(34)
where a is the accommodation coefcient, m/t is the measured rate

of evaporation in vacuum (calculated from the area data at a given
temperature and from density), A is the average surface of the
sample, R is the gas constant, T is the sample temperature, and M is
the molecular weight of the material. Following Johnston et al.
[237], the accommodation coefcient in Eq. (34) was assumed to
have the value unity. Using Eq. (33), the vapor pressure was
determined for few temperatures for the solid, liquid, and
supercooled phases. Furthermore, using the ClausiusClapeyron
equation applied to the vapor of a pure substance (assuming the
volume of the vapor large compared to that of the sample) and
using Vp given by Eq. (34), the latent heat of vaporization/
sublimation DHT (J/kg) at a given temperature can be calculated
from [232]:
dlogV p T
DHT
d1=T
2:303R
(35)

From the results of the mass loss (normalized with the initial
mass) as a function of time for liquid (1700, 1800, 1900, and
2050 K) and solid (1770, 1900, and 1940 K) titanium, and using
equation 34, it was possible to obtain values of the vapor pressure.
The data of supercooled, liquid, and high temperature solid
titanium are presented in Fig. 60 and are summarized in Table 14.
The uncertainty of the vapor pressure measurements was
estimated to be 3% for the liquid and 6% for the solid from the
resolution of the video grabbing capabilities and from the
10
Vapor Pressure (Pa)
38
1
4.5
5.5
6.5
Liquid
0.1
Solid
0.01
0.001
10000/T (K-1)
Fig. 60. Vapor pressure of titanium as a function of temperature [234].

Reprinted with permission from P.-F. Paradis et al., Eur. J. Phys. Appl. Phys. 22, 97
101. Copyright 2003, Cambridge University Press.
G Model

Table 14
Values for the vapor pressure of Ti. Vp(Tm) denotes the vapor pressure at the melting
temperature [229].
Phase
Log Vp(T) (Pa)
T range (K)
Vp(Tm) (Pa)
Liquid
Solid
9.15417,978 T1
16.63432,960 T1
17002050
17701940
0.795
0.469
uncertainties in mass and temperature measurements. Because

the shape of a solid sample departed from that of a sphere, it made
digitization less accurate which explains the higher uncertainty.
The vapor pressure of titanium, as that of other pure metals,
exhibited a non-linear nature as a function of temperature
[138,232]. When the data of other investigators are extrapolated
to the melting temperature, the ESL value for the solid case is,
within respective experimental uncertainties, identical to that of
Edwards et al. [238] and 34% lower than those of Carpenter et al.
[233] and Blocher and Campbell [239]. Note that at the melting
temperature, the vapor pressure datum for the solid is nearly 40%
lower than that for the liquid.
From the slope of the vapor pressure versus temperature of
Fig. 61, and with the help of Eq. (35), the average latent heat of
vaporization was calculated from the data of the liquid phase as
344.8 kJ/kg, which agrees, within the experimental uncertainties,
with the value reported by Vinet et al. [240]. Similarly, the heat of
sublimation was calculated from the data of the solid phase as
632.1 kJ/kg, which is 12% higher than that of Edwards et al. [237]
and less than 14% higher compared with those of Carpenter et al.
[233] and of Blocher and Campbell [239].
The vapor pressure results obtained for the liquid phase could
not be compared because no data were reported in the literature.
39
However, if we compare the ESL data for the solid phase with those
of other investigators, the difference could arise from the departure
from a perfect sphere of our solid sample that induced errors in the
digitization procedure. Additional discrepancies could be attributed to the difference in processing techniques and temperature
measurement. The use of electrostatic levitation and radiative
heating in vacuum isolated the samples from container walls and
gases, whereas the cited authors employed methods for which
possible chemical reactions between the highly reactive titanium
and the crucible or the residual surrounding gas could have
occurred. In addition, electron bombardment and induction
heating, used by the conventional instruments, might have
contaminated the specimen under study through evaporation
from the electrodes. The disappearing lament technique utilized
by some authors to measure temperature might also have
introduced some errors. As an additional potential source of
discrepancy, the Knudsen effusion equation was used to calculate
the vapor pressure for electrostatically levitated droplets. However, the physical reality between the geometry of the spheroid
sample and that of normally used samples (plane) was different. To
some extent, the atoms on the surface of the ESL sample had fewer
neighbors that those lying in a plane, which was the case for other
investigators [233,238,239]. Therefore, this could further explain
the lesser energy (or lower vapor pressure) observed in the ESL
experiments.
Electrostatic levitation with an imaging technique permitted
the measurement of the vapor pressure of liquid and supercooled
titanium. A drawback explaining that this method has not been
used for other materials is the coating of the window of the
chamber which required extensive cleaning and maintenance.
However, besides this issue, the method could also, in principle, be
applied to any solid or liquid materials, as long as they can be
levitated. However, as is the case with any other techniques, it
could be time consuming if low vapor pressure materials or if low
temperatures are investigated [232].
5. Short-range structure and atomic dynamics
Fig. 61. Comparison between the values obtained by experiment and calculation
based on the hard sphere model for surface tension (a) and viscosity (b) of hafnium
[250].
Recently, a lot of attention has focused on the utilization of

containerless techniques for the structure analysis of materials
[241244,128,245248]. In addition to the well known merits of
contactless processing listed in the introduction, levitation
methods offer samples with nearly spherical shape for which
the data correction can be easily performed on the diffraction data
analysis [249]. Moreover, because containerless processing
removes the risk of heterogeneous nucleation from the wall of
a container, the structural study of deeply supercooled liquids can
be performed [250254]. In addition, containerless processing
offers the additional advantage for scattering experiments that
the amount of scattering material in the vicinity of the sample is
reduced. This allows performing high quality neutron scattering
experiments with an excellent signal-to-background ratio.
Therefore, several efforts for implementing electromagnetic
[241244,128] and aerodynamic [245248] techniques to synchrotron X-ray or neutron source for structure analysis of liquids
have been undertaken. The motivation of implementing an
electrostatic levitator lies in the fact that it can handle various
kinds of materials and that it provides temperature homogeneity
of the sample better than that of the aerodynamic levitator.
Moreover, the electrostatic scheme allows experiments to be
carried out over wide temperature ranges because the mechanism
of levitation is independent of that of heating, contrary to
electromagnetic levitation. In addition, the positioning of sample
can be very accurately performed and there are no coils in the eld
of view of the interacting high-energy beam, which again
simplies the analysis.
G Model

40
Table 15
Comparison of hard sphere calculation and experimental values at the melting temperature for heat capacity (Cp), surface tension (g), and viscosity (h) [250].
Element
Heat capacity Cp(J/mol K)

