Search NASA⌕ Search

SEARCH · Search NASA

Results for “Microstructural Analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Inelastic Deformation of Metal Matrix Composites: Plasticity and Damage Mechanisms - Part 1

The deformation mechanisms of a Ti 15-3/SCS6 (SiC fiber) metal matrix composite (MMC) were investigated using a combination of mechanical measurements and microstructural analysis. The objectives were to evaluate the contributions of plasticity and damage to the overall inelastic response, and to confirm the mechanisms by rigorous microstructural evaluations. The results of room temperature experiments performed on 0 degree and 90 degree systems primarily are reported in this report. Results of experiments performed on other laminate systems and at high temperatures will be provided in a forthcoming report. Inelastic deformation of the 0 degree MMC (fibers parallel to load direction) was dominated by the plasticity of the matrix. In contrast, inelastic deformations of the 90 degree composite (fibers perpendicular to loading direction) occurred by both damage and plasticity. The predictions of a continuum elastic plastic model were compared with experimental data. The model was adequate for predicting the 0 degree response; however, it was inadequate for predicting the 90 degree response largely because it neglected damage. The importance of validating constitutive models using a combination of mechanical measurements and microstructural analysis is pointed out. The deformation mechanisms, and the likely sequence of events associated with the inelastic deformation of MMCs, are indicated in this paper.

Majumdar, B. S.↗
DOE OSTI2020

Mechanistic Analysis of Microstructural Attributes to Lithium Plating in Fast Charging

Metallic lithium deposition on graphite anodes is a critical degradation mode in lithium-ion batteries, which limits safety and fast charge capability. A conclusive strategy to mitigate lithium deposition under fast charging yet remains elusive. Herein, we examine the role of electrode microstructure in mitigating lithium plating behavior under various operating conditions, including fast charging. The multilength scale characteristics of the electrode microstructure lead to a complex interaction of transport and kinetic limitations that significantly governs the cell performance and the occurrence of Li plating. We demonstrate, based on a comprehensive mesoscale analysis, that the performance and degradation can be significantly modulated via systematic design improvements at the hierarchy of length scales. It is found that the improvement in kinetic and transport characteristics achievable at disparate scales can dramatically affect Li plating propensity.

25 ENERGY STORAGE↗
DOE OSTI2025

Geometry and size dependent microstructure and crack formation in Rene 41 superalloy fabricated by laser powder bed fusion

This study provides a systematic investigation into the size and geometry-dependent microstructural evolution and cracking susceptibility of LPBF-fabricated Rene 41. By coupling experimental microstructural analysis with thermal modeling, this research uniquely identifies the relationship between geometry-specific thermal histories, carbide coarsening, and liquation cracking. Four different geometries with varying thickness were fabricated with the identical process parameters. It was found that the grain size and morphology are not affected by the part size. However, the thinner parts exhibited coarser sub-grain structures compared to the thicker ones. The crack formation was observed for the parts with cross-sections smaller than 1 mm, whereas thicker parts had high density without any defects. Further, the cracks were observed in the interdendritic regions, suggesting that liquation cracking was the active micro-crack formation mechanism. The detailed microstructural analysis combined with a thermal finite element analysis proved that the heat extraction efficiency was lower for thinner parts causing a lower cooling rate and coarser carbides, making them more susceptible to constitutional liquation. Microhardness measurements were conducted for each geometry and correlated with the observed microstructural variations. The findings highlight the critical need for geometry-specific optimization of LPBF process parameters to mitigate cracking and achieve microstructural uniformity, offering valuable insights into the fabrication of complex, high-performance aerospace components.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Comparative analysis of microstructure and reactive sites for nuclear graphite IG-110 and graphite matrix A3

