Experimental Mechanics (2010) 50:37–45
DOI 10.1007/s11340-008-9210-9
Nanomechanical Testing of Gum Metal
E.A. Withey & J. Ye & A.M. Minor & S. Kuramoto &
D.C. Chrzan & J.W. Morris Jr.
Received: 28 May 2008 / Accepted: 1 December 2008 / Published online: 24 January 2009
# Society for Experimental Mechanics 2009
Abstract “Gum Metal” is a newly developed β-Ti alloy
that, in the cold-worked condition, has exceptional elastic
elongation and high strength. The available evidence
suggests that Gum Metal does not yield until the applied
stress approaches the ideal strength, and then deforms by
mechanisms that do not involve conventional crystal
dislocations. To study its behavior, submicron-sized pillars
of solution-treated and cold-worked Gum Metal were
compressed in situ in a quantitative compression stage in
a transmission electron microscope. Solution-treated speci-
mens and half of the cold-worked specimens exhibited
essentially monotonic hardening during compression, but
with serrated load-deflection curves that included periodic
partial relaxations of the stress. The other cold-worked
specimens exhibited pronounced shear instability. These
samples deformed by a stick-slip motion along a well-
defined shear plane, with a serrated load-deflection curve
demonstrating partial stress relaxation at each sliding event.
E.A. Withey (*) : J. Ye : A.M. Minor : D.C. Chrzan :
J.W. Morris Jr.
Department of Materials Science and Engineering,
University of California,
Berkeley, CA 94720, USA
e-mail: ewithey@berkeley.edu
J. Ye : A.M. Minor
National Center for Electron Microscopy,
Lawrence Berkeley National Laboratory,
Berkeley, CA 94720, USA
S. Kuramoto
Toyota Central R&D Laboratories, Inc.,
Nagakute, Aichi 480-1192, Japan
The pattern of deformation is consistent with prior work
showing deformation by the formation and growth of shear
bands and faults in a matrix that is densely decorated with
defects.
Keywords Gum metal . Titanium . Sub-micron pillars .
TEM . Compression
Introduction
The ideal strength of a material is reached when its atomic
bonds become so stretched that they can no longer support
the applied load. At that point of elastic instability the
material must fracture or deform. The ideal strength in
shear can be computed from first principles and, for a body-
centered-cubic (bcc) metal, is about 11% of the shear
modulus [1]. However, most metals yield at stresses
significantly lower than their ideal strength due to the
motion of dislocations. In order for a metal to reach its ideal
strength, the dislocations within it must be so efficiently
pinned that they cannot move until the ideal strength is
exceeded.
In 2003, researchers at Toyota Central R&D introduced
an intriguing new class of β-titanium alloys, coined Gum
Metal, that after severe cold-working appear to deform at,
or near, their ideal strength [2]. These alloys were designed
to have a near-zero shear modulus in the <111> direction
[3], the weakest direction in the bcc structure [1, 4], and
have a generic composition Ti–24(Nb+Ta+V)–(Zr+Hf)–O
(at.%) [5]. Examples of Gum Metal include Ti–12Ta–9Nb–
3V–6Zr–1.2O, Ti–23Nb–0.7Ta–2Zr–1.2O, Ti–20Nb–
3.5Ta–3.4Zr–1.2O (at.%). After extreme cold-working
38
(∼90%), these alloys display a number of “super” properties
including super elasticity, high strength, super cold-
workability, and Invar (low thermal expansion coefficient
over a temperature range) and Elinvar (constant elastic
modulus over a limited temperature range) properties [2].
Gum Metal is currently used in eyeglass frames, as
precision screws and fishing line, and in tennis rackets
and golf clubs. Given its low elastic modulus and high
strength, future biomedical, automotive, and aeronautical
applications are expected.
In the solution-treated (ST) condition, Gum Metal has a
microstructure and a set of properties that resemble other
bcc alloys: large equiaxed grains, ∼50–100 μm in diameter,
and a stress–strain curve with linear–elastic behavior
followed by yielding. In contrast, cold-worked (CW) Gum
Metal has a marble-like optical microstructure, which, on a
smaller scale, appears as fuzzy domains ∼200 nm in
diameter with ill-defined boundaries each rotated slightly
with respect to its neighbors. The tensile stress-strain curve
includes a large elastic deformation that becomes non-linear
before yielding. The plastic elongation is appreciable, but
includes very little hardening.