Calculation
Ti
Zr
Nb
Hf
34.2
33.8
33.4
33.8
Surface tension g (103 N m1)
Viscosity h (103 Pa s)
Experiment
Calculation
Experiment
Calculation
Experiment
35.9
41.7
40.3
34.3
1634
1445
2177
1646
1557
1500
1937
1614
3.0
3.6
4.7
5.4
4.4
4.7
4.5
5.2
5.1. Hard sphere model

One of the fundamental scientic interests of measuring the
thermophysical properties of refractory metals is to nd relationships between the microscopic structure and the macroscopic and
thermophysical properties of liquids. Compared to simple liquid
metals such as alkaline metals, which consist of s and p valence
electrons, liquid transition metals are partially lled with d-band
electrons and are more complicated. Due to the presence of these d
electrons, successful prediction could hardly be done for liquid
transition metals. Furthermore, the lack of accurate thermophysical properties of refractory metals prevented the progress of
theoretical research. However, the advent of containerless
techniques, electrostatic levitation, in particular, offered means
to obtain reliable thermophysical properties of transition metals.
Comparison between theoretically calculated values based on the
hard sphere model and data measured with electrostatic levitators
was carried out for heat capacity, surface tension, and viscosity of
titanium, zirconium, niobium, and hafnium [250]. The calculated
and measured values are listed in Table 15, and Fig. 61 shows, as an
example, the comparison between the measured and calculated
values based on the hard sphere model for surface tension and
viscosity of hafnium. Despite of the simplicity of the hard sphere
model, agreement between the measured data and the calculated
values is good and proved the reliability of the non-contact
thermophysical property measurements with electrostatic levitation.
5.2. Neutron scattering experiments
Neutron scattering is a powerful technique that allows
investigating both the short-range structure and the atomic
dynamics in liquids matter. By elastic neutron diffraction, the
static structure factors S(q) can be determined. These provide
information on the atomic structure of the liquid, which governs
macroscopic properties such as viscosity, density, and electrical
conductivity. Isotopic substitution provides the opportunity to
vary the scattering strength of alloy components, which enables
even to determine the full sets of partial structure factors that
provide information both on the topological and the chemical
structure of the melt. Partial structure factors are used as input in
numerical mode-coupling solutions to predict dynamic processes
in the liquids thus giving insight into the structure-dynamics
relations [251]. Dynamic processes in the melt can be studied
experimentally by inelastic or quasielastic neutron scattering. The
dynamic structure factor, S(Q,v), is measured in these techniques
as function of momentum transfer and energy. From S(Q,v) selfdiffusion coefcients can be determined for elements with a
sufciently high incoherent scattering length [252].
5.2.1. Preliminary experiments
For the reasons mentioned above, JAXA opted for the
electrostatic technology for the structure analysis of condensed
matter by neutron scattering. The facility, for which all instruments were located on an elevated table to avoid the incident and
scattered neutrons, consisted of a heating laser, a pumping unit,
and a stainless steel chamber that were easy to transport, assemble

and integrate with the high resolution powder diffractometer
(HRPD) at the Advanced Science Research Center of the Japan
Atomic Energy Research Institute (JAERI) in Tokaimura, Ibaraki,
Japan. The chamber contained the levitator and was surrounded by
various diagnostics probes and detectors (laser, neutron beam,
camera, neutron detector, pyrometer, etc.) (Figs. 62 and 63). The
overall layout of the neutron facility is reminiscent of the
pressurized facility, in particular with respect to electrode
conguration, sample handling, and laser heating [57,58,253].
However, the chamber was evacuated to a 105 Pa pressure prior
to processing. For sample observation and to ease the heating laser
beam alignment, one CCD camera gave a close view of the
specimen and another one looked through the pyrometer.
Once the sample was levitated and reached the required
temperature for an experiment, a 1 cm 5 cm cross-section beam
of thermal neutrons produced by the JRR-3 M nuclear reactor of the
Advanced Science Research Center of JAERI, was directed toward
the aluminum entrance port of the chamber [57]. The beam was
further collimated by a cadmium slit (large neutron absorption
coefcient) located 50 mm ahead of the sample position to make
the incident neutron beam size slightly larger than that of the
sample (slit width set to 3 mm), thus eliminating the background
intensity from the copper electrodes [58]. At the sample position,
the continuous ux was 105 unpolarized neutrons/cm2. The
scattered neutrons exit the chamber through an aluminum port.
Preliminary neutron diffraction experiments were performed
with a 3 mm diameter alumina polycrystalline sphere coated with
a few ten angstroms thick platinum layer [58]. The coating helped
to maintain the positive charge on the sphere. The sample could be
kept continuously levitated for more than 12 h. The sample
position oscillation was estimated to be less than 0.1 mm along
the three axes from the video images. The vacuum level of the furnace
was about 5 104 Pa. The intensity of scattered neutrons was
analyzed with the diffraction spectrometer. The diffractometer had a
Fig. 62. Illustration of the main system components, as viewed from the top, of the
JAXA vacuum electrostatic levitator dedicated to neutron beam interaction studies.
G Model

41
Fig. 63. Side view of the JAXA neutron vacuum electrostatic levitator.
0.2% Dd/d resolution that is comparable to conventional X-ray

instruments [254]. The HRPD has 64 detectors in the range of
scattered direction from 58 to 1658 measured from the incident
neutron beam direction. The neutron wavelength was 1.823 A. The
diffraction data of the levitated sample were obtained with and
without the cadmium slit. The background intensity from the furnace
was also obtained for both cases. The intensity data were obtained by
increments of 0.058 or 0.108 as a function of the scattering angle, 2u,
and were normalized to the incident neutron number, which were
recorded by a monitor counter. The whole measurement was
performed at room temperature.
The intensity data of the scattered neutron are shown in Fig. 64
for an alumina sample and the background, when the cadmium slit
was used [58]. The gure does not reveal sharp peaks in the
background and indicates that the levitator does not generate
sharp diffraction peaks which is an advantage compared to the
electromagnetic or aerodynamic methods for which the radiofrequency (RF) coil or the gas nozzle located in the vicinity of the
sample yielded such peaks. Peaks of platinum were not observed
because the diffraction intensity of the platinum coating of few ten
angstroms was quite small in comparison with that of alumina
Fig. 64. Intensity of alumina and background with the Cd slit: (a) alumina, (b)
background [58].
Reprinted with permission from H. Aoki et al., Rev. Sci. Instrum. 74, 11471149.
itself. The diffraction intensities of the alumina specimen after the

