Scripta Materialia 51 (2004) 825830

www.actamat-journals.com

Performance and applications of nanostructured materials

produced by severe plastic deformation
a,*
Yuntian T. Zhu , Terry C. Lowe a, Terence G. Langdon b

a
Los Alamos National Laboratory, Materials Science; Technology Division, MS G755, Los Alamos, NM 87545, USA
b
Departments of Aerospace & Mechanical Engineering and Materials Science, University of Southern California, Los Angeles, CA 90089-1453, USA
Accepted 4 May 2004
Available online 4 June 2004

Abstract
Nanostructured materials produced by severe plastic deformation can be tailored to have both superior performance and
superior properties. These materials are attractive for use in a range of applications from biomedical to aerospace industries.
2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Applications; Manufacturing; Nanostructured materials; Severe plastic deformation

1. Introduction tion domains (crystallites), which are often smaller than

Nanostructured (NS) materials are dened as solids
having microstructural features in the range of
1100
nm in at least one dimension [1]. Two complementary
approaches have been developed in attempts to synthe-
size NS solids. The rst is the bottomup approach in
which bulk NS materials are assembled from individual
atoms or from nanoscale building blocks such as nano-
particles. Techniques in this category include inert gas
condensation [2], electrodeposition [3], and chemical and
physical deposition [4].
The second approach is the topdown approach in
which existing coarse-grained materials are processed to
produce substantial grain renement and a nanostruc-
ture. The most successful topdown approach in-
volves the use of severe plastic deformation (SPD)
processing in which materials are subjected to the
imposition of very large strains without the introduction
of concomitant changes in the cross-sectional dimen-
sions of the samples. Materials produced by SPD tech-
niques usually have grain sizes in the range of 1001000
nm. However, they have subgrain structures, such as
subgrains, dislocation cells and X-ray coherent dirac-
*
Corresponding author. Tel.: +1-505-667-4029; fax: +1-505-667-
2264.
E-mail address: yzhu@lanl.gov (Y.T. Zhu).
1359-6462/$ - see front matter 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2004.05.006
100 nm. Therefore, they can be called NS materials [5].
Several SPD processing methods are now available,
including equal-channel angular pressing (ECAP) [6,7],
high-pressure torsion [5,8], accumulative roll-bonding
(ARB) [9,10], repetitive corrugation and straightening
[11,12], and friction stir processing (FSP) [13,14]. At-
tempts have also been made to combine some of these
procedures such as ECAP and cold rolling [15], ARB
and FSP [16] or ECAP and HPT [17,18]. An overall
review of these various techniques suggests that, at least
in terms of the commercial viability of the processing
route and the nature of the microstructures attained to
date, processing by ECAP has at least two advantages
that favor its adoption into manufacturing practice.
Firstly, it can be scaled up to produce relatively large
bulk samples [19,20]. Secondly, several groups have
incorporated it into conventional rolling mills for con-
tinuous processing [2123].
Processing through the use of SPD techniques pro-
vides the capability of producing large, bulk NS mate-
rials that may be utilized in structural applications. The
incorporation of ECAP into continuous production
techniques also holds out the promise of producing NS
materials with a competitive low cost. Current costs to
produce 520 mm diameter round bar of NS titanium
and titanium alloys by non-continuous ECAP range
between $50 and $150/kg. These costs are comparable to
those for intensive thermomechanical size reductions of
826 Y.T. Zhu et al. / Scripta Materialia 51 (2004) 825830
conventional metals as in, for example, the production
of wire. However, they are not competitive for many
larger-dimension higher-volume applications. As in any
commercialization, a successful combination of high
performance and low cost will be the factor that ulti-
mately determines whether NS materials move from the
laboratory to widespread industrial utilization. The
fabrication rate is a key determinant of nanomaterial
cost, ranging from a fraction of a nanometer/second
(nm/s) for synthesis using a scanning tunneling micro-
scope, to hundreds of nm/s for electroless forming, to
thousands of nm/s for photo-electroforming, to millions
of nm/s for conventional machining and forming. Thus,
SPD has a signicant potential for producing NS
materials at rates, and therefore at costs, comparable to
conventional material production methods.
