Characterization of Materials through High Resolution Imaging: High Resolution Characterization of Materials with Phase Contrast Imaging
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
Thursday 8:30 AM
March 18, 2021
Room: RM 14
Location: TMS2021 Virtual
Session Chair: Xianghui Xiao, Brookhaven National Laboratory
8:30 AM Invited
In Situ and Operando 3D Nano-imaging for Materials Science at the ESRF: Julie Villanova1; Richi Kumar1; Victor Vanpeene1; Jaime Segura-Ruiz1; Remi Tucoulou1; Pierre Lhuissier2; Luc Salvo2; 1ESRF; 2SIMAP/UGA
X-ray computed tomography is now well recognized as a powerful technique to investigate material properties from the micro to the nano-scale. The use of phase contrast imaging provides non-destructive access to 3D morphology, by highlighting small features of differing refractive index within structures that are otherwise uniform or within weak absorbing materials. Thanks to the high flux of synchrotron X-ray nano-beams and the constant improvement of the detectors, fast acquisition rates are now reachable at the nano-scale, leading to dynamic monitoring of phenomena through in situ and operando measurements. This work presents the in situ hard X-ray nanotomography setup that has been developed at the ID16B beamline of the ESRF. It details different examples of studies on metallurgy and energy materials, and the technical developments associated. Finally, the benefits and limitations brought to the technique by the new extremely brilliant X-ray source EBS of the ESRF are discussed.
9:00 AM
Evaluation of TATB Crystal Morphology for Predicting Sensitivity Using X-ray Computed Tomography: Lindsey Kuettner1; Brian Patterson1; John Yeager1; Larry Hill1; 1Los Alamos National Laboratory
Triaminotrinitrobenzene (TATB) explosive crystals are used within a variety of high explosive systems. The crystal loading and physical heterogeneity, crystal size and shape, and internal microstructure can all greatly affect the sensitivity of the explosive. The internal structure of dry-animated TATB is comprised of residual NH4Cl inclusions and voids that were created when washing out the NH4Cl. Quantifying these inclusions and voids, as well as whole crystal structure, could lead to predictions of detonation sensitivity of HE lots. In order to study the internal grain microstructural difference between TATB crystals, measurements were performed using nano- and micro-scale X-ray computed tomography (CT). MicroCT was used to image many distributed crystals simultaneously to obtain a value of the crystal size. NanoCT was used to image the NH4Cl and intra-crystal void sizes and distribution. It was found that the void fraction is approximately correlated and the NH4Cl inversely correlated with powder sensitivity.
9:20 AM
Megahertz X-ray Microscopy for Imaging High-speed Phenomena in Opaque Materials: Valerio Bellucci1; Tokushi Sato1; Pablo Villanueva Perez2; Jozef Ulicny3; Wataru Yashiro4; Henry Chapman5; Adrian Mancuso1; Patrik Vagovič5; 1European XFEL GmbH; 2Lund University; 3Pavol Jozef Šafárik University; 4Tohoku University; 5Center for Free-Electron Laser Science
X-ray phase-contrast microscopy with a sampling rate of 1.128 MHz was demonstrated at the European X-ray Free-Electron Laser with micrometre scale spatial resolution. The contrast and spatial resolution attained were superior in comparison to previous synchrotron MHz microscopy due to the high brilliance of the source. This work opens up the possibility of imaging dynamic stochastic phenomena in opaque systems with object velocities up to a few kilometres per second at nanosecond to microsecond time scales by using XFEL sources. Modern emerging technologies, such as additive manufacturing, bioprinting, and new material production, will benefit from this novel metrology tool to probe fundamental high-speed dynamics occurring in such systems. The high brilliance of modern XFEL sources paves the way for future developments of this technology with the introduction of 3D MHz microscopy for volumetric imaging of fast phenomena in opaque samples.
9:40 AM
Microstructural Characterization and Mechanical Behavior of a Meteorite Using Correlative Microscopy: Tai-Jan Huang1; Sridhar Niverty1; Arun Sundar1; Md Fazle Rabbi2; Laurence Garvie2; Aditi Chattopadhyay2; Desireé Cotto-Figueroa3; Nikhilesh Chawla1; 1Purdue University; 2Arizona State University; 3University of Puerto Rico at Humacao
Meteorites have a complex microstructure due to their multicomponent nature and the conditions in which they were formed. Their complex anisotropic structure and formation history makes it difficult to obtain reliable structure-property relationships in these materials. Thus, a comprehensive assessment of microstructural phase distribution and the connection to mechanical properties is important. In this study, a correlative microscopy-based approach was used to characterize the meteorite Aba Panu(L3). Absorption contrast X-ray tomography was employed to non-destructively obtain the 3D spatial distribution of constituent phases. Additionally, scanning electron microscopy, energy dispersive spectroscopy (EDS), and wavelength dispersive spectroscopy (WDS) were employed to obtain phase compositions and thereby, infer the types of mineral present in the meteorite. Nanoindentation and Vickers micro-indentation were performed on all identified phases to measure modulus and hardness properties. The variability in mechanical properties of the various phases were correlated with the compositional variability and will be discussed.
