Materials Science and Engineering A 463 (2007) 238244

Superplasticity and cooperative grain boundary

sliding in nanocrystalline Ni3Al
N.A. Mara a, , A.V. Sergueeva b , T.D. Mara b , S.X. McFadden c , A.K. Mukherjee b
a
b

Center for Integrated Nanotechnologies, Los Alamos National Laboratory, Los Alamos, NM 87545, United States
Materials Science Division, University of California, Davis, One Shields Avenue, Davis, CA 95616, United States
c Sandia Laboratories, Livermore, CA 94550, USA
Received 31 March 2006; received in revised form 22 August 2006; accepted 26 August 2006

Abstract
Cooperative grain boundary sliding (CGBS) has been shown to account for the majority of macroscopic strain seen in microcrystalline metallic
systems undergoing superplastic deformation. While CGBS has been observed on the surface of microcrystalline samples deforming superplastically
through the shifting of diamond scribe lines, there have been few transmission electron microscopy results showing such occurrences in the bulk
of the material, or the details behind the micromechanism of CGBS. In this work, nanocrystalline Ni3 Al produced via high-pressure torsion is
deformed superplastically in the electron microscope. High-temperature (700 C) in situ tensile testing shows the nature of CGBS at the nanoscale
through direct observation of this phenomenon.
2006 Elsevier B.V. All rights reserved.
Keywords: Nanocrystalline material; Superplasticity; High-temperature mechanical behavior; Nickel aluminide; Grain boundary sliding; Nanocrystalline plasticity

1. Introduction
The objective of this work is to investigate the high temperature plasticity of metallic materials at diminishing length
scales. The various mechanisms that can dictate mechanical
[1] response at elevated temperatures are handled phenomenologically through the use of the Mukherjee-Bird-Dorn equation
(MBD):
 
DGb b p  n
= A
(1)
kT
d
G
where is the strain rate, D the rate-controlling diffusivity term
(lattice, grain boundary, or darken interdiffusivity), G the shear
modulus, b the magnitude of the Burgers vector, k Boltzmanns
constant, T the test or service temperature in Kelvin, d the grain
size, p the grain size exponent, the applied stress, n the stress
exponent and A is a mechanism dependent constant. Various
values for the mechanism-defining parameters p, n, D and A
reveal the rate-controlling mechanism at hand for a given set of
test conditions.

Corresponding author. Tel.: +1 505 667 8665; fax: +1 505 665 9030.
E-mail address: namara@lanl.gov (N.A. Mara).

0921-5093/$ see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2006.08.123

From Eq. (1) at constant temperature, it is evident that forming rates can be increased by decreasing the grain size. In
addition, at constant strain rate, the decrease in grain size from
micrometer to nanometer scale can lead to lowering of the superplastic forming temperature. This effect is buried in the strongly
temperature dependent Arrhenius expression for diffusivity in
the MBD Eq. (1), and lower temperatures allow for decreased
grain growth, as well as the ability to lower forming temperatures into ranges suitable for conventional tooling [2]. These
attributes have been shown to be experimentally true in some
cases, but the general trend is decreasing total elongation with
decreasing grain size when grain diameters are reduced to the
nanoscale as was shown by Sergueeva et al. [3]. This trend is
contrary to the prediction of the MBD equation, but although
total ductility is reduced, the conditions under which superplasticity will occur can still be optimized (lower T, higher strain
rates). As mentioned earlier, optimization of superplastic forming temperatures and strain rates have been seen in nano 1420-Al
alloy [4] as well as nano-Ni3 Al [5], but can be at the expense of
total elongation.
In addition to the observations of optimized superplastic
forming conditions (albeit with a decrease in total elongation)
and the need to avoid grain growth, published results emphasize
some features specific to nanocrystalline structures undergoing

