Late News Poster Session: Characterization
Program Organizers: TMS Administration
Tuesday 5:30 PM
March 1, 2022
Room: Exhibit Hall C
Location: Anaheim Convention Center
L-51: An Innovative Mass Spectrometer Simplifies Elemental Characterization of Metals: Ellen Williams1; Jonathan Putman1; Jeffrey Williams1; 1Exum Instruments
This presentation describes an innovative mass spectrometer and its application for high-sensitivity, high-throughput elemental characterization of metals. Addressing many limitations of other techniques, Laser Ablation Laser Ionization Time of Flight Mass Spectrometer (LALI-TOF-MS) combines a dual-laser ionization source with a TOF mass analyzer into a compact, desktop package. The first laser ablates, or liberates, material from the sample’s surface, and then the second laser ionizes that liberated material. Directly analyzing solids eliminates the complicated sample preparation procedures required by other mass spectrometry techniques. After ionization, the particles move through the ion optics to the TOF mass analyzer, which measures the time required for ions of different masses to impact a detector. This results in a full mass spectrum, facilitating multielement quantification. Not only are its detection limits comparable with those of traditional mass spectrometry, LALI-TOF-MS also measures low-mass elements (e.g., carbon, oxygen, etc.) that other techniques fail to detect.
L-52: Application of HRTEM and LTEM for Investigations of Microstructure and Magnetic Domain Structure of Nanocrystalline Fe Based Soft Magnetic Materials after Ultra-rapid Annealing Process: Wojciech Maziarz1; Anna Wójcik1; Robert Chulist1; Maciej Szlezynger1; Maciej Kowalczyk2; Aleksandra Kolano-Burian3; Paweł Czaja1; 1Institute of Metallurgy and Materials Science, Polish Academy of Sciences; 2The Faculty of Materials Science and Engineering, Warsaw University of Technology; 3Lukasiewicz Research Network—Institute of Non-Ferrous Metals
The work presents application of high resolution transmission electron microscopy (HRTEM) and Lorentz microscopy (LTEM) in the study of crystal structure, microstructure, and magnetic domain structure of nanocrystalline Fe based soft magnetic materials. The Fe78Ni8B14 amorphous melt spun ribbons were subjected to ultra-rapid annealing (URA) process at 500 °C for time duration ranging from 0.5 to 14s. The crystallization of nanocrystalline alfa-Fe solid solution and microstructure evolution with grain sizes from 15 to 35 nm, depending on URA time processing, were observed. The longest URA time (14s) caused the largest grain growth and precipitation of Fe3B phase; the latter being unfavourable for soft magnetic properties. LTEM analysis, including in-situ dynamic observations under an applied magnetic field, allowed for visualization of the magnetic domain and domain walls movement that determine the magnitude of the magnetocrystalline anisotropy. National Centre for Research and Development (NCBiR) of Poland is acknowledged for funding (TECHMATSTRATEG 2/410941/4/NCBR/2019).
L-53: Computer Vision for Microvia Characterization: Nikhil Damani1; Pragna Bhaskar1; Mohan Kathaperumal1; Madhavan Swaminathan1; 13D Systems Packaging Research Center Georgia Institute of Technology
Microvia technology is essential to building high density interconnects for higher functionality/area and better performance for advanced computing and artificial intelligence applications. These vias are fabricated on the dielectric material by laser drilling. The laser drilling process is affected by material properties and the laser parameters. Fabrication of microvias involves optimizing these laser drilling parameters and follow-up processes to obtain clean, through-hole vias for each dielectric material. To ensure repeatability, multiple vias are drilled and the dimensions of all these need to be measured. Previous studies have used a combination of scanning electron microscopy and laser confocal microscopy techniques to image and measure these microvias. However, these are time consuming, destructive, and can be used only for characterizing a small number of vias. The present study uses a computer-vision (CV) based method to characterize the large number of vias drilled during the optimization of drilling process.
L-54: Correlative Microscopy and Applied Statistics – Development of a Simultaneous Electron Diffraction and Energy Dispersive X-ray Spectroscopy Data Analysis Method to Understand Interface Populations: Christopher Bilsland1; Andrew Barrow2; Ben Britton3; 1Imperial College London; 2Rolls-Royce; 3Imperial College London/ University of British Columbia
Engineering materials often consist of multiple phases that link together to form the underlying microstructure. The phases can have different structures and chemistries, and these are often connected. Manufacturing metallic materials determines the hierarchy of these structures, ranging across the mm to nm length scales, which ultimately determine components properties and lifetime. In this work, we apply simultaneous EBSD (electron backscatter diffraction) and EDS (energy dispersive x-ray spectroscopy) in a SEM (scanning electron microscope) which collects significant amounts of microstructural information. We use correlative processing of this data to yield quantitative results, that can be analysed using common statistical treatments (e.g. ANOVA) to understand systematic variation of the distribution of chemistry and structure within the hierarchical microstructure of wrought and HIP-ed powder metallurgy based nickel alloys. We have applied this method to understand the impact that sample size has on the inspected chemistry of precipitation in these material systems.
