Characterization of Minerals, Metals and Materials 2022: On-Demand Oral Presentations
Sponsored by: TMS Extraction and Processing Division, TMS: Materials Characterization Committee
Program Organizers: Mingming Zhang; Jian Li, CanmetMATERIALS; Bowen Li, Michigan Technological University; Sergio Monteiro, Instituto Militar de Engenharia; Shadia Ikhmayies; 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 U.S. Army Research Laboratory; Rajiv Soman, Eurofins EAG Materials Science LLC; Zhiwei Peng, Central South University

Monday 8:00 AM
March 14, 2022
Room: Characterization
Location: On-Demand Room

Session Chair: Mingming Zhang

Direct Correlation of Frank Loop Nature and Morphology in Self-ion Irradiated Nickel: Kan Ma1; Brigitte Décamps2; Anna Fraczkiewicz3; Frédéric Prima4; Marie Loyer-Prost1; 1DEN-Service de Recherches de Métallurgie Physique, CEA; 2IJCLab, Université Paris-Saclay; 3MINES Saint-Etienne, Université de Lyon; 4PSL Research University-Chimie ParisTech
    Face-Cubic Centered (FCC) materials such as novel austenitic materials present great potential for applications in Gen IV nuclear reactors. To better understand fundamental mechanisms of radiation damage in FCC structure, high-purity nickel and its alloys are irradiated using self-ions at 450/510°C as FCC model materials. Fine analysis of dislocation loops is performed in specimens prepared by by Focus Ion Beam followed by flash electropolishing using Transmission Electron Microscopy. For the first time to our knowledge, (i) vacancy loops are detected in irradiated nickel by the inside-outside method and stereo-microscopy and (ii) a drastic correlation between the Frank loop nature (vacancy-type v.s. interstitial-type) and their morphology (segmented v.s. circular) is identified. This correlation provides a new and simple TEM characterization method for the nature determination of Frank loops in nickel system.

Machine Learning Enabled Atom Tomographic Imaging of Chemical Short-range Order in Fe-18Al : Yue Li1; Zhangwei Wang2; Leigh T. Stephenson1; Baptiste Gault1; 1Max-Planck-Institut Fur Eisenforschung; 2Central South University
    Chemical short-range order (CSRO) refers to atoms of specific elements self-organising within a disordered crystalline matrix. These particular atomic neighbourhoods can modify the mechanical and functional performances of materials. CSRO is typically characterized indirectly, using volume-averaged (e.g. X-ray/neutron scattering) or through projection (i.e. two-dimensional) microscopy techniques that fail to capture the complex, three-dimensional atomistic architectures. Quantitative assessment of CSRO and concrete structure-property relationships remain unachievable. Here, we present a machine-learning enhanced approach to break the inherent resolution limits of atom probe tomography to reveal three-dimensional analytical imaging of the size and morphology of multiple CSRO. We showcase our approach by addressing a long-standing question encountered in a body-centred-cubic Fe-18Al (at.%) solid solution alloy that sees anomalous property changes upon heat treatment. After validating our method against artificial data for ground truth, we unearth non-statistical B2-CSRO (FeAl) instead of the generally-expected D03-CSRO (Fe3Al). We propose quantitative correlations among annealing temperature, CSRO, and the nano-hardness and electrical resistivity, supported by atomistic simulations. The proposed strategy can be generally employed to investigate short/medium/long-range ordering phenomena in a vast array of materials and help design future high-performance materials.

Leaching Cobalt from a Nickel-containing Copper-cobalt Zebesha Ore: Yotamu Hara1; Foibe Uahengo1; Rainford Hara1; Nachikonde Fumpa1; Alexander Old1; Golden Kaluba1; 1Copperbelt Univ
    Two copper – cobalt ore samples from Zebesha Mine in Zambia with varying amounts of nickel (0.02 – 0.45 weight %), manganese and iron were leached under different conditions with a purpose of understanding leaching characteristics. Leach test were conducted at different conditions such as pH, temperature and, in the presence and absence of reductant (SMBS). Acid consumption was decreasing with increase in leaching pH. Leach recoveries of Cu, Co, Ni, Mn and Fe were determined and the results were compared with thermodynamic predictions. Recoveries of Co, Ni and Mn were poor in the absence of SMBS. There was a good agreement between the experimental results and thermodynamic predictions. Recoveries of Cu and Ni were more sensitive to leaching pH. The feed samples were characterised using scanning electron microscopy and x-ray diffraction techniques.