N.A. Mara et al. / Materials Science and Engineering A 463 (2007) 238244

superplastic deformation (for details, see Refs. [5,6]). One of

the most important observations is a notably high degree of
strain hardening during tensile tests and high flow stresses as
compared to microcrystalline materials at comparable temperature and strain rate. Because of the grain size dependence in
the constitutive relationship for superplastic flow, strain hardening during superplasticity has been conventionally explained
in terms of grain growth. However, the ultimate tensile stress
(UTS) for nanocrystalline Ni3 Al increased by nearly 30 times
[5], while the grain size increased only two-fold. This finding
contrasts with superplastic behavior found in microcrystalline
materials in which the flow stress is proportional to grain size,
suggesting the presence of differences in the details of the deformation process that control the superplastic behavior in each type
of material. The issue of the high flow stresses witnessed during
superplastic deformation will be addressed later in this paper.
In addition to the exact nature of the high flow stresses seen
in superplastic nanomaterials, there is also little direct experimental data pertaining to the nature of the micromechanisms
behind superplasticity such as cooperative grain boundary sliding (CGBS) [79]. This mechanism is associated not only with
individual grains sliding and rotating relative to one another,
but entire groups of grains sliding along commonly oriented
grain boundaries, resulting in the large amount of mass transfer
responsible for elongations in the hundreds of percent.
It is the objective of this work to present experimental results
that provide direct insight to the nature of superplastic deformation of nanomaterials. These include new tensile results that
display the high flow stresses commonly seen in superplastic
deformation of nanomaterials, as well as results stemming from
a high-temperature in situ transmission electron microscopy
(TEM) investigation of Ni3 Al that show direct evidence of
individual grain boundary sliding, as well as cooperative grain
boundary sliding.
2. Experimental details
The in situ TEM specimens of nanocrystalline Ni3 Al
underwent a lengthy preparation procedure before undergoing
high-temperature in situ deformation in the transmission electron microscope at the National Center for Electron Microscopy
(NCEM) at the Lawrence Berkeley National Laboratory (LBL).
A hot extruded coarse-grained Ni3 Al rod with composition
Ni8.5Al7.8Cr0.8Zr0.02B (wt.%) approximately 30 mm in
diameter was produced at Oakridge National Laboratory. This
rod was then sectioned and sent to Ufa, Russia, where it underwent a high-pressure torsion (HPT) treatment that subjected the
material to 7 GPa normal stress, and 11 full rotations, resulting in an approximately 13 mm diameter disk of nanocrystalline
Ni3 Al.
The in situ tensile specimens were then shaped via electrical
discharge machining (EDM), and then ground to the appropriate final thickness with 600 grit SiC paper. These specimens had
dimensions of approximately 11 mm length, 2.5 mm width and
a thickness of 100 m. The sample is strained from pins located
at either end, while the center is thinned to electron transparency
for viewing in the transmission electron microscope. In order to

