Characterization of Minerals, Metals and Materials: Advanced Characterization Methods I
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, The University of Jordan

Monday 8:30 AM
March 20, 2023
Room: Aqua 313
Location: Hilton

Session Chair: Jian Li, CanmetMATERIALS; Yunus Kalay, Middle East Technical University


8:30 AM  
Non-local Means Denoising of EDS Spectra for Rapid Mapping of Composition in Nickel Aluminum Bronze: Patrick Callahan1; Dillon Watring1; David Rowenhorst1; 1US Naval Research Laboratory
    The goal of this work is to enhance composition determination in materials by energy dispersive X-ray spectroscopy (EDS) while reducing data collection time by using non-local means filtering. Non-local means filtering has been a successful image processing method for denoising images by replacing pixel intensities through a non-local smoothing kernel. This technique was recently advanced to operate on high-dimensional datasets for the denoising of electron backscatter diffraction patterns (EBSPs) within an EBSD scan, which are denoised by averaging an EBSP with patterns within a certain distance that are determined to be alike by a similarity metric. This work examines using similar high-dimensional non-local means denoising to hyperspectral EDS data from nickel aluminum bronze, comparing data collected at longer dwell times to data collected at shorter dwell times with non-local means filtering applied. This enables an enhancement in spectral data quality with reduced collection time without worsening the spatial resolution.

8:50 AM  
Analytical Polarized-light Microscopy: Specifications and Applications: Brian Hoover1; Cesar Ornelas-Rascon1; 1Advanced Optical Technologies, Inc.
    Polarized-light microscopy (PLM) has been used for nearly a century to visualize anisotropic materials, but has rarely been applied to quantitative analysis despite its obvious practical advantages compared to electron microscopy. Recent advancements in polarization metrology, optical components, and electrodynamic material models have led to new PLM modalities for quantitative analysis of metals and other materials. New PLM specifications are reviewed and example applications are highlighted, including super-wide-…eld quantitative imaging, martensite fraction, inclusion analysis, and orientation imaging of non-cubic metals, including AM Ti64, which is verified against EBSD.

9:10 AM  
Characterization of the Speed of Sound for Molten Metals at High Pressures: Elizabeth Rasmussen1; Mark McLinden1; 1National Institute of Standards and Technology
    Currently, a gap exists in thermodynamic material property data for metals in the liquid phase at elevated pressures. This gap stalls data-driven innovation in advanced manufacturing processes such as the additive manufacturing of metals, and extreme ultraviolet light (EUV) lithography in semiconductor fabrication. The thermodynamic property of speed of sound is advantageous as measurements with low uncertainties can be achieved across a range of temperature and pressure conditions in a rapid and automated manner. From sound speed, thermodynamic integration allows for density, isobaric heat capacity and isobaric expansivity values to be obtained. In this presentation, we will discuss a custom instrument that can measure the sound speed of molten metal at pressures from 0.1 to 50 MPa with an uncertainty of under 0.1%. Initial results will be presented as well as details on how the data will be used to aid in next-generation material simulations.

9:30 AM  
Critical Analysis of Intermetallic Phases in Cu-Sn Alloys by EBSD: Stefan Martin1; Andreas Leineweber1; 1Tu Bergakademie Freiberg
    Compounds of 3d transition metals and tin, form a series of intermetallic phases that are crystallographically very similar and/or differ only in the formation of an ordering of individual atomic species. The discrimination of these phases by EBSD can be very tricky. On the example of the Cu-Sn system, it will be shown which phases can be distinguished by their metrics and how pattern-matching can be used to identify the correct phases with the help of the superstructure bands and how domain states can be correctly identified.

9:50 AM  
Thermal Conductivity Measurements of Battery Components using the Flash Method: Heng Wang1; Peter Ralbovsky1; Guiquan Pan1; Marc-Antoine Thermitus1; 1Netzsch Instruments North America, LLC
    Thermal management is critical for battery performance and safety. The accurate measurement of thermal conductivity of internal components is essential for understanding and improving heat transfer inside batteries. In this paper, thermal diffusivity values of battery electrode and separator components are measured by using a light flash analyzer with the innovated adjustable flash pulse from 10 to 1500 µs, ZoomOptics, and analysis models. The influences of these features to insure reliable measurements are discussed. The thermal conductivity results are calculated from thermal diffusivity along with density and specific heat values as measured with a DSC.