In this paper, we shall focus on the performance and
possible applications of NS materials produced via SPD.
More specically, we shall focus on their mechanical
properties and structural applications. Nanostructured
and amorphous materials produced by other methods
and their physical properties will also be discussed
briey.
2. Performance
NS materials have unique mechanical and physical
properties which are derived from their unique micro-
structures. These properties make them attractive for
many potential commercial applications.
2.1. Strength and ductility
The strength of a coarse-grained material usually
follows the well-known HallPetch relationship,
r r0 Kd 1=2 , where r is the strength, d is the grain
size, and r0 and K are constants. NS materials deviate
from this relationship, with slower strength increase
(smaller K) as the grain size decreases. Below a certain
critical grain size, an inverse HallPetch relationship is
observed [24]. To have the desired combination of high
strength and high ductility for structural applications,
smaller grains are not always desired. Ductility usually
decreases with decreasing grain size in NS materials. NS
metals and alloys with grain sizes less than 20 nm or
amorphous alloys may have both lower strength and
lower ductility than materials with larger grain sizes.
There exists an optimum grain size range in which a NS
material has both high strength and good ductility.
The processing method also aects the strength and
ductility. NS materials produced by consolidation of
nanopowders usually are very brittle due to defects such
as oxidation, trapped gas and porosity [25]. Electrode-
posited NS lms may also be brittle due to impurities
from the electrolyte. NS materials produced by SPD
techniques are contamination-free and porosity-free so
that they usually have high strength and good ductility.
It can be shown that SPD processing decreases the
ductility to a smaller extent than conventional defor-
mation processes such as rolling, drawing and extrusion.
For example, experiments were conducted to compare
the strength and ductility of the 3004 aluminum alloy
processed by ECAP and cold rolling [26]. It was found
that processing by ECAP led to a greater retention of
ductility than cold rolling. In practice, the higher duc-
tility of materials processed by ECAP is a very attractive
characteristic for structural applications.
Some NS materials produced by SPD have been
found to have an extraordinary combination of both
high strength and high ductility. For example, pure Cu
processed via ECAP for 16 passes with a back-pressure
has a ductility close to that of coarse-grained Cu while at
the same time having a yield strength that is several
times higher [27]. High strength and good ductility
rarely exist simultaneously in any material. Therefore,
this combination is very attractive for advanced struc-
tural applications in areas such as aerospace and
sporting goods. Unfortunately, the mechanism for
achieving such good mechanical properties is not yet
understood although it is generally recognized that the
mechanical behavior of materials is determined by the
deformation mechanisms, which in turn are controlled
by the nature of the microstructures.
Some progress has been made recently in under-
standing these deformation mechanisms. For example,
the emission of partial dislocations from grain bound-
aries and the occurrence of stacking faults and defor-
mation twinning in NS aluminum provides a sharp
contrast to the behavior of coarse-grained aluminum
where twinning is absent [28,29]. Another example is NS
copper, which was found to twin abundantly when de-
formed under HPT at room temperature and low strain
rate [30]. In contrast, coarse-grained copper did not
deform by twinning under the same deformation con-
dition [31]. The low ductility of NS materials has been
attributed to their low work hardening because their
small grain sizes do not accommodate further disloca-
tion accumulation [32]. The twinning could be utilized to
increase work hardening of NS materials and to conse-
quently improve their ductility.
2.2. Other mechanical properties
Although strength and ductility are the two most
important mechanical properties, there are other
important properties for structural applications includ-
ing fracture toughness, fatigue strength and wear resis-
tance.
To date, the fracture toughness has not been studied
in NS samples because the measurements require large
samples in order to reach the required plane strain
 Y.T. Zhu et al. / Scripta Materialia 51 (2004) 825830
condition. It is reasonable to anticipate this will become
feasible within the next few years as facilities are
established to produce larger samples through SPD
techniques.
