Characterization of Minerals, Metals and Materials: Advanced Characterization Methods II
Sponsored by: TMS Extraction and Processing Division, TMS: Materials Characterization Committee
Program Organizers: Mingming Zhang, Baowu Ouyeel Co. Ltd; Zhiwei Peng, Central South University; Jian Li, CanmetMATERIALS; Bowen Li, Michigan Technological University; Sergio Monteiro, Instituto Militar de Engenharia; Rajiv Soman, Eurofins EAG Materials Science LLC; Jiann-Yang Hwang, Michigan Technological University; Yunus Kalay, Middle East Technical University; Juan Escobedo-Diaz, University of New South Wales; John Carpenter, Los Alamos National Laboratory; Andrew Brown, Devcom Arl Army Research Office; Shadia Ikhmayies
Monday 2:00 PM
March 20, 2023
Room: Aqua 313
Location: Hilton
Session Chair: Bowen Li, Michigan Technological University; Rajiv Soman, Eurofins EAG Materials Science LLC
2:00 PM
On the Feasibility of Back-scattered or Ion-induced Secondary Electron Imaging to Determine Grain Orientations: Marc De Graef1; 1Carnegie Mellon University
Electron backscatter diffraction (EBSD) is a standard microstructure characterization technique used to determine grain orientations over a region of interest. The experimental scan is performed in a serial fashion, one sampling point at a time. Other observation modalities in the scanning electron microscope, e.g. backscattered electron (BSE) imaging and ion-induced secondary electron (ISE) imaging, are comparatively much faster than an EBSD scan, which raises the question of whether or not these techniques can be used to acquire orientation information. In this contribution we will analyze how the experimental parameters (e.g., number of images at different sample tilts) affect the orientation accuracy of both BSE and ISE imaging approaches using physics-based forward models for both modalities. The combination of BSE/ISE imaging with dictionary matching for individual image pixel intensity profiles may result in a fast large area orientation determination with sufficient orientation accuracy to be competitive with the EBSD approach.
2:20 PM
Structure and Interfaces of MBE Grown Fe Thin Films on GaAs: Ramasis Goswami1; 1Naval Research Laboratory
Fe/GaAs is an important system to study spin injection behavior that can vary with the nature and interfaces of Fe films. Here we investigate the effect of interfacial strain on the microstructure, interfaces and phase formation behavior in epitaxially grown Fe films. To vary the strain, we have characterized Fe films of various thicknesses ranging from 10 to 1000 nm which were grown using molecular beam epitaxy on GaAs (011) and AlGaAs (001) substrates. High resolution x-ray diffraction studies reveal that films with higher thicknesses exhibit an equilibrium alpha-Fe phase, while the films with less than 10 nm thicknesses indicate the presence of delta-Fe. Transmission electron microscopy reveals the interface for 10 nm thick films has strain lobes with no interfacial phase formation for films deposited at room temperature. At higher deposition temperature, 175ºC, similar strain lobes were observed for a 10 nm thick film.
2:40 PM
Development of Bearing Temperature Monitoring Technology in Railway Vehicle: Jeongguk Kim1; 1Korea Railroad Research Institute
The axle bearing of a railway vehicle is one of the parts that play an important role in driving the axle. In case of bearing damage or abnormality, a major accident may occur while the railway vehicle is running. Therefore, it is important to manage the abnormal condition of the axle bearings. Bearing abnormalities are usually managed by monitoring the bearing temperature. European EN standards monitor the temperature by installing a temperature monitoring device around the wayside, and recommends that a bearing temperature monitoring device for high-speed railways over 250km/h. In this study, infrared thermography technology was applied to monitor the axle bearing temperature. A temperature monitoring system was developed by installing a small infrared camera on the upper part of the axle and measuring the temperature outside the axle box on the vehicle. In this presentation, infrared thermal imaging sensing, operation program, and experimental results will be introduced.
