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Updates on the Predictive Materials Modeling Software Tools

Updates on NASA‘s efforts to build a Predictive Material Modeling (PMM) framework from the micro-scale to the macro-scale are presented in this abstract. The PMM effort is part of the Entry Systems Modeling (ESM) project under NASA’s Game Changing Development (GCD) program. To reduce the need for extensive testing and accelerate the design cycle process, ESM is developing simulation and modeling tools that enable the characterization of the properties of thermal protection materials and their response to extremely hot plasma. The Porous Microstructure Analysis (PuMA) software has been developed to compute effective material properties and perform material response simulations on digitized microstructures of porous media. PuMA is able to import three-dimensional digital images obtained from X-ray microtomography or to generate artificial microstructures that mimic real materials. PuMA also provides a module for interactive 3D visualizations. Version 3, which was recently released as open-source, includes modules to compute simple morphological properties such as porosity, volume fractions, pore diameter, and specific surface area. Additional capabilities include the determination of effective thermal and electrical conductivity (both radiative and solid conduction - including the ability to simulate local anisotropy for the latter); effective diffusivity and tortuosity from the continuum to the rarefied regime; techniques to determine the local material orientation, as well as mechanical properties (elasticity coefficients), and permeability. Computed properties are then used to inform a macro-scale material response model, such as those implemented in the Porous material Analysis Toolbox based on OpenFOAM (PATO) software developed within ESM. The computational model in PATO is a generic heat and mass transfer model for porous reactive materials containing several solid phases and a single gas phase. The detailed chemical interactions occurring between the solid phases and the gas phase are modeled at the pore scale, assuming Local Thermal Equilibrium. Recent efforts include the development of a mechanical erosion model as well as a unified model allowing an intrinsic coupling between fluid and material. Comparison to flight data (Mars Science Laboratory [MSL] Entry Descent and Landing Instrument [MEDLI] and Mars 2020 MEDLI2) is critical in order to validate these computational tools. Examples of ablative material response using the code will be presented, including 3D simulations of the full-scale heatshield of the MSL capsule. The simulations demonstrated the ability of the modern material response code, PATO, to handle the material response of geometrically complex and large domains through the use of massively parallel computations.

material modeling↗
DOE OSTI2013

Edward's sword? - A non-destructive study of a medieval king's sword

Non-destructive and instrumental methods including photon activation analysis were applied in an examination of an ancient sword. It was tried to find indication of forgery or, if authentic, any later processing and alteration. Metal components of the hilt and the blade were analysed by instrumental photon activation. Non-destructive metallurgical studies (hardness measurements, microscopic microstructure analysis) are briefly described, too. The results of these investigations did not yield indication of non-authenticity. This stood in agreement with the results of stylistic and scientific studies by weapon experts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Effect of Oxide Additives on Phase Evolution and Tribological Behavior of Zirconia-Toughened Alumina Composite

Four different zirconia-toughened alumina added with different pairs of oxides (CeO{sub 2}, TiO{sub 2}, CuO, ZnO and SnO{sub 2}) were prepared through the co-precipitation technique. Conventional sintering resulted in relative densities ≥96%. Phase analyses of these composites were performed by x-ray diffraction. Vicker’s hardness and tribological behavior of all ZTA composites were studied. Microstructure analysis of polished and worn surfaces was carried out to understand and correlate the mechanical/tribological behavior with the microstructure. A different wear mechanism is observed in ZTA containing CeO{sub 2} and TiO{sub 2} which resulted in considerable improvement in tribological behavior with a minimum specific wear rate of 9 × 10{sup −7} mm{sup 3}/Nm.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Magnesium Alloy ZK60 Tubing made by Shear Assisted Processing and Extrusion (ShAPE)

ZK60 Magnesium tubing has been friction extruded from as-cast billets and T5 conditioned bars using Shear Assisted Processing and Extrusion (ShAPE). Tubes having an outer diameter of 50.8 mm and wall thickness of 1.9 mm were extruded with >20 times less ram force compared to conventional extrusion due to the unique shearing conditions and tooling inherent to ShAPE. Microstructures of the as-cast billet and T5 bar feedstock materials were significantly different from each other in terms of grain size, texture, and second phase distribution; yet the resulting microstructures after ShAPE were remarkably similar. An average grain size of 4-5 microns, 20o tilt of basal texture away from the extrusion axis, and refined second phases having a uniform distribution were achieved independent of the feedstock material. Hardness for as-extruded and artificially aged tubes are presented with isotropic behavior explained by detailed microstructural analysis. This work suggests that bulk ZK60 magnesium alloys extrusions may be fabricated in a single step, with microstructures that are unobtainable with conventional extrusion.