10:00 AM Invited
Imaging Materials on the Run: Shedding Light on Fast Structural Processes Using Time-resolved Synchrotron X-ray Tomographic Microscopy: Christian Schlepuetz1; Federica Marone1; Anne Bonnin1; Marco Stampanoni1; 1Paul Scherrer Institute
Properties of high-tech materials are highly influenced by transient processing conditions. A thorough understanding of their structural evolution during fabrication thus allows tailoring performance for specific purposes. However, many dynamic processes, such as crack propagation in composites, bubble formation in metal foams, dendrite growth during solidification, etc., occur within opaque materials usually hosted in complex conditioning environments on microscopic length scales and sub-second time scales, making them elusive to common characterization methods. To overcome these limitations, the latest developments in time-resolved synchrotron microtomography have pushed the routinely achievable time resolution well into the sub-second regime, reaching up to hundreds of tomographies per second for selected material systems, while allowing for ever more complex environments to produce realistic sample conditions. With the development of advanced tomographic reconstruction algorithms, even a live preview of virtual slices through 3D volumes in nearly real time is possible.
10:30 AM
Quantitative Data Analysis of Dynamic Tomography Data with Motion Artifacts: Xianghui Xiao1; Yang Yang1; Zhenrui Xu2; James Steiner2; Yijin Liu3; Feng Lin2; 1Brookhaven National Laboratory; 2Virginia Tech; 3SLAC National Accelerator Laboratory
X-ray tomography has been widely used in inspecting opaque objects’ structures nondestructively. With the bright light sources and advanced detector techniques, x-ray tomography can be used to detect rapid dynamic structure changes in samples under various stimulus conditions. However, the temporal resolution of the tomography technique has still been handicapped by the intrinsic limitations in the data acquisition speed and the lack of a suitable data processing method. In this talk, I will present a novel quantitative data analysis method that can tolerate the ‘imperfect’ tomography reconstruction data in which there are severe sample motion artifacts. An application in the drying film cases will be discussed in the presentation.
10:50 AM Invited
High Speed, High Resolution, High Temperature 3D Imaging of Spacecraft Materials during Atmospheric Entry Conditions: Dilworth Parkinson1; Harold Barnard1; Alastair MacDowell1; Sam Schickler1; Shawn Shacterman1; Talia Benioff-White1; Kara Levy1; Francesco Panerai2; Collin Foster2; Benjamin Ringel2; Christian Schlepuetz3; 1Lawrence Berkeley National Laboratory; 2University of Illinois, Urbana-Champaign; 3Paul Scherrer Institute
During atmospheric entry, spacecraft experience extreme conditions, and it is important to better understand how materials in current use by NASA behave under these conditions, to work towards developing new materials. We performed high speed, high resolution, high temperature 3D imaging--using synchrotron propagation-based phase contrast microCT--of spacecraft heat shield and parachute materials under conditions meant to simulate re-entry. The data was reconstructed and analyzed using machine learning approaches on high performance computing systems, and simulations of each experimental run were performed to check the ability of the models to capture all of the relevant features observed in the experiments. In this presentation, both the experimental and computational methods for this work will be described, and both visual and quantitative comparisons of experiment and simulation will be shown.
11:20 AM
Study of Structure of Beam-sensitive Supported Nanoparticle Catalysts by Low-dose High Resolution Phase Contrast Imaging: Cheng-Han Li1; Joerg Jinschek1; 1The Ohio State University
Phase contrast imaging (PCI) in scanning / transmission electron microscopy (S/TEM) has been widely utilized to reveal the structure of materials with high spatial resolution and high sensitivity. In general, acquisition of an image series, such as focal series, are necessary to generate sufficiently high S/N data that is further processed using algorithm to restore the phase contrast and amplitude contrast images. However, such extended exposure to high-energy electrons might be too invasive for electron-beam-sensitive materials, such as highly active supported nanoparticles catalysts. Thus, strategies have to be applied managing electron dose and minimize invasive electron-beam effects. In this study, high-resolution PCI with optimized electron-dose exposure and fast-speed direct electron detection have been utilized to reveal the pristine microstructure of supported noble metals model catalysts, correlated with simulated images. Low-dose PCI methods are essential to characterize beam-sensitive materials with high spatial resolution.
11:40 AM
Indexing Grains: A Comparison between Three-dimensional Synchrotron X-ray Diffraction and Electron Backscatter Diffraction Techniques: Karim Louca1; Hamidreza Abdolvand1; 1Western University
Understanding deformation mechanisms of metals and alloys at meso- and nano- scales is necessary for developing predictive models that estimates service life of engineering components. In this study, three-dimensional synchrotron X-ray diffraction (3D-XRD) technique is used to measure the center-of-mass (COM), orientation, volume and elastic strain of individual grains in a pure zirconium specimen. In addition, electron backscatter diffraction technique is used to measure the orientations and morphologies of the grains located at the surface of the same specimen. Indexed grains from both techniques are compared. This is followed by using the weighted Voronoi method to simulate grain morphologies from the 3D-XRD data. The simulated grain map is compared to the one measured by EBSD. It is shown that more than 80 percent of the grain neighbors are correctly matched between the two techniques.