Exploring Three Dimensional Orientation and Residual Stresses in Railway Steels: Can Yildirim1; Yubin Zhang2; Erika Steyn3; Fang Liu3; Carsten Detlefs1; Casey Jessop3; Johan Alstrom3; 1European Synchrotron Radiation Facility; 2Technical University of Denmark; 3Chalmers University of Technology
    Railway wheel steels, typically comprising a fine lamellar pearlitic microstructure, undergo a combination of thermal and mechanical loads in service that may lead to material failure due to increased residual stress levels. Here, we use an advanced synchrotron technique, dark field X-ray microscopy, to map 3D lattice variations including both the crystallographic orientation and lattice strain, within individual pro-eutectoid ferrite grains. In addition to an as-manufactured sample, we studied samples that underwent low cycle fatigue tests followed by isothermal heat treatments at 300– 600°C. The as-manufactured sample shows an orientation variation up to 0.5° and compressive elastic strain up to 1.8 × 10−3, but no direct correlation between the measured compressive strain and lattice orientation. The LCF tested samples exhibit an increase in orientation spread up to 3-4°, while the grain-level residual stresses show a non-monotonous trend as a function of annealing temperature.

Microstructural Characterisation of AA5083 in AA5083/SiC Co-continuous Ceramic Composites (C4) Fabricated by Gravity and Gas Pressure Infiltration: Georgia Warren1; Jianshen Wang1; AS Prasanth2; Krishna Shankar1; V Krishnaraj3; R Ramesh4; Juan Escobedo-Diaz1; 1School of Engineering and Information Technology, University of New South Wales, Canberra, Australia; 2Department of Mechanical Engineering, PSG College of Technology, Coimbatore, India; 3Department of Production Engineering, PSG College of Technology, Coimbatore, India; 4Department of Mechanical Engineering, PSG Institute of Technology and Applied Research, Coimbatore, India
    AA5083/SiC co-continuous ceramic composites (C4) were fabricated using gas pressure and gravity infiltration. SiC foams had 10 pores per inch (PPI) and 20 PPI. The aluminum metal matrix in C4 composites were characterized using optical microscopy and a microhardness measurements. Results show that the properties of the aluminium matrix in the composites were affected by the infiltration pressure during manufacturing and the pore size of SiC foams. The Al phase in specimens fabricated by gas pressure infiltration exhibited a smaller average grain size, a higher average hardness, and lower average porosity level compared to that fabricated by gravity infiltration. Also the specimens manufactured with 10 PPI foams displayed a larger average grain size, a higher average hardness and higher porosity level compared to the composites with 20 PPI foams. The hardness in the Al matrix was observed to increase with decreasing distance from the SiC struts.

Temperature Monitoring of Bearings in Railway Vehicles Using Infrared Thermography Technology: Jeongguk Kim1; 1Korea Railroad Research Institute
    Axle bearing failure in railway vehicles is a factor that prevents the safe operation of rail vehicles. One indication of axle bearing failure is the build-up of heat generated by the bearing. In order to monitor the bearing temperature, conventionally, a temperature sensor has been built into the axlebox to manage the bearing temperature. In this study, a temperature monitoring system based on infrared thermography technology was developed to monitor the temperature of axlebox bearings in railway vehicles. It was attempted to secure the driving safety of railway vehicles through monitoring the temperature outside the axlebox by using a small infrared thermal imaging camera. In this paper, the development of an axlebox bearing temperature monitoring system based on infrared thermography technology will be introduced. Moreover, the results of performance evaluation and temperature monitoring using an actual bearing tester will be presented.

Interaction between Iron Ore and Magnesium Additives during Pellet Roasting Process: Lianda Zhao1; Jingsong Wang1; Qingguo Xue1; Hong Su1; 1State Key Laboratory of Advanced Metallurgy,University of Science and Technology Beijing
     To study the interaction between iron ore and magnesium additives, several types of interaction couples were prepared and SEM-EDS was used to measure the diffusion distance of Mg2+. Results showed that prolonging the roasting time was beneficial to the diffusion of Mg2+ in the iron ore. When the basicity (CaO/SiO2) of iron ore increased from 0.2 to 1.0, the diffusion distance of Mg2+ increased from 15μm to 35μm. Among three magnesium additives, the diffusion distance of Mg2+ in dolomite was the longest, while that in serpentine was the shortest. Serpentine contains a large amount of SiO2, which can not participate in the chemical reaction. The presence of SiO2 hindered the contact between MgO and Fe2O3, thus reducing the diffusion distance of Mg2+. The roasting experiment of high magnesium pellets was further carried out to study the influence of basicity on the compressive strength of pellets. Result shows that the compressive strength of pellets decreased from 2701N to 2556N when 2% dolomite was added. The basicity of high magnesium pellets was adjusted by adding CaO into the pellets. The compressive strength of pellets with basicity of 1.2 was 2629N. The compressive strength of pellets with basicity of 1.5 was 2654N. Adding CaO to high magnesium pellets can improve the compressive strength.