Nuclear graphite and graphite matrix are both high-purity, fine-grain, graphitized materials designed for use in Fluoride-Salt Cooled High Temperature Reactors (FHRs), High Temperature Gas Cooled Reactors (HTGRs), and Molten Salt Reactors (MSRs). Their ability to chemisorb radioisotopes (such as tritium) and their chemical stability is dependent upon the density of reactive carbon sites (RCS), which varies among grades of graphite and changes with neutron irradiation. While nuclear graphites have been extensively characterized, much less data is available for graphite matrix. The current study performs a comparative analysis of IG-110 nuclear graphite and A3 graphite matrix, by X-ray Diffraction (XRD), Raman, and H 2 uptake at 700 °C with H 2 partial pressure range of 300 Pa and 22 kPa. At 10 kPa, the RCS occupied by H 2 uptake per number of carbon atoms at the edge of a crystallite, H/C edge , is 600(300) appm for IG-110 and 2300(200) appm for A3. Prior empirical studies for nuclear graphite establish a linear relationship between H/C and C edge /C and degree of graphitization. The present study shows that these correlations no longer hold when extrapolating to graphite matrix; the type of defects and the defect density at the crystallite surface are different between IG-110 and A3 due to differences in raw materials and manufacturing method.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

ROADRUNNER MiniFuel Experiment: Irradiation Target Design and Sample Characterization

High-density uranium nitride (UN) is a fuel candidate for several advanced nuclear reactor designs currently under development. Because there are limited UN performance data relative to fuel fabrication impurity and density variation, an irradiation campaign has been developed as part of a collaborative effort among the University of Texas at San Antonio (UTSA), Westinghouse Electric Company, Oak Ridge National Laboratory (ORNL), and Los Alamos National Laboratory (LANL) under the Nuclear Science User Facilities program. This project, entitled ROADRUNNER, or Research On ADvancing the peRformance of UraNium Nitrides in Extreme enviRonments, aimsto support UN fuel qualification for advanced reactors by investigating the impact of density and impurity variations on UN performance as a function of irradiation temperature and burnup. The MiniFuel experiment vehicle developed by ORNL, which leverages the High Flux Isotope Reactor, was selected to perform this accelerated separate-effects irradiation testing. The experiment test matrix consists of six MiniFuel targets containing miniature UN fuel disks, and targets three distinct burnup levels (37.5, 60, and 75 MWd/kg U) and three distinct temperatures (600, 900, and 1200°C). Neutronics and thermal analyses were performed to determine the experimental parameters needed to meet the desired irradiation conditions and to predict the experiment components temperatures. UN pellets were fabricated at LANL with tightly controlled parameters to produce specimens with three distinct densities and three levels of carbon content. The pellets were then thinned down by UTSA to the experiment-required thickness. The pre-characterization of the specimens includes density measurements, carbon and oxygen contents, microstructure analysis, and x-ray computed tomography. The selected specimens will be assembled into the MiniFuel experiment, and the first ROADRUNNER MiniFuel targets are intended for HFIR insertion during the Fall of 2024. After irradiation, the targets will be shipped to ORNL’s hot cell facility for disassembly. The post-irradiation examination on the fuel specimens includes fission gas release measurements, visual inspection, fuel swelling measurements, gamma spectroscopy, and microstructure analysis. The data collected post-irradiation will be used to develop fuel performance models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1981

Microscopy and microstructure of Shuttle thermal protection system materials

Examples of the contribution of microstructural analysis to the development of the Space Shuttle tile insulation system are presented, with photographic examples of the scanning electron microscope (SEM) investigations. After the basic thermal protection system materials had been selected, it was neccessary to analyze the mechanical responses of the combined materials; which included: (1) the polymer strain isolation pad (SIP), (2) the room temperature-vulcanizing silicone rubber bond, (RTV), and (3) rigid ceramic fiber reusable surface insulation (RSI). Microstructural analysis was used to provide information on deformation and fracture mechanisms, load transfer mechanisms, and structural alterations occurring before final failure. Both quantitative and qualitative information was obtained in the open, three-dimensional fibrous structures of the ceramic tiles by means of novel techniques of encapsulation and dissolution.

