Characterization of Materials through High Resolution Imaging: High Resolution Characterization of Materials with General Coherent Imaging Techniques
Sponsored by: TMS Structural Materials Division, TMS: Advanced Characterization, Testing, and Simulation Committee
Program Organizers: Richard Sandberg, Brigham Young University; Ross Harder, Argonne National Laboratory; Xianghui Xiao, Brookhaven National Laboratory; Brian Abbey, La Trobe University; Saryu Fensin, Los Alamos National Laboratory; Ana Diaz, Paul Scherrer Institute; Mathew Cherukara, Argonne National Laboratory

Wednesday 2:00 PM
March 17, 2021
Room: RM 14
Location: TMS2021 Virtual

Session Chair: Richard Sandberg, Brigham Young University


2:00 PM  Keynote
The Fourth is Strong in These Ones!: Ian McNulty1; 1MAX IV Laboratory
     Three new x-ray sources form the vanguard of a fourth generation of synchrotron machines offering 100-fold greater brightness than the previous generation. At least two more fourth-generation sources are under construction with several others envisioned worldwide. The short wavelengths of x-rays offer large penetration depth, sensitivity to atomic, electronic, and magnetic structure, and imaging at a resolution approaching atomic dimensions. These sources open entirely new vistas for high resolution coherent x-ray imaging of materials due to its hunger for source brightness. The first, MAX IV in Sweden, began operating in mid-2016. Five of the sixteen beamlines at MAX IV have dedicated experimental stations for soft and hard x-ray imaging. Early imaging results have already been obtained with the latest sources, ESRF-EBS in France and SIRIUS in Brazil. This talk reviews recent progress and considers new opportunities for material imaging with these super-bright x-ray sources.

2:30 PM  
X-ray Based Nanodiffraction to Study Strain in Materials for Nuclear Energy: Ericmoore Jossou1; Mehmet Topsakal1; Xiaojing Huang1; Khalid Hattar2; Hanfei Yan1; Yong Chu1; Cheng Sun3; Lingfeng He3; Jian Gan3; Lynne Ecker1; Simerjeet Gill1; 1Brookhaven National Laboratory; 2Sandia National Laboratories; 3Idaho National Laboratory
    Understanding microstructural and strain evolutions induced by fission gas in nuclear fuel is crucial for designing next generation of nuclear reactors, as it is responsible for volumetric swelling and catastrophic failure in metallic fuels. Depth-resolved synchrotron X-ray nanodiffraction uniquely permits the measurement of lattice strain associated with irradiation-induced defects with sub-micron spatial resolution while X-ray fluorescence (XRF) enables 2D imaging of fission gas bubble positions with nanoscale resolution. Here, our recent work on residual lattice strain caused by krypton-ion-implantation in tungsten using a correlative multi-modal approach will be presented. For instance, the heterogeneous distribution of local defects accounts for the compressive and expansive lattice strain observed in the tungsten matrix. Beyond providing a detailed understanding of irradiation-induced microstructural changes in ion irradiated single crystal materials, this work demonstrates the utility of multi-modal scanning nanofocused X-ray measurements for the optimization of materials for the future nuclear reactors.

2:50 PM  Invited
Imaging Phase Transitions of Quantum Materials with Bragg Coherent X-ray Diffraction: Tadesse Assefa1; Yao Cao2; Jiecheng Diao3; Wonsuk Cha2; Ross Hardar2; Kim Kisslinger1; Mark Dean1; Genda Gu1; John Tranquada1; Ian Robinson1; 1Brookhaven National Laboratory; 2Argonne National Laboratory; 3University College London
    Structural symmetry breaking and recovery in condensed matter systems are closely related to exotic physical properties such as superconductivity, collective charge, and magnetic orders. The interplay between different order parameters is intricate and often subject to intense debate, as in the case of charge order and superconductivity. Recently we have applied coherent X-ray diffraction to visualize the domain structures associated with these symmetry changes directly during phase transition. In this talk, I will describe experimental challenges to push Bragg Coherent Diffractive Imaging (BCDI) into the cryogenic regime where most phase transitions in quantum materials reside. As an example, I will present our work on La1.875Ba0.125CuO4 (LBCO) where we image the structural evolution of LBCO microcrystal samples during the high-temperature tetragonal to low-temperature orthorhombic phase transition. Besides, I will show preliminary results from 34-ID-C beamline, APS to imaging Charge-order domains IrTe2 flakes, efforts towards magnetic BCDI on Sr2IrO4, and other examples.