239

thin the center region to the necessary 100 nm or so thickness,

mechanical polishing via dimpling followed by electropolishing
in a 10% perchloric acid/15% acetic acid/75% methanol bath in
a Tenupol 3 jet polisher was employed. Electrolytic bath conditions were 30 V DC, 30 to 40 C bath temperature, and an
approximate current of 300 mA.
After being thinned to electron transparency, the samples
were strained in the Gatan Model 672 in situ heating/straining
stage. This stage is equipped with a mechanical stepper motor
whose rate of speed and actuation is determined by the operator. Heating up to 700 C is achieved via an annular furnace
that surrounds the viewable area of the in situ sample. Temperature readings are made by a thermocouple placed on the annular
furnace itself.
Focused ion beam (FIB) milling has opened up new possibilities to fabricate custom parts and shapes at the micron scale and
below. While the FIB has been used to create thin-film samples
for viewing in the transmission electron microscope of specific
areas/interfaces and construction of micro-pillars for mechanical testing at small length scales through nanoindentation [10],
it was appropriate in this work to use the FIB for milling a gage
section into the electron transparent area of the in situ samples.
Through this technique, a gage section approximately 5 m wide
and 20 m long could be cut out of an area that showed the best
microstructural images in terms of clearly defined grain boundaries and good diffraction contrast between separate grains, and
was best oriented to result in a true tensile state.
During the in situ experiments, a standard 30 frame/s video
recorder was used to capture footage while the sample was
brought to about (700 15 C). Once at 700 C, the sample was
strained to failure. All of the samples to be presented underwent
a 600 C pre-thinning anneal to grow the grains to approximately
75 nm, and to relieve internal stresses that could obscure observations of dislocation activity. All in situ TEM was carried out
using 300 kV electrons in a JEOL 3010 transmission electron
microscope.
Tensile results were obtained through the use of a custombuilt mini tensile tester with samples having a 1 mm 1 mm
gage section with thicknesses ranging from approximately
200 m down to 20 m. Logging of the tensile data was carried
out using LabView software and a National Instruments data
acquisition card (DAQ) installed in a personal computer. After
analog to digital conversion, the load resolution was 0.1 N, and
displacement resolution was 5 m. A NiCr element furnace
was used to heat the specimen in air or argon as the circumstances dictated. Temperature of the specimen was controlled
within 1 K using an Omega controller as measured via Ktype thermocouple placed on the grips as near to the sample
as possible.
3. Results
In past results presented by the current authors, one comment
has consistently arisen which relates to nanocrystalline sample sizes as compared to their microcrystalline counterparts. In
Fig. 1(a), a tensile plot comparing past nanocrystalline Ni3 Al
results by McFadden et al. [5] with microcrystalline results by

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Fig. 1. Tensile curves for Ni3 Al for superplastic deformation under different
conditions. While (a) uses a sample under somewhat different conditions, as
well as significantly more grains across the thickness of the nanocrystalline
sample and (b) illustrates the same general trend for very similar conditions and
a similar number of grains through the thickness of the sample. Note the high
flow stresses in the nanocrystalline sample in both cases.

Mukhopadhyay et al. [11] is presented. Remarkably high flow

stresses are seen in the nanocrystalline case, as well as low temperature superplasticity compared to the microcrystalline state
for an equivalent amount of total deformation. However, the
strain rates are different and sample sizes in this study differ considerably, and so Fig. 1(b) shows the results of two tensile tests
with more directly comparable results. In the new nano-Ni3 Al
results, the material is tested under comparable conditions as the
micro-Ni3 Al. Most importantly, the number of grains through
the thickness of the material in the nanocrystalline sample, as
well as the strain rate, is substantially equivalent to those found
in the microcrystalline sample. While the flow stresses in the
nanocrystalline sample are affected by the decrease in strain
rate from Fig. 1(a and b), as well as the total elongation affected
by the decrease in gage thickness, the overall characteristics of
the flow curve remain largely the same. There is a clear sixfold increase in flow stress for the nanocrystalline Ni3 Al over
microcrystalline Ni3 Al.
Fig. 2 shows a series of TEM images that depict the
microstructure of (a) Ni3 Al in its as-received form, (b) after
annealing at 650 C for 3 min, and (c) after deformation at
650 C. While there is evidence of twin formation, there is
little evidence of dislocation storage, and certainly no dislo-

Fig. 2. Ni3 Al (a) before heating, (b) at test temperature (650 C) and (c) after
deformation at 650 C. Note the minimal amount of grain growth and equiaxed
nature of the grains. This microstructure correlates with the nanocrystalline
tensile curve depicted in Fig. 1(a).

cation substructure. When coupled with the information from

Fig. 1(a), several questions arise, namely, what is the cause of
the high flow stresses, and what occurs during the test (transition from Fig. 2(b and c) to facilitate superplastic deformation in
terms of grain boundary sliding and associated accommodation
mechanisms?
The micrographs in Fig. 2, while giving important
microstructural details at discrete points during the deformation/testing process have a significant drawback, in that there
are crucial observations to be made during the tensile test, e.g.