10:10 AM Break

10:25 AM  
Characterization of Lunar and Martian Meteorites using Scanning Electronic Microscope (SEM): Hussain Al Halwachi1; 1Bahrain Society of Chemists
    Lunar and Martian meteorites are rare rocks found on earth and classified by meteoritical experts depending on their physical and chemical features. Three different types of certified lunar rock samples and one Martian rock sample were tested and scanned by Scanning electronic microscope (SEM) to obtain the chemical composition, explore the elemental mapping, and provide a statistical comparison between the different types. The SEM was able by EDX channel to provide accurate chemical compositions, in addition to microstructure images and elements mapping. The data provided by SEM were treated statistically by the principal component analysis (PCA) technique to obtain the relation between the elements and obtain a statistical model to help in differentiating similar rocks in the future.

10:45 AM  Cancelled
Characterization of Pearls using EDXF and Omnian Standard Less Application: Hussain Al Halwachi1; 1Aluminium Bahrain (Alba)
    Pearls are precocious gemstone that required to be certified using non destructive method in order to know whether it is natural or artificial. EDXRF with small spot camera was able to provide the accurate chemical composition of pearls using the modified Omnian standard less calibration. The calibration lines of the modified calibration was improved by adding extra Pearls standards in order to provide very accurate results

11:05 AM  
X-ray Tomography as a 3D Metrology Technique: Brian Patterson1; Bryan Hunter1; Steven Young1; Theresa Quintana1; Thomas Day1; Derek Schmidt1; Adam Wachtor1; 1Los Alamos National Laboratory
    The 3D imaging of materials using X-ray tomography is a powerful technique to understand the interior of materials and their defects. No other technique can be used to non-destructively examine voids, cracks, or inclusions, and is useful for a variety of material systems including polymers, metals, 3D printed, or machined parts. The acquisition of a 3D image of the material is a complicated multi-step process in which a variety of conditions can greatly affect the final image and can make quantification of any features complicated. Each of these steps often rely on decisions by the scientist which affect their accuracy and precision. Here, we will discuss a variety of material systems in which we attempt to quantify surface quality, thin shelled objects, and 3D printed foams dimensions. It is critical to understand the process, assure the numerical validity and that the associated error is as small as possible.

11:25 AM  
Online Electron Microscope for 3D Microstructure Data: Zachary Varley1; Allison Weller1; Gregory Rohrer1; Marc De Graef1; 1Carnegie Mellon University
    Microstructure analysis in the electron microscope is increasingly performed in 3D via serial sectioning due to the direct, relatively high-resolution, measurement of phase and orientation, especially grain size and shape statistics. Previous work proposed an unsupervised dynamic sampling routine to leverage the organized granular structure of orientation data present in 3D microstructure data. Herein, an online electron microscope is proposed. By bringing together EMSoft and Dream3D, expedited validation and development of sampling, indexing, and characterization is made possible. EMSoft brings forward models of electron diffraction while Dream3D handles the microstructure synthesis and analysis. This software is written in Python and packaged in a Docker container, allowing simple installation and operating system agnostic usage. The Docker container includes parallel Dream3D pipeline execution on the CPU with Python’s multiprocessing library as well as an OpenCL runtime for EMsoft.

11:45 AM  
Unveiling Effect of Alloying Elements on Recrystallization Behavior of Platinum Alloys: Gaeun Song1; So-Yeon Lee2; In-Suk Choi1; 1Seoul National University; 2Kumoh National Institute of Technology
     Platinum alloys are widely used in various industries. Nevertheless, there is a limited understanding of the alloying effect on structural properties. In this study, we investigated the effect of the alloying elements of Pt alloys on recrystallization behavior. We fabricated three different Pt alloys using Co, Cu, and W as alloying elements, and observed how the microstructure varied using EBSD. Interestingly, the Pt-W alloy showed retarded recrystallization compared to the Pt-Co and the Pt-Cu alloy. To investigate how W retards recrystallization behavior of Pt alloys, we calculated each Pt alloys’ dislocation density and recrystallization activation energy using XRD and observed the distribution of alloying elements using TEM. Also, we utilized DFT simulation to figure out the unique characteristic of W that affects the recrystallization behavior of Pt alloys.This research will help in-depth understanding of Pt-based alloys and become a good guideline to process Pt-based alloys suitable for the purpose.

12:05 PM  
The Power and Limitation of Ion Beam Imaging in Focused Ion Beam Microscopes: Pei Liu1; 1CanmetMATERIALS
    In the past three decades, the focused ion beam microscope has evolved from a semiconductor production tool into an advanced microstructure characterization instrument. The FIB microscopes have changed from the first generation of single ion beam systems to multi-beam systems that often couple with various types of analytical instruments. However, the powerful FIB system are often recognized as an advanced TEM specimen preparation machines due to its superior capability of making high-quality, site-specific thin foils from almost any types of materials and any geometry. This is a vast under usage of such powerful systems. Most users do not take advantage of the primary ion beam imaging capability that can provide high quality images to reveal important microstructure features. In this paper, the author uses practical examples to demonstrate the power of ion beam imaging.