subtraction of the background are shown in Fig. 65. Ten peaks were
clearly observed and were identied as those derived from the
mirror indices of hexagonal structure of alumina. The observed
peaks were in complete agreement with the literature [255]. The
lattice parameters were determined with the use of these ten peaks
by the standard procedure. The determined lattice constants were
a = 54.760 A and c = 513.00 A. These values were in close
agreement with the literature data [255]. The background intensity
of the present data was weaker than that of a previous neutron
diffraction experiment of solid alumina performed with an
aerodynamic levitator [247]. The ESL study exhibits sharp peaks,
as shown in Fig. 66, compared to the rather broad peaks reported in
the previous study [247]. These preliminary results indicated that
an electrostatic levitator coupled with neutron diffraction is a
promising method for structural study of condensed matter.
5.2.2. Elastic and quasi-elastic experiments
For about ten years, electromagnetic (EML) [128,256] and
aerodynamic levitation techniques (ADL) [257,258] have been
used in order to investigate the short-range order of melts using
elastic neutron scattering. Later, quasielastic neutron scattering
experiments were also performed to study the atomic dynamics of
liquids [259,260]. The ESL technique, however, appeared less
attractive at rst for neutron scattering studies because the early
generations of electrostatic levitation facilities were only able to
process comparatively small samples with volume of up to about
10 mm3. For weakly interacting neutron radiation, signicantly
larger sample sizes are preferable. Moreover, when considering the
Fig. 65. Intensity of alumina with the corresponding mirror indices [58].
Reprinted with permission from H. Aoki et al., Rev. Sci. Instrum. 74, 11471149.
G Model

42
Fig. 66. Schematic drawing (vertical cut) of the DLR electrostatic levitator for
neutron scattering experiments. Sample: S; top electrode: TE; ground electrode:
GE; side electrodes: SE; high voltage feed through: HV; positioning laser with beam
expander: L; mirror: M3; position sensitive detector: PSD; neutron window: NW;
turbo molecular pump: TP; UV lamp: UV [261].
use of neutron time-of-ight spectrometers for quasielastic

scattering experiments, the geometrical constraints given by such
instruments request a levitator with a very compact design which
is technically challenging.
Recently, a compact electrostatic levitator specically designed
for elastic and quasielastic neutron scattering experiments on
liquids has been developed at DLR [261]. By applying levitation
voltages of up to 40 kV, samples of about 100 mm3 in volume can
be processed. This is an increase of the sample size by one order of
magnitude as compared to earlier ESL-facilities, providing
scattering volumes that match those offered by electromagnetic
levitators. A schematic sketch of the device is depicted in Fig. 66.
Fig. 67 shows the levitator integrated in a neutron scattering
environment. The electrically charged sample (S) is levitated by the
electrostatic eld of two vertically arranged electrodes (TE, GE).
Two pairs of side electrodes (SE) are used to control the horizontal
position of the sample. The electrode system is installed within a
vacuum chamber that can be evacuated to a pressure of 107 mbar
within 1 h by use of a turbo molecular pump.
To allow for a compact facility and a large free-scattering angle,
the two laser beams used for sample position detection are
introduced through windows from the top of the chamber and
reected by mirrors within the chamber on the specimen. Two of
the mirrors (M1, M2) are located in the scattering plane. M1
reects the rst laser beam onto the sample and subsequently M2
reects the shadowgraph of the sample on the rst PSD at the top
of the chamber (Fig. 67). Another mirror (M3) is placed below the
scattering plane and reects the second laser beam on the sample.
The beam then directly passes to the second PSD (Fig. 67). In order
to avoid the shading of this laser beam by the horizontal electrodes,
the laser beam is tilted by 458 with respect to the electrodes. With
this design, a range of 1308 of unobstructed scattering angle is
reached.
Fig. 67. Schematic drawing (horizontal cut) of the electrostatic levitator integrated
in the neutron scattering environment. Neutron beam guide: NG; neutron beam:
NB; neutron slit system: NS; neutron B4C aperture: NA; neutron window: NW;
neutron beam stop: BS; neutron detector: D; mirrors: M1-3; position sensitive
detector: PSD; high voltage feedthrough: HV; side electrodes: SE; UV lamp: UV;
laser head containing the coupling optics of the heating laser, the pyrometer, and
the CCD video camera: LH; window for sample exchange: W [261].
For heating the specimen, a 75 W infrared ber coupled diode

laser emitting at the wavelength of 808 nm is utilized (well suited
for melting metallic samples). The facility also comprises a ber
coupled two-color pyrometer for measurement of the sample
temperature and a CCD-video camera (LH) for observation of the
specimen. These are along the same path as that of the laser beam
to ensure a compact facility and to ease adjustment of the heating
laser. To guarantee laser safety, the levitation facility is light-tight
and all openings are secured by safety interlocks.
In order to compensate charge losses during the heating of the
sample before thermionic emission charging becomes efcient, the
specimen is illuminated by ultraviolet light that generates charges
to the specimen through photoelectric effect. As UV source, a He
discharge lamp is used because it combines a compact design with
high photon energy (20 eV) and ux. Because no transparent
window material exists for this photon energy, the discharge
chamber of the lamp is directly connected with the chamber of the
levitator via a differentially pumped capillary of 1 mm diameter
that points toward the sample.
The neutron beam is adjusted in size by a system of slits (NS) at
the end of the beam tube and then enters into the vacuum chamber
of the levitator through an Al window (NW). The window has a
thickness of 2 mm and covers an angular range of 2208 horizontally
and 208 vertically. An aperture (A), made from densely sintered
neutron absorbing B4C, is installed inside the chamber and shapes the
beam right in front of the sample. It is tilted by an angle of 458 with
respect to the incident beam to prevent that the range of high
scattering angles is obstructed by the aperture. In case of elastic
neutron diffraction experiments, the direct beam is blocked inside the
chamber by a Cd beam stop (BS) to avoid disturbing the scattering at
the backside of the chamber.
While the primary aim of the development at DLR was to design
a mobile electrostatic levitator for neutron scattering experiments,
it has also been successfully utilized for performing X-ray
scattering experiments using high-energy synchrotron radiation
with only minor modications to the device. Such experiments aim
the study the short-range order of the liquid phase of ZrCu alloy
G Model

