Results for “microstructural analysis” — Page 5

NASA NTRS2026

PROTECT: Production and Reuse of Thermally Efficient Ceramic Thermal Protection Systems

PROTECT (Production and Reuse Of Thermally Efficient Ceramic TPS) is a NASA Early Career Initiative focused on developing the next generation of reusable ceramic thermal protection systems (TPS). This project addresses key challenges in TPS design, including temperature capability, thermal stability, and refurbishment time, by integrating novel material development with predictive modeling. Leveraging enhanced capabilities in NASA’s Porous Microstructure Analysis (PuMA) software, PROTECT introduces new modeling tools to predict the thermal and mechanical behavior of fibrous ceramic materials. These tools enable accurate prediction of performance metrics such as thermal conductivity and structural integrity, reducing reliance on costly physical testing. Preliminary advances in these areas will be presented. To support model validation, PROTECT is building a comprehensive database of raw material properties using advanced characterization techniques, including micro computed tomography (CT) scanning in collaboration with the University of Illinois Urbana-Champaign (UIUC). The presentation will detail the sampling workflows and analysis methods used to generate this detailed microstructural data and how it is used to develop improved models in PuMA. This multi-center collaboration, spanning NASA (JSC, ARC, KSC, GRC), Oak Ridge National Laboratory, UIUC, and SpaceX, is developing tailored TPS solutions for LEO, lunar, and Martian missions. By bridging heritage systems with the demands of modern spaceflight, PROTECT contributes to the advancement of reusable TPS technologies for future exploration missions.

Propulsion, Refractory, and Coating Materials↗

NASA NTRS2026

PROTECT: Production and Reuse of Thermally Efficient Ceramic Thermal Protection Systems

PROTECT (Production and Reuse Of Thermally Efficient Ceramic TPS) is a NASA Early Career Initiative focused on developing the next generation of reusable ceramic thermal protection systems (TPS). This project addresses key challenges in TPS design, including temperature capability, thermal stability, and refurbishment time, by integrating novel material development with predictive modeling. Leveraging enhanced capabilities in NASA’s Porous Microstructure Analysis (PuMA) software, PROTECT introduces new modeling tools to predict the thermal and mechanical behavior of fibrous ceramic materials. These tools enable accurate prediction of performance metrics such as thermal conductivity and structural integrity, reducing reliance on costly physical testing. Preliminary advances in these areas will be presented. To support model validation, PROTECT is building a comprehensive database of raw material properties using advanced characterization techniques, including micro computed tomography (CT) scanning in collaboration with the University of Illinois Urbana-Champaign (UIUC). The presentation will detail the sampling workflows and analysis methods used to generate this detailed microstructural data and how it is used to develop improved models in PuMA. This multi-center collaboration, spanning NASA (JSC, ARC, KSC, GRC), Oak Ridge National Laboratory, UIUC, and SpaceX, is developing tailored TPS solutions for LEO, lunar, and Martian missions. By bridging heritage systems with the demands of modern spaceflight, PROTECT contributes to the advancement of reusable TPS technologies for future exploration missions.

Propulsion, Refractory, and Coating Materials↗

DOE OSTI2020

Notch-tensile behavior of Al0.1CrFeCoNi high entropy alloy

Notch-tensile behavior of an Al0.1CrFeCoNi high entropy alloy (Al0.1-HEA) was studied using V-notch geometry and with local strain mapping using digital image correlation (DIC). A notch-strength ratio of 1.51 indicated notch strengthening. Further analysis of stress-strain response supplemented with microstructural analysis revealed that, while the presence of notch results in strengthening due to work hardening by twinning induced plasticity, the notch also contributes strongly to geometrical softening in the non-uniform ductility regime, and accounts for the onset of failure. The strain localization behavior of Al0.1-HEA due to the presence of V-notch was compared with three conventional alloys: Inconel 625 nickel-based superalloy, 304 stainless steel and Ti–6Al–4V titanium alloy. The study revealed that the nature of notch widening with increasing strain was dependent on material characteristics. The extent of notch widening impacted the local strain field and stress distribution, thereby influencing the propensity for crack initiation and growth. The experimental results were verified by finite element analysis.

