Assessing Experimental Parameter Space for Achieving Quantitative Electron Tomography for Nanometer-Scale Plastic Deform

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Assessing Experimental Parameter Space for Achieving Quantitative Electron Tomography for Nanometer-Scale Plastic Deformation YA-PENG YU, HIROMITSU FURUKAWA, NORITAKA HORII, and MITSUHIRO MURAYAMA Integrating in situ deformation and electron tomography (ET) techniques allows us to visualize the materials’ response to an applied stress with nanometer spatial resolution. The capability of structural, chemical, and morphological characterization in three-dimension real time and at sub-microscopic levels alleviates several persistent problems of two-dimensional imaging such as the projection effect and postmortem appearance. On the other hand, implementing deformation mechanism introduces additional experimental constraints that could influence the accuracy of the reconstructed volumes in a different way. To materialize quantitative and statistically relevant microstructure interpretation by time-resolved ET, we evaluated several key parameters such as angular tilt range, tilt increment, and reconstruction algorithms to characterize their influences on the accuracy of size and morphology reproducibility. https://doi.org/10.1007/s11661-019-05345-3 Ó The Minerals, Metals & Materials Society and ASM International 2019

I.

INTRODUCTION

DEVELOPMENT of nanomaterials has become a prevalent field in science. With the increasing complexity of materials, interpretations provided based on two-dimensional (2D) characterization results show signs of plateauing due to the projection effect. Electron tomography (ET) is an invaluable technique with the capability of carrying out thorough three-dimensional (3D) structural, chemical, and morphological characterization of materials at nanometer scale. Studies have proven ET robust to provide informative measurements. For instance, the effects of heavy-ion irradiation on dislocation process in stainless steels were investigated using ET to retrieve the dislocation state in 3D[1]; phase transitions between the bicontinuous double gyroid and hexagonally packed cylindrical structures of a poly(styrene-block-isoprene) block copolymer were examined at nanometer scale in 3D.[2] ET is a powerful technique; however, its applicability and reliability can be restricted by several factors. Except some special cases such as the stereo microscopy YA-PENG YU is with the Institute for Critical Technology and Applied Science, Virginia Tech, 1991 Kraft Dr, Blacksburg, VA 24061. HIROMITSU FURUKAWA and NORITAKA HORII are with the System In Frontier, Inc., 2-8-3, Akebono-Cho, Tachikawa, Tokyo 1900012, Japan. MITSUHIRO MURAYAMA is with the Materials Science and Engineering, Virginia Tech, 1991 Kraft Dr, Blacksburg, VA 24061. Contact email: [email protected] Manuscript submitted March 1, 2019.

METALLURGICAL AND MATERIALS TRANSACTIONS A

for dislocation visualization,[3–5] acquisition of tilt-series projection images over the entire angular tilt range (± 90 deg) with small tilt interval is required for ideal 3D volume reconstruction by ET. Due to the hardware geometry of the electron microscope and the location of th