Characterization of Minerals, Metals and Materials: Advanced Microstructural Characterization Methods
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
Tuesday 8:00 AM
March 21, 2023
Room: Aqua 313
Location: Hilton
Session Chair: John Carpenter, Los Alamos National Laboratory; Jiann-Yang Hwang, Michigan Technological University
8:00 AM
Microstructural Effects on the Shock Hugoniot: David Jones1; Daniel Martinez1; Jesse Callanan1; Darby Luscher1; Saryu Fensin1; 1Los Alamos National Laboratory
It is well accepted that the Hugoniot – the locus of all shock states, a path through the equation-of-state – is strongly affected by “macro” properties such as density, chemistry, and phase fraction. However, microstructural properties that affect strength, such as texture and dislocation density, are often ignored. In this work we study a single pedigree of copper, investigating the effect of cold work (and therefore dislocation density and grain size) on the Hugoniot. Gas-gun plate impact experiments are used to measure the equation-of-state with sub-percent uncertainties, revealing a trend where both the Hugoniot elastic limit and shock velocity increase with cold work. The two Hugoniots for the cold-rolled and annealed copper samples intersect and collapse into one at stresses above the weak shock limit. Simulations are used to hypothesize what is driving this difference in the low-stress Hugoniot for copper.
8:20 AM
Quantitative Microstructural Characterization of Precipitates and their Distributions in Nickel Alloys: Chris Bilsland1; Thomas Britton2; 1Imperial College London; 2University of British Columbia
We present a new correlative framework to develop quantitative microstructural characterisation of precipitates in Ni-based alloys. For component manufacturing, precipitate distribution is controlled to optimise performance, such as optimising strength and stress corrosion cracking (SCC) resistance. In this work, we use simultaneous energy dispersive X-ray spectroscopy (EDS/EDX) and electron backscatter diffraction (EBSD), together with statistical testing, to explore the similarity and differences of precipitate distributions in Inconel 625. Our new approach draws together new image processing algorithms for particle classification (using EDS spectra), automated correlation with grain boundary character (from EBSD), statistical testing and verification of the area studied, as well as visualisations of the co-distribution of elements against different boundary types. These methods have been useful to understand measured differences in SCC performance for wrought and hot isostatic pressed (HIP'ed) components.
8:40 AM
Correlative Microscopy Characterization of Afterburner Thermal Barrier Coating: Bartlomiej Winiarski1; 1Thermo Fisher Scientific
Correlative microscopy (CM) workflows allow and aid solving a broad range of scientific and industrial problems (e.g. battery research, 3D printing, smart materials, integrated circuits, multi-physics simulation, etc.) previously unreachable by the typical experimental operando. CM workflows involve coordinated in 2D / 3D space and time (temporal 4D imaging) characterization of materials and components across a range of length scales. Various apparatus and imaging modalities contribute to the workflow, for example light, electron/ion microscopy, X-Ray computed tomography (CT), SIMS, EBSD, EDS, WDS, CL, XPS, Raman, STEM and TEM imaging and metrological techniques. As a practical example of CM for aviation and aerospace industries we study a thermal barrier coating (TBC) used in the afterburner JT11D-20 engine. The CM workflow used in this study correlates 3D data from micro X-Ray CT, Plasma FIB-SEM serial sectioning tomography and S/TEM study across the length scales.
9:00 AM
Electron Transport Properties in Metal Nanowhiskers: Gunther Richter1; Olga Iaroslavtseva1; 1Mpi For Intelligent Systems
One-dimensional nanostructures attracted in the past years a high interest due to their properties. They are thought to be the future building blocks for novel (nano-)technological devices. Especially semiconductor nanowires are under investigation for their unique properties. However, metals as one of the oldest were so far difficult to fabricate in sub-micrometer diameter dimensions. We report the successful growth of defect scarce nanowhiskers with aspect ratios up to 1000. The unique microstructure allow for probing the genuine physical properties in such structures. In this report we will focus on the electron transport properties of metal nanowhisker with diameters ~100 nm. The room temperature conductivity is at the same value as the bulk one, this is in stark contrast to common interconnects. We will discuss the influence of the microstructure and especially the surface on conductivity. The room temperature findings are supported by observations at 10K temperature.
9:20 AM
Evaluation And Construction of Microstructural Property Distributions For Advanced Material Characterization: Noah Wade1; Lori Graham-Brady1; 1Johns Hopkins University
As part of the ongoing development of material characterization many computational models are incorporating parameter distributions in place of average values, such as the mean grain size. Other structural and morphology measurements such as aspect ratio, shapes properties, and grain boundary lengths also being incorporated, however, many of these measurements don’t have accepted standards for the reporting and minimizing of associated measurement errors. In this work an uncertainty quantification tool for the evaluation of these measurements is proposed. Using a numerical simulation of the microstructural data collection process and a Bayesian framework, a prediction of the range true property measurements given a measure value is obtained. Results are presented for the construction of several different property distributions showing how the variability of measurements is different for various morphological measurements. These distributions are then used to show how material characterization can be optimized based on the desired morphological measurements being made.