L-55: Digital Image Processing for the Analysis of Spray Coated Porous Films: Noah McAllister1; Robert Green-Warren1; Jae-Hwang Lee2; Assimina Pelegri1; Jonathan Singer1; 1Rutgers School of Engineering; 2University of Massachusetts Amherst
Self-limiting electrospray deposition (SLED) has been shown to be a means of creating thin, porous polymeric films conformally on complex surfaces. Thickness measurements are needed to quantify the porosity of these films. However, current optical film measurement techniques are only applicable for dense films; or, the technique is destructive in nature. Here, we present a means of non-destructively measuring the thickness of porous polymeric thin films deposited through SLED. This technique compensates for the scattering associated with porous films by using image processing on reflection and transmission optical micrographs. A Savitzky-Golay-based differentiator is used to find the inflection points of the image which represent the interface and boundary of the film, as shown in reflection and transmission, respectively. A comparative study between cross-sectional SEM (where scattering effects are diminished) and optical microscopy verifies that our optical microscopy technique can be used to consistently, non-destructively measure film thickness.
L-56: High Resolution STEM and LM STEM DPC Studies of Ni-Mn-Ga Based Precursor Powders and 3D Printed Magnetic Shape Memory Alloys: Pawel Czaja1; Anna Wójcik1; Robert Chulist1; Maciej Kowalczyk2; Wojciech Maziarz1; 1Institute of Metallurgy and Materials Science PAS; 2The Faculty of Materials Science and Engineering Warsaw University of Technology
The Ni-Mn-Ga based magnetic shape memory alloys have been longed researched with reference to the magnetic field induced strain (MFIS) offering high frequency actuation response and strain output of up to 12% in single crystalline alloy, depending on martensite crystal structure. The structure itself is sensitive to composition and fabrication routes. Special consideration should be given to alloys produced by additive manufacturing in respcet of various powder feed sources, compositional homogeneity and resulting microstructure of 3D printed parts. In this contribution advanced high resolution scanning transmission electron microscopy (HR-STEM) and low magnification STEM (LM STEM) combined with differential phase contrast analysis (DPC) are applied to pin point minute local compositional changes, structure identity and magnetic domain arrangements in precursor powders and in as selected laser melted Ni-Mn-Ga based magnetic shape memory alloys. Acknowledgement: National Centre for Research and Development (NCBiR) of Poland is acknowledged for funding (TECHMATSTRATEG 2/410941/4/NCBR/ 2019).
L-57: Enhancement of Electrical, Thermal and Mechanical Properties of Epoxy-carbon Nanotube/Egg Shell Ash Particles Nanocomposites: Suleiman Hassan1; Sunday Aigbodion2; 1Nigerian Institute of Mining and Geosciences; 2University of Nigeria, Nsukka, Nigeria
Carbon nanotubes (CNT) are promising material due to its outstanding properties, however the electrical percolation threshold of epoxy/carbon CNT nanocomposites is one of lowest among the conductive nanocomposites. Research was conducted to improve the electrical percolation threshold of epoxy/CNT with calcium carbonate. This work used eggshell ash particles (ESAp) to replace CaC for enhanced electrical properties. The nanocomposites were produced by varying CNT from 0.5 - 1.5wt% with 0.5wt% ESAp constant. The morphology, X-ray diffractometer, electrical, thermal properties and tensile strength of the developed epoxy-CNT/ESAp nanocomposites were determined. The results show increment in the tensile strength, electrical conductivity of the epoxy/CNT with the addition of ESAp, increases the glass transition temperature of the composites and enhancement of the thermal properties. The work established that the addition of ESAp to epoxy-CNT can be used to improved electrical percolation threshold of the composites.Keywords: Carbon nanotube, Eggshell, Epoxy, Electrical, Mechanical, Thermal properties
L-58: Experimental and Computational Investigations of TiIrB: A New Ternary Boride with Ti1+xRh2−x+yIr3−yB3-type Structure: Kate Gibson1; Jan Scheifers1; Boniface Fokwa1; 1University of California, Riverside
A new ternary phase, TiIrB, was synthesized by arc-melting of the elements and characterized by powder X-ray diffraction. The compound crystallizes in the orthorhombic Ti1+xRh2−x+yIr3−yB3 structure type, space group Pbam (no. 55) with the lattice parameters a = 8.655(2), b = 15.020(2), and c = 3.2271(4) Å. Density Functional Theory (DFT) calculations were carried out to understand the electronic structure, including a Bader charge analysis. The charge distribution of TiIrB in the Ti1+xRh2−x+yIr3−yB3-type phase has been evaluated for the first time, and the results indicate that more electron density is transferred to the boron atoms in the zigzag B4 units than to isolated boron atoms.
