6th International Congress on 3D Materials Science (3DMS 2022): Emergent Characterization Techniques II: Tomography
Program Organizers: Dorte Juul Jensen, Technical University of Denmark; Marie Charpagne, University of Illinois; Keith Knipling, Naval Research Laboratory; Klaus-Dieter Liss, University of Wollongong; Matthew Miller, Cornell University; David Rowenhorst, Naval Research Laboratory
Wednesday 8:20 AM
June 29, 2022
Room: Columbia A&B
Location: Hyatt Regency Washington on Capitol Hill
Session Chair: Michael Uchic, Air Force Research Laboratory
8:20 AM Invited
Multiple Modal X-ray Microtomography for Material Science: Tiqiao Xiao1; Biao Deng2; Guohao Du2; Yanan Fu2; Han Guo2; Ke Li3; Guanyun Peng2; Fen Tao2; Honglan Xie2; Yanling Xue2; Fucheng Yu3; Guangzhao Zhou2; Haipeng Zhang3; 1Shanghai Synchrotron Radiation Facility/Zhangjiang Laboratory, Shanghai Advanced Research Institute, Chinese Academy of Sciences; Shanghai Institute of Applied Physics, Chinese Academy of Sciences; University of Chinese Academy of Sciences; 2Shanghai Synchrotron Radiation Facility/Zhangjiang Lab, Shanghai Advanced Research Institute, Chinese Academy of Sciences; 3Shanghai Institute of Applied Physics, Chinese Academy of Sciences
X-ray microtomography (XMCT) is the dominated method for BL13W at SSRF, more than 70% user experiments were carried out with XMCT and about one half of researches are on material science. X-ray microtomography based on a variety of contrast mechanisms including absorption, phase, fluorescence, diffraction and scattering, have been developed. With the combination of multi-contrast information, X-ray microtomography is capable for nondestructive and quantitative investigation on microstructures and components of low Z and high Z materials, elements distribution, crystal grain distribution and orientation, nanoparticle distribution and morphology etc. Microscope with multiscale from 20nm to 50nm and to microns can be provided for static and dynamic analysis to microstructures. Dynamic X-ray tomography up to 26 Hz has also developed at SSRF. Novel X-ray imaging modalities including ghost imaging and move contrast imaging may provide new solutions for low dose or in operando researches on material science.
8:50 AM
New Insights in Materials Characterization – Spectral Computed Tomography: Wesley De Boever1; Frederik Coppens1; 1Tescan
Micro-CT can be used to study the structure of samples from a centimeter to micrometer scale. One of the main limitations in this, however, is the inability to perform true material identification without prior knowledge, as contrast inside a micro-CT scan is mainly caused by the atomic number of the sample.To overcome this limitation, we present the integration of an energy-sensitive spectral detector inside laboratory-based micro-CT scanners. Using this type of detector, not only the attenuated intensity of the X-ray beam when travelling through samples could be measured, but the entire energy spectrum (20-160 keV) of the X-ray beam was measured. Measurements were performed on various types of samples, from simple plastic specimen as proof of concept to economically important samples such as batteries and raw materials for the mining industry.
9:10 AM
X-ray Microscopy Analysis of Functionally Graded SiC Particle Reinforced Aluminum Matrix Composites Using Dual-energy Tomography: Eshan Ganju1; Hamid Torbatisarraf1; Caitlin O'Brien1; Meet Jaydeepkumar Oza2; Siddhartha Roy3; Tapas Laha4; Günter Schell2; Claudia Bucharsky2; Nikhilesh Chawla1; 1Purdue University; 2Karlsruhe Institute of Technology; 3Indian Institute of Technology Kharagpur ; 4Indian Institute of Technology Kharagpur
Al-SiC composites are important materials for high strength, high stiffness, and lightweight applications. The problem with using X-ray microscopy to study Al-SiC composites is that the densities of Al and SiC are very similar. In this study, we used a novel dual-energy X-ray Computed Tomography (DE-XCT) approach to segment the different phases of a functionally graded Al-SiC composite fabricated by spark plasma sintering. Using the DE-XCT data and 2D histogram-based annotated segmentation, we segmented the different phases of the composite and performed watershed analysis on the SiC phase to quantify the size, shape, orientation, and spatial distribution of the SiC particles in the composite. The segmentation and watershed analyses showed that the SiC particles are homogeneously distributed in the Al matrix and appear to have a preferred orientation. The combined use of DE-XCT scans and watershed analysis allowed us to gain important insights into the microstructure of the Al-SiC composite.
