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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
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N.A. Mara et al. / Materials Science and Engineering A 463 (2007) 238244
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.
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).
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.
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.
242
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).
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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.
References
[1] A.K. Mukherjee, J.E. Bird, J.E. Dorn, Trans. ASM 62 (1969) 155179.
[2] A.K. Mukherjee, Mater. Sci. Eng. A 322 (2002) 122.
[3] A.V. Sergueeva, N.A. Mara, R.Z. Valiev, A.K. Mukherjee, Mater. Sci. Eng.
A 410411 (2005) 413416.
[4] R.S. Mishra, R.Z. Valiev, S.X. McFadden, R.K. Islamgaliev, A.K. Mukherjee, Philos. Mag. A (Phys. Condens. Matter: Struct. Defects Mech.
Properties 81 (1) (2001) 3748.
[5] S.X. McFadden, R.S. Mishra, R.Z. Valiev, A.P. Zhilyaev, A.K. Mukherjee,
Nature 398 (6729) (1999) 684686.
[6] A. Sergueeva, A. Mukherjee, in: H.S. Nalwa (Ed.), Encyclopedia of
Nanoscience and Nanotechnology, American Scientific Publishers, 2004,
pp. 305316.
[7] M.G. Zelin, A.K. Mukherjee, Acta Metall. Mater. 43 (6) (1995) 23592372.
[8] M.G. Zelin, Q. Li, A.K. Mukherjee, in: Superplasticity and Superplastic
Forming 1995; Proceedings of the Minerals, Metals, and Materials Society,
Las Vegas, Nevada; USA; 1315 Feb. 1995.
[9] O.A. Kaibyshev, Mater. Sci. Eng. A 324 (12) (2002) 96102.
[10] M.D. Uchic, D.M. Dimiduk, J.N. Florando, W.D. Nix, Science 305 (5686)
(2004) 986989.
[11] J. Mukhopadhyay, G. Kaschner, A.K. Mukherjee, Scripta Metall. Mater.
24 (5) (1990) 857862.
[12] M.Y. Gutkin, I.A. Ovidko, N.V. Skiba, Acta Mater. 52 (6) (2004)
17111720.
[13] M.G. Zelin, M.R. Dunlap, R. Rosen, A.K. Mukherjee, J. Appl. Phys. 74
(8) (1993) 49724982.
[14] Y. Champion, C. Langlois, S. Guerin, S. Lartigue-Korinek, P. Langlois,
M.J. Hytch, Mater. Sci. Forum 482 (2005) 7176.
[15] J. Markmann, P. Bunzel, H. Rosner, K.W. Liu, K.A. Padmanabhan,
R. Birringer, H. Gleiter, J. Weissmuller, Scripta Mater. 49 (7) (2003)
637644.
[16] M. Zelin, A. Mukherjee, Philos. Mag. Lett. 68 (4) (1993) 207214.
[17] M.G. Zelin, A.K. Mukherjee, J. Mater. Sci. Lett. 13 (17) (1994) 12581260.
[18] V.V. Astanin, S.N. Faizova, K.A. Padmanabhan, Mater. Sci. Technol. 12
(6) (1996) 489494.
[19] S.X. McFadden, Superplasticity of nanocrystalline nickel aluminide alloy
and nanocrystalline nickel, Ph.D. Dissertation, University of California,
Davis, p. 126, 2001.