Cancelled
L-59: Seeing More with Machine Learning and Electron Backscatter Diffraction (EBSD): Tom McAuliffe1; David Dye1; Thomas Britton2; 1Imperial College London; 2University of British Columbia
In this presentation, we will show how we can use principal component analysis (PCA), non-negative matrix factorisation, and an autoencoder to cluster and classify gamma and gamma-prime phases in a Ni-based superalloy. This enables us to non-locally average conventionally captured diffraction patterns and amplify signal to noise. Analysis of these patterns using spherical projection and a spherical band profile analysis enables us to see differences in the diffraction patterns between the two phases. We compare these differences to high quality simulations, based upon dynamical scattering theory, and find reasonable agreement. Finally, we use these band profiles to perform spherical-angular dark field imaging where we image based upon the scattering intensity of a particular lattice plane. We focus this work to explore how we can develop EBSD techniques further to provide insight into the spatial distribution of phases in high temperature Ni-based superalloys used in jet-engine applications.
L-60: Study of the Martensitic Transformation by Deformation of Traction in the Steels AISI 304 through Electrical Resistivity: Edgar Apaza Huallpa1; Helio Goldenstein2; Esequiel Nicolas Collado Cardenas1; Elmer Antonio Mamani Calcina1; Juan Carlos Negron Lopez1; Lino Reynaldo Quispe Cardenas1; Alejandro Boris Marquez Guevara1; Erick Omar Tunqui Labra1; 1Universidad Nacional de San Agustin de Arequipa, Perú; 2Universidade de São Paulo
Studies related to martensitic transformation have been increasing in recent years, for this case, tensile deformation (uniaxial tension) was experienced using AISI 304 stainless steel as a study material, the specimens were machined under the ASTM E8 / E8M standard. This phase change was measured by the four-point resistivity test consisting of the passage of electrical current through the alloyed metal and the voltage supplied by a source, this was analyzed by the voltage changes using a voltmeter. To corroborate this phase change, its microstructure was observed by metallographic analysis in specimens, without deformation and with tensile deformation, where you can see the presence of martensite after the test, so that a characterization method could be established to identify the martensite formed during the mechanical test.
L-61: Thermogravimetric and FTIR Analysis of Amazonian Oils: Luana Demosthenes Demosthenes1; Waldeir Silva Dias2; Foluke Salgado de Assis3; Kleynice kazumy de lima Yamaguchi4; Sergio Neves Monteiro1; Wendell Bruno de Almeida Bezerra1; Benjamin Lazarus5; 1Military Institute of Engineering (IME); 2Universidade do Estado do Amazonas; 3Instituto de Pesquisas da Marinha; 4Universidade Federal do Amazonas; 5UCSD
The Brazilian Amazon forest has a very rich diversity of plants and fruits. And from these plants and fruits, natural oils are produced. These natural oils are sold in local markets in northern Brazil for various purposes. The most commercialized natural oils are copaiba (Copaifera l.), andiroba (Carapa g.), buriti (Mauritia f.) and tucumã (Astrocaryum v.). This research aimed to analyze the thermal degradation by TGA and perform the FTIR analysis of these natural oils. It was possible to verify, in a comparative way, which of the four oils showed the greatest mass loss. The oil that had the highest degradation temperature was also observed. In addition, this work also presents the Tonsets of each oil. According to the FTIR analysis of the oils, the presence of functional groups in organic samples was noted, such as hydroxyls, carboxyls and epoxies. The data obtained corroborate the data found in the literature.
L-62: X-ray Tomography In-situ Mechanical Testing: Alex Arzoumanidis1; 1Psylotech
Mechanical testing inside industrial microCT scanners provides exciting insight into microstructure and damage accumulation in composites, metals and additively manufactured metamaterials. Digital Volume Correlation can reveal small-scale mechanism that collectively produce a material’s continuum level response. Support posts in typical load frames obstruct X-rays during sample rotation. A test system that rotates the load train within the frame is presented. The rotating load train maximizes spatial resolution by enabling source placement close to the sample. The frame constrains out-of-plane motion and wobble though precision machining and design symmetry. A sub-micron alignment correction algorithm is also presented.
L-63: XRD and SEM Characterization of Amazon Biomass Residues: Euterpe Oleracea, Theobroma Grandiflorum and Astrocaryum Vulgare Mart: Luana Demosthenes Demosthenes1; Waldeir Silva Dias2; Foluke Salgado de Assis3; Kleynice kazumy de lima Yamaguchi4; Sergio Monteiro1; Wendell Bruno de Almeida Bezerra1; 1Military Institute of Engineering (IME); 2Universidade do Estado do Amazonas; 3Instituto de Pesquisas da Marinha; 4Universidade Federal do Amazonas
The Brazilian Amazon region is well known for its fruit diversity. Some of these fruits are traded all over the world, for example açaí (Euterpe o.). Other fruits that are well known worldwide are cupuaçu (Theobroma g.) and Tucumã (Astrocaryum v.) which present appreciable flavors in the food industry. However, after consuming the fruit pulp, tons of waste are generated because these fruits have fractions of 40 to 80% of peel and seeds. In view of this problem, this research aims to characterize these residues by XRD and to verify the morphology by SEM. The results obtained for the XRD diffractograms showed an amorphous halo at approximately 10° for each of the organic samples. The morphologies of the samples were observed by SEM and with the measuring tool coupled to the equipment, PS of the samples were measured.