9:30 AM
Atomic-resolution 3D Analysis of Pt-Ru Alloy Nanoparticles by Electron Tomography: Tomokazu Yamamoto1; Koji Shigematsu1; Kohei Kusada2; Hiroshi Kitagawa2; Syo Matsumura1; 1Kyushu University; 2Kyoto University
Electron tomography (ET) is an important characterization tool for the investigation of catalytic alloy nanoparticles because their properties depends on morphological and structural factors; their size, shapes, surface compositions, segregation patterns and so on. Aberration-corrected scanning transmission electron microscopy (STEM) imaging and recent progress of tomographic reconstruction algorism such as a generalized Fourier iterative reconstruction (GENFIRE) developed by A. Pryor Jr. et al. has enabled atomic-resolution tomographic reconstruction of metal nanoparticles. In this study, we applied atomic-resolution ET on 3D structural analysis of multiple twined Pt-Ru alloy nanoparticles which is a promising anode catalyst for direct methanol fuel cells. The GENFIRE reconstructions from 45 STEM images of the nanoparticles reveals 3D segregated element distributions and multiple twined structure with {111} twin boundary. The resolution of the reconstructed images varied with direction due to missing-wedge artifacts from limited angle reconstruction and diffraction contrasts in STEM images.
9:50 AM Break
10:10 AM
Visualizing and Analyzing 3D Dislocation Structures in Metals with Dark-field X-ray Microscopy: Leora Dresselhaus-Marais1; 1Stanford University
Metals' properties are usually describe via dislocation density, but effects of 3D dislocation structures are often overlooked, as limited characterization methods can resolve 3D defects that span Angstrom to mm lengthscales. Dark Field X-ray Microscopy (DFXM) measures deep subsurface deformations in crystalline materials. My group has developed DFXM approaches to measure dynamics and 3D structures of dislocations across 100-300μm3 regions. This talk will introduce our use of “section-DFXM” to map 3D structures of dislocations - enabled by computer-vision. Reconstructing 4D (x,y,z,φ) scans into 3D maps, we identify hundreds of dislocations using segmentation and classification tools. I will show how annealed single-crystal metals seen by 3D DFXM give new insights into dislocation patterning. Our findings present key opportunities to establish how specific types of microstructural features give rise to the dynamics of dislocation theory.
10:30 AM
Dynamic In-situ Imaging of Methane Hydrate Formation and Self-preservation in Porous Media: Viktor Nikitin1; 1Max IV Laboratory
We present the results of dynamic in-situ 3D X-ray imaging of methane hydrates microstructure during methane hydrate formation and dissociation in sand samples. Short scanning times and high resolution provided by synchrotron X-rays allowed for better understanding of water movement and different types of gas-hydrate formation. Complementing previous observations, we conclude that gas-hydrate formation is accompanied by the water movements caused by cryogenic water suction that happens in sequences of short fast movements with longer equilibrium states in between (when the water is immobile). Based on the 3D microstructure we identified two types of gas-hydrate formation: i) into the gas pockets and ii) inside water volumes. The rate of dissociation in the self-preservation mode (pressure drop at negative temperatures) appears to be different for these two types of gas hydrates. This means that the history of gas-hydrate formation may influence its behaviour at the dissociation stage (e.g. gas-hydrate production).
10:50 AM Invited
In Operando 3D Characterization of Materials with Sub-15 nm Spatial Resolution Nano-tomography with the Transmission X-ray Microscope at APS: Vincent De Andrade1; Alex Deriy1; Michael Wojcick1; Sunil Bean1; Deming Shu1; Doga Gursoy1; Viktor Nikitin1; Francesco De Carlo1; 1Argonne National Laboratory
The TXM at beamline 32-ID of the APS at Argonne National Laboratory has been tailored for high throughput and high spatial resolution in operando nanotomography experiments. Thanks to a constant R&D effort, it emerged as a highly productive instrument, especially in the domain of Materials Science.Here, we will report recent upgrades that led the instrument to unprecedented level of performance. New optics conjugated with the enhancement of key mechanical components enabled 1 mn long tomographic acquisitions, to improve Zernike phase contrast measurement for materials like graphite and to achieve 3D spatial resolution of 13 nm, which is a record for a TXM and comparable to the resolution of the best hard X-ray ptychography microscopes. Then, we will present 3D characterization of material and systems in operando, like Portland cement formation over 10h with 1 min temporal resolution, Al-Cu alloy experiencing deformation or PGM-free electrocatalysts undergoing pyrolysis.