Fig. 68. Raw diffractogram of liquid Zr36Ni64 (0.6 g mass) at a temperature of 1370 K
measured using a neutron wavelength of 0.94 A. Also shown is the background of
the empty ESL, which is one order of magnitude smaller than that of the signal of the
sample.
[262], in particular the investigation of the phase formation during

non-equilibrium solidication of supercooled melts with a subsecond timely resolution [263] and to examine high-temperature
phase transformations of GdZr under conditions close to
equilibrium [264].
The rst elastic neutron scattering experiments on melts using
DLRs mobile facility were performed at the high ux diffractometer D20 of the Institut Laue-Langevin in 2010 using a neutron
wavelength of 0.94 A [261]. Fig. 68 shows the scattering signal of a
liquid Zr64Ni36 sample of 0.6 g mass at T = 1370 K normalized to
monitor counts and corrected for the detector efciency only. Also
shown in the gure is the background signal of the empty levitator.
In the usable range of scattering angles of 48 < 2u < 1348,
corresponding to a range of momentum transfer of about
0.6 A1 < q < 12 A1, the scattering intensity from the sample is
about one order of magnitude larger than that of the background
intensity. The structure factors determined from the diffraction
data for liquid Zr64Ni36 in a broad range of temperatures including
the metastable regime of supercooled liquids are shown in Fig. 68.
The peak positions and the general shape of the structure factor do
not signicantly vary with temperature indicating that the shortrange order remains essentially unchanged. Small changes with
temperature can be observed in the amplitudes of the oscillations.
As observed also for other metallic melts [128] the characteristic
features of the structure factors become more pronounced if the
temperature is decreased.
In recent years the short-range order (SRO) of Zr-based glass
forming alloys, has been extensively studied in the liquid and the
glassy state, both experimentally [265,266] and by molecular
dynamics (MD) [267269] simulations. A strong controversy
remains concerning the role of an icosahedral SRO in such Zrbased liquids. While some authors [265267] report indications
for a signicant degree of icosahedral SRO, other investigations
[268,269] suggest that icosahedral SRO does not play a dominant
role. However, most of the experimental studies suffer from the
fact that only total X-ray structure factors were measured. For
conclusive structural investigations of alloy melts partial structure
factors must be determined.
By isotopic substitution of Ni partial structure factors of stable
Zr64Ni36 melts at T = 1375 K have been determined in 2009 using
the electromagnetic levitation technique [269]. The partial
structure factor SNN reveals a large nearest neighbor coordination
number of ZNN 13.8 that is incompatible with the assumption of
a dominant icosahedral short-range order in the melt. While the
partial structure factors have been determined at one temperature
43
Fig. 69. Total static structure factor of liquid Zr64Ni36 for different temperatures in
the stable liquid and in the regime of the supercooled melt below the liquidus
temperature of TL = 1283 K. The structure factors are shifted by multiples of 0.5 for
better visibility [261].
above the melting temperature only, the electrostatic levitation

results of Fig. 69 demonstrate that there is no fundamental change
of the short-range order in the investigated broad temperature
regime (1085 K < T < 1370 K).
ZrCu alloys exhibit an even better glass-forming ability than
ZrNi alloys as reported by Xu et al. [270]. As discussed in the
literature [262] for the special case of liquid ZrCu, good
approximations of the two partial Bhatia Thornton structure
factors SNN and SNC can be determined if the total structure factors
measured with both neutrons and X-rays are available. Therefore
neutron scattering and diffraction of synchrotron radiation have
been combined in order to investigate the SRO in ZrCu melts that
were processed by electrostatic levitation [262]. The neutron
scattering experiments were performed with the D20 diffractometer at the Institut Laue-Langevin using incident neutrons with a
wavelength of l = 0.94 A and the X-ray diffraction studies were
performed at beamline BW5 of the Hasylab at the German electron
synchrotron (DESY) using monochromatic X-rays of 100 keV
energy. The total structure factors determined by these two
diffraction techniques for liquid Zr50Cu50 at different temperatures
are shown in Fig. 70. At the same temperature, both total structure
factors exhibit signicant differences indicating that the Cu and Zr
atoms are not randomly distributed in the liquid.
The partial structure factors, SNN and SNC, determined from the
two total structure factors measured with neutrons and X-rays for
Fig. 70. Total structure factors measured by neutron scattering and X-ray diffraction
for liquid Zr50Cu50 at different temperatures above and below the liquidus
temperature of TL = 1226 K [262].
G Model

44
Fig. 71. Partial structure factors SNN (upper curves) and SNC (lower curves) for liquid
Zr50Cu50 at T = 1280 K (red) and T = 1175 K (blue) [262] (For interpretation of the
references to color in this gure legend, the reader is referred to the web version of
the article.).
a Zr50Cu50 melt at different temperatures are illustrated in Fig. 71.

SNN describes exclusively the topological short-range order of the
melt, while SNC describes the correlation between density and
chemical composition. From SNN and SNC the corresponding pair
correlation functions gNN and gNC can be calculated. From gNN(r)
simple parameters that describe the topological short-range order
in the melt, like the mean distance of nearest neighbors, r1, and of
second neighbors, r2, as well as the nearest neighbor coordination
number, ZNN, are determined. These are compiled in Table 15 for
different ZrCu melts. The ZNN values are considerably larger than
coordination numbers reported for monatomic metallic melts
(Z 12) [128], but they are similar to those determined for liquid
Zr64Ni36 (ZNN 13.8) [270]. Because a dominant icosahedral SRO
(as well as a fcc- or hcp type SRO) implies ZNN = 12, the much higher
ZNN observed for liquid ZrCu and ZrNi highlights that the SRO
cannot be dominated by icosahedral aggregates. This result is in
contradiction with speculations on the decisive role of icosahedral
SRO for glass formation in Zr-based alloy melts (Table 16).
Quasielastic neutron scattering experiments were also performed at the time-of-ight spectrometer TOFTOF [271] of the
Munich research reactor (FRM II) in Garching, Germany, for liquid
Ni36Zr64 at different temperatures ranging from temperatures
above the liquidus temperature TL down to temperatures in the
metastable regime of an supercooled melt below TL [261]. Fig. 72
shows a raw time-of-ight spectrum measured for a Zr64Ni36 melt
at T = 1478 K acquired within a span of scattering angles of
598 < 2u < 748. Also shown is the spectrum of the empty levitator.
Due to the containerless processing setup, the background is about
2 orders of magnitude smaller than the signal measured with
sample. Fig. 73 illustrates the quasielastic range of the scattering
law S(q,v) for liquid Ni36Zr64 for two temperatures, T = 1116 K and
T = 1460 K, at a wave vector of q = 0.5 A1 [272]. The quasielastic
signal can be well described with a Lorentzian function convoluted
with the instrumental energy resolution function determined from
a measurement on vanadium at 290 K (lines in Fig. 74). It can be
clearly seen that the full width at half maximum, , of the
Fig. 72. Raw time-of-ight spectrum measured for a Zr64Ni36 melt at T = 1478 K
acquired within a range of scattering angles of 598 < 2u < 748. Also shown is a
spectrum of the empty levitator.
Fig. 73. Scattering law S(q,v) of liquid Zr64Ni36 for q = 0.5 A1 at T = 1115 K (lled
symbols) and T = 1460 K (open symbols) tted with Lorentzian proles [272].
Lorentzian function at constant q decreases with decreasing