Development of Surface Tension and Heat Capacity Measurement Techniques for Molten Materials Using Aerodynamic Levitation: Yifan Sun1; Hiroaki Muta1; Yuji Ohishi1; 1Osaka University
    For aerodynamic levitation, the interaction between the levitation gas and the sample has always been a problem for measuring thermophysical properties. This study will introduce two novel measurement techniques: the ‘drop-bounce’ method for surface tension evaluations and the ‘multiple-gas cooling’ method for heat capacity analysis. The ‘drop-bounce’ method incorporates the idea of free-fall into aerodynamic levitation and allows the sample to oscillate without the influence of the levitation gas. Under such conditions, the sample oscillates as if under microgravity condition, and its ‘true’ surface tension can be obtained. The ‘multiple-gas cooling’ method utilizes two types of inert cooling gas to obtain two cooling curves for the same sample. By solving the radiative and convective heat loss terms together, we can obtain the heat capacity of the liquid sample without prior knowledge of its emissivity. The methods developed in this study are significant for research in aerodynamic levitation and high-temperature melts.

Coking Coal Macromolecular Structural Characteristic and Its Correlations with the Compressive Strength of CaO-containing Carbon Pellets: Xiaomin You1; Xuefeng She1; Jingsong Wang1; Qingguo Xue1; 1State Key Laboratory of Advanced Metallurgy, University of Science and Technology Beijing
    CaO-containing carbon pellets (CCCP) preparing from well-mixed coking coal (CC) and calcium oxide (CaO) were roasted at different pyrolysis temperatures(400–800°C). To investigate the effect of roasted temperature on the compressive strength of CCCP, Raman spectroscopy and X-ray diffraction were adopted to characterized macromolecular structure changes of CC in CCCP. The results showed that the compressive strength of CCCP increased with the increase of temperature. The compressive strength of CCCP was negatively correlated with the peak intensity ratio (ID1/IG ) value and positively correlated with the peak intensity ratio ( IG/IAll ) value. A linear relationship between the compressive strength of CCCP and the carbon layer spacing of CC was established. As temperature increased, the structural defects and imperfections of carbon crystallites were gradually decreased. The aromatic carbon layers were more closely packed, which formed high-order CC. As a result, the compressive strength of CCCP increased.

SAXS Tomography of Multilayered Al-Zn-Mg Alloy Sheets: Shan Lin1; Hiroshi Okuda1; 1Kyoto University
     Multilayered structure has been used from a viewpoint of designing composite materials, to manufacture strong materials in the industry. In the present work, we used the method developed in the last report to examine nanostructure distribution in a layered structure containing macroscopic compositional modulation. A tomographic measurement using synchrotron radiation Small Angle X-ray Scattering (SAXS) signal was conducted for a 3-layered rectangular rod specimen of Al-Zn-Mg alloys, prepared by hot rolling and cut from a 3-layered sheet. A 2D absorption coefficient tomography in the absolute value was reconstructed for a cross section of specimen pillar. The 2D integrated intensity tomography was also reconstructed in the same cross section, caused by the nanoscopic precipitates from SAXS measurement, in the direction normal to the cross section. Measurements have been performed at the beam-line 40XU of SPring-8, Japan.

Low-temperature Preparation and Mechanism Study of Vanadium Nitride: Yongjie Liu1; Qingqing Hu1; Donglai Ma1; Yue Wang1; Zhixiong You1; 1Chongqing University
    In this study, VN was successfully prepared from V2O5 in an ammonia atmosphere at 600℃. Factsage 8.0 software was used to analyze the gas composition in the reaction process. Meanwhile, based on the first principle of density functional theory, the adsorption model of NH3 on V2O5(001) surface was established. The adsorption of NH3 on V2O5(001) surface was revealed by analyzing the structure change and adsorption energy of the adsorption model. The results show that the adsorption of NH3 on V2O5(001) surface makes the bond length of the surrounding V-O bond longer, which describes the reaction situation of NH3 and V2O5 microscopic surface interface to a certain extent. Therefore, through thermodynamic calculation and first-principles calculation and analysis, the microscopic mechanism of the reaction is revealed, which is of great significance to the determination of process parameters in the actual reaction.