According to Gutkin et al., the formation of the marble-
like structure develops through the formation of and shear
along “giant” faults, which are defined planar regions
∼1 nm thick within which localized plastic strain reaches
thousands of percent [6]. These defects were first seen by
Saito et al. while pulling ST Gum Metal in uniaxial tension
to 10% strain [2]. The direction of the faults was ∼45° from
the tensile axis, but did not parallel typical slip planes or
slip directions for the bcc structure. Subsequent investiga-
tion of giant faults and their role in developing the
microstructure of CW Gum Metal showed that as the
amount of work increased, the faults became visible across
the large grains of the ST Gum Metal [5, 6]. Giant faults
were not observed to penetrate the high-angle grain
boundaries, but did produce steps in the grain boundaries
they intersected. Near the giant faults, the orientations of
the grains were rotated from their original orientations. As
the amount of work increased further, the grains became
more elongated and serrated eventually leading to the
marble-like structure seen in 90% CW Gum Metal.
Prior work in this laboratory (Withey et al. [7]) on the
nanoindentation of one composition of Gum Metal in
the ST condition revealed thick arrays of dislocations in
the peripheries of the indentation pits, while the fuzzy
domains typical of cold-worked material filled the severely
deformed volume along the sides and bottoms of the pits.
The dislocations were dipoles connected by tightly serrated
end segments indicating the presence of nanoscaled
obstacles spaced ∼25 nm apart. Parallel theoretical work
(Li et al. [8]) found that the obstacle spacing required to pin
dislocations at stresses above the ideal strength of Gum
Exp Mech (2010) 50:37–45
Metal is on the order of 10 nm. Thus, the microstructure is,
at least, generally consistent with the requirements for a
material to reach its ideal strength. However, the nature of
the obstacles that pin the dislocations remains unclear.
The domain structure inside the nanoindentation pits
studied in [7] mimicked the microstructure of the material
in the CW condition. Examination of this structure in both
bulk and deformed CW and deformed ST Gum Metal
samples has shown that there are slight rotations from one
domain to the next suggesting that there is a nearly
continuous rotation across multiple fuzzy domains. The
structure of the boundaries between domains is not yet
clear.
In the work reported here the mechanism of plastic
deformation of Gum Metal in the ST and CW conditions
was investigated by compressing sub-micron-sized pillars
of Gum Metal in an indentation stage mounted in a
transmission electron microscope (TEM). This technique
was chosen because it allows the deformation process to be
followed in situ in samples whose small size ensures that
internal stresses are reduced and substantial heterogeneities
are avoided.
Experimental Procedure
Gum Metal with a composition of Ti–35.9Nb–2Ta–2.7Zr–
0.3O (wt.%) was obtained from Toyota Central R&D
Laboratories, Nagoya, Japan in the form of two 4 mm
diameter rods. Each rod was processed from elemental
powders cold isostatically pressed into cylindrical form
before sintering at 1,300°C and hot forging at 1,150°C in
air, and solution-treating at 900°C in Ar. Rods were then
cold-rotary swaged by 90%. One rod was subsequently
solution-treated a second time at 900°C for 30 min, thus
producing one CW or cold-rotary swaged rod and one ST or
solution-treated rod [9].
Sections of each rod were cut parallel to the swaging
direction (rod axis) with thicknesses of ∼500 μm. These
sections were mechanically thinned to ∼20 μm and attached
with super glue to a copper substrate. They were then
machined in a FEI 235 dual focused ion beam (FIB) using
an annular pattern and low current (∼10 nA) to produce
cylindrical pillars 100–200 nm in diameter. Each pillar had
a sidewall taper of 4–5° defined by the angle of the sidewall
with respect to the axis of the pillar, and length up to 1 μm.
The copper substrate with the attached Gum Metal
pillars was placed in a Hysitron PicoIndenter® stage in
a JEOL 3010 TEM located in the National Center for
Electron Microscopy (NCEM) at the Lawrence Berkeley
National Laboratory. The PicoIndenter® is equipped with a
boron-doped diamond flat punch tip with an area much
larger than the contact areas of the pillars. The indentation
Exp Mech (2010) 50:37–45 39

