Characterization of Materials through High Resolution Coherent Imaging: Phase Contrast Imaging II
Sponsored by: TMS Structural Materials Division, TMS: Advanced Characterization, Testing, and Simulation Committee
Program Organizers: Ross Harder, Argonne National Lab; Xianghui Xiao, Argonne National Laboratory; Richard Sandberg, Los Alamos National Laboratory; Saryu Fensin, Los Alamos National Laboratory; Brian Abbey, LaTrobe University; Ana Diaz, Paul Scherrer Institut

Tuesday 2:00 PM
February 28, 2017
Room: 25B
Location: San Diego Convention Ctr

Session Chair: Ross Harder, Argonne National Lab

2:00 PM  
Anisotropic Growth Patterns in Four Dimensions: Ashwin Shahani1; Xianghui Xiao2; Peter Voorhees1; 1Northwestern University; 2Argonne National Laboratory
    Four-dimensional X-ray tomography (4D-XRT) has made it possible to follow microstructural evolution in three dimensions and as a function of time. The advent of novel techniques in reconstruction, data processing, visualization, and analysis now opens the door to a class of problems previously unexplored due to the lack of real-time 4D experiments. This is especially true of microstructures that have complex interfacial morphologies, such as group IV semiconductor crystals. For instance, silicon and germanium exhibit “mixed morphologies,” i.e., both faceted and rounded, due to the prevalence of defects that intersect the solid-liquid interfaces. Examples of our 4D-XRT results on the growth forms of such structures, collected in the absorption and phase mode, will be presented and discussed.

2:30 PM  
In-situ Phase Contrast Nano-tomography at ID16B: Julie Villanova1; Richi Kumar1; Rémi Daudin2; Pierre Lhuissier2; Luc Salvo2; David Jauffrès2; Christophe L. Martin2; Rémi Tucoulou1; 1ESRF - The European synchrotron; 2SIMAP-Univ. Grenoble Alpes
    In the framework of the European Synchrotron Radiation Facility (ESRF) upgrade program, a new nano-analysis beamline has been recently built on ID16 port(1). At 165m from the in-vacuum undulator source, ID16B endstation which offers a multimodal approach has been designed to accommodate several micro-analytical techniques (X-ray fluorescence, X-ray absorption, and X-ray diffraction) combined with 2D/3D X-ray imaging (XRI, such as magnified tomography and laminography). In this work, we present the in-situ nano-tomography set-up that has been developed to perform high temperature experiments. Thanks to different materials studies, the capabilities of the technique will be reviewed. Current challenges as well as future possibilities offered by the Extremely Brilliance Source upgrade program at the ESRF will be discussed. (1) G. Martínez-Criado, J. Villanova, R. Tucoulou, et al., ID16B: A hard X-ray nanoprobe beamline at the ESRF for nano-analysis. J. Synchr. Radiat., 23 (2015), p 344, 352.

2:50 PM  
High Speed Tomographic Imaging of Materials during Uniaxial Loading: Brian Patterson1; Nikhilesh Chawla2; Sudhanshu Singh2; Angel Ovejero2; Jason Williams2; Xianghui Xiao3; Kevin Henderson1; Robin Pacheco1; Nikolaus Cordes1; James Mertens1; 1Los Alamos National Laboratory; 2Arizona State University; 3Argonne National Laboratory
    Understanding the effects of material composition, geometry, aging, and processing upon the overall material performance requires a detailed understanding of their initial morphology and how the morphology changes under external stimuli. Synchrotron light sources, such as the APS, afford materials researchers unprecedented X-ray flux to help unravel these complex materials science challenges. Full 3D tomographic data in ~0.25 seconds with a ~five micrometer voxel size while uniaxially loading materials makes it possible to study the dynamic in situ deformation of materials at greater than 10-2 strain rates. The in situ imaging of polymer foams during uniaxial compression was completed and used to model the mechanical performance of these hyper elastic materials. Experiments of 3D printed materials during uniaxial tension shows the 3D flow of the glass filled nylon material and the delamination of the filler material and the polymer binder during the plastic flow and breakage.