Sinha, Subhasis↗

DOE OSTI2020

Rietveld Refinement for Macromolecular Powder Diffraction

Powder X-ray diffraction (PXRD) has been employed extensively for the structural characterization of materials, quantitative analysis of multicomponent mixtures, phase identification, texture, and microstructural analysis. At the heart of all those lies the Rietveld method, which has revolutionized the use of powder diffraction for materials studies. Initially applied to minerals and inorganics, the Rietveld method has progressively been used for more complex materials, for instance, zeolites and pharmaceuticals. A major advance of the method came some 20 years ago, when the first protein structure was successfully refined. Because of the sheer complexity of macromolecules, several new approaches and algorithms had to be pioneered or adapted from macromolecular single-crystal diffraction experiments, thus constituting macromolecular PXRD a quite unique field of study. This review aims to provide necessary elements of theory and application of structure solution and refinement via the Rietveld method for macromolecular PXRD data. Here, practical explanations and highlighted case studies are also presented.

36 MATERIALS SCIENCE↗

DOE OSTI2022

In situ melt pool measurements for laser powder bed fusion using multi sensing and correlation analysis

Laser powder bed fusion is a promising technology for local deposition and microstructure control, but it suffers from defects such as delamination and porosity due to the lack of understanding of melt pool dynamics. To study the fundamental behavior of the melt pool, both geometric and thermal sensing with high spatial and temporal resolutions are necessary. This work applies and integrates three advanced sensing technologies: synchrotron X-ray imaging, high-speed IR camera, and high-spatial-resolution IR camera to characterize the evolution of the melt pool shape, keyhole, vapor plume, and thermal evolution in Ti–6Al–4V and 410 stainless steel spot melt cases. Aside from presenting the sensing capability, this paper develops an effective algorithm for high-speed X-ray imaging data to identify melt pool geometries accurately. Preprocessing methods are also implemented for the IR data to estimate the emissivity value and extrapolate the saturated pixels. Quantifications on boundary velocities, melt pool dimensions, thermal gradients, and cooling rates are performed, enabling future comprehensive melt pool dynamics and microstructure analysis. The study discovers a strong correlation between the thermal and X-ray data, demonstrating the feasibility of using relatively cheap IR cameras to predict features that currently can only be captured using costly synchrotron X-ray imaging. Such correlation can be used for future thermal-based melt pool control and model validation.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

Effects of high-dose neutron irradiation at light-water reactor relevant temperature on the mechanical properties of SiC/SiC composites

For this study, the neutron dose-dependent evolutions and the underlying mechanisms of properties of SiC fiber-reinforced SiC matrix (SiC/SiC) composites at a temperature relevant to light-water reactors (∼600 K) were investigated and analyzed. Chemical vapor infiltrated (CVI) SiC/SiC composites reinforced with Hi-Nicalon Type S or Tyranno SA3 fiber were neutron-irradiated to doses up to 30 dpa. The irradiated composites retained their flexural strengths. The thermal diffusivity and dimensional changes were mostly retained from 2.0 to 30.2 dpa. Discrepancies in irradiation responses among CVI SiC/SiC composites from different sources were found. Additional microstructural analysis using Raman spectroscopy and numerical analysis on irradiation effect on residual stress were used to explain how the microstructural variables, especially of carbon interphases, affect the mechanical properties in the 30–40 dpa dose range.

Continuous fiber-reinforced ceramic matrix composi↗

NASA NTRS2001

C-Coupon Studies of CMCS: Fracture Behavior and Microstructural Characterization

A curved beam 'C-coupon' was used to assess fracture behavior in a Sylramic(tm)/melt infiltration (MI) SiC matrix composite. Failure stresses and fracture mechanisms, as determined by optical and scanning electron microstructural analysis, are compared with finite element stress calculations to analyze failure modes. Material microstructure was found to have a strong influence on mechanical behavior. Fracture occurs in interlaminar tension (ILT), provided that the ratio of ILT to tensile strength for the material is less than the ratio of radial to hoop stresses for the C-coupon geometry. Utilization of 3D architectures to improve interlaminar strength requires significant development efforts to incorporate through thickness fibers in regions with high curvatures while maintaining uniform thickness, radius, and microstructure.

Hurwitz, Frances I.↗

NASA NTRSDate not supplied

Impact of Powder Supply Variation on Mechanical Properties for Additive Manufacture of Alloy 718

The Additive Manufacturing Structural Integrity Initiative (AMSII) examined how a number of different Alloy 718 powder lots can create variation in microstructure and mechanical properties in parts fabricated using Laser Powder Bed Fusion. Being a common alloy, Alloy 718 powder can be found in a variety of compositions, fabrication techniques, and powder size distribution. Sixteen virgin powders, and three recycled powders were used to build samples for microstructure analysis, fatigue and tensile testing. The major impacts of the different powders manifested in variations in the microstructure, such as minor phases and grain size variation. There were corresponding variations in mechanical properties. A down-selection of powders were chosen for additional analysis, and a powder recyclability study was completed to look at the effect of reused powder.