Results

During the compression of both ST and CW pillars, stress

and deformation was localized at the tops of the pillars
apparently due to their sidewall tapers. All pillars had a
speckled appearance before compression, which was
ascribed to damage on the outside layer of the pillars due
to FIB processing. The density of these speckles differed
with local orientation of the pillars.
The basic results of the compression experiments are
documented in Figs. 2, 3 and 4, which illustrate the two
distinct behavioral patterns that were observed. Each figure
compares load–displacement curves for two metallurgically
similar samples that exhibited similar behavior. In each
case, the deformation of the two samples is compared at
roughly similar stages of overall deformation by extracting
frames from the test films. The three frames were taken at
the points indicated on the load deflection curves. The
deformation patterns are compared directly in Fig. 5.
Figure 5(a) shows sample load deflection curves corre-
sponding to the superimposed traces of the sample profiles

Fig. 1 (a) Indentation stage and (b) TEM image of the flat punch and
an ST pillar after a compression test showing the large size of the
punch compared to the pillar

stage and flat punch are shown in Fig. 1(a) and (b),
respectively. Load and displacement resolutions were,
nominally, 0.1 μN and 0.5 nm, respectively. More detailed
information about the PicoIndenter® can be found in [10].
Before each compression experiment, diffraction patterns
were taken from several locations on the pillars to charac-
terize their initial microstructure and orientation to be
compared with their microstructure and orientation after
compression. Each compression test was done under
displacement control at a displacement rate of 20 nm/s in
either bright-field or dark-field imaging modes. The com-
pressions were recorded in real time at 30 frames per second
by a camera within the microscope. Load–displacement data
was measured continuously throughout each test by a
Fig. 2 (a) Load–displacement data for two ST pillars with the black
feedback loop in the indentation stage, and matched frame- data corresponding to the frames extracted in (b–d) and the grey data
by-frame with test film. to those in (e–g)
40 Exp Mech (2010) 50:37–45

region of deformation which is defined by a scallop on

the edge of the deformed pillar. The diffraction patterns of
the deformed regions of the ST pillars [Fig. 6(b)] are
streaked to form a broken ring pattern about the <110> zone
axis, in contrast to the sharp diffraction spots in the <110>
zone axis orientation of the pillar before deformation
[Fig. 6(a)] indicating the formation of several new domains.
The deformed regions are, slightly rotated from their original
orientation, as was previously observed in studies of ex-situ
nanoindentation [7].
Figure 2(e–g) shows the comparable behavior for the
other ST pillar. In this case multiple streaks also appear, but
are roughly perpendicular to the pillar axis. Given the
similarity of the two load-deflection curves, we believe that
the slip lines are at 45° to the axis in this case as well, but
are oriented into the plane of the figure.
The serrated load-deflection curves measured on these
specimens are not unusual. However, the serrations
observed here are significantly less pronounced than those
seen in prior pillar compression tests of more conventional
crystalline materials [10]. The pronounced load drops
observed in the prior tests could usually be associated with

Fig. 3 (a) Load–displacement data for two non-sliding CW pillars

with the black data corresponding to the frames extracted in (b–d) and
the grey data to those in (e–g)

shown in Fig. 5(b–d) taken at three similar points along the

load deflection curves.
Figures 2 and 3 show sets of ST and CW specimens
that have roughly similar behavior. The load–displacement
curves have a serrated stair-step shape that shows a general
hardening trend with periodic load drops.

Solution-Treated (ST) Specimens

The load-deflection curves of the two ST pillars virtually

superimpose for the first 80 nm of displacement [Fig. 2(a)].
The general hardening trend is punctuated by a few
significant load drops interspersed with regions of slight
softening where the load appears to decrease linearly with
increasing displacement before increasing to another local
maximum. The softening portion of the curve persists over
about 15–20 nm of displacement, and terminates in a well-
defined minimum. Figure 2(b–d) and (e–g) shows the
corresponding frames of the video for each of the two
pillars. In Fig. 2(b–d), as the flat punch compresses the pillar,
four dark streaks form at approximately 45° to the pillar Fig. 4 (a) Load–displacement data for two non-sliding CW pillars
axis. Closer investigation of still images taken after with the black data corresponding to the frames extracted in (b–d) and
compression [Fig. 6(b)], show that each streak borders a the grey data to those in (e–g)
Exp Mech (2010) 50:37–45 41