3:00 PM
Enhancing the Reliability of Reconstruction for Small Grains Using Novel Laboratory Diffraction Contrast Tomography (Lab DCT) Acquisition and Reconstruction Approaches: Eshan Ganju1; Eugenia Nieto-Valeiras2; Javier LLorca2; Nikhilesh Chawla1; 1Purdue University; 2IMDEA Materials Institute
Laboratory Diffraction Contrast Tomography (LabDCT) in tandem with Absorption Contrast Tomography (ACT) has enhanced our understanding of 3D and 4D phenomena over the last decade. One of the biggest challenges presently in Lab DCT technique is the reliable reconstruction of small grains (< 20 µm). Here we present a systematic study of different LabDCT acquisition and reconstruction strategies with the aim of improving the reliability of reconstruction of smaller grains. Two metallic samples (pure Ni and Ti) were scanned to obtain diffraction radiographs under Laue-focusing and magnified acquisition geometries. A sophisticated forward modeling-based approach was used to enhance the reconstruction reliability of the smaller grains within the samples. Furthermore, the LabDCT grain maps were compared to EBSD grain maps to assess reconstruction accuracy of the smaller grains. Finally, recommendations will be made regarding the optimal acquisition and reconstruction approaches to reliably capture small grains with the Lab DCT technique.
3:20 PM
Film Structure of Polymerized Synthetic Dopamine by Neutron Reflectometry: Matthew Herman1; Erik Watkins1; John Yeager1; 1Los Alamos National Laboratory
Synthetic dopamine, capable of undergoing self-polymerization under ambient conditions and becoming polydopamine (PDA), has been demonstrated to form controllable nanometer thickness films. These films have been applied to various substrates, including high explosives and particle composites, promoting adhesion between the polymer binder and filler interface. These films are thought to form a core-shell architecture consisting of a rigid polymer shell over the substrate. The effects of PDA film in application and chemical composition of the polymer are well understood, but the general structure of the polymerized dopamine is lacking in the literature. Neutron reflectometry, performed on the Asterix beamline at the Los Alamos Neutron Science Center, has been employed to demonstrate the controllable nature of PDA film growth and the film’s structure. Thin film composite stack-ups of inert crystal, PDA, and polymer binder system were investigated to determine the nature of the various interfaces.
3:40 PM Break
3:55 PM
Material Characterization by Neutron Imaging and Neutron Grating Interferometry: Yuxuan Zhang1; Leslie Butler2; Hassina Bilheux1; Kyungmin Ham2; Jean Bilheux1; Erik Stringfellow1; Wieslaw Stryjewski2; Michael Vincent2; 1Oak Ridge National Laboratory; 2Louisiana State University
Neutron imaging, similar to X-ray imaging, is a non-destructive technique that investigates the internal features/structures of an object. Neutron’s high penetration through metals and its high sensitivity to light elements (H, Li, etc.) have made neutron imaging a unique tool in many research fields such as energy storage materials, additive manufacturing, geology, nuclear materials, etc. Recently, neutron grating interferometry (nGI) has been implemented at the cold neutron imaging instrument at Oak Ridge National Laboratory (ORNL). Such technique enables simultaneous access to three imaging modalities: attenuation, differential phase contrast, and small angle scattering. Therefore, cracks, voids, and porosity ranging from hundreds of nanometers to a few micrometers can be spatially resolved in bulk materials. This work will present existing and recently developed neutron imaging capabilities at ORNL.
4:15 PM
Machine learning-enabled tomographic imaging of chemical short-range atomic ordering: Yue Li1; Zhangwei Wang2; Baptiste Gault1; 1Max-Planck-Institut Fur Eisenforschung; 2Central South University
In solids, chemical short-range order (CSRO) refers to the self-organisation of atoms of certain species occupying specific crystal sites. CSRO is increasingly being envisaged as a lever to tailor the mechanical and functional properties of materials. Yet quantitative relationships between properties and the morphology, number density, and atomic configurations of CSRO domains remain elusive. Herein, we showcase how machine learning-enhanced atom probe tomography (APT) can mine the near-atomically resolved APT data and jointly exploit the technique’s high elemental sensitivity to provide a 3D quantitative analysis of CSRO in a CoCrNi medium-entropy alloy. We reveal multiple CSRO configurations, with their formation supported by state-of-the-art Monte-Carlo simulations. Quantitative analysis of these CSROs allows us to establish relationships between processing parameters and physical properties. The unambiguous characterization of CSRO will help refine strategies for designing advanced materials by manipulating atomic-scale architectures.