Alloy 718↗

DOE OSTI2022

TEM Specimen Manufacturing to Support Analysis of IASCC Mechanisms in Irradiated Austenitic Steels – Light-Water– Relevant Materials

The present report describes the manufacturing of samples for advanced microstructure studies of mechanisms of irradiation-assisted stress corrosion cracking (IASCC) in the materials of light-water reactor (LWR) internal components. The samples were manufactured via FIB (focused ion beam milling) from 4-point-bend specimens subjected to oxidation and mechanical loading in a simulated LWR environment (primary water, PW). The corrosion tests were conducted at the University of Michigan (UM), and the tested specimens were transported to ORNL to perform FIB work. Finally, the manufactured FIB specimens were shipped back to the UM for microstructure characterization. Section 1 in the report provides a brief introduction; Section 2 describes materials, their in-service and irradiation history, and the geometry of specimens for IASCC testing. Section 3 documents typical work steps (specimen mapping) and reports the number of manufactured FIB objects. Section 4 briefly describes the preliminary results of microstructure analysis performed at the University of Michigan and highlights the key findings. The summary and conclusions section discusses future possible future steps and generalizes the obtained results, their unique character, and their importance for the nuclear industry.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRSDate not supplied

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 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↗

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 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↗

NASA NTRSDate not supplied

Predictive Modeling of Carbon Ablators

Efforts to build a Predictive Material Modeling (PMM) framework from the micro-scale to the macro-scale are presented in this abstract. To reduce the need for extensive testing, accelerate the design cycle process, and reduce uncertainty margins applied to final designs, NASA is developing simulation and modeling tools that enable characterization of material properties and response to high-enthalpy environments. The Porous Microstructure Analysis (PuMA) code has been developed for computing macroscale (volume averaged) properties of porous materials using microscale images from micro-computed tomography (micro-CT). Microscale modeling requires a realistic representation of a material microstructure; these are obtained either synthetically during the design of the material or through X-ray micro-CT. Volume averaged properties are then used to inform macroscale material response models, such as those implemented in the Porous-material Analysis Toolbox based on OpenFOAM (PATO) software, also actively developed by NASA. 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. These tools were developed to efficiently interface with other pre-existing codes such as SPARTA (direct simulation Monte Carlo), DPLR (hypersonic CFD), NEQAIR (radiative transport) and DAKOTA (uncertainty quantification and optimization). Detailed flight data (Mars Science Laboratory [MSL] Entry Descent and Landing Instrument [MEDLI]) is critical for validating these computational tools for NASA applications. Examples of modeling ablative material response using these codes will be presented including 3D simulations of the full-scale heatshield of the MSL capsule. The simulations demonstrate 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.

Thermal Protection Systems↗

NASA NTRSDate not supplied

Predictive Modeling of Carbon Ablators Using Micro and Macro-Scale Modeling

Efforts to build a Predictive Material Modeling (PMM) framework from the micro-scale to the macro-scale are presented in this abstract. To reduce the need for extensive testing, accelerate the design cycle process, and reduce uncertainty margins applied to final designs, NASA is developing simulation and modeling tools that enable characterization of material properties and response to high-enthalpy environments. The Porous Microstructure Analysis (PuMA) code has been developed for computing macroscale (volume averaged) properties of porous materials using microscale images from micro-computed tomography (micro-CT). Microscale modeling requires a realistic representation of a material microstructure; these are obtained either synthetically during the design of the material or through X-ray micro-CT. Volume averaged properties are then used to inform macroscale material response models, such as those implemented in the Porous-material Analysis Toolbox based on OpenFOAM (PATO) software, also actively developed by NASA. 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. These tools were developed to efficiently interface with other pre-existing codes such as SPARTA (direct simulation Monte Carlo), DPLR (hypersonic CFD), NEQAIR (radiative transport) and DAKOTA (uncertainty quantification and optimization). Detailed flight data (Mars Science Laboratory [MSL] Entry Descent and Landing Instrument [MEDLI]) is critical for validating these computational tools for NASA applications. Examples of modeling ablative material response using these codes will be presented including 3D simulations of the full-scale heatshield of the MSL capsule. The simulations demonstrate 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.

Thermal Protection Systems↗