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 1,585 records · Page 88
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Formation of the {gamma}ʹʹʹ-Ni2(Cr, Mo, W) phase during a two-step aging heat treatment in HAYNES® 244® Alloy

Precipitation hardening is the dominant method of achieving high strength in most Ni-based superalloys. The formation of nanoscale precipitates during thermal exposure is often studied to determine the optimal methods of attaining high strength. The commercial Ni-based superalloy, HAYNES® 244® alloy, is strengthened through a novel -Ni2(Cr, Mo, W) intermetallic phase that forms during a two-step aging cycle. The precipitation kinetics of this intermetallic phase are sluggish for single-step aging in comparison to the γʹ phase in precipitation-strengthened Ni-based alloys, but a two-step aging treatment has shown to reliably harden the alloy and improve high-temperature properties compared to a single-step aging heat treatment. To investigate the formation and coarsening of this phase, heat-treated samples of the 244 alloy were analyzed with high-energy in situ and ex situ X-ray techniques such as small angle X-ray scattering and wide angle X-ray scattering as well as Vickers micro-hardness, electron microscopy, and atom probe tomography. The relationship between hardness, aging parameters, and microstructure evolution is discussed. The enthalpy of formation and precipitate solvus temperature were determined with high-temperature differential scanning calorimetry and dilatometry analysis.

Ni-based Superalloys↗
DOE OSTI2018

Optimization of Process Parameters for the Axial Distortion and Distortion Range During Die Quenching of a Spiral Bevel Gear

The strength of high-duty gears can be improved by carburizing and quenching processes. Quenching distortion is inevitable during the process, and it has direct effects on the precision of the gear. For spiral bevel gear with big diameter and small thickness, die quenching process is applied in the manufacturing to control the distortion in axial direction. Die quenching parameters must be optimized to minimize the distortion while considering non-uniformity of chemical compositions and loads. In this paper, material models of gear material (22CrMoH) built based on the phase transformation kinetics, static mechanical properties and phase transformation plasticity equations. Finite element analysis (FEA) models are conducted to study the whole die quenching process based on the production process. Die quenching experiments and testing of microstructures and distortions are conducted to verify the accuracy of the FEA models. The effects of loads and bottom die obliquity on the final distortion are studied to set the appropriate range and control distortion. The distortion was very sensitive to the bottom die obliquity and some part of load ranges. The distortion changes little when the load of inner die was in the range of 1.38-2.07 MPa and the load of outer die was in the range of 2.07-2.76 MPa. The distortion range is fitted the production requirements by setting the inclination angle of bottom die between 0.12° and 0.29°.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Lead sheathing of ship hulls in the Roman period: Archaeometallurgical characterisation

An archaeometallurgical analysis of samples of lead sheathing from five ships of the Roman period was carried out in order to determine their composition and microstructure, and to obtain a better understanding of their manufacturing processes. The examinations included optical microscopy of metallographic cross-sections, microhardness tests, scanning electron microscopy, including energy dispersive spectroscopy, and X-ray photoelectron spectroscopy. The results show that the samples were all composed of lead covered with an oxide layer. The sheet thicknesses, microhardness values and microhardness distribution, as well as the grain size distribution, led to the conclusion that all of the sheets were produced by the same technology, using hammering, and were probably used for the same purpose. The presence of antimony was observed in the sample from the Roman ship from Caesarea, which may hint at an Italian (Sardinian) origin of the material, and perhaps of the ship. - Research Highlights: {yields} During the Roman period ship hulls were sheathed with lead. {yields} Five samples have been analysed for their characteristics and manufacturing process. {yields} The process was cold-working (strain-hardening) using hammering. {yields} The lead was open-casted on a flat stone, and later hammered at room temperature. {yields} Antimony in the Caesarea shipwreck may indicate an Italian origin of construction.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Abnormal grain growth in AISI 304L stainless steel

The microstructural evolution during abnormal grain growth (secondary recrystallization) in 304L stainless steel was studied in a wide range of annealing temperatures and times. At relatively low temperatures, the grain growth mode was identified as normal. However, at homologous temperatures between 0.65 (850 °C) and 0.7 (900 °C), the observed transition in grain growth mode from normal to abnormal, which was also evident from the bimodality in grain size distribution histograms, was detected to be caused by the dissolution/coarsening of carbides. The microstructural features such as dispersed carbides were characterized by optical metallography, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, and microhardness. Continued annealing to a long time led to the completion of secondary recrystallization and the subsequent reappearance of normal growth mode. Another instance of abnormal grain growth was observed at homologous temperatures higher than 0.8, which may be attributed to the grain boundary faceting/defaceting phenomenon. It was also found that when the size of abnormal grains reached a critical value, their size will not change too much and the grain growth behavior becomes practically stagnant. - Highlights: • Abnormal grain growth (secondary recrystallization) in AISI 304L stainless steel • Exaggerated grain growth due to dissolution/coarsening of carbides • The enrichment of carbide particles by titanium • Abnormal grain growth due to grain boundary faceting at very high temperatures • The stagnancy of abnormal grain growth by annealing beyond a critical time.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Revealing the nanostructure of calcium phosphate coatings using HRTEM/FIB techniques