Friction Stir Extrusion, Friction Consolidation an↗
DOE OSTI2020

Fabrication of UN-Mo CERMET Nuclear Fuel Using Advanced Manufacturing Techniques

Ceramic-metallic nuclear fuels are a candidate fuel for nuclear thermal propulsion systems due to their high heat transport properties, which are necessary in very high-temperature environments. The conventional fabrication of uranium nitride–molybdenum fuel has been thoroughly studied in the past, but modern manufacturing techniques have presented a unique opportunity for further development within this field. This work demonstrates the use of advanced manufacturing techniques to produce nuclear fuel pellets composed of uranium nitride microspheres encased in a molybdenum matrix. Binder jetting is used to print molybdenum disks that are filled with uranium nitride microspheres and afterward sintered using spark plasma sintering. Two fuel pellets were fabricated to demonstrate the methodology and to provide a baseline analysis of the effects of temperature and pressure processing conditions. Characterization of the sintered fuel pellets includes detailed microstructural analysis and thermal conductivity measurements.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

STEM imaging of irradiation induced defects in Eurofer97 steel variants irradiated in the EUROfusion collaboration

Ten exploratory variants of Eurofer97 reduced activation ferritic martensitic (RAFM) steel were irradiated in HFIR to ~2.94 – 32.4 dpa, 300±30 °C as a part of the EUROfusion collaboration. The irradiations were performed in rabbit capsules. ES21-22 capsule were used for irradiating SS-J3 tensile samples while M4CVN bend bar samples were irradiated in ES31-35 capsules. The mechanical properties and multi-length scale characterization of the microstructures of these ten steels, designated as H, I, P, J, K, L, M, N, O, P and reference E, in the nonirradiated form was reported in "Mechanical properties and microstructure characterization of unirradiated Eurofer-97 steel variants for the EUROfusion project, ORNL/SPR-2018/882," while their irradiated properties and some microstructure analysis was reported in "Post-irradiation examination of Eurofer97 steel variants irradiated to 2.5 dpa, ~300 °C in HFIR for the EUROfusion program, ORNL/SPR-2020/1440." Here, additional microstructures using TEM/STEM and STEM-EDX of the irradiated steels is presented. Characterization was performed at the Low Activation Materials Development and Analysis (LAMDA) laboratory.

36 MATERIALS SCIENCE↗
DOE OSTI2023

EDS-PhaSe: Phase Segmentation and Analysis from EDS Elemental Map Images Using Markers of Elemental Segregation

Scanning electron microscopy (SEM), combined with energy-dispersive spectroscopy (EDS), is an extensively used technique for in-depth microstructural analysis. Here, we present the EDS-Phase Segmentation (EDS-PhaSe) tool that enables phase segmentation and phase analysis using the EDS elemental map images. Importantly, it converts the EDS map images into estimated composition maps for calculating markers of selective elemental redistribution in the scanned area and creates a phase-segmented micrograph while providing approximate fraction and composition of each identified phase. EDS-PhaSe offers two unique advantages. Firstly, it enables the direct processing of EDS elemental map images without requiring any raw or proprietary data/software, thereby allowing the analysis of EDS results available in the published literature as images. Secondly, it enables segmentation and analysis of phases even when the phase contrast is missing in backscattered micrographs, assisting in correlating the XRD and SEM-EDS data as shown in this work for a AlCoCrFeNi high-entropy alloy.

