5th International Congress on 3D Materials Science (3DMS 2021): Characterization Methods I
Program Organizers: Dorte Juul Jensen, Technical University of Denmark; Erica Lilleodden, Fraunhofer Insitute for Microstructure of Materials and Systems (IMWS); Scott Barnett, Northwestern University; Keith Knipling, Naval Research Laboratory; Matthew Miller, Cornell University; Akira Taniyama, The Japan Institute of Metals and Materials; Hiroyuki Toda, Kyushu University; Lei Zhang, Chinese Academy of Sciences
Tuesday 9:50 AM
June 29, 2021
Room: Virtual B
Location: Virtual
Session Chair: Matthew Miller, Cornell University
A New Generation of Synchrotron-based Design Tools at MSN-C (The Materials Solution Network at CHESS): Matthew Miller1; Paul Shade2; 1Cornell University; 2Air Force Research Laboratory
Over the past decade at high energy synchrotron light sources around the world, a broad range of x-ray scattering experiments have been transitioning to materials characterization measurements, thereby shifting the focus from the x-rays and photon science to the materials themselves and their applications in engineering design. This talk describes several examples examining the processing and performance of structural alloys within the new Materials Solution Network at CHESS (MSN-C) funded by AFRL. MSN-C provides beamtime to DoD researchers on two x-ray beamlines – one at high energy for metals and the other at lower energy for polymers and composites - to utilize these developing tools on some of the most pressing DoD materials challenges.
Advanced In-situ Loading Environments for Synchrotron X-ray Diffraction Experiments: Paul Shade1; Basil Blank2; Mark Obstalecki1; William Musinski1; Peter Kenesei3; Jun-Sang Park3; Jon Almer3; Darren Pagan4; Kelly Nygren4; Peter Ko4; Christopher Budrow5; David Menasche6; Joel Bernier7; Robert Suter8; Todd Turner1; 1Air Force Research Laboratory; 2PulseRay; 3Advanced Photon Source; 4Cornell High Energy Synchrotron Source; 5Budrow Consulting; 6Hamiltonian Group; 7Lawrence Livermore National Laboratory; 8Carnegie Mellon University
High energy x-ray characterization methods hold great potential for gaining insight into the behavior of materials and providing comparison datasets for the validation and development of mesoscale modeling tools. A suite of techniques have been developed by the x-ray community for characterizing the 3D structure and micromechanical state of polycrystalline materials; however, combining these techniques with in situ mechanical testing under well characterized and controlled boundary conditions has been challenging due to experimental design requirements. In this presentation, we describe advanced in situ loading environments that have been developed for communal use at the Advanced Photon Source and the Cornell High Energy Synchrotron Source. Example 3D datasets that have been collected using this hardware and their application for materials modeling efforts will be discussed.
Application of High Energy Imaging CT to Investigate Local 3D Short Fatigue Crack Closure Behavior in Ti-6Al-4V Alloy: Valary Tubei1; Hiroyuki Toda1; Kyosuke Hirayama1; Meysam Hassanipour1; Akihisa Takeuchi2; Masayuki Uesugi2; 1Kyushu University; 2Japan Synchrotron Radiation Research Institute
High energy imaging CT has been utilized for the in-situ observation of local 3D short fatigue crack closure behavior in Ti-6Al-4V alloy at SPring-8 synchrotron radiation facility in Japan. In recent years, projection CT with a resolution of ~1 µm has been employed to non-destructively observe crack closure. However, the short crack tip opening displacement is usually below 1µm and thus this technique cannot be used to accurately visualize crack front closure behavior. Recent CT technology advances have led to the achievement of ultra-high resolution imaging that is realized by focusing the high energy X-ray beams using the apodization Fresnel Zone Plate. This imaging CT was utilized in this study with X-ray energy of 30 keV. In combination with the high contrast attained by using the Zernike Phase Plate, the internal microstructure, crack and crack closure occurrence at the crack front were readily visualized at a resolution of 130 nm.
Phase Change of Pyrolitic Material: In-situ Transformation and Induced Microstructures at 660 km Depth: Jeff Gay1; Estelle Ledoux1; Matthias Krug2; Anna Pakhomova3; Ilya Kupenko2; Julien Chantel1; Carmen Sanchez-Valle2; Sébastien Merkel1; 1University of Lille; 2University of Münster; 3DESY, Hamburg, Germany
Phase transformations within the Earth’s mantle can cause crystal growth in preferred orientations among other phenomena. These phase changes are a result of changes in pressure and temperature with depth. At 660 km, ringwoodite and garnet decompose to form bridgmanite and ferropericlase. These transformations generate microstructures, cause seismic reflectors, and viscosity changes that impact mantle dynamics. Understanding these transformation microstructures will hence better constrain processes in the Earth’s mantle. These transformations are not martensitic, but grains grow with preferred orientations through diffusive processes. Here we implement synchroton multigrain x-ray diffraction in a laser heated diamond anvil cell. We are able to track individual grains, crystal structures, and orientations, while being compressed in-situ at pressures ranging from 18 to 55 GPa and temperatures of ~1800 K. Using this experimental approach, we can then use obtained transformation textures to refine current seismic models to better understand seismic observables in the Earth’s mantle.
Redefining ESRF's Tomography Ecosystem for the EBS Upgrade: Nicola Viganò1; 1ESRF - The European Synchrotron
The scheduled ESRF EBS upgrade will offer unprecedented opportunities for tomographic applications. The higher available X-ray photon flux and coherence will allow to overcome current limitations in imaging and microstructure characterization techniques like: X-ray phase contrast tomography (XPCT), X-ray diffraction computed tomography (XRD-CT) and X-ray fluorescence computed tomography (XRF-CT). The increased X-ray flux and the consequent reduction of acquisition times allow to increase the acquisition rate and data throughput. This will unlock a number of time-lapse observation studies and multi-modal techniques that were not possible before, but it will also put more strain on the current data processing pipeline.In this oral presentation, I will present the undergoing restructuring of the ESRF tomography acquisition and processing ecosystem. I will also discuss the plans for improving the currently offered tomographic reconstruction tools, by leveraging advances in multi-channel/multi-modal reconstructions and machine-learning.
Three-dimensional Sub-grain Mapping of Lattice Strains and Orientations in Polycrystals: Peter Reischig1; Wolfgang Ludwig2; 1InnoCryst Ltd; 2CNR / ESRF
We demonstrate the capability of efficiently mapping the complete local strain and orientation tensor field at the sub-grain level in three dimensions inside a polycrystal, in a non-destructive way. Diffraction Contract Tomography can provide detailed 3D grain maps of moderately deformed polycrystals at the micrometre scale, utilising high-energy, monochromatic synchrotron X-rays. Using full-beam illumination and a single sample rotation enables fast and efficient scans. The ESRF source upgrade will bring scanning times of the order of minutes in in-situ experiments within reach. The highly convoluted experimental data pose a large-scale, 12-dimensional, ill-posed, non-linear reconstruction problem. A forward model and iterative solver has been developed to infer the grain shapes, sub-grain orientation and strain fields (order of 10-3 to 10-4). Furthermore, the single crystal elastic moduli are fitted from the strain data. The data acquisition and processing method, and experimental validation on a Gum metal sample under tensile load will be discussed.