Newquist, C. W.↗
DOE OSTI2025

Survey of baffle plate samples, specimen machining, and hydrogen measurements

This report outlines preliminary results on the survey and characterization of irradiated baffle plate, baffle former, and flux thimble tube specimens as part of the ongoing investigation into irradiation-induced embrittlement in austenitic stainless steels at ambient (room temperature) conditions. The specimens originated from commercial pressurized water reactor (PWR) components, covering displacement damage doses ranging from approximately 0.065 to 75 dpa. Initial scanning electron microscopy (SEM) surveys revealed that specimen surfaces exhibited fine machining marks and in-service-formed oxide layers on the side surfaces of the analyzed specimens. The oxide layers revealed specific features resembling localized "pitting-like" corrosion. An additional set of specimens representing in-service oxidation is being preserved for future microstructure analysis work. As believed, this will provide additional insights into long-term material degradation in PRWs. Specimen machining challenges emerged due to a complex failure of the electric discharge machining (EDM) system located in hot area. Despite partial restoration, issues persist with the EDM’s secondary power supply, necessitating the exploration of alternative EDM or computer numerical control (CNC) machining approaches to facilitate tensile specimen preparation. Currently, low speed saw cutting is in progress to prepare specimens for hydrogen measurements and general microstructure analysis. The near-term goals include completing tensile specimen machining for advanced mechanical testing and characterizing fracture mechanisms, and stress-corrosion cracking testing, ultimately aiming to identify and mitigate the ambient-condition intergranular cracking through targeted post-irradiation annealing strategies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRSDate not supplied

3D Printed Ceramic Reinforced Polymer Composites Microstructure and Mechanical Properties

In Fused Filament Fabrication (FFF) 3D printing a part is made by extruding material layer by layer. Benefits of FFF are the ability to print complex shapes quickly and at a lower cost compared to other manufacturing methods. In this work, filaments composed of either silicon carbide (SiC) or zirconium silicate ceramic particulates in a polylactic-acid (PLA) matrix were used to print specimens for microstructural analysis and mechanical testing. Pure PLA samples were also printed and tested as a baseline for comparison. A Design of Experiments approach was used to test the interactions between three different parameters and their effect on ultimate strength, Young’s modulus, and yield strength. For compression test specimens, these parameters were infill percentage, number of shells, and print orientation angle. For tensile test specimens, the parameters were layer height, number of shells, and infill orientation angle. Pre- and post-compression test samples were evaluated by scanning electron microscopy for microstructural analysis. Infill percentage had the greatest effect on mechanical properties while number of shells and print orientation angle had minor effects. When changing the layer lines from perpendicular to parallel, relative to the loading direction, SiC-PLA had higher mechanical properties while pure PLA properties had decreased, and zirconium silicate-PLA had mix results.

Fused filament fabrication↗
NASA NTRS1996

Tensile Strength and Microstructural Characterization of Uncoated and Coated HPZ Ceramic Fibers

Tensile strengths of as-received HPZ fiber and those surface coated with BN, BN/SiC, and BN/Si3N4 have been determined at room temperature using a two-parameter Weibull distribution. Nominally approx. 0.4 micron BN and 0.2 micron SiC or Si3N4 coatings were deposited on the fibers by chemical vapor deposition using a continuous reactor. The average tensile strength of uncoated HPZ fiber was 2.0 +/- 0.56 GPa (290 +/- 81 ksi) with a Weibull modulus of 4.1. For the BN coated fibers, the average strength and the Weibull modulus increased to 2.39 +/- 0.44 GPa (346 +/- 64 ksi) and 6.5, respectively. The HPZ/BN/SiC fibers showed an average strength of 2.0 +/- 0.32 GPa (290 +/- 47 ksi) and Weibull modulus of 7.3. Average strength of the fibers having a dual BN/Si3N4 surface coating degraded to 1.15 +/- 0.26 GPa (166 +/- 38 ksi) with a Weibull modulus of 5.3. The chemical composition and thickness of the fiber coatings were determined using scanning Auger analysis. Microstructural analysis of the fibers and the coatings was carried out by scanning electron microscopy and transmission electron microscopy. A microporous silica-rich layer approx. 200 nm thick is present on the as-received HPZ fiber surface. The BN coatings on the fibers are amorphous to partly turbostratic and contaminated with carbon and oxygen. Silicon carbide coating was crystalline whereas the silicon nitride coating was amorphous. The silicon carbide and silicon nitride coatings are non-stoichiometric, non-uniform, and granular. Within a fiber tow, the fibers on the outside had thicker and more granular coatings than those on the inside.