Fig. 5 (a) Load displacement curves for ST, non-sliding CW, and sliding CW pillars indicating the points from which the traces of the respective
pillars are shown in (b), (c), and (d)

bursts of dislocation activity, producing a spontaneous
stress relaxation that essentially relieved the imposed load.
Since no dislocation motion was directly observed during
the compression of the ST pillars, it is difficult to say
whether the load drops seen here were due to dislocation
mobility or to some other mechanism. However, the sample
does not relax in obvious bursts; the relaxation is gradual
and stops while the sample remains under significant load.
The deformation mechanism appears to involve the gradual
growth of planar “shear bands” against a significant resis-
tance that leads to an overall monotonic hardening.
Cold-Worked (CW) Specimens: Monotonic Hardening
The cold-worked specimens exhibited two very different
patterns of behavior during pillar compression: monotonic
hardening (Fig. 3) and “shear instability” (Fig. 4).
The load-deflection curves of two CW samples that
exhibited monotonic hardening are shown superimposed in
Fig. 3 along with captured frames that show the change in
shape during deformation. A sequential trace of the profile
of the specimen associated with the black curve in Fig. 3 is
shown in Fig. 5(c). Before and after pictures of the
specimen that produced the load-deflection curve that is
colored gray in Fig. 3 are shown in Fig. 7.
As in the case of the solution-treated material, the two
load-deflection curves almost superimpose. As in the ST
case, the curves are serrated. But the serrations are much
less pronounced; the load drops are smaller. Deformation is
narrowly confined to the sample tip. As the indentation
proceeds, the pillar slowly and progressively develops a
sheared “foot”. The slow development of the deformation is
evident from the superimposed sample profiles in Fig. 5(c);
the sheared tip is most apparent in the post-test micrograph

Fig. 6 TEM images taken

(a) before and (b) after com-
pression of the ST pillar shown
in Fig. 2(b–d). The top diffrac-
tion pattern in (b) corresponds
to the deformed volume of the
pillar and the bottom to the
undeformed volume. The dif-
fraction pattern in (a) gives the
orientation of the pillar
before deformation
42 Exp Mech (2010) 50:37–45

Fig. 7 TEM images taken (a) before and (b) after compression of the CW pillar shown in Fig. 3(e–g). The top diffraction pattern in (a)
corresponds to the first third of the pillar from the tip and the bottom pattern from the second third. In (b) the top pattern corresponds to the
deformed volume of the pillar and the bottom pattern to the volume right below the deformed region

in Fig. 7(b). The diffraction patterns included in Fig. 7
show that this sample contained at least two crystallographic
domains. The upper domain is severely deformed, and its
diffraction pattern shows spots that are slightly streaked.
The lower domain appears unchanged. The profile of the
sheared tip bears a general resemblance to the final
profile of the ST sample in Fig. 6(b), but the boundary
between the sheared and unsheared material is much
sharper in this case.
Cold-Worked (CW) Specimens: Shear Sliding
The load-deflection curves of the two samples that
exhibited shear sliding are plotted in Fig. 4, along with
micrographs that were taken at critical points in the defor-
mation to illustrate its pattern. The pillar in Fig. 4(b–d)
show an obvious shear instability; a section of the sample
tip is displaced by sliding on a narrow shear band angled
∼45° to the pillar axis. The development of the offset is
shown in the superimposed traces in Fig. 5(d). The final
configuration of the offset sample is shown in Fig. 8(b),
along with the relevant diffraction patterns. The second
sample, in Fig. 4(e–g), appears to have deformed by a
similar shear instability, but in this case the plane of shear is
angled into the plane of the figure and was difficult to
image in the TEM.
The load-deflection curves for these specimens are
serrated, like the curves for the ST specimens in Fig. 2,
but differ in three important respects. First, the loads are
significantly smaller (both ST pillars and the sliding CW
pillars had similar initial diameters), reflecting the ease of
deformation along the well-defined shear band. Second,
there is little monotonic hardening. In fact, the sample in
Fig. 4(b–d), that develops the visible shear offset, softens in
the later stages of its compression. This is presumably due
to the decreasing area of contact on the plane of shear.
Third, the depths of the serrations are comparable to those
in the ST samples and significantly greater than those in
the CW samples in Fig. 3, but have a very different
significance than in the ST pillars. In the ST samples the
successive minima in the load–displacement curves appear
to be associated with the formation of spatially discrete slip

