Characterization of Minerals, Metals and Materials 2021: Advanced Characterization Methods III
Sponsored by: TMS Extraction and Processing Division, TMS: Materials Characterization Committee
Program Organizers: Jian Li, CanmetMATERIALS; Mingming Zhang, Baowu Ouyeel Co. Ltd; 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; Alex Moser, Naval Research Laboratory
Wednesday 2:00 PM
March 17, 2021
Room: RM 15
Location: TMS2021 Virtual
Session Chair: Jian Li, CanmetMATERIALS; Kim Jeongguk , Korea Railroad Research Institute
2:00 PM
Nanotwinned Ni-Mo-W Alloys with Ultrahigh Strength and Localized Plasticity: Gianna Valentino1; Jessica Krogstad2; Timothy Weihs1; Kevin Hemker1; 1Johns Hopkins University; 2University of Illinois Urbana-Champaign
The engineering of mechanical properties and performance of materials has traditionally relied heavily on the exploitation of the processing-structure-property relations, as a design tool to synthesize new materials. Nanostructured materials are no exception and have received considerable attention in recent years for thin film protective coatings, microelectromechanical systems (MEMS), and many other engineering applications aiming to achieve a balance of strength and ductility. Sputter deposited Ni-Mo-W films have been shown to possess ultrahigh strength, highly anisotropic plasticity, low electrical resistivity and low thermal expansion that stem from the finely spaced growth twins that form during the deposition process. Here we report on in-situ SEM micropillar compression and post-mortem microstructural analysis to elucidate the fundamental deformation mechanisms that underpin the extreme strength and plasticity in nanotwinned Ni-Mo-W. Emphasis will be placed on the loading orientation with respect to the twin planes, which will be key to understanding and utilizing these materials.
2:20 PM
FIB-SIMS in a Multi-Ion Source Plasma FIB: Daniel Murray1; Xiaofei Pu1; 1Idaho National Lab
FIB-SIMS is an emerging technique that has been gaining attention in recent years. This is due to its ability to analyze light elements, isotopic compositions, its ability to directly correlate SIMS datasets with results from other analytical techniques in FIB, and a significant cost reduction relative to standalone SIMS instruments. The major limitation of traditional FIB-SIMS, however, comes from the primary ion beam in the standard FIB instrument, which is normally Ga or Xe. Both primary ions give lower secondary ion yields relative to O2+ or Ce+, which are commonly used in standalone SIMS instruments. Here we show that by incorporating a TOF-SIMS detector onto a Thermo Helios Hydra PFIB, which has O2+ available as a primary beam, the sensitivity of the instrument is increased, and thus the utility expanded. We will present studies of secondary ion yields and characterization of various materials demonstrating enhanced utility of this one-of-a-kind instrument.
2:40 PM
In-situ Nanoscale Characterization of Phase Transformations in Materials Undergoing Ultra-fast Heating and Cooling: Azin Akbari1; James Ranney1; 1ThermoFisherScientific
Conventional in-situ characterization of materials at high temperatures in Scanning Electron Microscopes (SEM) has relied on resistive heating of bulk samples in oven-style crucibles. While these techniques can provide valuable insight in microstructural transformations of materials at elevated temperatures, they fail to capture the complex heating and cooling dynamics of real-world applications and more advanced manufacturing techniques such as Additive Manufacturing (AM). In this study, the Thermo Scientific µHeater was utilized to achieve ultra-fast heating and cooling rates on a variety of materials: Ti-6-4, Cu, Ag, Au, and Al alloys. Using the µHeater, a Micro-Electromechanical Systems (MEMs) device for in-situ experiments, enables acquisition of Energy Dispersive X-Ray Spectroscopy (EDS) and Electron Backscattered Diffraction (EBSD) while studying the microstructure inside the SEM. This more complete analytical characterization yields a better understanding of the material’s response under extreme conditions, further driving application-based material development.