4:35 PM
Structure and Substructure Characterization of Ni50.3Ti29.7Hf20 High-temperature Shape Memory Alloy: Jiaqi Dong1; Umale Tejas1; Benjamin Young1; Dexin Zhao1; Ibrahim Karaman1; Kelvin Xie1; 1Texas A&M University
Twinning types and martensite interfaces play a significant role in the cyclic stability and fatigue life of shape memory alloys (SMAs). Therefore, we investigate the structure and substructure of the aged and solution-treated martensitic Ni50.3Ti29.7Hf20 high-temperature SMA in detail by transmission electron microscopy and precession electron diffraction (PED). Most martensite plates contain high-density internal (0 0 1) compound twins. Orientation relationships between martensite variants were studied using PED. In the solution-treated sample, (1 1 0.64) Type II twins and (1 1 1) Type I twins were observed, as well as the junction planes (i.e. (1 1 1) in variant A are parallel to (1 1 0.64) in variant B). (0 1 1) type I twin was observed in aged samples. Some of these orientation relationships are rarely observed in other NiTi or NiTiHf SMAs, which offers new insight to understand the phase transformation behavior in Ni50.3Ti29.7Hf20 SMAs.
4:55 PM
Nano-scale Spatially Resolved Analysis of Hydrogen in Stainless Steels: Dallin Barton1; Mark Wirth1; Dan Nguyen1; Mengkong Tong1; Tingkun Liu1; Zihua Zhu1; Daniel Perea1; Arun Devaraj1; 1Pacific Northwest National Laboratory
Increased hydrogen concentration in stainless steel causes a noticeable reduction in ductility known as hydrogen embrittlement. The relationship of the bulk mass composition of hydrogen in stainless steel to its mechanical behavior has been thoroughly researched. Spatially resolved characterization techniques with high sensitivity for hydrogen can elucidate hydrogen behavior at the nano-scale. This talk will discuss analysis of hydrogen in model austenitic FeCrNi alloys. A rigorous coupling of electrochemistry, including cyclic voltammetry, and nanoscale characterization, including atom probe tomography and nano secondary ion mass spectrometry, is used to understand hydrogen segregation to material properties such as phase, crystal orientation and structure, and features such as dislocations, twin boundaries, and high-angle grain boundaries. Hydrogen can quickly diffuse out of alloys at room temperatures. Therefore, cryogenic transfer and operation techniques have been developed to decrease unwanted H diffusion before proper characterization. Details concerning cryo-characterization and resulting hydrogen diffusion behavior will be given.
5:15 PM
Curing Behavior of Plasmonic Spiky Gold Nanoparticles Integrated in an Epoxy System: Cynthia Sangang1; 1Texas Tech University
Novel nanocomposites are in high demand in various industries. Namely automotive and aerospace sectors where they are commonly used as adhesives and coatings. They demonstrate unique physical and chemical properties, such as high strength-to-weight ratio, excellent chemical, and corrosion resistance. Noble metallic plasmonic nanoparticles have been integrated into epoxy systems in recent years owing to their outstanding optical properties. Spiky gold nanoparticles (SAuNPs) with localized surface plasmon resonance (LSPR) of up to 1320 nm were successfully synthesized and integrated into a thermoset resin system. Transmission electron microscopy (TEM) and UV-Vis-NIR confirmed the size, morphology, and absorbance peak of the SAuNPs. The curing behavior of the nanocomposite is herein reported. Non-isothermal differential scanning calorimetry (DSC) scans of SAuNPs-epoxy systems suggest that SAuNPs facilitated the exothermic reactions of epoxy resins.