temperature. For small momentum transfers, the measured signal
is dominated by the incoherent scattering of the Ni atoms
(incoherent scattering cross sections: sinc(Ni) = 5.2 barn,
Table 16
Nearest neighbor (r1) and second neighbor (r2) distances, and nearest neighbor
coordination numbers, ZNN, for ZrCu melts at different temperatures [262].
Zr66.7Cu33.3
Zr50Cu50
Zr41.2Cu58.8
T (K)
r1 (A)
r2 (A)
ZNN
1325
1175
1280
1110
1260
2.95 0.01
2.79 0.01
2.79 0.01
2.75 0.01
2.74 0.01
5.37 0.05
5.10 0.05
5.13 0.05
5.01 0.05
4.94 0.05
13.7 0.5
13.8 0.5
13.6 0.5
13.8 0.5
13.6 0.5
Fig. 74. Temperature dependence of the Ni self-diffusion coefcient in liquid

Zr64Ni36 processed by electromagnetic (EML) [269] and electrostatic [261]
levitation.
G Model

sinc(Zr) = 0.02 barn) and the Ni self-diffusivity is related to by

D = q2/2 [273,274].
5.2.2.1. Diffusivity. In Fig. 74, the Ni self-diffusion coefcient, D, in
liquid Zr64Ni36, determined from the quasielastic neutron scattering data measured by means of ESL [261] as well as electromagnetic levitation (EML) [269], is shown as a function of the
temperature. Both sets of data are in excellent agreement with
each other. Due to the clean environment of the high vacuum of the
ESL, it was possible to extend the temperature range to lower
temperatures, thus enabling measurements at maximum supercoolings of about 170 K below the liquidus temperature of 1283 K.
In the diffusion data measured using the ESL, small deviations from
the Arrhenius-type temperature dependence D(T) = D0 exp(EA/
kBT) with EA = (0.64 0.02) eV and D0 = (2.1 0.3) 107 m2/s (line
in Fig. 74) are observed at the highest supercoolings, indicating
approaching the critical temperature of mode coupling theory.
5.3. Synchrotron scattering experiments
5.3.1. Inelastic scattering
Inelastic scattering can be detected when strong X-ray and
neutron beams are targeted onto materials and yield useful
information on physical properties of materials. The intensity of
inelastic scattering, however, is much smaller than that of elastic
scattering. Inelastic scattering could be buried into noise extrinsic
to sample. By levitating a sample, the observed data are mostly due
to the sample, which signicantly improves the signal-to-noise
ratio. This is a remarkable advantage when performing inelastic Xray scattering experiments.
So far, high-resolution inelastic scattering (HRIS) and highenergy inelastic scattering, the so-called Compton scattering, have
been performed using levitation technique. HRIS observes a
dynamic structure factor S(q,v). S(q,v) gives information on the
MeV excitation in materials which are mainly due to phonons.
HRIS provides a useful method for studying collective atomic
dynamics in liquids. A pioneering work was performed on the
microscopic dynamics of liquid aluminum oxide using gas levitator
by Sinn et al. [275]. HRIS experiments have been also performed on
liquid boron [276] and liquid titanium [277].
Compton scattering refers to the inelastic X-ray scattering
process at large energy and momentum transfers. To date, the
technique has been applied primarily to investigate the electronic
structure and ferrmiology of solid-state systems, where the
measured Compton prole is directly related to the momentum
density distribution of the electronic ground state within the
impulse approximation. Since no charged particles entering or
leaving the sample are involved, the Compton technique is a
genuinely bulk probe, which is not complicated by surface effects
present in photoemission or electron scattering experiments.
Recently, Compton scattering coupled with electrostatic levitation
has been used to investigate electronic properties of high
temperature liquids such as liquid Si [61]. To investigate the
electronic structures of condensed matters, soft X-ray spectroscopy is usually used. Soft X-ray measurements require a clean and
stable sample surface. The surface of high temperature liquids,
however, is not stable due to thermal convection, and evaporation
from the melt could disturb bulk sensitive measurements by soft
X-ray. Hard X-ray measurements are needed to investigate bulk
properties of high temperature liquids. The Compton scattering
beamline at SPring-8 (BL08W) uses 116 keV X-rays which allow
investigating bulk properties of high temperature liquids.
Si transforms into a metal accompanied by a density increase of
about 10% upon melting. The resistivity of liquid Si (l-Si) at the
melting temperature (1683 K) is 0.75 Vm, which is comparable to
that of simple liquid metals such as l-Al. Molecular dynamics
45
simulations of molten Si at 1800 K suggest that approximately 30%

of the bonds are covalent and that these covalent bonds possess a
highly dynamic nature, forming and breaking up rapidly on a time
scale of 20 fs [278]. It is remarkable that two completely different
types of bonds, metallic and covalent, can coexist in l-Si. In fact, the
coexistence of two forms of liquid in a single component substance
has been predicted to undergo a phase transition as a function of
temperature and/or pressure. A recent study reports that l-Si could
undergo a liquidliquid phase transition (LLPT) below about
1232 K and above about 12 kB, separating into a high-density
metallic liquid (HDL) and a low-density semi-metallic liquid (LDL)
[279]. However, 1232 K is far below the melting temperature of Si,
and, as a result the supercooled state has remained inaccessible to
current experimental techniques so that the experimental
conrmation of an LLPT in Si remains an open question. A key
requirement for the possibility of an LLPT obviously is that the
metallic and covalent bonds coexist in l-Si. Although experimental
investigations of the atomic conguration hint at the existence of
covalent bonds in l-Si, soft X-ray and magnetic susceptibility
measurements of electronic properties so far do not support this
viewpoint in that all four valence electrons in l-Si appear to behave
like free electrons.
Molten Si is highly reactive with most crucibles. To hold the
sample without contamination, an electrostatic levitator was used.
The facility levitates a spheroid sample of 2 mm diameter (Fig. 75)
in a high vacuum environment (approximately 105 Pa) using
electrostatic forces via a feedback computer control. The sample
(Si, 99.9999% purity) was heated and melted using the focused
radiation of three 50 W semiconductor laser beams emitting at
808 nm. The temperature was controlled within 15 K and was
measured by pyrometry.
Compton proles of polycrystalline (300 K) and molten Si
(1787 K) were measured by high-energy (116 keV) inelastic X-ray
scattering at the BL08W beamline of SPring-8. In order to analyze
the Compton proles, Car-Parrinello molecular dynamics (CPMD)
simulations were performed with the Quantum ESPRESSO package
within the framework of the density-functional theory using the
generalized gradient approximation. Fig. 76 presents the differences between the Compton proles for the solid and liquid phases
[DJ(pz) = Jsolid(pz) Jliquid(pz)]. The results of CPMD simulation are
obtained by taking the difference of the liquid Compton prole and
the spherically averaged prole of the solid. The CPMD results
agree very well with the experimental results. In order to analyze
the bonding character in l-Si obtained through CPMD simulation,
the maximally localized Wannier functions (MLWF) analysis
method is used. MLWF are sorted into three groups to categorize
Fig. 75. Interior view of an electrostatic levitator with a 2 mm diameter sample