36 MATERIALS SCIENCE↗
NASA NTRS1995

The effect of gravity on the combustion synthesis of Ni-Al and Ni3Al-TiB2 composites from elements

Previous studies on the combustion synthesis of advanced materials indicate that combustion and structure formation mechanisms involve several stages including melting of reactants and products, spreading of the melt, droplet coalescence, diffusion and convection, buoyancy of solid particles, and densification of the liquid product. Most of these processes are affected by gravity. Conducting the combustion synthesis under microgravity conditions is expected to help elucidate the reaction mechanisms. Two systems were examined. The first involves Ni/AI cladded particles, which is an ideal system to examine the individual particle and liquid flow before combustion occurs. For comparison, elemental Ni and Al powders with the same stoichiometry as that of the cladded particles were also used in some experiments. The second system was the Ni3AITiB2 composite in which the Ni3AI (-delta H(sub f) = 153.1 kJ/mol) phase melts during reaction enabling us to examine settling of the liquid phase. The amount of liquid phase was controlled by varying the TiB2 (-delta H(sub f) = 323.8 kJ/mol) content which generates the additional heat. The overall reactions for the two systems can be expressed as follows. System 1: 4Ni + 2AI yields Ni3AI + NiA and System 2: 3Ni + Al + x (Ti + 2B) yields Ni3Al + x(TiB2). For the first system, pellets were pressed directly from the cladded particles, at green densities about 77 +/- 3% of theoretical value. For the second, the pellets were prepared by mixing the elemental reactant powders in the required stoichiometry by ball-milling and then pressing uniaxially at green densities about 70 +/- 3 percent of theoretical. The pellets were cylindrical in shape, 10 mm in diameter and length typically 20-30 mm. The pellet samples were reacted in UHP Argon (1 atm) using the experimental setup and procedure described previously. After reaction, the samples were sectioned axially in order to conduct the microstructural analysis in the longitudinal direction. The phase composition of the reacted product was determined by X-ray diffraction (XRD) and the microstructure was analyzed using scanning electron microscopy (SEM) along with energy dispersive X-ray spectrometry (EDX).

Varma, Arvind↗
DOE OSTI2017

Studying Unirradiated TRISO-coated Particles from the Second Advanced Gas Reactor Experiment

Combined precession electron diffraction and point resolved chemical imaging have been used to provide an analysis of the material structure and chemical information of unirradiated uranium oxy-carbide (14.0 wt% enriched) kernelled tristructural isotropic-coated (TRISO) coated particle fuel. The detailed microstructural analysis includes examination of the structure associated with kernel, IPyC and SiC layers, as well as the IPyC-SiC interface. The analysis serves as a baseline for future studies on the potential effects of fission product and defect release through intact SiC layers and possible grain restructuring with irradiation. The baseline microstructure is thereby identified to understand the subtle effects of fabrication that may influence fission product precipitate release associated with different fuel types. Results indicated a Si:C gradient in the SiC layer which could influence fission transport reactivity and the high resolution imaging at the IPyC-SiC interface shows the gradual chemical composition change at this interface.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Hydrothermal synthesis of vanadium pentoxide nanowires

Nanowires of V{sub 2}O{sub 5} were prepared via hydrothermal route using NH{sub 4}VO{sub 3} as precursor in the presence of sulfuric acid at 120°C for 24 h. This synthesis process is free of any templates and reducing agents. Thermal analysis showed a phase change at 350°C and the samples were annealed at 500°C. The XRD analysis showed the monoclinic phase for the as-prepared and orthorhombic phase of V{sub 2}O{sub 5} when annealed at 500°C. Characteristic Raman peaks also expressed the same structural features. Microstructure analysis by SEM showed the nanowire structure of V{sub 2}O{sub 5} with thickness in the range of 20–50 nm and length in micrometers. The possible mechanisms of formation of the nanowires were schematically explained based on the layered structure of V{sub 2}O{sub 5}.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS1993

Readying advanced composites for the microscope

Concerns related to the proper preparation of composite specimens for microstructural analysis are examined. Proper preparation will minimize the amount of surface and subsurface damage at each stage of the procedure so that the microstructural features of the final-polished specimen can be accurately determined as a function of the composite's response to processing, testing, or service conditions. This requires that an optimum combination of abrasive type, size, and bond be applied during each grinding, lapping, and polishing step. Machine settings, such as polishing speed, force, and relative polishing direction, are also important. Guidelines are given for each step of the six-stage specimen preparation process: sectioning, planar grinding, sample integrity, polishing, and etching.

