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The mechanical behavior of nanocrystalline metals has been a research topic of interest for the past two decades. The current understanding is summarized in several recent reviews. [1][2][3] Researchers have been investigating the deformation mechanisms in nanocrystalline metals and alloys through experimental and modeling routes. [4][5][6][7][8][9][10] Modeling results [8][9][10] indicate that there is a transition from dislocation generation at sources within grains to grain-boundary mediated dislocation generation in the grain size range between about 100 to 10 nm. Below 10 nm, grain boundary deformation modes (sliding, rotation, etc.) become dominant and inverse Hall-Petch effects have been reported. Experimental evidence to confirm these predictions is an active area of research. Two important experimental parameters that are useful in characterizing the deformation kinetics of materials are the strain rate sensitivity m and the activation volume V*. [5,11,12] These are related by m = kT/V*r where k is Boltzmann's constant, T is temperature (K) and r is the stress. There is a limited amount of data available on m and V* measurements for nanocrystalline metals. [4,5,[11][12][13][14] One aspect of this is the fact that research-scale synthesizing techniques often produce small quantities of material and mechanical testing procedures suited to small sample sizes are required. [4,5,7,[13][14][15][16][17][18] In addition to this fact there is a tremendous scarcity of testing methodologies for testing the materials at small scales such as Micro-Electro-Mechanical-Systems (MEMS) where micro tensile and nanoindentation tests are used for understanding the deformation behaviour. [19,20] The aim of the present work was to extend the shear punch test (SPT) technique to the measurement of activation volumes on small scale specimens of few millimeters (∼ 1 mm to 3 mm). The advantage of SPT over nanoindentation and micro tensile tests is the deformation zone where a large number of grains undergo deformation within the shear zone and overcomes the problem of strain gradient plasticity effects, gain size effects as well as the specimen size effects. [21] The SPT has been used for evaluating the yield and ultimate stress by numerous researchers, including us. [21][22][23][24][25][26][27][28] The SPT shear yield or ultimate strength value s can be correlated with its tensile test counterpart r using the relation r = as. The correlation factor a depends upon the testing setup and data analysis methods. [22][23][24][25][26][27][28] The Von Mises (VM) yield criterion predicts a = 3 p if the SPT approximates pure shear loading conditions. This was the case in [21] where the details and standardization of the SPT technique used in the present research work are given.The stress relaxation method has been used to determine activation volumes and dislocation dynamics in coarse-grain metals and alloys [29] and in nanocrystalline Ni. [14] The tests are normally done using uniaxial loading conditions. In the present study, we use the s...

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