Herein, we report on the micro- and nanostructure of the calcium phosphate coating produced by pulsed laser deposition (PLD), using focused ion beam (FIB) lamella sample preparation and transmission electron microscopy (TEM) as the characterization technique. The initial selected area electron diffraction (SAED) data demonstrated the presence of hydroxyapatite (HA) over any other possible calcium phosphate crystalline structure and the polycrystalline nature of the coating. Moreover, the SAED analyses showed clear textured ring patterns coherent with the presence of a preferred orientation in the HA nano-crystal growth. The SAED data also indicated that the coating appears to be textured in the 〈002〉 crystalline direction. Dark-field images obtained using 002 as the working reflection showed a clear oriented crystal growth in columns, from bottom to top. These columns have a peculiar arrangement of nano-crystals since, in some cases, the preferred orientation appears to start at a certain distance from the substrate. Direct d-spacing measurements on high-resolution TEM images provided further proof of the presence of an HA nano-crystal structure. The reported data may be of interest in the future to adjust the microstructure of the HA coatings. - Highlights: •The FIB lift-out technique allows a very site-specific sample preparation method for HRTEM analysis. •It also permits a fast assessment of the HA coating thickness and elemental composition (EDS). •The coatings exhibit a nano-crystalline nature, with a texturing effect along the 002 planes. •PLD is suitable for the production of crystalline c-axis oriented hydroxyapatite coatings. •The crystalline HA phase in the PLD coating is very similar to the present in bone.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Initial examination of fuel compacts and TRISO particles from the US AGR-2 irradiation test

Post-irradiation examination was completed on two as-irradiated compacts from the US Advanced Gas Reactor Fuel Development and Qualification Program’s second irradiation test. These compacts were selected for examination because there were indications that they may have contained particles that released cesium through a failed or defective SiC layer. The coated particles were recovered from these compacts by electrolytic deconsolidation of the surrounding graphitic matrix in nitric acid. The leach-burn-leach (LBL) process was used to dissolve and analyze exposed metallic elements (actinides and fission products), and each particle was individually surveyed for relative cesium retention with the Irradiated Microsphere Gamma Analyzer (IMGA). Data from IMGA and LBL examinations provided information on fission product release during irradiation and whether any specific particles had below-average retention that could be related to coating layer defects or radiation-induced degradation. A few selected normal-retention particles and six with abnormally-low cesium inventory were analyzed using X-ray tomography to produce three-dimensional images of the internal coating structure. Four of the low-cesium particles had obviously damaged or degraded SiC, and X-ray imaging was able to guide subsequent grinding and polishing to expose the regions of interest for analysis by optical and electron microscopy. Additional particles from each compact were also sectioned and examined to study the overall radiation-induced microstructural changes in the kernel and coating layers.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Tuning gas separation performance of polyimide membranes with macrocyclic crown ether units

Membrane-based gas separation is an energy-efficient alternative to conventional thermally-driven separation processes. However, polymer membranes face the permeability-selectivity trade-off challenge, which stems from the broad size distribution of free volume voids. Here, this study reports a molecular design strategy to address this challenge through incorporating macrocyclic crown ether (CE) moieties into the backbone of Matrimid® polyimide, a commercial gas separation membrane. A series of CE-containing Matrimid®-like copolyimides were synthesized with systematically varied CE molar contents ranging from 3 to 20%. These copolyimides formed ductile, defect-free thin films suitable for membrane fabrication. Gas permeation tests revealed a non-monotonic relationship between permeability/selectivity and CE content. Notably, the copolyimide with only 5% CE demonstrated a 61% increase in CO 2 /CH 4 selectivity and a 13% increase in CO 2 permeability relative to pristine Matrimid®. Higher CE contents did not yield further performance improvements, which is likely due to the competing effects of chain packing disruption and π–π interactions among CE moieties at high content. This hypothesis was supported by wide-angle X-ray scattering (WAXS) analysis, density measurements, and fractional free volume calculations. These findings highlight the potential of macrocyclic crown ether incorporation strategies in fine tuning the microstructure of commercial polyimide gas separation membranes to surpass the traditional permeability-selectivity trade-off.