Zipperian, Donald C.↗
DOE OSTI2018

The relationship between low-temperature toughness and secondary crack in low-carbon bainitic weld metals

Highlights: • The crack propagation plane was identified with the decreasing possibility of {110}/{100}, {112} and {123}. • Crack path deviates at some middle-angle misorientation boundaries with high strain concentration. • The most effective barrier to arrest crack in Ni0 and Ni2 is the boundaries of inter-Bain in a CPP packet, while in Ni4 the boundaries of inter-CPP and intra-Bain packets impede crack propagation. - Abstract: This paper aims to reveal the relationship among low-temperature toughness, microstructure and secondary crack from both microstructural and crystallographic perspectives. Instrumented Charpy tests were carried out in the upper platform, transition temperature range, as well as at lower temperatures. Quantitative fractographic analysis, microstructural characterization and secondary crack observation were conducted on half of the impact specimen. Crystallographic features were identified in the secondary crack proximity, e.g. variant selection, orientation relationship, cleavage plane of the corresponding crack matrix. Some results in literature are confirmed. Nickel addition is beneficial to hindering crack propagation as a result of microstructure improvement. The most effective barrier for crack propagation is high-angle misorientation boundaries between Bain packets and the boundaries of ferrite matrix with the microstructure of granular bainite. Additionally, high-angle misorientation boundaries between closed-packed plane packets arrest cracks in the mixed microstructure of fine lath bainite and intricate acicular ferrite. Most preferred crack propagation planes are {110} and {100} in our low carbon bainitic weld metals, with the decreasing possibility of {112} and {123}.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Localized Deformation Investigation in Irradiated Materials via Electron Microscopy, EBSD, and In-Situ Mechanical Testing

This report describes the preliminary results of an analysis of dislocation defect structures in nondeformed and deformed austenitic stainless steels – materials of light water reactor internal components. The analysis was performed using an advanced modern approach: high-resolution electron backscatter diffraction (HR-EBSD). Work was performed at Oak Ridge National Laboratory’s Low Activation Materials Development and Analysis (LAMDA) facility. The report is divided into sections describing specific aspects of the project. Section 1 describes the necessity and importance of the defect microstructure analysis and demonstrates that there are very limited data regarding dislocation and defect population at the meso-level (i.e., a grain or group of interacting grains). Section 1 also introduces the HR-EBSD approach used in this research and provides a limited background. Section 2 describes the scanning electron microscope/EBSD systems available at the LAMDA facility, materials investigated in the present work, and hardware and software requirements for the HR-EBSD analysis. Section 3 provides preliminary HR-EBSD results for nonirradiated austenitic stainless steel in contrast to and in comparison with the conventional EBSD outcome. Section 4 describes the HR-EBSD results for austenitic stainless steel irradiated in a commercial-type nuclear power plant and subjected to in-situ mechanical testing. The analysis is focused on mapping and analyzing the geometrically necessary dislocations before and after deformation at small strain levels. As expected, the results will be beneficial for performing corrosion tests, including electrochemical microscopy, which is currently being performed within the Light Water Reactor Sustainability program at the University of California–Los Angeles (Dr. G. Sant). Section 5 summarizes the work performed, presents conclusions, and discusses future activities for this research.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2021

Machine Learning Based Software Package for Reproducible Data Analysis for Electron Microscopy

Advances in hardware and computation technologies are enabling large hyperspectral imaging during Electron Microscopy (EM), resulting in datasets being produced at rapidly increasing spatial and temporal resolutions. This presents exciting opportunities for microstructure analysis, but also poses great challenges in data analysis. Under this STTR program, QuesTek Innovations LLC, a leader in the field of integrated computational materials engineering (ICME), collaborated with Lawrence Livermore National Laboratory and Argonne National Laboratory. The team developed an open-source machine learning (ML) powered tool for EM data analysis of multiple systems and data types, and collected EM data for ML model development using the cutting-edge PicoProbe equipment at Argonne National Laboratory.