being laser heated and subject to synchrotron radiation.
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46
Fig. 76. Difference between the Compton proles for the solid and liquid phases,
[DJ(pz) = Jsolid(pz) Jliquid(pz)]: experiment (black) and CPMD simulation (red) [61]
(For interpretation of the references to color in this gure legend, the reader is
referred to the web version of the article.).
different types of electrons pairs in l-Si: covalent bond pairs, lone

pairs, and diffuse pairs. It is found that on the average, there are
17%, 83%, and less than 1% of covalent bonds, diffuse pairs, and lone
pairs, respectively.
In Fig. 77 is shown a snapshot from the simulation carried out
on l-Si. The key point of the analysis is that the existence of
covalent bonds in metallic l-Si is clearly conrmed, and that l-Si is
not homogeneous at the atomic scale. The coexistence of two
different bonding natures in a single component liquid is a
precondition for LLPT. This study thus supports the possible
occurrence of LLPT in deeply supercooled l-Si. Future Compton
experiments with intense X-ray pulses are needed to probe how
the silicon bonding properties evolve from metallic to covalent
character and how a LLPT may occur.
5.3.2. Elastic scattering
It has been thought that liquids are an intermediate phase
between crystals and gases, since the density of the liquids is close
to that of crystals, but the atomic mobility in the liquids is similar
to that in the gases. This is particularly true for most liquid metals.
Therefore, a fragment of crystal phase is thought as the structure of
a liquid phase. This is the well known microcrystalline model.
However, this model could not explain the deep supercooling
phenomenon, demonstrated by Turnbull [139]. On the other hand,
a dense randomly packed structure based on a hard sphere model
Fig. 77. Snapshot from the simulation on l-Si at 1787 K illustrating Si atoms
(yellow), covalent bond pairs (green), lone pairs (red), and diffuse pairs (translucent
blue). Note that bonds connecting Si atoms are only guide for the eyes [61] (For
interpretation of the references to color in this gure legend, the reader is referred
to the web version of the article.).
Fig. 78. Calculated structure factors of possible local cluster types in liquid: (a)
tetrahedron, (b) bi-tetrahedron (the dotted line is for a distorted tetrahedron), (c)
icosahedron, and (d) decahedron are energetically favored structures as well as (f);
(e) the Z14 polyhedron in FrankKasper phases is a prominent cluster type in
glasses [127].
was suggested for the liquid structure [280]. However, this model
did not agree with the structure of early transition liquid metals
obtained in experiments [281]. The disagreement may be caused
by either modeling or experiments. From the experimental view,
the combination of electrostatic levitation and high energy
synchrotron X-ray scattering can give accurate structural information of the liquid metals, since the scattered intensity from a
levitated liquid does not need correction by a container holding the
liquid sample, and the transmitted scattering can give the bulk
structural information of the liquid metals. The characteristic
feature of the local order of the liquid appears in high q range with
high energy X-ray scattering experiment as seen in Fig. 78.
In Fig. 79, the structure factor (S(q)) of liquid metals (Ni, Ti, and
Zr) is shown. The calculated structure factors cannot t the
Fig. 79. Experimentally measured structure factors for pure elemental liquids (Ni,
Ti, and Zr) in the equilibrium and supercooled states. The dashed lines indicate an
optimized t to the PercusYevick hard sphere model [127].
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47
Fig. 81. Comparison of the experimental data (open circles) and the calculated S(q)
of Ti with ISRO (thin line) and DISRO (thick line) including DebyeWaller (DW)
factor. The inset shows the calculated S(q) for different degrees of distortion
without DW factor; the solid line is calculated for the above distortions, and the
dotted and thin lines are for D3d (threefold) and D2d (twofold) [282] distortions,
respectively [126].
Reprinted with permission from G.W. Lee et al., Phys. Rev. Lett. 93, 037802.
Fig. 80. X-ray structure factors for liquid Ni (liquidus temperature, TL = 1728 K) (a)
and Ti (TL = 1940 K) (b) as a function of temperature (connected open circles); the
curves are displaced vertically for clarity. Dashed lines are from the PercusYevick
hard sphere model. Selected (for clarity) neutron diffraction data from EML
experiments [128] for Ni are shown as closed circles in (a) and the X-ray data from
earlier work on Ti [286] are shown by the dotted line in (b). Insets show the t of the
experimental data (connected open circles) to a 13-atom icosahedron (solid lines),
above and below the melting temperatures [126].
experimental structure factors of the supercooled and stable

liquids. Interestingly, the second oscillation of S(q) has characteristic features, i.e., a small shoulder (marked by arrows). In the case
of Ni, the shoulder on the high q side on the second oscillation,
indicated by an arrow, is lower than that on the low q side. This
shape corresponds to a signal for icosahedral short range order
(ISRO), suggested by Frank for the rst time as the local order of
liquid metals [89]. In neutron scattering experiment, the shoulder
was observed [128]. On the other hand, the shape symmetry of the
second oscillation on S(q) becomes reverse for Ti, and the intensity
of the shoulder at high q side is comparable to that at low q side for
Zr. As seen in Fig. 80, the oscillation shape on S(q) reects various
local orders. In the case of Ni, S(q) with ISRO composed of 13 atoms
gives a good agreement, while it does not agree with the S(q) of
liquid Ti (Fig. 80) [126]. Based on theoretical cluster calculation
[282], Lee explained the S(q) of liquid Ti with distorted ISRO
(DISRO) (Fig. 81) [126]. The DISRO is attributed to the competition
of electronic and density of the cluster. The DISRO was found in a
reverse Monte-Carlo (RMC) simulation [283] and ab-initio
molecular dynamics [284,285]. In particular, the DISRO is
attributed to the atoms with short bond lengths (Short range
order (SRO) clusters) [285]. Fig. 82 illustrates that the SRO clusters
reproduce the reversed second oscillation on S(q) of liquid Ti.
In the case of liquid Si, the local structure changed during
cooling. The structural change was detected by in situ X-ray
diffraction study combined with an electrostatic levitator (Fig. 83).
The S(q) indicates that the local order changes from A5 (white tin)
to A4 (diamond) structure [290] with decreasing temperature.
Interestingly, the coordination number (CN) of the supercooled
liquid does not change during cooling, which is contrary to the
previous measurements (Fig. 84). Furthermore, the coordination
number (CN) decreases and approaches a value of approximately

