5th International Congress on 3D Materials Science (3DMS 2021): Practical Applications
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
Wednesday 12:10 PM
June 30, 2021
Room: Virtual D
Location: Virtual
Session Chair: Ashley Spear, University of Utah
3D Characterization of Grain Structure and In-situ Deformation of Open-cell Metal Foam Using Micro-computed Tomography and High-energy X-ray Diffraction Microscopy: Quinton Johnson1; Jayden Plumb2; Peter Kenesei3; Hemant Sharma3; Jun-Sang Park3; Ashley Spear1; 1University of Utah; 2University of California, Santa Barbara; 3Advanced Photon Source, Argonne National Laboratory
Ultra-low-density foams have complex hierarchical structures that give rise to desirable properties like high strength-to-weight ratio and excellent energy absorption. The sparse, fragile network of struts in open-cell foams makes characterizing sub-strut-scale material structure especially challenging. In this work, 3D grain and precipitate structures are characterized for open-cell aluminum foam using synchrotron characterization techniques. X-ray computed tomography and high-energy X-ray diffraction microscopy data were collected in-situ at interrupted loading intervals during compression. A novel scanning strategy developed at the APS 1-ID beamline enabled complete characterization of a 6%-dense foam sample that was four times larger than the X-ray beam width. A data-analysis procedure was developed to track grains through large strut displacement and deformation. The 3D precipitate maps were used to correlate ligament failure to precipitate distributions. The methods and procedures developed here can be applied to other low-density structures (e.g., AM lattices) and enable new possibilities for high-fidelity modeling.
In-situ 3D Imaging of Mechanical Failure in TRISO Particles: Stephen Kelly1; Hrishikesh Bale1; Peter Hosemann2; 1Carl Zeiss Microscopy; 2University of California
Tri-structural isotropic (TRISO) particles are leading candidates for use as fuel in advanced, high temperature nuclear reactors. They are small (~1 mm diameter) composite spheres containing a nuclear fuel core surrounded by concentric layers of carbon and SiC. Their composite construction allows them to operate at high temperatures with excellent resistance to corrosion, oxidation, and neutron irradiation. The robust containment of the fuel core and fission products depends critically on the integrity of the SiC layer, and the mechanical properties of this layer must be understood for proper fuel particle design and integration into larger scale reactor systems. We present here a 3D in situ investigation into the fracture properties of the SiC layer in a surrogate (non-radioactive core) TRISO particle. We apply a compressive load while simultaneously imaging the 3D microstructure using sub-micrometer x-ray microscopy to visualize crack propagation in the SiC layer.
Possibilities and Limitations of Tomography Methods for the Detailed Analysis of Lithium-ion Battery Cathode Microstructures: Jochen Joos1; Stephen Kelly2; Tobias Volkenandt2; Stefanie Freitag2; André Weber1; Ellen Ivers-Tiffée1; 1Institute for Applied Materials (IAM-WET), Karlsruhe Institute of Technology (KIT); 2Carl Zeiss Microscopy
Deep knowledge of the 3D microstructure is essential for optimizing performance in Lithium ion batteries electrodes. Tomography methods like focused ion beam-secondary electron microscopy (FIB-SEM) and X-ray tomography are the most frequently used 3D characterization techniques for battery electrodes. While each method has advantages and disadvantages, understanding the complex morphology of electrodes requires a complementary, multi-scale 3D approach. In this work, the possibilities and limitations for both 3D techniques, X-ray and FIB-SEM tomography, are studied using the example of a LiNiCoAlO2-LiCoO2 blend cathode from a commercial cell. The same cathode sample was analyzed with both techniques and moreover with different devices to enable a comparison of the obtained data quality. The material fractions, porosity, surface area and tortuosity are calculated from the different data sets and the results are compared with special emphasis on the differentiation of the different active materials and the carbon-binder phase.