N.A. Mara et al. / Materials Science and Engineering A 463 (2007) 238244

241

may explain the high degree of work hardening seen in nanomaterials undergoing superplastic deformation [12], and may
be a precursor to alignment of grain boundaries into long-range
sliding surfaces (stringers) in microcrystalline materials.
The relatively small local rotations that take place in the
1.5 min span between Fig. 3(a and b) can be more clearly seen
through highlighting the grain boundaries as in Fig. 3(c). In this

Fig. 3. (a and b) TEM images taken approximately 1.5 min apart and show
grain displacement as depicted in (c) especially note the displacement in the
area marked by the arrows.

between the microstructures seen in Fig. 2(a and b). Fig. 3

presents new findings that stem from a high temperature in
situ TEM straining experiment which show local grain displacement. In this experiment, nano-Ni3 Al was strained at
approximately 700 C, at a strain rate estimated to be on the
order of 1 103 s1 , although due to the lack of a proper
gage section, this could be as low as 1 104 s1 or as high
as 1 102 s10 . The differences in grain orientation are small,
but quite significant, and are marked by arrows in Fig. 3(a and
b). These small reorientations have been modeled before, and

Fig. 4. Progression of TEM images through 81 s. Note differences in grain orientation (some of which are marked by arrows) up until 81 s, where cooperative
grain boundary sliding is about to take place.

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N.A. Mara et al. / Materials Science and Engineering A 463 (2007) 238244

figure, the group of grains shown as dashed lines are the original
grain orientations from Fig. 3(a), and the solid lines represent the
deformed orientations from Fig. 3(b). It is clear from this figure
that the contrast changes seen between the two micrographs do
result in a significant amount of deformation, although signs of
dislocation activity were not observed. It should be noted that
although one may consider these changes to be insignificant,
they are occurring within 1.5 s.
Fig. 3 shows experimental evidence of the small rotations
that are necessary on the scale of a single grain diameter, but
does not show the CGBS event that could explain the elongations of hundreds of percent that are commonly seen in materials
undergoing superplastic deformation. While the phenomenon of
CGBS has been observed in micrometer-scale materials through
in situ straining of PbSn eutectic in a scanning electron microscope [13], these results show the first such deformation in situ
in nanomaterials. Fig. 4 shows a progression of excerpts from
an in situ experiment carried out on Ni3 Al at approximately
750 C. Small re-arrangements of grains in accordance with the
evidence shown in Fig. 3 take place up until the 81 s mark,
and then a massive re-arrangement over the order of several
grains along planes of cooperative grain boundary shear ensues
as shown in Fig. 5. This change in orientation occurs along the
stringers shown by the arrows in Fig. 5(a), and is further highlighted when the individual grains are outlined as in Fig. 5(b).
It is important to note that this deformation event took place
within the length of one captured frame, consisting of one thirti-

Fig. 5. TEM images taken just after CGBS. Note stringers formed in (a) as
highlighted in (b).