CO2 separation↗
DOE OSTI2021

Effect of heat treatments on superconducting properties and connectivity in K-doped BaFe2As2

Abstract Fe-based superconductors and in particular K-doped BaFe 2 As 2 (K-Ba122) are materials of interest for possible future high-field applications. However the critical current density ( J c ) in polycrystalline Ba122 is still quite low and connectivity issues are suspected to be responsible. In this work we investigated the properties of high-purity, carefully processed, K-Ba122 samples synthesized with two separate heat treatments at various temperatures between 600 and 825 °C. We performed specific heat characterization and T c -distribution analysis up to 16 T and we compared them with magnetic T c and J c characterizations, and transmission-electron-microscopy (TEM) microstructures. We found no direct correlation between the magnetic T c and J c , whereas the specific heat T c -distributions did provide valuable insights. In fact the best J c -performing sample, heat treated first at 750 °C and then at 600 °C, has the peak of the T c -distributions at the highest temperatures and the least field sensitivity, thus maximizing H c2 . We also observed that the magnetic T c onset was always significantly lower than the specific heat T c : although we partially ascribe the lower magnetization T c to the small grain size (< λ , the penetration depth) of the K-Ba122 phase, this behaviour also implies the presence of some grain-boundary barriers to current flow. Comparing the T c -distribution with J c , our systematic synthesis study reveals that increasing the first heat treatment above 750 °C or the second one above 600 °C significantly compromises the connectivity and suppresses the vortex pinning properties. We conclude that high-purity precursors and clean processing are not yet enough to overcome all J c limitations. However, our study suggests that a higher temperature T c -distribution, a larger H c2 and a better connectivity could be achieved by lowering the second heat treatment temperature below 600 °C thus enhancing, as a consequence, J c .

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

Enhanced thermal conductivity of polycrystalline aluminum nitride thin films by optimizing the interface structure

The growth-temperature dependency and interface structure effects on the thermal conductivity of the highly textured AlN thin films on (001) Si substrates were systematically studied by characterizing the crystal structures, surface morphologies, interface structures, chemical compositions, and thermal conductivity using x-ray diffraction analysis, atomic force microscopy, high resolution transmission electron microscopy, x-ray photoelectron spectroscopy, and 3-omega method, respectively. By optimizing the interface microstructure and the growth temperature, thermal conductivity of polycrystalline AlN thin films can be greatly enhanced from 9.9 to 26.7 W/mK, when the growth temperature increases from 330 to 560 Degree-Sign C. This achievement is considered to be associated with the diminishment of the amorphous and disordered layer at the AlN/Si interface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Focused acoustic beam imaging of grain structure and local Young's modulus with Rayleigh and surface skimming longitudinal waves

The interaction of a focused acoustic beam with materials generates Rayleigh surface waves (RSW) and surface skimming longitudinal waves (SSLW). Acoustic microscopic investigations have used the RSW amplitude and the velocity measurements, extensively for grain structure analysis. Although, the presence of SSLW has been recognized, it is rarely used in acoustic imaging. This paper presents an approach to perform microstructure imaging and local elastic modulus measurements by combining both RSW and SSLW. The acoustic imaging of grain structure was performed by measuring the amplitude of RSW and SSLW signal. The microstructure images obtained on the same region of the samples with RSW and SSLW are compared and the difference in the contrast observed is discussed based on the propagation characteristics of the individual surface waves. The velocity measurements are determined by two point defocus method. The surface wave velocities of RSW and SSLW of the same regions of the sample are combined and presented as average Young's modulus image.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Experimental and theoretical examination of shock-compressed copper through the fcc to bcc to melt phase transitions

Recent studies show a face-centered cubic (fcc) to body-centered cubic (bcc) transformation along the shock Hugoniot for several metals (i.e., Cu, Au, and Ag). Here, we combine laser-shock compression of Cu foils on nanosecond timescales with in situ x-ray diffraction (XRD) to examine the microstructural changes with stress. We study the fcc phase and the phase transition from fcc to bcc (pressures greater than 180 GPa). Textural analysis of the azimuthal intensities from the XRD images is consistent with transformation into the bcc phase through the Pitsch-distortion mechanism. We use embedded atom model molecular dynamics simulations to determine the stability of the bcc phase in pressure–temperature space. Finally, our results indicate that the bcc phase is stabilized only at high temperatures and remains stable at pressures greater than 500 GPa.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Decoding diffraction and spectroscopy data with machine learning: A tutorial