Lin, Yu↗
DOE OSTI2013

Observation of crystallization and characterizations on thiourea cadmium iodide: A semi-organic optical material

Graphical abstract: - Highlights: • Thiourea cadmium iodide (TCI) was grown by slow evaporation solution technique. • Morphology and growth rate of the grown compound are determined with the help of inverted microscope. • Optical band gap has been determined. • Microstructure analysis has been reported. • Electrical study has been reported and discussed. - Abstract: In this work, the single crystals of thiourea cadmium iodide were grown by slow evaporation solution technique in two different ratios 2:1 and 1:1. During the formation of their single crystals the morphological features and its live growth process were recorded with the help of inverted microscope. Structural studies of the grown crystals have been carried out by powder X-ray diffraction to confirm the crystal system and vibrational modes by Raman spectroscopy. The optical energy band gaps were investigated through UV–vis spectroscopy study. The surface morphology of the grown single crystals was analyzed by using Scanning Electron Microscope and thermal analysis was carried out by using thermogravimetric analysis. The electrical properties were also studied as a function of frequency and the obtained results are discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Crystallization dynamics in glass-forming systems

Crystallization under far-from-equilibrium conditions is investigated for two different scenarios: crystallization of the metallic glass alloy Cu 50 Zr 50 and solidification of a transparent organic compound, o-terphenyl. For Cu 50 Zr 50 , crystallization kinetics are quanti ed through a new procedure that directly fits thermal analysis data to the commonly utilized JMAK model. The phase evolution during crystallization is quantified through in-situ measurements (HEXRD, DSC) and ex-situ microstructural analysis (TEM, HRTEM). The influence of chemical partitioning, diffusion, and crystallographic orientation on this sequence are examined. For o-terphenyl, the relationship between crystal growth velocity and interface undercooling is systematically studied via directional solidification.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Characterization of basin concrete in support of structural integrity demonstration for extended storage

Concrete core samples from C basin were characterized through material testing and analysis to verify the design inputs for structural analysis of the L Basin and to evaluate the type and extent of changes in the material condition of the concrete under extended service for fuel storage. To avoid the impact on operations, core samples were not collected from L area, but rather, several concrete core samples were taken from the C Basin prior to its closure. C basin was selected due to its similar environmental exposure and service history compared to L Basin. The microstructure and chemical composition of the concrete exposed to the water was profiled from the water surface into the wall to evaluate the impact and extent of exposure. No significant leaching of concrete components was observed. Ingress of carbonation or deleterious species was determined to be insignificant. No evidence of alkali-silica reactions (ASR) was observed. Ettringite was observed to form throughout the structure (in air voids or pores); however, the sulfur content was measured to be consistent with the initial concrete that was used to construct the facility. Similar ettringite trends were observed in the interior segments of the core samples. The compressive strength of the concrete at the mid-wall of the basin was measured, and similar microstructural analysis was conducted on these materials post compression testing. The microstructure was determined to be similar to near-surface segments of the core samples. The average strength was 4148 psi, which is well-above the design strength of 2500 psi. The analyses showed that phase alterations and minor cracking in a microstructure did not affect the design specification for the concrete.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

Effect of nano-SiO{sub 2} particles and curing time on development of fiber-matrix bond properties and microstructure of ultra-high strength concrete

Bond properties between fibers and cementitious matrix have significant effect on the mechanical behavior of composite materials. In this study, the development of steel fiber-matrix interfacial bond properties in ultra-high strength concrete (UHSC) proportioned with nano-SiO{sub 2} varying between 0 and 2%, by mass of cementitious materials, was investigated. A statistical model relating either bond strength or pullout energy to curing time and nano-SiO{sub 2} content was proposed by using the response surface methodology. Mercury intrusion porosimetry (MIP) and backscatter scanning electron microscopy (BSEM) were used to characterize the microstructure of the matrix and the fiber-matrix interface, respectively. Micro-hardness around the embedded fiber and hydration products of the matrix were evaluated as well. Test results indicated that the optimal nano-SiO{sub 2} dosage was 1% in terms of the bond properties and the microstructure. The proposed quadratic model efficiently predicted the bond strength and pullout energy with consideration of curing time and nano-SiO{sub 2} content. The improvement in bond properties associated with nano-silica was correlated with denser matrix and/or interface and stronger bond and greater strength of hydration products based on microstructural analysis.

36 MATERIALS SCIENCE↗