Characterization of Minerals, Metals and Materials 2022: Advanced Characterization Methods I
Sponsored by: TMS Extraction and Processing Division, TMS: Materials Characterization Committee
Program Organizers: Mingming Zhang, Baowu Ouyeel Co. Ltd; Jian Li, CanmetMATERIALS; Bowen Li, Michigan Technological University; Sergio Monteiro, Instituto Militar de Engenharia; Shadia Ikhmayies, The University of Jordan; Yunus Kalay, Middle East Technical University; Jiann-Yang Hwang, Michigan Technological University; Juan Escobedo-Diaz, University of New South Wales; John Carpenter, Los Alamos National Laboratory; Andrew Brown, Devcom Arl Army Research Office; Rajiv Soman, Eurofins EAG Materials Science LLC; Zhiwei Peng, Central South University

Monday 8:30 AM
February 28, 2022
Room: 207B
Location: Anaheim Convention Center

Session Chair: Rajiv Soman, AnalytiChem Group, USA; Bowen Li, Michigan Technological University


8:30 AM Introductory Comments

8:35 AM  
A Review of Atom Probe Tomography Technology: The Present and Future: Robert Ulfig1; David Larson1; David Reinhard1; Peter Clifton1; 1Cameca Instruments Inc.
    Over the past decade, the improvements in the capability of 3D nanoscale characterization using atom probe tomography (APT) have been remarkable. The advances have enabled the analysis of material systems and structures far beyond the early limitations of APT to bulk metals. In addition, the maturation of FIB-based specimen preparation methods and the use of in-situ t-EBSD/STEM has made site-specific analyses truly routine. This presentation will provide an overview of the state-of-the-art hardware, software, and applications with a perspective on the performance needs of various selected applications that have moved APT from pure research to development and manufacturing support.

8:55 AM  
Characterization of Platinum Nanoparticles on a Non-conductive Perovskite Catalyst through Tailored Imaging Conditions in Scanning Electron Microscopy: Andy Holwell1; Maadhav Kothari1; John Irvine2; Yukwon John3; Andrea Pascuii4; 1Carl Zeiss Microscopy Llc; 2University of St Andrews; 3Yonsei University; 4Johnson Matthey
    Platinum (Pt), generally dispersed on a solid oxide support, has been widely used for catalytic chemical reactions in automobile, petroleum and energy industries. During the reactions, Pt is exposed to severe conditions, for example, heat and impurities, that cause Pt agglomeration and poisoning, respectively, resulting in activity/stability losses. Here, perovskite materials are designed with Pt for significant catalytic properties through novel doping and exsolution methods. In order to accurately determine the catalytic ability of Pt nanoparticles it is important to understand the structure and morphology of nano particles, typical scanning electron microscopy methods do not reveal the morphological characteristics of nanoparticles due to the lack of electron beam stability. Here we demonstrate imaging techniques employed to accurately determine activity, morphology as well as confirming metal dispersion using energy dispersive x-ray spectroscopy (EDX). This method can improve the catalytic analysis of Pt loading, size, dispersion, and active sites determination.

9:15 AM  
The Needle in the Haystack: The Role of New Advances in Correlative Light, Electron, Ion Beam and X-ray Microscopy in Finding, Imaging and Understanding Ever Fewer and Smaller Inclusions and Features in Steel: Andy Holwell1; 1Carl Zeiss Microscopy Llc
     Relentless process improvements in the steel industry have rendered non-metallic inclusions, once common and conspicuous impurities, now the needle in the haystack. The role of smaller and fewer inclusions in ever cleaner steel remains acute in increasingly demanding applications, but characterizing them is increasingly challenging. Locating, imaging, analyzing and understanding nanoinclusions requires a connected approach whereby multimodal submicron and nanometer-scale data is combined, from light, electron, x-ray and ion beam microscopy. We will present advances in sub-nanometer inclusion and feature analysis, femtosecond laser ablation to access deeply-buried features, and how integrated in situ heating, tensile and spectroscopic and crystallographic experiments reveal previously inaccessible structural and elemental detail on inclusions. We also describe a previously unknown effect whereby certain inclusions are only visible at specific beam conditions.

9:35 AM  
Characterization of Explosive Crystals with X-ray Micro and Nano-scale Tomography: Brian Patterson1; Lindsey Kuettner1; Steven Young1; Larry Hill1; Alexandra Burch1; John Yeager1; 1Los Alamos National Laboratory
    Explosives are a very exciting system to study in materials science. Not only for their chemical performance, but also the many challenges for scientists in understanding their morphology (voids and cracks), as well as their interfacial and mechanical performance. Explosive crystals have multiple length scales (10’s of nm scale through centimeter scale) that must be characterized and understood to predict their sensitivity, mechanical properties and performance. X-ray computed tomography on both the micro and nano-scale is being used to understand the salient features on these size scales. We will show nano-scale CT images of various lots of explosive powder and how the wormholes contained may affect the detonation performance, mechanical testing results of bicrystal experiments to understand interfaces between explosive crystals and the polymer binder, and show how dual-energy micro-CT imaging is used to segment plastic-bonded explosive composite materials to measure crystal distribution.

9:55 AM Break

10:15 AM  
Simulating Electron Microscopy to Elucidate Connections between Structural Measurements and Properties of Glassy Materials: Nicholas Julian1; Robert Rudd2; Jaime Marian1; 1University of California Los Angeles; 2Lawrence Livermore National Laboratory
    The inherently disordered atomic configurations of glassy materials impede definitive determination of structure-property relationships. While experimental measurements of atomic configurations and medium range order in glassy materials have been established, e.g. fluctuation electron microscopy or atomic electron tomography, the number of measured atomic configurations remains low. In this work we use established computational construction methods, molecular dynamics, and electron microscopy simulations to enhance the number and variety of configurations sampled and more definitively resolve connections between atomic structures, measurements, and properties of glassy materials.