This Tutorial provides a step-by-step guide on how to apply supervised machine-learning techniques to analyze diffraction and spectroscopy data. This Tutorial details four models—a reconstruction-focused model, a regression-focused model, a hybrid reconstruction/regression model, and a multimodal model—that use x-ray diffraction profiles and vibrational density of states spectra to predict various microstructural descriptors. In this Tutorial, we cover data pre-processing steps, constructions of the models via dimensionality reduction and regression, training, and analysis of these models. Comparisons of the model’s performance are provided, highlighting the strength and weakness of the various approaches utilized.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding Complex Magnetic Spin Textures with Simulation-Assisted Lorentz Transmission Electron Microscopy

There is an increased interest in topologically nontrivial magnetic spin textures such as skyrmions and chiral domain-wall solitons, both from a point of fundamental physics understanding as well as potential technological interest in low-power memory applications. In order to control their behavior, it is necessary to understand their complex spin texture at the nanoscale. Lorentz transmission electron microscopy (LTEM) is a suitable technique for studying these systems due to its high spatial resolution and capability to simultaneously characterize magnetic texture and microstructure. In this work, we present the application of PyLorentz, an open-source software suite that we have developed, for quantitative image analysis of Neel-type skyrmions in thin-film heterostructures. PyLorentz enhances LTEM capabilities by enabling reconstruction of magnetic induction maps from experimental images, as well as simulating LTEM images using micromagnetic simulation data. We demonstrate this for simulated Neel skyrmions as well as experimental data from [Pt/Co/W] multilayer heterostructures. Finally, we also show how simulation-assisted LTEM analysis is crucial for understanding these complex magnetic spin textures, in which the reconstructed magnetic induction map (seen in the LTEM images) differs significantly from the magnetization configuration.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Predicting and Controlling Corrosion (Abbreviated Final Report)

Corrosion accumulates significant replacement costs in the transportation, utility, manufacturing, and infrastructure sectors. It also underpins several of LLNL’s core missions in stockpile stewardship, defense, and energy security. Whereas most corrosion and aging models are empirically parameterized to describe well-defined conditions late in the reaction, the factors that determine the early stages of corrosion—during which mitigation could be most impactful— are poorly understood. This project addressed the critical need for new approaches to predict the kinetics of corrosion initiation based on firm physical and chemical understanding. The activities encompassed degradation of relevant metals in both hydrogen-rich and environmental corrosion scenarios. The team integrated state-of-the-art multiscale simulation, in situ characterization, and data science within three technical thrusts: hydriding of Ti alloys; aqueous corrosion of Al and Ni-Cr alloys; and degradation of additively manufactured 316L stainless steel. In each case, novel capabilities were developed to identify and track the impacts of key atomistic, compositional, and microstructural features on the metal systems. For hydriding, protocols were developed to tightly integrate multiscale models, advanced multimodal characterization, and machine learning to determine how hydrogen interacts with native passivating surface oxides and nucleates new undesired phases, shedding new light on the critical role of grain boundaries, interfaces, and atomically disordered regions. For aqueous corrosion, the project demonstrated methods to predict dissolution rates of metal surfaces in corrosive solutions, to measure and understand microstructural and grain orientation effects on corrosion susceptibility, and to investigate competing growth and dissolution kinetics of surface oxides. For additively manufactured metals, analysis using state-of-the-art microscopy techniques revealed the role of specific heterogeneities invoked during laser processing, including cellular structure, dislocations, and precipitates, on corrosion susceptibility. In addition to new capabilities and understanding, the project provided an avenue for workforce development, as well as key partnerships with stakeholders in corrosion science.

08 HYDROGEN↗
DOE OSTI2016

Initial examination of fuel compacts and triso particles from the US AGR-2 irradiation test - 18443

Post-irradiation examination was completed on two as-irradiated compacts from the US Advanced Gas Reactor Fuel Development and Qualification Program's second irradiation test. These compacts were selected for examination due to indications that they may have contained particles that released cesium due to a failed or defective SiC layer. The coated particles were recovered from these compacts by electrolytic deconsolidation of the surrounding graphitic matrix in nitric acid. The leach-burn-leach (LBL) process was used to dissolve and analyze exposed metallic elements (actinides and fission products), and each particle was individually surveyed for relative cesium retention with the Irradiated Microsphere Gamma Analyzer (IMGA). Data from IMGA and LBL examinations provided information on fission product release during irradiation and whether any specific particles had below-average retention that could be related to coating layer defects or radiation-induced degradation. A few selected normal-retention particles and six with abnormally-low cesium inventory were analyzed using x-ray tomography to produce three-dimensional images of the internal coating structure. Four of the low-cesium particles had obviously damaged or degraded SiC, and x-ray imaging was able to guide subsequent grinding and polishing to expose the regions of interest for analysis by optical and electron microscopy. Additional particles from each compact were also sectioned and examined to study the overall radiation-induced microstructural changes in the kernel and coating layers. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2013