4.5, from the supercooled liquid to crystal during recalescence
which is marked by an arrow in the inset of Fig. 84. A CN of 4.5 is
appropriate to tetrahedral coordination in crystalline silicon.
Since the ISRO is the energetically favored structure, the
evolution of the ISRO should be shown with supercooling. The
evidence appears in the second oscillation of S(q) as marked by an
arrow in Fig. 85 [127]. The shoulder intensity of the second
oscillation on the high q side does not change with supercooling,
but the intensity on the low q side near 4.6 A1 increases with
supercooling. The change of intensity or shape on the S(q) is an
Fig. 82. (a) Calculated S(q) for supercooled liquid Ti, short-bond length atoms (SRO
clusters, black line), and background atoms with long bonds (gray line); (b) bond
angle distributions [285].
Reprinted with permission from B. Lee et al., J. Chem. Phys. 129, 024711. Copyright
2008, AIP Publishing LLC.
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48
Fig. 85. Structure factor of the equilibrium and supercooled liquids of a

Ti39.5Zr39.5Ni21 alloy liquid (Tl = 1093 K) that crystallizes to a metastable i-phase.
The insets show the growing intensities of the rst [inset (I)] and second peaks
[inset (II), marked by an arrow] with decreasing temperature [127].
indication of changes in short range order, since the S(q) is

determined by the distance between atoms, i.e.,
Sq
1=N
i; j
!
2
f i f j sinqr i; j =qri; j h f i
2
h fi 1
(36)
where N, f, q, and r are respectively the number of atoms, the

atomic form factor, the wave-momentum, and the atomic distance.
Fig. 83. (a) Structure factors and (b) reduced radial distribution functions for liquid
Si, obtained from diffraction patterns taken at a frame rate of 1 Hz during cooling at
13 K/s [287].
Reprinted with permission from T.H. Kim et al., Phys. Rev. Lett. 95, 085501.
Fig. 84. The coordination number of supercooled liquid Si (left). In order to show the
change in coordination during recalescence, a time series is displayed in the inset.
The arrow denotes the onset of recalescence. The data were taken with 10 Hz frame
rate [287]. Temperature dependence of the coordination number obtained by
previous measurements (* [244]), & [288], ~ [289]).
Reprinted with permission from T.H. Kim et al., Phys. Rev. Lett. 95, 085501.
Fig. 86. (a) A 13-atom icosahedral cluster showing the bond types considered for the
calculation of S(q); (b) total S(q) and the contributions of each bond type to S(q); (c)
the combinations of the various bond types to S(q) [127].
G Model

Fig. 87. Honeycutt and Anderson indices as a function of temperature calculated

from the t RMC structures for Ti39.5Zr39.5Ni21 supercooled liquids. With
supercooling, the number of pairs associated with icosahedral order (1551,
1541, and 1431) and bcc order (1661) increases. The number of pairs associated
with fcc and hcp order (1421 and 1422) does not change signicantly [292].
Reprinted with permission from T.H. Kim et al., J. Phys. Condens. Matter 19, 455212.
Copyright 2007, IOP Publishing.
For the ISRO with 13 atoms and with four type lengths, S(q) is given
as follows.
1=1324 f 1 f 2 sinqr1=qr1 60 f22 sinqr2=qr2
49
Microstructure analysis using Honeycutt and Anderson indices

[291] showed the same aspect with increasing population of 1551,
1431, and 1541 types (Fig. 87) [292]. This result veries Franks
hypothesis [89].
ISRO may not be the only SRO of liquid metals. It is well known
that distorted ISRO or decahedral order is more stable than perfect
ISRO in atomic cluster study [282,293295]. This is true for nonmetals. In case of metals, liquid Ti has distorted ISRO (DISRO).
Fig. 88 shows an evidence that liquid Ti40Zr30Ni30 exhibits a
different S(q) from that of i-phase forming Ti39.5Zr39.5Ni21
[127,282]. Since the C14 Laves phase on Ti40Zr30Ni30 with hcp
structure is composed of three distorted ISRO [286], the SRO differs
from the perfect ISRO. Fig. 89(a) shows a calculated S(q) as a
function of distortion angle. As distortion increased with u
direction, the third and forth peak shapes are changed. The mixed
structure with ISRO and DISRO reproduces the S(q) obtained in
experiment (Fig. 89(b)).
An evidence of chemical short range order was revealed by
combining X-ray beam scattering and electrostatic levitation
[296]. The presence of a pronounced pre-peak at q 1.78 A1 in the
static structure factor indicates a medium-range order (MRO) in
the liquid (Fig. 90). The position and intensity of the pre-peak
remain constant with cooling, indicating that the MRO is already
present in the liquid above its melting temperature. It should be
emphasized here that the detailed study of liquid structures with
S(q) is possible by combining electrostatic levitation and X-ray
Sq
60 f22 sinqr3=qr3 12 f22 sinqr4=qr4 h f i

2
h fi 1
(37)
The partial S(q) for each bond length is shown in Fig. 86(a).
Among the bond lengths, r2 and r3 type-bonds dominantly affect
the second peak shape of the total S(q). Therefore, when the
number of r2 and r3 bonds increases, the behavior of the second
oscillation on S(q) can be reproduced with supercooling in
Fig. 86(b). The r2 and r3 type-bonds are found in the distorted
tetrahedral order in Fig. 86(a), which is the unit structure for
ISRO. Therefore, it can be concluded that the fragments of ISRO,
i.e., distorted tetrahedral order, increase with supercooling.
Fig. 88. Structure factor of Ti40Zr27Ni33 (Tl = 1194 K) as a function of supercooling.