Bansal, Narottam P.↗
DOE OSTI2026

Directed energy deposition of Haynes 282 nickel superalloy

Laser powder directed energy deposition was employed to fabricate Haynes® 282 Ni-based superalloy for high temperature creep testing. Material was heat treated using a single-step aging heat treatment of 800 °C for 4 h. Microstructural analysis was conducted in the as-deposited, solution-annealed, and age-hardened conditions. γ′ precipitates were absent in the as-deposited and annealed condition but formed during aging with an average size of 48.5 ± 12 nm. γ’ denuded zones ranging in thickness from 73 to 469 nm were observed adjacent to an effectively continuous grain boundary carbide film that covered 72.5% of the measured boundary length. The heat-treated material contained a high-volume fraction of TiC carbides ranging in size from 38 to 457 nm. Electron backscatter diffraction showed partial recrystallization, with 77-83% recrystallized area and a heterogeneous grain-size distribution. Creep testing at 750 °C at 300, 320, and 350 MPa revealed significantly inferior performance compared to wrought material, with higher strain rates, earlier tertiary onset, and shorter rupture lives. Fractography shows that failure was dominated by intergranular rupture. Post rupture microstructural analysis results suggest that the creep behavior was primarily governed by the non-equilibrium interface network rather than the bulk γ/γ’ matrix. In conclusion, the findings indicate that achieving wrought-like creep performance necessitates substantial improvements in the additive process, specifically focusing on enhanced homogenization, full recrystallization, and precise control over the morphology and distribution of carbides.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

Voltage cycling as a dynamic operation mode for high temperature electrolysis solid oxide cells

Solid Oxide Electrolysis Cells (SOECs) have emerged as a promising technology for the efficient production of H2 via high-temperature electrolysis. However, power input from dynamic energy sources remains a significant challenge for their long-term stability. It is important to analyze the tolerance of cells under dynamic operation conditions. This study focuses on evaluating the impact of voltage cycling on the performance and durability of electrode-supported SOECs. We explore the operational limits and degradation mechanisms of SOECs subjected to various voltage conditions and find that the cells have high tolerance for dynamic voltage. Voltage cycling between 1.3 V and 1.5 V for 9000 cycles does not damage the cell. Conversely, cycling to higher voltages (≥1.7 V) results in accelerated degradation. Advanced characterization is used to screen for various degradation modes post operation. Within the oxygen electrode, XRD and STEM EDS find compositional and phase evolution in all voltage cycled samples including increased decomposition of the air electrode resulting in cation migration. Microstructural analysis of the fuel electrode from nano-CT data shows minimal change throughout the sample set and no evidence of Ni migration, indicating the fuel electrode is stable and not impacted by cycling to higher voltages within the timeframe studied.

Zhu, Zhikuan↗
DOE OSTI2026

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics↗
DOE OSTI2019

A Comparative Analysis on Microstructure and Fracture Mechanism of X100 Pipeline Steel CGHAZ Between Laser Welding and Arc Welding

The objective of this study is to compare and contrast the differences in microstructure and fracture mechanism between CGHAZ of laser welding and submerged arc welding in X100 pipeline steel. The single-pass welding thermal simulation test of laser welding and submerged arc welding was carried out in MMS-200 thermal simulation test machine using self-made fixtures. The results indicated that the microstructure of laser welding CGHAZ and submerged arc welding CGHAZ was lath martensite and granular bainite, respectively. The impact energy of laser welding CGHAZ was 27 J, and the fracture mode was ductile fracture; the impact energy of submerged arc welding CGHAZ was 7.7 J, and the fracture mode was brittle fracture. The nucleation and propagation mechanism of cracks in different welding modes was established. Microcracks nucleated at the position of dislocation accumulation and remained austenite suppressed crack nucleation in laser welding CGHAZ. The nucleation site was at the M–A constituents in submerged arc welding CGHAZ. The main crack of laser welding CGHAZ was formed by one or a small number of microcracks. The main crack in submerged arc welding CGHAZ was formed by a large number of microcracks. The difference between crack nucleation and propagation mechanism is the reason why the impact energy of laser welding CGHAZ is higher than of submerged arc welding CGHAZ.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Analysis of microstructural facet fatigue failure in ultra-fine grained powder metallurgy Ti-6Al-4V produced through hydrogen sintering