Synthesis of porous sheet-like Co{sub 3}O{sub 4} microstructure by precipitation method and its potential applications in the thermal decomposition of ammonium perchlorate

Porous sheet-like cobalt oxide (Co{sub 3}O{sub 4}) were successfully synthesized by precipitation method combined with calcination of cobalt hydroxide precursors. The structure, morphology and porosity properties of the products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption-desorption measurement. The as-prepared sheet-like microstructures were approximately 2-3 {mu}m in average diameter, and the morphology of the cobalt hydroxide precursors was retained after the calcination process. However, it appeared a large number of uniform pores in the sheets after calcination. In order to calculate the potential catalytic activity, the thermal decomposition of ammonium perchlorate (AP) has been analyzed, in which cobalt oxide played a role of an additive and the porous sheet-like Co{sub 3}O{sub 4} microstructures exhibited high catalytic performance and considerable decrease in the thermal decomposition temperature of AP. Moreover, a formation mechanism for the sheet-like microstructures has been discussed. - Graphical abstract: Porous sheet-like Co{sub 3}O{sub 4} were synthesized by facile precipitation method combined with calcination of {beta}-Co(OH){sub 2} precursors. Thermogravimetric-differential scanning calorimetric analysis indicates potential catalytic activity in the thermal decomposition of ammonium perchlorate. Highlights: Black-Right-Pointing-Pointer Synthesis of sheet-like {beta}-Co(OH){sub 2} precursors by precipitation method. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} were obtained by calcining {beta}-Co(OH){sub 2} precursors. Black-Right-Pointing-Pointer The possible formation mechanism of porous sheet-like Co{sub 3}O{sub 4} has been discussed. Black-Right-Pointing-Pointer Porous sheet-like Co{sub 3}O{sub 4} decrease the thermal decomposition temperature of ammonium perchlorate.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Nonlinear modeling and performance analysis of cracked beam microgyroscopes

Cracks constitute a common structural defect in microelectromechanical systems that may arise during manufacturing, mechanical fatigue, or shock loading. Areas weakened by cracks increase the flexibility of the microstructure. Furthermore, depending on the crack severity, the increased flexibility can cause dramatic changes in the static and dynamic behaviors of electrically actuated MEMS. In this study, a numerical investigation of the depth and location of multiple edge cracks on the performance of beam microgyroscopes is conducted. Applying the Griffith strain energy release theorem for an edge crack, the vibrational characteristics of microgyroscopes with multiple cracks including the static deflection, natural frequencies, and mode shapes are studied analytically. Then, the differential quadrature method is employed to model the nonlinear dynamic behaviors of the cracked gyroscope system. Cracks initiated along the driving or sensing directions of the microgyroscope are found to have differing effects on its nonlinear dynamic response. This numerical study reveals that the onset of severe single cracks or a series of multiple cracks can significantly affect the sensitivity of the microgyroscope to base rotations and therefore leads to a degradation in the performance of the damaged MEMS sensor. This study also shows that a potential design approach for broadband microgyroscope systems manufactured with cracks can be proposed.

42 ENGINEERING↗
DOE OSTI2024

Analysis of radially resolved thermal conductivity in high burnup mixed oxide fuel and comparison to thermal conductivity correlations implemented in fuel performance codes

The thermal diffusivity and thermal conductivity of high burnup (19 % FIMA) mixed oxide (U, Pu)O 2 nuclear fuel has been measured along the radial direction using a thermoreflectance-based method. Measured thermal conductivity exhibits a notable radial variation consistent with the expectations that a large temperature gradient across the annular fuel pellet leads to a heterogeneous microstructure. A common fuel performance model of thermal conductivity, the Lucuta-Inoue model, is used to analyze the measured thermal conductivity profile. Further, this model adequately captures the radial dependence of thermal conductivity except in the periphery. The analysis suggests that the characteristic radial shape of the thermal conductivity profile follows the burnup profile within the fuel pin. In the periphery, the high burnup structure is formed and the conductivity model, not capturing this effect, likely overestimates the thermal conductivity.

36 MATERIALS SCIENCE↗