Fig. 8 TEM images taken (a) before and (b) after compression of the CW pillar shown in Fig. 4(b–d). The top diffraction patterns in (a) and (b)
correspond to the top domain, the domain that slid, and the bottom patterns are taken from the second domain from the top of the pillar
Exp Mech (2010) 50:37–45
bands, while in the CW specimens they appear to be due to
a frictional stick-slide motion on a narrow, well-defined
shear plane. The effective friction that opposes this sliding
is, apparently, considerable since the sample supports a
significant load even at the minima of its serrations.
The diffraction patterns in Fig. 8 show that the offset
sample in Fig. 4(b–d) has multiple domains. The severe
deformation is confined to the domain at the sample tip.
The apparent planarity of the shear band and its orientation
near 45° from the tensile axis suggests that it is confined to
a single domain and does not cross the boundary.
Discussion
Patterns of Deformation
The results show that the indentation of Gum Metal
produces at least two distinct deformation patterns: the
monotonic hardening pattern observed in the solution-
treated and two of the four cold-worked specimens, and
the shear instability experienced by the other two cold-
worked specimens.
The reason for the different behaviors of the cold-
worked specimens appears to be crystallographic. Figures 7
and 8 include micrographs of the specimen in Fig. 3(e–g),
which showed monotonic hardening, and the specimen in
Fig. 4(b–d), which exhibited the clearest shear instability,
respectively. In both cases <110> and <112> directions are
in the plane of the figure, taken from the diffractions patterns
near the sample tip. The {110} and {112} preferred slip
planes are, of course, perpendicular to these directions.
Figure 8 shows that the well-defined slide plane of the pillar
is parallel (or nearly so) to the trace of the (110) close-
packed plane, a preferred plane for the formation of a sharp
shear band like the one that developed in the sample.
Figure 7 does not include a similar plane for the mono-
tonically hardened CW pillar, though the post-test data,
which includes the deformation-induced rotations of the
crystal axes, suggests that the severely deformed material at
the tip has rotated so that the deformed region is bounded by
a {110} plane.
While this crystallographic explanation seems persua-
sive, it is not sufficient to explain all of the data. For
example, the ST sample shown in Fig. 2(b–d) also had a
{110} plane oriented for easy shear, and the sample does
appear to shear on this plane. But the shear appears on
multiple {110} planes, leading to a more diffuse deforma-
tion that does not produce a sharp offset like that in CW
pillars that had distinct sliding.
Moreover, work by Shan et al. [11] includes evidence
that crystallographic slip is not necessarily required to
produce the well-defined offsets seen here. In their study,
43
the compression of submicron-sized pillars of metallic glass
led to the formation of a shear band along which the
majority of subsequent deformation seemed to occur
through the offset of the top of the pillar at an angle to
the base of the pillar. Like the sliding tip, the offset of the
top of the metallic glass pillar moved jerkily in spurts
accompanied by large load drops.
Hardening
A second interesting feature of the compression behavior is
the frictional resistance to shear and the pronounced
hardening that follows it. In typical in situ TEM deforma-
tion experiments on crystalline materials, the deformation
occurs primarily through a series of bursts in which
dislocations or showers of dislocations are generated and
flow relatively freely through the crystal. This is not the
case in Gum metal. Even the most pronounced serrations
relax only part of the applied load, indicating a substantial
resistance to shear, and the relaxation is followed by a
pronounced and continuous hardening (the only apparent
exception—the macroscopic softening of the CW pillar in
Fig. 4(b–d)—is almost certainly a geometric effect due
to the decreasing area of contact in the shear plane). Since
the diffraction patterns of the material in these submicron-
sized pillars are well-defined before deformation occurs,
this behavior cannot be attributed to residual stresses or
lattice distortions, even in the severely cold-worked
material.
Prior work [7] has shown that the matrix of ST Gum
metal is densely decorated with features that strongly resist
dislocation glide. While the precise nature of these obstacles
remains unclear, they appear to be responsible for the
suppression of dislocation activity in the cold-worked
material. Assuming that those obstacles are present and
active in these samples (though they are not resolved in the
diffraction patterns) they provide an obvious source for the
friction and hardening that occurs in these tests.
Deformation Mechanism
There are three mechanisms that may be relevant to the
deformation of Gum metal: dislocation plasticity, micro-
shearing leading to shear bands, and phase transformations.
Dislocation plasticity plays some role in the deformation of
the solution-treated material, but has not been observed in
cold worked specimens. Microshears and shear bands are
reasonably well documented in both solution-treated and