3:20 PM Break

3:40 PM  
In-situ Deformation and Damage Assessment in Materials under Dynamic Loading Using High Speed Synchrotron X-ray Phase Contrast Imaging: Niranjan Parab1; Zherui Guo1; Matthew Hudspeth1; Benjamin Claus1; Jou-Mei Chu1; Tao Sun2; Kamel Fezzaa2; Weinong Chen1; 1Purdue University; 2Argonne National Laboratory
    A high speed synchrotron X-ray phase contrast imaging setup (PCI) is integrated with a modified Kolsky bar setup to study the deformation and fracture behavior of materials under high strain rate loading at beam line 32-ID, Advanced Photon Source, Argonne National Laboratory. The synchrotron X-ray imaging technique provides a significant advantage over the traditional optical imaging in terms of ability to observe in-situ sub-surface fracture in materials under dynamic loading. In this study, the dynamic loading is applied on the specimens using a modified miniaturized Kolsky bar apparatus. The resulting deformation and fracture history is recorded using the high speed synchrotron X-ray PCI. The effectiveness of the novel union between these two powerful experimental techniques is demonstrated by a series of dynamic experiments on different material systems, including fracture of particles in a granular system, ligament-bone junction damage, fracture of concrete and other geo-materials, and fiber pull-out from composite materials.

4:10 PM  
In-Situ and In-Operando Examination of Structure-Functional Relations in Porous Materials for Energy Conversion and Storage with Nano- and Micro- Synchrotron X-ray Computed Tomography: Andrew Shum1; Vincent De Andrade2; Xianghui Xiao2; Dilworth Parkinson3; Adam Weber4; Iryna Zenyuk1; 1Tufts University; 2Advanced Photon Source, Argonne National Laboratory; 3Advanced Light Source, Lawrence Berkeley National Laboratory; 4Lawrence Berkeley National Laboratory
    Porous carbon materials make up the essential components of polymer-electrolyte fuel cells (PEFCs) and redox-flow batteries (RFBs). Understanding the morphology and associated liquid and gas transport in these porous carbon papers is critical to optimizing the performance of RFBs and PEFCs. These materials are selected based on their structural stability, high electrical and thermal conductivity, large surface area, and high fluid transport properties due to their relatively large pores (10 um) and high porosity. To improve transport phenomenon in these high surface area media, three-dimensional studies are necessary to fully resolve the complex and anisotropic structure. Synchrotron nano- and micro- X-ray computed tomography (CT) utilizing phase contrast imaging is used to characterize these materials for energy applications. We will discuss various in-situ and in-operando experimental procedures for synchrotron imaging to further fundamental understanding of structure-property phenomena in these multi-scale materials and provide a roadmap for the design of next-generation materials.

4:40 PM  
Zernike Phase Contrast for Hard X-ray Microscopy: Ken Vidar Falch1; Ragnvald Mathiesen1; Anatoly Snigirev2; Irina Snigireva3; Mikhail Lyubomirskiy3; Daniele Casari1; 1NTNU; 2Immanuel Kant Baltic Federal University; 3ESRF
    While high resolution microscopy is available at soft x-ray energies, some types of samples require better transmission in order to give sufficient signal. As phase contrast is significantly stronger than absorption contrast, it is in most cases beneficial to rely on the former. A hard x-ray Zernike phase contrast (ZPC) microscope based on refractive X-ray optics has been implemented with 17 keV photon energy, utilizing both monochromatic and pink beam radiation with 0.3% bandwidth. Significantly increased contrast has been achieved in a series of weakly absorbing samples, such as organic micron-sized colloid particles and Al-Si alloy microstructures. Contrast enhancement and the use of non-monochromatized radiation from undulator harmonics can reduce the exposure times required, and pave the way for ultra-fast microscopy imaging at high photon energies.

5:10 PM  
Phase Contrast Tomography to Document Gypsum Dehydration in Single Crystals and Polycrystalline Materials: Florian Fusseis1; Xianghui Xiao2; John Bedford3; Henri Leclere3; 1University of Edinburgh; 2Argonne National Laboratory; 3Liverpool University
    Gypsum (CaSO4.2H2O) is one of the most abundant naturally occurring sulphates and of immense significance for several research communities, ranging from construction materials, trough artifact preservation to tectonic processes. At the core of most research is the dehydration path of gypsum upon heating, from gypsum to hemihydrate (CaSO4.1/2H2O) then anhydrite (CaSO4). Despite a century worth of research, key aspects of the dehydration process are still poorly understood. For the first time, we used synchrotron-based phase contrast microtomography to document the hemihydrate formation during the dehydration of gypsum in situ. Our 4D data comprise several tens of time steps and capture the advance of the reaction in sufficient detail to determine the reaction rate and identify the key parameters governing reaction advance. the new data not only advances our understanding of this ubiquitous material significantly but also outlines a novel direction in the study of chemical reactions.