The fatigue strength is another important mechanical
property but the studies reported to date are fairly
limited. Preliminary investigations suggest that most
SPD-processed metals have an enhanced high-cycle fa-
tigue life but a shorter low-cycle fatigue life [33]. The
explanation for this trend lies in observations that the
high-cycle fatigue life correlates strongly with strength
whereas the low-cycle fatigue life correlates strongly
with ductility and, as already documented, NS metals
usually have higher strength and lower ductility than in
their coarse-grained counterparts. Moderate annealing
after SPD processing may improve the ductility without
signicantly sacricing the strength, thereby improving
the low-cycle fatigue life. Surface hardening techniques
such as shot-peening are generally eective in improving
the fatigue life of coarse-grained materials but appear to
be ineective in improving the fatigue life of NS mate-
rials [20].
Since NS materials have a higher hardness than their
coarse-grained counterparts, it is reasonable to antici-
pate an increased wear resistance. This is supported by
recent experiments on NS low-carbon steel where the
wear resistance was increased [34]. In addition, NS
materials have lower friction coecients [34,35].
2.3. Thermal stability
NS materials are expected to have low thermal sta-
bility because of their high densities of crystalline defects
such as grain boundaries and dislocations. Surprisingly,
most NS metals produced by SPD exhibit relatively
good thermal stability. For example, NS commercially-
pure Ti processed by ECAP and cold rolling can be
annealed at temperatures below 400 C without a sig-
nicant decrease in the strength [36]. Thus, NS pure Ti is
suciently thermally stable for most applications
including for use as medical implants. Materials pro-
duced by cryogenic ball-milling have even more stable
NS structures. For example, an NS AlMg alloy pro-
cessed by cryogenic ball-milling in liquid nitrogen has
been reported to maintain the NS structure after
annealing at temperatures higher than 250 C [37],
which is remarkable considering the low melting tem-
perature of Al alloys. It can be shown that low tem-
perature annealing is benecial in NS materials
produced by SPD techniques because it signicantly
improves the ductility without markedly aecting the
strength. This provides an opportunity to combine the
deformation and annealing to make stable and strong
metals and alloys, as demonstrated in a recent example
with Cu [38].
827
2.4. Corrosion resistance
Little information is available to date on the corro-
sion resistance of NS materials. However, there is evi-
dence that NS Ti has better corrosion resistance than
coarse-grained Ti [39]. Several researchers have reported
no signicant dierence in the corrosion resistance of
NS materials by comparison with their coarse-grained
counterparts and the enhancement in the corrosion
resistance of NS Ti is probably due to the more uniform
nature of the corrosion. In coarse-grained Ti the disso-
lution of the material is heavily concentrated at the grain
boundaries because they have a higher energy than in
the grain interior; but in NS Ti the high defect density
inside the grains tends to equilibrate the energies across
the material, leading to a more uniform corrosion.
2.5. Physical properties
Amorphous and NS solids also have unique optical
and magnetic properties [2]. As the grain sizes change
from amorphous to the nanometer range, the solids will
change color and/or transparency [2,40]. Amorphous Fe
and Co-based alloys have very good soft magnetic
properties [2] and can be cast into cylinders or melt-spun
into ribbons [4]. NS magnetic materials are found to
have lower Curie temperature and lower saturation
magnetization than their CG counterparts [4,6].
Attractive soft magnetic properties are observed in NS
Fe-based alloys [4]. They can be made with specic core
loss, time variability of core-loss, and low magneto-
striction that are desired for high frequency transform-
ers, magnetic heads, etc. [2].
3. Applications
The potentials for using NS materials in structural
applications are being driven primarily by two separate
factors: (1) superior properties and (2) superior manu-
facturability. NS materials produced by SPD have the
greatest potential for large-scale industrial applications
because they make use of equipment that has many
similarities with that used in conventional deformation
processing, thereby incurring only a relatively modest
investment in capital equipment. It should be noted also
that, since SPD processing may produce metals having
characteristics that are only modestly dierent from
conventional metals, there is a low initial risk in the
utilization of SPD metals although the payo over time
may be very high. Another signicant advantage of the
SPD processing is its capability of producing bulk, large
NS material stocks for real structural applications. For
example, ECAP has been used to produce large Ti billets
(see Fig. 1) [20].