Application of Flue Gas Desulfurization Waste for the Production of Geopolymer Tiles: Markssuel Marvila1; Afonso Azevedo; Felipe Gama1; Euzébio Zanelato1; Sergio Monteiro1; Carlos Maurício Vieira1; 1Universidade Estadual do Norte Fluminense Darcy Ribeiro
    Geopolymers are eco-friendly materials that efficiently replace cementitious and ceramic materials. In this context, the objective of this work was to carry out the production of geopolymer tiles using commercial metakaolin and flue gas desulfurization waste (FGD). The tiles were produced in the molar ratio SiO2/Al2O3=3.00, using a composition with 0, 10 and 20% substitution of metakaolin by FGD. Prismatic specimens were produced, with tests of tensile strength, mass density, water absorption and linear shrinkage being carried out. Curing was carried out at 25ºC and 65ºC for a period of 7 days. The results obtained demonstrate that the use of FGD improved the mechanical behavior of the tiles, due to the formation of phases different from geopolymerization of metakaolin alone. It is concluded that the application of geopolymer tiles with FGD is viable, as the values obtained are compatible with the proposed application.

Separation of Nickel and Cobalt from Nickel and Cobalt Solution by Cyanex272: Yan Ganggang1; Wang Zibiao2; Le Dinghao2; Sun Xintao2; Zhang Xijun1; Chen Dalin1; 1State Key Laboratory of Nickel and Cobalt Resources Comprehensive Utilization; 2Central south university
    Due to the close physical and chemical properties of nickel and cobalt, it is difficult to separate them. At present, the main separation methods include ion exchange method, membrane separation method and solvent extraction method. In this study, the solvent extraction method was used for the experiment, in which the nickel cobalt simulation liquid was prepared according to the material liquid data after removing impurities by P204 in the industry, and then the nickel cobalt separation experiment was carried out using the modified Cyanex272 extraction agent. The experimental results show that the optimal extraction conditions are as follows: comparison is 1:1, initial pH value is 5.5, reaction temperature is 25 °C, reaction time is 10 min. Under these conditions, the extraction rate of single-stage cobalt can reach about 96%, and the three-stage extraction rate of cobalt can reach more than 99% after the extraction equilibrium diagram is drawn by experiments.

Evolution of the Thermal Conductivity of Sintered Ag Paste as a Function of the Density, the Roughness of the Interface and Aging: Anas Sghuri1; Yann Billaud1; Loïc Signor1; Pascal Gadaud1; Didier Saury1; Xavier Milhet1; 1Pprime Institut
    This work presents a methodology to estimate the evolution of thermal conductivity of sintered silver deposited on pure copper, used as die-attach in the microelectronics industry. The study is based on a comparative assessment of the effect of silver porosity, interface roughness and aging on the conductivity of the material. The porosity and interface roughness are estimated by means of image analysis. The conductivity estimation method is based on solving an inverse problem by minimizing the squared deviation between the response of a 3D semi-analytical model and the measurement from a single flash-type experiment. The chosen estimator, known as ENH (Estimation by Normalization of Harmonics), consists in dividing the measurements by a reference harmonic. This method allows the simultaneous estimation of the in-plane conductivity components. The results of the experimental measurement of the thermal conductivity of sintered silver as a function of the density and aging are presented and discussed.

High-speed X-rays for Quantitative Analyses of Dynamic Events: Andrew Brown1; Thomas Plaisted1; Hans Broos2; Frits Hilvers2; 1DEVCOM U.S. Army Research Laboratory; 2TNO
    X-ray imaging of dynamic events has evolved in recent decades from the traditional sequencing of flash x-ray images to utilizing continuous x-ray sources and synchrotrons in combination with scintillator screens and high-speed cameras to capture dynamic events at frame rates on the order of 102-106 s-1. High-speed x-ray (HSX) imaging produces a single imaged plane for the duration of a dynamic event and is advantageous for tracking the motion of non-symmetric objects. In this study, a HSX system at TNO (Netherlands) is used to image ballistic impacts on a commercially available helmet backed by a 3D printed frangible human skull surrogate system developed at DEVCOM U.S. Army Research Laboratory. The HSX videos allow for quantitative analyses of the evolving helmet backface and subsequent interactions with the frangible skull surrogate that are otherwise not achievable via synchrotron sources (field-of-view limitations) or flash x-rays (limited frames and varying imaging planes).