The hydrogen sintering and phase transformation (HSPT) process is a powder metallurgy method that produces Ti-6Al-4V with fatigue properties rivaling wrought processed Ti-6Al-4V. Previous fatigue work on HSPT Ti-6Al-4V has shown failure to be frequently caused by microstructural facets, which were believed to be grain boundary (GB) α phase. This belief conflicts with other reports as fatigue failure typically occurs across α colonies or primary α grains, not GB α. In this work, electron backscattered diffraction is used to identify these facets as GB α. Furthermore, a simple geometric model predicting the effective slip length of GB α is presented.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure and high temperature properties of tungsten processed via electron beam melting additive manufacturing

There is considerable interest in the adoption of additive manufacturing for processing refractory metals. The layer-wise fabrication approach enables opportunities for producing complex geometries which cannot be otherwise be achieved via powder metallurgy. However, the processing science is still in its nascent stages and structure–property relations are relatively unexplored. Fundamental research is needed to further develop the technology and enable the fabrication of refractory metals for high temperature applications. Here we focus on the processing of pure tungsten using electron beam melting additive manufacturing. Experimentally we develop a suitable processing window for achieving high density crack free material. Microstructural analysis reveals that the microstructure generally consists of a columnar structure with a (111) build direction fiber preference, although, fiber switching was observed. Process induced deformation is believed to drive the formation of subgrains whose boundaries exhibit a high dislocation density. Additionally, high temperature tensile testing reveals that the material exhibits excellent properties closer to that of annealed tungsten. Significant mechanical anisotropy was observed to be present which is likely driven by strong crystallographic texture.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Characteristics of Premature Creep Failure in Over-tempered Base Metal of Grade 91 Steel Weldment

Characteristics of premature creep failure in the over-tempered base metal (OT-BM) of a Grade 91 steel weldment are investigated with specially designed creep experiments and advanced microstructure characterization. In situ digital image correlation (DIC) strain measurements reveal that local creep strain as high as 100% accumulated in the OT-BM, compared with only 10% nominal strain over the gauge length. The creep strain rate in the OT-BM is identical to that in the intercritical heat-affected zone and fine-grained heat-affected zone at the secondary creep stage and early tertiary stage, but faster at the late tertiary stage. Microstructural analysis shows that highly recovered microstructure in the OT-BM leads to the lowest hardness, the largest grain size, the lowest fraction of coincidence site lattice boundaries, and the lowest localized strain energy. Dislocation creep and transgranular creep fracture are the dominant deformation and fracture mechanisms in the OT-BM under the current creep testing condition of a low temperature (550 °C) and a high stress (215 MPa).

42 ENGINEERING↗
DOE OSTI2020

Image-driven discriminative and generative machine learning algorithms for establishing microstructure–processing relationships

We investigate methods of microstructure representation for the purpose of predicting processing condition from microstructure image data. A binary alloy that is currently under development as a nuclear fuel was studied for the purpose of developing an improved machine learning approach to image recognition, characterization, and building predictive capabilities linking microstructure to processing conditions. Here, we test different microstructure representations and evaluate model performance based on classification accuracy. A classification accuracy of 95.8% was achieved fordistinguishing between micrographs corresponding to ten different thermo-mechanical material processing conditions.We find that our newly developed microstructure representation describes image data well, and the traditional approachof utilizing area fractions of different phases is insufficient for distinguishing between multiple classes using a relativelysmall, imbalanced original data set of 272 images. To explore the applicability of generative methods for supplementing such limited data sets, generative adversarial networks were trained to generate artificial microstructure images. Two different generative networks were trained and tested to assess performance. Challenges and best practices associated with applying machine learning to limited microstructure image data sets is also discussed. Our work has implications for quantitative microstructure analysis, and development of microstructure-processing relationships in limited data sets typical of metallurgical process design studies.

36 MATERIALS SCIENCE↗