3:20 PM  
Mesoscale Defect Dynamics in the Bulk with Time-resolved Dark-field X-ray Microscopy: Leora Dresselhaus-Marais1; 1Lawrence Livermore National Laboratory
    Materials respond to their surroundings based on their native properties and how their defects interact. Mesoscale defect interactions connect atomic imperfections to the continuum properties. Experimental tools in this regime struggle to time-resolve measurements of defects buried deep beneath the surface. Dark-field X-ray microscopy (DFXM) can now directly image defects in single- and poly-crystals, resolving distortions deep beneath the surface over a wide field of view, with high sensitivity to strain and inclination in the lattice. We have extended DFXM to time-resolved studies at synchrotron and X-ray free electron laser facilities to collect movies of mesoscale deformation processes in-situ. With these early studies, I will show how time-resolved DFXM now presents opportunities to study mesoscale dynamics to inform multi-scale models. This work was performed in part under the auspices of the U.S. Department of Energy by Lawrence Livermore National Laboratory under Contract DE-AC52-07NA27344.

3:40 PM  Invited
Laboratory and Synchrotron-based X-ray Tomographic Imaging during In Situ Loading of Materials: Brian Patterson1; Lindsey Kuettner1; Cindy Welch1; Paul Welch1; Axinte Ionita1; Nikhilesh Chawla2; Xianghui Xiao3; 1Los Alamos National Laboratory; 2Arizona State University; 3Brookhaven National Laboratory
    The X-ray 3D imaging and collection of material response during loading allows materials researchers to directly identify failure mechanisms. Laboratory-based sources are used to acquire the initial morphology of the material which is often used as a starting point for mechanical modeling. Synchrotron light sources, such as the Advanced Photon Source, are useful in that the high X-ray flux allows researchers to acquire high speed, 3D images during loading. The uniaxial loading of a variety of soft, composite, as well as 3D printed materials up to ~0.4 /s strain rates will be used to highlight the lessons learned for these types of experiments. Analysis of the images through the use of advanced techniques, such as eigenvector centrality, digital volume correlation, as well as finite element modeling, will be shown. These techniques provide opportunities to validate material models by the side-by-side comparison of the modeled performance to the mechanical response.

4:10 PM  
Magnetic Correlations and Time Fluctuations in Assemblies of Fe3O4 Nanoparticles Probed via X-rays: Karine Chesnel1; 1Brigham Young University
    Magnetic nanoparticles are increasingly used in biomedical applications such as drug-delivery, gene delivery, hyperthermia, or contrast agents for MRI. Magnetite (Fe3O4) nanoparticles are good candidates for these applications due to their non-toxicity and long-life in the bloodstream. Here we show inter-particle magnetic correlations probed at the nanoscale via x-ray resonant magnetic scattering (XRMS). We show the dependence on particle size, varying from 5 to 11 nm, suggesting an enhancement of magnetic couplings for bigger particles. Additionally, we show a model based on chains of nanoparticles. The data fitting suggests ferromagnetic ordering when an external magnetic field is applied, but the emergence of antiferromagnetic ordering at remanence. Additionally we will present photon correlation data that show the dynamics of fluctuation throughout the superparamagnetic blocking transition.

4:30 PM  
Using the Rotation Vector Base Line Electron Back Scatter Diffraction (RVB-EBSD) Method to Characterize Single Crystal Cast Microstructures: Pascal Thome1; Felicitas Scholz1; Jan Frenzel1; Gunther Eggeler1; 1Ruhr-University Bochum
    We present the Rotation Vector Base Line Electron Back Scatter Diffraction (RVB-EBSD) method, a new correlative orientation imaging method for scanning electron microscopy (OIM/SEM). The RVB-EBSD method was developed to study crystal mosaicity in as-cast Ni-base superalloy single crystals (SX). The technique allows to quantify small crystallographic deviation angles between individual dendrites and to interpret associated accommodation processes in terms of geometrically necessary dislocations (GNDs). The RVB-EBSD method was inspired by previous seminal approaches which use cross correlation EBSD procedures. A rotation vector approximation and a correction procedure, which relies on a base line function, are used. The method moreover features a novel way of intuitive color coding. We show an in-depth analysis of the crystallographic relations which arise from the competitive growth of dendrites. Emphasis is placed on a comparison between SX produced by a conventional Bridgman process and SX produced by selective electron beam melting (SEBM).