Precipitation and Strengthening in AlCoCrFeNi High Entropy Alloys as Studied by Atom Probe Tomography: Keith Knipling1; Patrick Callahan1; David Beaudry2; 1Naval Research Laboratory; 2University of Florida
High entropy alloys (HEAs) typically contain five or more principal elements in nearly equiatomic proportions, significantly expanding the composition space and achievable properties of novel metallic materials. In this study we present the complex three-dimensional nanoscale microstructures formed in Al0.5CoCrFeNi (atomic fraction) HEAs in the as-cast state and after thermal aging at 700 and 1000 °C. The alloy solidifies into dendritic regions that have a face-centered cubic (FCC) crystal structure enriched in Co, Cr, and Fe, and interdendritic regions that are comprised of a disordered body-centered cubic (BCC, A2) phase and an ordered BCC phase (B2) formed by spinodal decomposition. During aging these regions form a variety of strengthening precipitates, including NiAl (B2 structure), Ni3Al (L12), and α-Cr (BCC). Atomic-scale clustering and ordering is assessed in three dimensions using atom-probe tomography and these experimental results are compared with the equilibrium phases predicted by thermodynamic modeling.
Properties Relied on Internal Structure of Ceramics from 3D View of X-ray Tomography: Lei Zhang1; Shaogang Wang1; Zhen Wu1; Lei Cao1; 1Chinese Academy of Sciences
Highly porous ceramic was quantitatively characterized for the morphological parameters within the 3D volume. The size, shape of the pores as well as their distribution and connectivity, can be evaluated for the property of thermal insulation with the supplementary of modeling and analysis. As a bio-inspirited material, sea urchin spine is composed of bio ceramic and organic substance with a hierarchical structure. The complex 3D volume of a sampled structure was digitalized with the XRT techniques. The meshed 3D volume can be input Finite Element Analyses (FEA) for mechanical test with the 3D global scale. Compression of the real structure model revealed that the stress concentrates along the dense growth rings and dissipates through the strut structures. It implied that the rationally constructed hierarchical structure in nature play an important role in high strength-to-weight property. Its mechanical property might be optimized for potential applications of bone defect repair.
Revealing Complex Materials Structure in Dealloying and Energy Storage by Synchrotron X-ray Nano-tomography: Yu-chen Karen Chen-Wiegart1; 1Stony Brook University
Synchrotron X-ray nano-tomography with operando analysis and chemical sensitivity is powerful to study complex structures. We will discuss two types of such systems – porous metals fabricated by dealloying and energy storage materials in batteries. Dealloying, a selective etching process, can fabricate a variety of nanoporous metals with a characteristic bi-continuous structure with promising applications in catalysis, energy storage and bio-sensing. Our work includes addressing the processing-structure correlation in different dealloying systems, from solid-state interfacial dealloying, chemical dealloying, molten salt corrosion, and vapor phase dealloying. We utilized both full-field and scanning techniques. In addition, by combining X-ray imaging with other modalities, we applied a multimodal approach to address the complex chemical, morphological and structural evolution in energy storage materials. Novel systems with nanoporous electrodes, beyond-lithium batteries and aqueous batteries, will be discussed. These works highlight how X-ray nano-tomography methods can advance our understanding in complex materials for future materials design.
Three-dimensional Characterization and Modelling of Cyclic Deformation in Magnesium Alloys by High-energy X-ray Diffraction Microscopy: Duncan Greeley1; Mohammadreza Yaghoobi1; Darren Pagan2; Veera Sundararaghavan1; John Allison1; 1University of Michigan; 2Cornell High Energy Synchrotron Source
Fatigue behavior is a primary concern for lightweight structural components. To accurately predict the effect of microstructure and composition on low-cycle fatigue in rare-earth magnesium alloys, it is necessary to understand the effect of texture and grain size on micromechanical evolution during fatigue cycling. High-energy X-ray diffraction microscopy (HEDM) was utilized to analyze the three-dimensional character of deformation during a fully reversed tension-compression cycle in coarse and fine-grain size Mg-2.4wt.%Nd. Grain average strains in each microstructure were tracked in-situ with far-field HEDM. Slip activity and localization of strain were modelled with the PRISMS-Plasticity crystal plasticity finite element software using unloaded 3D grain morphologies and grain orientations characterized using near-field HEDM. The results of these crystal plasticity predictions are compared to far-field measurements. The dataset from this study is published publicly in the Center for Predictive Integrated Materials Science (PRISMS) Materials Commons data repository.