828 Y.T. Zhu et al. / Scripta Materialia 51 (2004) 825830
Fig. 1. An ECAP-processed Ti rod, which is about 50 mm in diameter
and 170 mm in length. The unit on the ruler is inch.
3.1. Applications driven by superior properties
It is generally easier to process the lower strength
metals such as Al or Cu. Also, a more thorough
knowledge base is currently available for these metals
[18]. For the SPD processing of Al and Cu, special
applications requiring limited-production volumes will
undoubtedly initiate the rst applications of these
materials. Later, after the economics of SPD processing
are well established, it is reasonable to assume that high-
volume production will become attractive. Lightweight
structures of Al alloys, as in weight-sensitive products
such as aircraft, bicycles, automobiles and boats, will
probably appear rst. Limited production demonstra-
tions for components manufactured in small volumes
will lead the way. One example is bicycle components.
For both mountain bikes and road racers, the added
strength achievable in the SPD-processed alloy equates
directly to weight savings in the structural frame tubing
and hardware components such as the gearing, pedals,
shifters, rims and spokes. Since the cost of bicycle
frames purchased by enthusiasts can often exceed $3000,
there is ample opportunity for incorporating high-per-
formance materials into these specialist applications.
Other early uses of SPD metals will develop for
applications where there are strong market drivers. For
example, there is a high level of competition and inno-
vation with advanced materials in the medical device
industry and this is supported by the growing societal
interest in products that extend or enhance the quality of
life. One example is plate-implants for bone osteosyn-
thesis made of NS Ti (see Fig. 2) [20]. The enhanced
fatigue performance that is possible in SPD metals is
particularly attractive for Ti and Ti alloys used for
prosthetics. Specic requirements for medical devices
are wide ranging, depending upon the impact that the
enhanced properties may have on the market advantage
that is imparted to a given product. Generally speaking,
an enhancement of greater than 25% over the properties
of conventional metals is necessary to motivate adopting
Fig. 2. Plate-implants for bone osteosynthesis made of nanostructured
Ti.
a new material. One specic example is the use of NS
pure Ti for dental implants. Typical implants have
diameters greater than 3 mm because the cyclic loads
associated with chewing can reach levels that push
conventional Ti towards the fatigue performance limit.
However, the small lower front teeth can be so closely
spaced that they require smaller diameter implants. By
introducing NS Ti possessing signicantly higher fatigue
strength, it will be possible to use 2 mm or smaller
diameter implants to replace the lower front teeth. For
dental implants, and many other medical devices, the
virtues of superior material properties are determined
not through specic materials properties requirements
or testing but through the fabrication of devices from
the new material and the subsequent simulated or in-
service evaluation of the performance of the device.
Thus it is critical to be able to fabricate manufacturing-
scale sizes and quantities of NS materials for evaluation
in specic applications.
The high strength of NS materials also makes them
ideal for making micro-devices and this is an exciting
and rapidly developing eld. For example, high strength
micro springs and gears have been made of NS NiMn
alloys via electrodeposition [3].
3.2. Applications driven by superior manufacturability
3.2.1. Machinability and forgability
For products that are directly machined to shape
from SPD-processed mill products, the feed rates and
cutting depths can be increased because of the manner in
which the deformation occurs under the machining
conditions. Processing by SPD leads to a smoother
surface nish and a reduction in tool wear. For some
specialized products, the largest portion of the cost may
be associated with the machining. For example, the ratio
of the machining cost to the material cost is greater than
a factor of 10 for some sporting goods products, thereby
creating a signicant incentive for reducing the
machining cost through material substitution. In some
cases the superior surface nish from machining of the
 Y.T. Zhu et al. / Scripta Materialia 51 (2004) 825830
SPD-processed metals may obviate the need for sub-
sequent surface nishing steps. This will reduce the
manufacturing cost by eliminating or simplifying the
processing steps. Forging is used to create product
shapes in the aerospace and automotive industry and
there is evidence that the forging temperatures can be
signicantly reduced when forging SPD-processed alu-
minum alloys for aerospace applications. In addition,
the times for subsequent heat treatments may be re-
duced by as much as 50%. Thus, for alloys with heat
treatments in excess of 12 h, the energy and time savings
are substantial.