Lowering the Presence of Heavy Metals in Textured Coat Using Recycled Post Consumer Glass: Andrew Adejo1; Adele Garkida2; Clement Gonah2; Eric Opoku2; 1Federal University of Lafia; 2Ahmadu Bello University
    Four extender batches of 95.7% recycled post-consumer glass, 0.25% colourant and 4% acrylic binder each were processed into extenders of yellow, blue, red and black separately. Textured coat batches of 20.1% Solvent, 12.0% binder, 67.0% extender, 0.2% Natrosol, 0.2% Texanol, 0.2% biocides and 0.1% ammonia were developed and characterized using atomic absorption spectroscopy (ASTM D3335). Results showed that Yellow coat has concentration of 170.65 ±0.031ppm lead, 3.40±0.025ppm Cobalt and 24.25±0.08ppm Cadmium, Red coat has concentration of 27.25±0.015ppm lead, 0.30±0.045ppm Cobalt and 9.85±0.065ppm Cadmium, Blue coat has concentration of 115.15±0.125ppm Lead, 0.30±0.01ppm, Cobalt and 9.85±0.065ppm Cadmium while Black coat has concentration of 33.10±0.37ppm Lead, 1.70±0.01ppm Cobalt and 0.30±0.02ppm Cadmium. This study shows that recycled post-consumer glass can be employed to produce textured coat with lower concentrations of heavy metals for buildings as compared to contemporary textured coats whose concentrations are greater than 90ppm for Lead, 100ppm for Cadmium and 100ppm for Cobalt.

Adsorption of Iron, Copper, Chromium and Cadmium in Cobalt Sulfate Solution by Goethite: Sujun Lu1; Jiang Cao2; Yuanyuan Li2; Guoju Chen1; Priska Jesika2; Guanwen Luo2; 1State Key Laboratory of Nickel and Cobalt Resources Comprehensive Utilization; 2Central South University
    Battery grade cobalt sulfate is an important raw material for the production of cathode materials for lithium-ion batteries. Crude cobalt sulfate solution often contains a variety of impurities. The existence of these impurities will affect the performance of cathode materials, so it needs deep purification and impurity removal. In this project, we used goethite and direct oxidation for adsorption to remove Fe, Cu, Pb, Cd, Cr and other impurity elements in cobalt sulfate solution. The result shows that the order of goethite adsorbing heavy metal ions is chromium, cadmium/nickel and cobalt. We used direct oxidation adsorption method to adsorb iron, chromium and copper ions from the solution. Under the conditions of pH value 4.0 and temperature 60℃, the removal rate of iron ions in the solution can reach 89%, which provides guidance for the study of adsorption and impurity removal of cobalt sulfate solution in the future.

Degradation of Structure and Properties of Coke in Blast Furnace: Effect of High Temperature Heat Treatment: Jingbo Chen1; Shengfu Zhang1; Yan Guo1; 1Chongqing Unversity
    To clarify the relationship between mineral phases transformation, carbon matrix structure and coke properties of metallurgical coke during high temperature in blast furnace, metallurgical coke made from different coking coals were subjected to annealing under N2 at 1100 ℃-1600 ℃ (corresponding from the lumpy zone to the dropping zone). A new method for quantitative analysis of mineral phases combined with X-Ray diffraction was used to describe the transformation of minerals phases. RT-Raman spectra, Optical microscope and Universal material testing machine were used to characterize the change of carbon matrix structure and coke properties. It was found that annealing caused the mineral transformation in coke, including the decomposition of kaoline and mullite, the formation of moissanite, cementite and gehlenite which result in the increase of coke porosity. Then, annealing can affect the carbon structure (crystalline structure and carbon skeleton), including promoting graphitization of carbon structure and cleavaging of large aromatic ring.

Strength and Failure Characterization of the Gibeon (IVA) Iron Meteorite: Md Fazle Rabbi1; Khaled Khafagy1; Laurence Garvie1; Erik Asphaug2; Desiree Cotto-Figueroa3; Aditi Chattopadhyay1; 1Arizona State University; 2University of Arizona; 3University of Puerto Rico at Humacao
    Iron meteorites are thought to be remnants of the cores of differentiated planetesimals, exposed to interplanetary space by collisional events. Since their phases (kamacite and taenite) are unique from the traditional steel phases, it is crucial to understand their material properties and failure mechanisms. In this study, eight specimens are used to characterize the strengths and failure mechanisms of Gibeon meteorite under quasi-static compressive and tensile loading. Although several authors reported Gibeon’s properties under different loading conditions, this paper shows the full-field strain and displacement contours using an in-situ three-dimensional digital image correlation technique that aids in better understating the initiation and propagation of damage surfaces. Further characterization of the post-fracture surfaces will be studied and correlated to the DIC effective strain contours to better study the influence of different phases on the failure mechanisms. These new findings will improve our understanding towards the asteroidal breakup of iron-rich bodies.