3:00 PM
A Study of the Absorption Edge of ZnO Thin Films Prepared by the Spray Pyrolysis Method: Shadia Ikhmayies; 1
Zinc oxide (ZnO) thin films are produced by the spray pyrolysis method on glass substrates at 450 °C. The films are characterized using X-ray diffraction (XRD), and UV-VIS transmittance spectroscopy. XRD pattern showed that the films are polycrystalline with hexagonal (wurtzite) structure. Transmittance was measured at room temperature in the wavelength range 350-1100 nm, and used to deduce the absorbance. The fourth derivative of the absorbance is used to detect the peaks in the near band edge region. Several peaks are found in the region of interest, from which are the free exciton peaks A, B, and C, bound exciton peaks related to defects and impurities, and very weak peaks assigned to longitudinal optical phonon replicas. These results are important for solar cells, room temperature UV-laser, and other photonic and optoelectronic applications.
3:20 PM
Modeling Empirical Estimators for the 3D Particle Size, Distribution, and Expected Error from 2D Cross Sections of a Lognormal Distribution of Spherical Particles: Austin Gerlt1; Amanda Criner2; Lee Semiatin2; Katelun Wertz2; Eric Payton2; 1The Ohio State University; 2Air Force Research Lab
Accurately estimating the mean size of 3D features within an opaque material using only 2D observations is a common and often difficult requirement in material characterization. Employing numerical methods to obtain an accurate estimate of the full 3D size distribution, which is often important for calculating structure-dependent properties, is yet more challenging. In this talk, two alternative methodologies are presented which circumvent the error propagation issues seen in classical numerical approaches via direct the direct simulation and cross sectioning of populations of spheres with lognormal size distributions to directly forward model the 2D to 3D stereological transformation. These empirical equations of fit are used to develop a set of 5 equations for transforming 2D cross sectional measurements into estimates of the full 3D distribution. The accuracy of this transformation is, for the first time, characterized as a function of the population size and measurement resolution.
3:40 PM
Imaging Materials and their Evolution with High-Energy X-rays: Jonathan Almer1; Peter Kenesei1; Jun-Sang Park1; Meimei Li1; Paul Shade2; 1Argonne National Laboratory; 2Air Force Research Laboratory
High-energy x-rays from 3rd generation synchrotron sources, including the Advanced Photon Source (APS), possess a unique combination of high penetration power and spatial, reciprocal space, and temporal resolution. These characteristics, coupled with extensive worldwide efforts over the past decades, have produced a variety of 3D imaging techniques using both density and diffraction/scattering contrast. These techniques operate in air with large working distances between optics, samples and detectors. This has enabled development and use of a variety of in-situ environments, with an overarching goal to best simulate the (often extreme) service conditions of materials. I will describe several of these environments, including thermo-mechanical loading systems and additive manufacturing platforms, while highlighting some key scientific results – particularly in the area of structural materials. Future developments will also be discussed in the context of the upcoming APS upgrade to a diffraction-limited source.
4:00 PM
General Guideline of FIB Milling of Metal Alloys: Jian Li1; 1CanmetMATERIALS
This report summarizes the routines we have developed that enhances milling efficiency while avoiding un-wanted artifacts during Ga ion milling process. Focus include: control of ion beam for enhanced milling efficiency, factors to be aware of for artifacts reduction, consideration of specimen temperature increase, and potential introduction of un-wanted phase transformation during ion beam milling. Generalized guidelines for efficient and safe FIB milling of engineering materials are summarized in this paper
4:20 PM
Integrated, Table-top Instrumentation for High-temperature Thermal Property Measurements of Molten Salts: Haoxuan Yan1; Federico Coppo1; Uday Pal1; 1Boston University
There is a growing need to measure the thermophysical behaviors of molten salts at high temperatures as a variety of processes rely on these properties. Molten salts are used in a variety of high-temperature industrial applications, such as metal electrolysis, nuclear reactors, energy storage, etc. The measurement of their thermal properties, however, has long been a difficult task due to measurement difficulties at high temperatures and reactivity with the container materials. In this work, a novel, highly-integrated, table-top instrumentation is developed to measure the viscosity, surface tension, density, and vapor pressure of molten fluorides utilizing a micro-heater device. Incorporating falling sphere viscometry and maximum bubble pressure method, rapid, accurate measurements are made with only a few grams of a given sample. Measured values are compared with simulated results yielding low margins of error, demonstrating the validity of this novel instrumentation for investigation of unknown molten salt systems.