3.2.2. Formability through superplasticity
The NS alloys processed by SPD can be formed su-
perplastically at lower temperatures and faster rates
than is possible in conventional superplastic alloys.
Superplasticity is a ow process in which polycrystalline
materials exhibit high elongations prior to ultimate
failure. This type of ow is the characteristic feature of
the superplastic forming industry in which complex
components, often having multiple curved surfaces, are
formed from superplastic sheet metals. The essential
requirements for achieving a superplastic forming
capability are small grain sizes, typically less than
10
lm, and high forming temperatures, typically above

0.5 Tm , where Tm is the absolute melting point of the
material. At the present time, the superplastic forming
industry occupies a small but viable cost-eective niche
through the production of high-cost low-volume com-
ponents associated primarily with the aerospace, archi-
tectural and sports industries [41]. Expansion beyond
this niche, into automotive and other high-volume
applications, is currently restricted by the slow strain
rates involved in the forming process (typically
103
s1 ) and the consequent long forming times (
2030
min) associated with the production of each separate
component.
The introduction of bulk NS materials provides a
potential for overcoming the inherent limitations asso-
ciated with conventional coarse-grained superplastic
materials. Thus, it is now well established, both theo-
retically and experimentally [42,43], that the rate of ow
within the superplastic regime varies inversely with the
grain size raised to a power that is close to
2. It is
anticipated, therefore, that a decrease in the grain size
by one order of magnitude will lead to an increase in the
optimal superplastic forming rate by approximately two
orders of magnitude and thus, in eect, the total forming
time will be reduced to
2030 s. It can be shown also
that this reduction in grain size will lead to the advent of
a superplastic forming capability which occurs at lower
temperatures than those generally associated with con-
ventional superplastic ow. Early experimental results
provided very clear demonstrations of the occurrence of
both high strain rate superplasticity [44] and low tem-
829
perature superplasticity [45] in bulk nanostructured
materials, where high strain rates refer to the tensile
testing of samples at rates at and above 102 s1 and low
temperatures refer to tensile testing at homologous
temperatures below 0.5Tm . For example, there are re-
ports of tensile elongations of up to >2000% at a strain
rate of 1 s1 in a ZnAl alloy processed by ECAP [46]
and the occurrence of superplasticity at homologous
temperatures as low as
0.36Tm for an electrodeposited
nickel [45].
The production of bulk nanostructured alloys in
sheet form, with ultrane grains that are fairly stable at
elevated temperatures, has the potential to expand the
superplastic forming niche into a processing regime that
will be eective in producing components for a very wide
range of commercial applications. The recent demon-
stration of the ECAP processing of plate samples [47]
suggests that it may be a fairly easy task to produce
superplastic NS materials that can be readily utilized in
forming operations. However, even in the absence of
sheet production, there are several potential applications
for these materials in bulk form: an example of current
interest is the production of superplastic seismic damp-
ing devices [48].
4. Summary and conclusions
1. Processing through the application of SPD is attrac-
tive for the production of bulk NS materials. These
materials can be tailored to exhibit both superior per-
formance and superior properties.
2. A primary advantage of SPD is the development of
materials having good machinability, forgability,
and formability at potentially low processing cost.
This makes these NS materials especially attractive
for use in specialized structural applications such
as medical implants, biomedical devices, and high-
performance bicycles. In the longer term, when
continuous-processing methods are developed, it is
reasonable to anticipate large-scale applications in
the automotive and other elds.
3. Amorphous and NS materials also have unique phys-
ical properties that are attractive for optical and elec-
trical applications. The high strength of NS materials
makes them ideal for micro-devices.
Acknowledgements
This work was supported by the US Department of
Energy IPP program (YTZ & TCL) and by the National
Science Foundation under Grant No. DMR-0243331
(TGL).
830 Y.T. Zhu et al. / Scripta Materialia 51 (2004) 825830
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