eth of a second. While contrast changes such as shown between

these figures can be due to a number of different phenomena,
including localized bending, these images show additional evidence that rules out such artifacts. One such case is the fact
that many of the grains outside the area showing the contrast
change, especially to the bottom of the area shown, are not
showing a change in contrast and function as marker grains.
Another, more substantial piece of evidence is that the sliding
event took place along obvious planes of long-range shear, as
marked by the arrows. Such features have been observed before
[14,15] in nanomaterials that underwent grain boundary sliding, but have never been captured during the actual sliding
event.
4. Discussion
While the sliding and rotation of individual grains is certainly
an important aspect of superplasticity, it is difficult for such a
mechanism to solely explain the elongations of hundreds of percent seen in superplastic materials. At the microscale, it has
been shown by authors including Zelin et al. [7,13,1618] that
grain boundary sliding actually occurs in groups in a process
known as CGBS. Through the use of diamond scribe lines in
microcrystalline Ti alloy as well as PbSn eutectic (conducted
in situ in the scanning electron microscopy), Zelin showed that
grains slide relative to one another along sets of grain boundaries that have aligned themselves to form planes of long-range
shear. Since the mass transport associated with a cooperative
event is much greater than that carried by singular grains, CGBS
can easily account for the large elongations seen in superplastic
deformation. Of course, the alignment of the grain boundaries
to form these stringers, as the boundaries of long-range shear
are commonly referred to, must occur by some process, which
is where local grain rotation and/or dislocation accommodation
must come into play. Kaibyshev [9] has shown that in microcrystalline materials undergoing superplastic deformation, grain
boundaries that are configured to reduce total grain boundary
line length will slide preferentially as a properly oriented stress
is applied. If an unfavorably oriented grain is found along one
of these stringers, the grain will either rotate on its own until
it comes into alignment with the rest of the grain boundaries
comprising the stringer, or it will undergo a significant amount
of dislocation motion to accommodate the cooperative grain
boundary sliding event. As such, a two-step process for superplastic deformation can be envisioned: (1) local grain rotation
and sliding accommodated by dislocation motion and/or diffusional processes to align grain boundaries into stringers in
accordance with applied stress. (2) Once aligned, large groups
of grains will slide cooperatively until an unfavorably oriented
grain/grain boundary stops the event. This process will repeat
itself throughout the material in different areas as changing local
stress states alter the planes of long-range shear throughout the
material.
Closer examination of Fig. 1 shows that while the flow
stresses seen in the nanocrystalline sample are much higher than
those seen in the microcrystalline sample, the testing conditions
are quite different. Specifically, one issue is that if one follows

N.A. Mara et al. / Materials Science and Engineering A 463 (2007) 238244

the model of Kaibyshev, mentioned earlier, that some grains

throughout the sample will have a statistical probability of being
unfavorably oriented to CGBS, and then a sample with more
grains through the thickness will have a greater probability of
encountering such an unfavorably oriented grain. Therefore, the
flow stresses will be higher in order to provide a driving force for
reorientation of these grains, or for dislocation motion (which
at these length scales will be difficult at best) to shear across the
grain. In Fig. 1(b), some of these issues are addressed, in that the
sample in the nano and micro states have a comparatively similar number of grains through their thickness. There still remain
some discrepancies between the two tests, however, but these are
not easily overcome. While the nano-Ni3 Al shows remarkable
resistance to grain growth due to its ordered crystalline structure,
it still must be tested 325 C below its microcrystalline counterpart to avoid uncontrollable grain growth. On the other hand,
if the microcrystalline Ni3 Al were to be tested at 700 C, it
would not exhibit superplasticity, as the test temperature would
be insufficient for adequate diffusivity in this microcrystalline
state. However, it is important to note that the work by McFadden
et al. has shown that this material shows a strain rate exponent,
as well as a grain size exponent that correlates nicely with values
that are commonly associated with superplasticity as a dominant
deformation mechanism [5,19]. Despite these small inconsistencies, Fig. 1(b) only serves to confirm what Fig. 1(a) has
depictedextraordinarily high flow stresses, followed by strain
softening, for nanomaterials undergoing superplastic deformation.
A recently proposed model by Gutkin et al. [12] makes one of
the first attempts to explain the extreme work hardening followed
by softening exhibited during nanocrystalline superplasticity.
This model uses grain boundary dislocations as the primary
mode of mass transport, and gradually has the interaction of
these dislocations at triple points account for the hardening
and softening of these materials. As grain boundary dislocations interact at triple points, a net displacement of the triple
point leaves a sessile dislocation behind, as well as gives an
offset to the triple point (triple point migration). As more grain
boundary dislocations approach the triple point, the sessile dislocation serves to repel them, resulting in work hardening up
until the point of ultimate tensile strength. All the while that
these grain boundary dislocations are overcoming the repulsive
stress and merging with the sessile dislocation, the grain boundary has continued to migrate in accordance with the respective
mobile dislocations Burgers vectors. As a result, the triple point
has migrated to where CGBS is facilitated, and strain softening
quickly ensues. Such a model is the first attempt to explain the
high flow stresses and strain softening seen in nanocrystalline
superplasticity.
The microstructural information given in Fig. 2 adds some
crucial information to the flow curves shown in Fig. 1. Fig. 2
essentially outlines the progression of the flow curve seen in
Fig. 1(a), and accounts for (a) the as-received condition, (b) the
state of the microstructure immediately before tensile testing
and (c) after undergoing superplastic deformation. The progression to test temperature shows a good amount of grain
growth, and relief of the internal stresses that characterize an