cold-worked material [2, 6]. There is preliminary evidence
for phase transformation during deformation, both to
nanoparticles of ω-phase and to a reversible orthorhombic
phase (Dye D, private correspondence, 2008). While these
likely play a role in the elastic deformation there is no
44
clear evidence of their contribution to bulk plasticity
(Khachaturyan AG, private correspondence, 2008).
The presence and persistence of sample preparation
damage (FIB damage) prevented the direct observation of
the deformation mechanism during these tests. On the other
hand, the very persistence of that damage, which consists
largely of dislocation loops, indicates that dislocations are
not mobile in these specimens. In pure monocrystalline
pillar specimens, the FIB damage is swept out of the
specimen in the earliest stags of compression [10]. Further,
there is no clear evidence of ω-phase or orthorhombic
phase in the post-test diffraction patterns, even after
extensive deformation. It therefore appears that the defor-
mation occurs primarily through the formation of micro-
shears or shear bands, as previously observed for bulk
deformation [2, 5, 6]. The difficulty of developing planar
shear in a microstructure that is densely decorated with
nanoparticles would then explain the significant friction
that opposes deformation, particularly when no crystallo-
graphically preferred shear plane is well oriented for slip.
Strength
One of the most interesting features of Gum metal is its
very high strength, particularly in the cold worked state,
which approaches the predicted ideal strength of the
material. That strength is apparent in these pillar compres-
sion tests. The ST pillars reach near ideal strengths and the
CW pillars have strengths just over half of the measured
strengths of the ST pillars.
If we estimate the yield strength of the pillars by
dividing the load at the first indication of plastic deforma-
tion by the cross-sectional area of the pillar at its apex, the
highest yield strengths are those of the ST specimens
(2,900–3,600 MPa), followed by the monotonically hard-
ening CW samples (∼1,900 MPa), followed by the speci-
mens that deform by planar sliding (1,600–1,900 MPa).
This is opposite of bulk behavior where the CW material
yields at a higher strength than the ST material. This
suggests a stronger size effect in the solution-treated Gum
Metal. It is strongly suspected that the lower yield strength
of the CW pillars is due to residual stresses retained in the
material by the domain structure. While the source of this
early yielding in the CW pillars is not clear, the pattern of
deformation suggests that shear instabilities emanate from
free surfaces and propagate along well-defined planes.
Since the geometry of the sample and indenter are not
perfectly controlled, there is the possibility that large stress
concentrations develop on first contact, generating local,
planar instabilities that propagate, driven by the stress
concentration at the periphery. Resolution of this issue will
require further investigation.
Exp Mech (2010) 50:37–45
On the other hand, as discussed above, the pattern of
deformation suggests that deformation occurs by local shear
rather than dislocation glide, which is consistent with
deformation at the limit of elastic stability.
Conclusions
Submicron-sized pillars of Gum Metal were compressed in
situ in a quantitative compression stage in a transmission
electron microscope. The samples included solution-treated
and heavily cold-worked Gum Metal; the latter condition
leads to and exceptionally high strength in bulk material
that may reach the ideal strength of the material. The load-
deflection curves and deformation patterns of the samples
show two rather different responses. The two solution-
treated specimens and two of the four cold-worked speci-
mens exhibited essentially monotonic hardening during
compression, but with serrated load-deflection curves that
included periodic, partial relaxations of the stress. The other
two cold-worked specimens exhibited pronounced shear
instability, with the samples deforming by a stick–slip
motion along a well-defined shear plane, with a serrated
load-deflection curve with partial stress relaxation at each
sliding event. While the defects that produced deformation
could not be observed directly, the pattern of deformation is
consistent with prior work showing deformation by the
formation and growth of shear bands and faults in a matrix
that is densely decorated with defects. This pattern is
consistent with deformation at the limit of strength.
However, in the CW pillars the estimated stresses at yield
are well below the predicted values at the limit of strength.
The low strength may be due to geometric or surface effects
that are not yet understood.
Acknowledgements This research was supported by the National
Science Foundation under Grant DMR 0706554 and by Toyota Motor
Corporation under a grant to the University of California Berkeley.
EW also acknowledges support from NSF through a graduate research
fellowship. Research at the National Center for Electron Microscopy
was supported by the Scientific User Facilities Division of the Office
of Basic Energy Sciences, U.S. Department of Energy under Contract
# DE-AC02-05CH11231.
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