Bragg coherent diffractive imaging of single-grain defect dynamics in polycrystalline films

Watching defects in heated thin films The response of materials to external conditions depends on small-scale features such as defects and grain boundaries. Yau et al. heated gold thin films and used coherent x-ray diffractive imaging to track how these microstructures developed during grain growth (see the Perspective by Suter). The technique allowed nondestructive visualization of the features in three dimensions. The method should help link external stimuli to material response through changes in microstructure, thereby allowing development of novel materials through microstructural engineering. Science, this issue p. 739; see also p. 704 Bragg coherent diffractive imaging can track defects and grain boundaries during heating in a gold thin film. Polycrystalline material properties depend on the distribution and interactions of their crystalline grains. In particular, grain boundaries and defects are crucial in determining their response to external stimuli. A long-standing challenge is thus to observe individual grains, defects, and strain dynamics inside functional materials. Here we report a technique capable of revealing grain heterogeneity, including strain fields and individual dislocations, that can be used under operando conditions in reactive environments: grain Bragg coherent diffractive imaging (gBCDI). Using a polycrystalline gold thin film subjected to heating, we show how gBCDI resolves grain boundary and dislocation dynamics in individual grains in three-dimensional detail with 10-nanometer spatial and subangstrom displacement field resolution. These results pave the way for understanding polycrystalline material response under external stimuli and, ideally, engineering particular functions.

[1]  Sandra Piazolo,et al.  Quantification of mineral behavior in four dimensions: Grain boundary and substructure dynamics in salt , 2012 .

[2]  J. Weissmüller,et al.  Grain boundary segregation, stress and stretch : Effects on hydrogen absorption in nanocrystalline palladium , 2007 .

[3]  R Harder,et al.  High-resolution three-dimensional partially coherent diffraction imaging , 2012, Nature Communications.

[4]  David B. Menasche,et al.  Comparison between diffraction contrast tomography and high-energy diffraction microscopy on a slightly deformed aluminium alloy , 2016, IUCrJ.

[5]  R. Harder,et al.  Coherent X-ray diffraction imaging of strain at the nanoscale. , 2009, Nature materials.

[6]  Defect‐Rich Metal Nanocrystals in Catalysis , 2016 .

[7]  D. Hull,et al.  Introduction to Dislocations , 1968 .

[8]  David L. Olmsted,et al.  Survey of computed grain boundary properties in face-centered cubic metals: I. Grain boundary energy , 2009 .

[9]  Jesse N. Clark,et al.  Coherent diffraction imaging of nanoscale strain evolution in a single crystal under high pressure , 2013, Nature Communications.

[10]  A. M. Kowalczyk,et al.  Phase Retrieval for a Complex-Valued Object Using a Low-Resolution Image , 1990, Signal Recovery and Synthesis III.

[11]  E. Holm,et al.  How Grain Growth Stops: A Mechanism for Grain-Growth Stagnation in Pure Materials , 2010, Science.

[12]  A. Korsunsky,et al.  Mesomechanics 2009 Crystal plasticity and hardening: a dislocation dynamics study , 2009 .

[13]  R. Harder,et al.  Coherent X-Ray Diffraction Imaging of Morphology and Strain in Nanomaterials , 2013 .

[14]  Sergei V. Kalinin,et al.  Nanoscale mapping of ion diffusion in a lithium-ion battery cathode. , 2010, Nature nanotechnology.

[15]  P Zapol,et al.  Avalanching strain dynamics during the hydriding phase transformation in individual palladium nanoparticles , 2015, Nature Communications.

[16]  P. Cloetens,et al.  New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging , 2009 .

[17]  M. Newton,et al.  Three-dimensional imaging of strain in a single ZnO nanorod. , 2010, Nature materials.

[18]  T. Cornelius,et al.  New insights into single-grain mechanical behavior from temperature-dependent 3-D coherent X-ray diffraction , 2014 .

[19]  J R Fienup,et al.  Phase retrieval algorithms: a comparison. , 1982, Applied optics.

[20]  D. Hull,et al.  Chapter 2 – Observation of Dislocations , 2011 .

[21]  F. C. Frank,et al.  The influence of dislocations on crystal growth , 1949 .

[22]  S Marchesini,et al.  Invited article: a [corrected] unified evaluation of iterative projection algorithms for phase retrieval. , 2006, The Review of scientific instruments.

[23]  M. Rudneva,et al.  In situ transmission electron microscopy imaging of grain growth in a platinum nanobridge induced by electric current annealing , 2011, Nanotechnology.

[24]  H. Gleiter,et al.  Nanostructured materials: basic concepts and microstructure☆ , 2000 .

[25]  S. Zwaag,et al.  Grain Nucleation and Growth During Phase Transformations , 2002, Science.

[26]  M. Vieira,et al.  In situ TEM study of grain growth in nanocrystalline copper thin films , 2010, Nanotechnology.

[27]  R. Harder,et al.  Nanoscale Hard X-Ray Microscopy Methods for Materials Studies* , 2013 .

[28]  Yonina C. Eldar,et al.  Phase Retrieval with Application to Optical Imaging , 2014, ArXiv.

[29]  S. Mackay MATERIALS: ENGINEERING, SCIENCE, PROCESSING AND DESIGN , 2011 .

[30]  J. Greer Nanotwinned metals: It's all about imperfections. , 2013, Nature Materials.

[31]  Ian K. Robinson,et al.  Three-dimensional imaging of dislocation propagation during crystal growth and dissolution , 2015, Nature materials.

[32]  Kazuto Yamauchi,et al.  Bragg x-ray ptychography of a silicon crystal: Visualization of the dislocation strain field and the production of a vortex beam , 2013 .

[33]  Shoushan Fan,et al.  Grain-boundary-dependent CO2 electroreduction activity. , 2015, Journal of the American Chemical Society.

[34]  Mukul Kumar,et al.  Electron Backscatter Diffraction in Materials Science , 2000 .

[35]  J. Miao,et al.  Application of optimization technique to noncrystalline x-ray diffraction microscopy: Guided hybrid input-output method , 2007 .

[36]  Robert M. Suter,et al.  Adaptive reconstruction method for three-dimensional orientation imaging , 2013 .

[37]  Garth J. Williams,et al.  Three-dimensional mapping of a deformation field inside a nanocrystal , 2006, Nature.

[38]  J. R. Patel,et al.  Local plasticity of Al thin films as revealed by x-ray microdiffraction. , 2003, Physical review letters.

[39]  Y. S. Meng,et al.  Topological defect dynamics in operando battery nanoparticles , 2015, Science.

[40]  S. Marchesini,et al.  Invited article: a [corrected] unified evaluation of iterative projection algorithms for phase retrieval. , 2006, The Review of scientific instruments.

[41]  H. Ohta,et al.  Atomic structures and oxygen dynamics of CeO2 grain boundaries , 2016, Scientific Reports.

[42]  Jesse N. Clark,et al.  3D Imaging of Twin Domain Defects in Gold Nanoparticles. , 2015, Nano letters.

[43]  B. Abbey,et al.  High energy transmission micro-beam Laue synchrotron X-ray diffraction , 2010 .

[44]  M. Nastasi,et al.  Enhanced hardening in Cu/330 stainless steel multilayers by nanoscale twinning , 2004 .

[45]  James R. Fienup,et al.  Phase-retrieval stagnation problems and solutions , 1986 .

[46]  B. Mitchell,et al.  Crystal growth kinetics of nanocrystalline aluminum prepared by mechanical attrition in nylon media , 2005 .