243

HPT-processed material. However, despite the twinning seen in

Fig. 2(c), there is little sign of dislocation storage, and therefore, little sign of conventional work hardening. For this reason,
in situ high-temperature TEM straining was employed to fill in
the missing link between the pre-deformed and post-deformed
microstructures.
The coupling of Figs. 35 show the definite progression
between discrete grain boundary sliding and cooperative grain
boundary sliding. The small re-alignments of grains in Fig. 3 are
very much consistent with the model of Gutkin et al. [12], and
form the first step of stringer formation before a long-range shear
event occurs. Fig. 4 shows a different area, and also exhibits
slight grain rearrangements captured in the 81 s leading up to
the massive rearrangement exhibited in Fig. 5. It is clear that
up until the cooperative grain boundary sliding event seen in
Fig. 5, there are minor grain rotations seen that help to form
the stringers seen in Fig. 5. After the very fast (within 1 frame)
CGBS event, the stringers are easily observed. The exhibited
behavior is very similar to that pointed out earlier by Zelin et
al. during in situ straining of microcrystalline PbSn eutectic in
the scanning electron microscopy. While these results show the
first direct evidence of CGBS in nanomaterials, there still remain
several questions to be answered. These in situ TEM straining
results show the macroscopic deformation of the superplastically
deforming grains but do not show the accommodation mechanisms working beneath the macroscopic shear of the material.
Whether dislocation accommodation plays an important role in
superplastic accommodation at length scales below 100 nm still
has yet to be directly observed. It would be best, as well as most
conclusive, to point out direct evidence of dislocation emission
and triple point behavior in this material undergoing superplastic deformation. This is a subject of the ongoing investigation of
nanocrystalline Ni3 Al, and this study should show some of the
crucial details as to the nature of high-temperature deformation
of nanocrystalline materials.
5. Conclusion
In this work, new sample thicknesses, as well as testing
parameters of nanocrystalline Ni3 Al show that the high degree
of work hardening during superplastic deformation is a unique
feature of nanocrystalline superplasticity, and is not merely due
to a statistical effect of increased numbers of unfavorably oriented grains through the thickness of nanocrystalline specimens.
Specifically, superplastically deformed nanocrystalline Ni3 Al
with approximately 250 grains through the sample thickness
showed a nearly six-fold increase in flow stress over its microcrystalline counterpart. In addition, new in situ high-temperature
straining in the TEM reveals a two-step process for superplastic
deformation in nanomaterials similar to that observed in materials with micron-sized grains. A series of small re-orientations
of grains and grain boundaries serves to set up planes of
long-range shear. Once these small changes in microstructure have been made, macroscopic sliding via cooperative
grain boundary sliding ensues, accounting for the majority of
strain seen in nanocrystalline materials undergoing superplastic
deformation.

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Acknowledgement
The authors would like to acknowledge the support of
the National Science Foundation, grant number NSF-DMR0240144. All in situ microscopy was carried out with
the generous support of the National Center for Electron
Microscopy (NCEM) at the Lawrence Berkeley National Laboratory.
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