9:40 AM Break
9:55 AM
Effect of Single Crystal Growth Techniques on Dendritic Microstructures and Small Orientation Defects in Ni-based Superalloys: Felicitas Werner1; Felicitas Scholz1; Paul Git2; Alexander Richter1; Pascal Thome1; Carolin Körner2; Gunther Eggeler1; Jan Frenzel1; 1Ruhr-University Bochum; 2Friedrich-Alexander-University Erlangen-Nürnberg
We investigate how different Bridgman single crystal solidification techniques affect dendritic microstructures and low angle misorientation defects. In general, Ni-based single crystal (SX) superalloys contain low angle grain boundaries between slightly misoriented dendrites. This type of defect is referred to as crystal mosaicity. We use two approaches to prepare SX material states. First, we use the seeding method where the formation of the SX is governed by epitaxial growth from a pre-oriented seed crystal. Second, we use the helix technique, where the solid/liquid interface has to pass a narrow spiral-shaped grain selector. The different material states were characterized by advanced microscopy techniques (e.g. tomography and cross-correlation EBSD) and Laue x-ray mappings. Our results suggest that the helix technique is associated with lateral solidification growth which results in line-shaped zones with slight misorientations. In contrast, these zones have a globular character for seeded crystal growth, where no significant lateral growth occurs.
10:15 AM
Optical Parameters of ZnO Thin Films: Shadia Ikhmayies1; 1Jabal El-Hussain
Zinc oxide is a very important material (ZnO) of diverse uses in solar cells, optoelectronic devices, and other applications. Optimizing the optical properties is required in such applications. In this work the influence of annealing in nitrogen atmosphere and aluminum doping on the optical properties was investigated. undoped (ZnO) and aluminum doped (ZnO:Al) thin films were deposited using spray pyrolysis (SP) method on glass substrates. The microstructure of the films was explored using X-ray diffraction and the films are polycrystalline. Transmittance of the films was recorded as a function of wavelength in the range 300-1100 nm. Transmittance was used to calculate absorption coefficient, extinction coefficient, reflectance, refractive index, real and imaginary parts of the dielectric constan, and optical conductivity. All these parameters are found to be affected by Al-doping and annealing.
10:35 AM
Correlative Microscopy Materials Characterization Using fs-laser Plasma FIB-SEM: Bartlomiej Winiarski1; Remco Geurts1; 1Thermo Fisher Scientific
Multi-scale correlative microscopy methods, which involve the coordinated characterization of materials across a range of length scales using various apparatus, allow solving a broad range of scientific problems previously unreachable by the typical experimental operando. The advent of FIB-SEM allowed for automated SST, 3D-EBSD/EDS of material volumes <40×40×40µm3. Plasma_FIB-SEM expanded these techniques to volume ~250×250×250µm3 keeping the voxels sizes in the dozens of nm-ranges. Recently, femtosecond Laser_PFIB-SEM pushed these 3D techniques further to mm-scale volumes, setting the standards for multi-modal data collection from nm to mm scales. Now, the Laser_PFIB-SEM platform is extended with multi-ions allowing for use of Xe, Ar, O and N focused beams. In this work we address current developments in 3D materials characterization with Laser_Hydra_PFIB-SEM and in the framework of correlative microscopy. We discuss the effects of ultra-short pulse laser ablation on the EBSD results and we present various practical examples and applications of the TriBeam.
10:55 AM
Optical Properties of Iridium at High Temperatures: Minsu Oh1; John McElearney1; Kevin Grossklaus1; Thomas Vandervelde1; 1Tufts University
With a melting point over 2400°C and oxidation resistance comparable to platinum, iridium (Ir) has many potential applications where thermal stability is desired. As material properties are generally a function of temperature, so it is not surprising that optical properties, such as refractive index, also vary with temperature. In fact, the temperature-dependent variation of material properties may cause the material’s performance to differ from what is expected or modeled based on its properties at room temperature. Thus, temperature-dependent material properties are needed to achieve more accurate modelling. In this work, we present optical properties of sputtered Ir at higher temperatures. An optically thick layer of Ir is sputter-deposited, using argon as a sputtering gas. The optical properties of as-deposited and annealed Ir samples are characterized by ellipsometry. The results of atomic force microscopy (AFM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) will also be provided.