The inset shows the magnied S(q) at higher q compared to that for the i-phase
forming liquid (dotted curve); the arrows point to the approximate position of the
third and fourth peaks [127].
Fig. 89. Calculated S(q) for Ti40Zr30Ni30 as a function of distortion angle (a), and a
comparison of the calculated S(q) for different degrees of distortion (b). The thick
line was computed for a combination of perfect icosahedra (55%) and distorted
icosahedra with u = 78 (45%). The arrows indicate the position of the third and fourth
peaks [136].
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50
Fig. 90. Static structure factor for (a) liquid Zr80Pt20 at 1607 8C, 1474 8C, 1345 8C,
1217 8C, 1090 8C, and 978 8C. The insets show the evolution of S(q) with decreasing
temperature for (b) the primary peak, (c) the second peak, and (d) the pre-peak
(indicated with an arrow in the total structure factor) [296].
Reprinted gure with permission from N.A. Mauro et al., Phys. Rev. B 83, 184109 (8
pp.), 2011. Copyright 2011 by the American Physical Society.
scattering technique, since the technique can highlight or detail

subtle information which otherwise would have to be removed by
a container correction.
6. Conclusions and outlook
As was illustrated in the above sections, electrostatic levitation
is a wonderful tool to process, characterize, and study materials for
both fundamental and applied endeavors in materials science. So
far, it has also shown promise for the synthesis of novel materials
with new properties. However, electrostatic levitation is still in its
infancy. As far as processing is concerned, the technique has been
mainly used with metals and a better knowledge of the charging
mechanisms is essential to permit systematic levitation of
ceramics, in particular oxides. Because thermionic effect cannot
be used to initiate launch of low melting temperature materials in
vacuum, charging has to rely on UV photoelectric effects, which is
very time consuming. Therefore, efforts shall be directed to
improve charging either by using shorter wavelength sources such
as table top X-ray lasers or by cleaning the surface by atomic beams
to alleviate this shortcoming.
Property measurements would also benet from several
improvements and additions to the current techniques. The
density measurement technique is quite mature but a further
improvement might permit resolving the changes in the liquid
density due to the structural changes occurring in some liquid
phase transitions, especially glass forming materials. The use of
VUV or X-ray sources as a background illumination source to the
sample would offer improved imaging, in particular for samples
near 4000 K. The surface tension and viscosity data obtained so far
are remarkable in a sense that they provided several data,
unknown before the advent of electrostatic levitation, and that,
all the way up to tungsten (>4000 K). However, some scatters still
appear in the viscosity data due to the motion of the sample upon
exciting the drop oscillation as the feedback control system tends
to bring back a perturbed sample to its original position. This issue
still needs to be addressed to allow more rene experiments.
Moreover, since the electrostatic scheme does not input any heat, a
high temperature sample in vacuum experiences pure radiative
cooling when the heating sources are shut off. From the
simplication of the energy equation governing the cooling, the

ratio of constant pressure heat capacity and hemispherical total
emissivity can be determined. Efforts are currently being pursued
to measure independently the hemispherical total emissivity and
to measure the isobaric heat capacity, for example by adding a drop
calorimeter to the levitator. Another problem is that when a
sample is molten, it becomes spherical with a smooth surface and
it is hard to measure its rotation frequency by current method.
Therefore, a novel technique is required to accurately measure the
rotation rate in the liquid phase and allow the measurement of the
electrical conductivity. Although a strong focus was devoted on the
thermophysical property measurements of refractory materials, in
particular elemental metals, over the last decades, the emphasis
will gradually shift toward the property measurements of
industrial ceramic and metallic alloys. Parallel efforts will also
continue in the arena of atomic structure characterization of liquid
and supercooled melts by neutron and synchrotron radiation
scattering.
Although several successes were achieved with the groundbased electrostatic levitation furnaces, difculties were faced
when handling iron, certain alloys, and oxides due to insufcient
electrical surface charges before the sample could reach the
melting point [297]. Reduced gravity conditions offered the
International Space Station would allow non-contact positioning
and processing of these materials or larger samples while
providing a quieter hydrothermal environment. This would
facilitate solidication studies of oxides and alloys as well as
the property measurements of materials of vital industrial
importance [298], and would help to further understand the uid
dynamics of drops [19,209,299]. The impact on solidication of the
modied ow within the molten sample in reduced gravity could
also be scrutinized. Even though the improved procedure for
viscosity measurement minimizes the effect of the positioning
force, the levitated sample cannot be free from external forces.
Microgravity is an ideal environment to alleviate this difculty
because no large forces will be needed to maintain the sample
position. Rather, only weak forces will be applied along the three
axes to counter the residual accelerations. Currently, an electrostatic levitator [63] is planned to be launched to the International
Space Station, and thermophysical property measurements in
microgravity will be conducted. This facility is expected to offer
viscosity data with higher accuracy. However, some questions
remain about how easy the surface tension measurement in
microgravity would be. This is because the drop charge (needed to
calculate the surface tension [29]) is determined by the levitation
conditions, which involve the gravitational acceleration, which, in
turn, virtually disappears in microgravity.
Experiments performed under microgravity would not only
help to address these issues but would also offer an attractive
platform to carry out nucleation and solidication studies from
deep supercooled phases. The resulting microstructure between
materials processed on the ground and those produced in orbit
could be compared and analyzed and could hopefully offer clues on
how to improve or optimize materials processing not only on Earth
but also in reduced gravity to, one day, support future Mankinds
efforts to colonize celestial bodies. This could also help to
understand the formation of planets and asteroids [300].
Acknowledgments
The authors (PFP, TI, and JTO) would like to express their
deepest gratitude to the Japan Society for the Promotion of Science
for their Grant-in-Aid for Scientic Research (B), and to Dr. J.K.R.
Weber (Materials Development Inc.) and Dr. K.C. Mills (Imperial
College) for several fruitful and challenging discussions over the
years. These authors are also thankful to personnel of AES Co. Ltd.,
G Model

especially Y. Watanabe, Y. Saita, and H. Tomioka for technical help

in numerous experiments and post-levitation microstructure
analysis. Part of the presented research (GWL) was supported
by the Converging Research Center Program through the Ministry
of Education, Science and Technology of Korea (2012K001240) and
by the Korea Research Institute of Standards and Science under the
project Establishment of National Physical Measurement Standards and Improvements of Calibration/Measurement Capability,
grant 13011001. The authors (DHM and JB) would like to
acknowledge DLR colleagues and collaborators, in particular J.
Gegner, D.M. Herlach, I. Kaban (IFW-Dresden), F. Kargl, S. Klein, T.
Kordel, G. Lohofer, N. Mattern (IFW-Dresden), T. Meister, A. Meyer,
C. Panofen, J. Peters (FRM-II, Garching), A.I. Pommrich, O.
Shuleshova (IFW-Dresden), M. Sperl, T. Unruh (FRM-II, Garching),
T. Voigtmann, and F. Yang for scientic cooperation as well as
several institutes (FRM-II (Garching), Hasylab@DESY (Hamburg),
and Institut Laue-Langevin (Grenoble)) for beam time allocation
and support. At last but not the least, one of the authors (PFP)
would like to dedicate this paper to his beloved mother, Francoise
(France) Gelinas Paradis, who passed away during the writing of
this paper. He will be grateful forever for her genuine and
continuous encouragement in the pursuit of his endeavors and for
showing him the path of creativity and achievement.
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