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 667 records · Page 37
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

DE-NE0000724 - Research Performance Final Report - Investigation of Thermal Aging Effects on the Evolution of Microstructure and Mechanical Properties of Cast Duplex Stainless Steels

This report details the research activities carried out under DOE-NEUP award number DE-NE0000724 concerning the evolution of structural and mechanical properties during thermal aging of CF–3 and CF–8 cast duplex stainless steels (CDSS). The overall objective of this project was to use state-of-the-art characterization techniques to elucidate trends and phenomena in the mechanical and structural evolution of cast duplex stainless steels (CDSS) during thermal aging. These steels are commonly used as structural materials in commercial light water nuclear power plants, undergoing aging for decades in operation as cooling water pipes, pump casings, valve bodies, etc. During extended exposure to these conditions, CDSS are known to undergo a change in mechanical properties resulting in a loss of ductility, i.e. embrittlement. While it is generally accepted that structural changes within the ferrite phase, such as decomposition into iron (Fe)-rich and chromium (Cr)-rich domains, lead to the bulk embrittlement of the steels, many questions remain as to the mechanisms of embrittlement at multiple length scales. This work is intended to shed insight into the atomic level composition changes, associated kinetic mechanisms, and effects of changing phase structure on micro- and nano-scale deformation that lead to loss of impact toughness and tensile ductility in these steels. In general, this project provides a route to answer some of these major questions using techniques such as 3-dimensional (3-D) atom probe tomography (APT) and real-microstructure finite element method (FEM) modeling, which were not readily available when these steels were originally selected for service in light water reactors. Mechanical properties evaluated by Charpy V-notch impact testing (CVN), tensile testing, and microhardness and nanohardness measurements were obtained for each condition and compared with the initial baseline properties to view trends in deformation behavior during aging. Concurrent analysis of the microstructure and nanostructure by atom probe tomography (APT) and transmission electron microscopy (TEM) provide mechanistic insight into the kinetic and mechanical behavior occurring on the nano-scale. The presence and morphology of the ferrite, austenite, and carbide phases have been characterized, and formation of new phases during aging, including spinodal decomposition products (α- and α'-ferrite) and G-phase, have been observed. The mechanical and structural characterization have been used to create accurate FEM models based on the real micro- and nano-structures of the systems. These models provide new insight into the local deformation behavior of these steels and the effects of each individual phase (including ferrite, austenite, carbides, and spinodal decomposition products) on the evolving bulk mechanical behavior of the system. The project was divided into three major tasks: 1. Initial Microstructure and Mechanical Property Survey and Initiate Heat Treatment; 2. Microstructural Characterization and Mechanical Property Testing During Aging; and 3. Microstructure-based Finite Element Modeling. Each of these tasks was successfully executed, resulting in reliable data and analysis that add to the overall body of work on the CDSS materials. Baseline properties and aging trends in mechanical data confirm prior observations and add new insights into the mechanical behavior of the steels. Structural characterization on multiple length scales provides new information on phase changes occurring during aging and sheds light on the kinetic processes occurring at the atomic scale. Furthermore, a combination of mechanical testing and microstructural characterization techniques was utilized to design FEM models of local deformation behavior of the ferrite and austenite phases, providing valuable new information regarding the effects of each of the microstructural components on the hardening and embrittlement processes. The data and analysis presented in this report and the publication associated with this project (§V) increase the understanding of aging and deformation in CF–3 and CF–8 steels. These results provide valuable information that can be utilized to aid in making informed decisions regarding the ongoing use of these steels in commercial nuclear infrastructure.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2022

Preliminary benchmarks and analysis of boundary conditions in a trenched microstructured silicon radiation detector

Microstructured neutron detectors have the benefit of enhanced neutron detection efficiency as compared to planar devices, achieved by etching 6 LiF-filled trenches on the top surface of a silicon PIN diode. This sensor geometry results in a complex electric field distribution and depletion characteristics within the diode under reverse bias. For the first time on record, the effects of a fixed oxide charge on the microstructured device depletion characteristics and mobile carrier transport is investigated. Prototype detectors were fabricated with non-conformal surface doping. Capacitance voltage and current voltage measurements were performed for these prototypes and compared with COMSOL Multiphysics simulations. A spectral response from an 241Am alpha particle source was acquired and analyzed. It was found that monoenergetic alpha particles produce three prominent peaks in the pulse height spectrum output by the device. The peaks were confirmed by simulations to correlate with dead layers and incident trajectories into the microstructure. It was also found that significant differences in pulse rise time result, corresponding with events arriving in a low-field region in the fins and a high-field region in the bulk. Geant4 was utilized for radiation transport, interaction modeling, and benchmarking the spectral data. The results of this simulation work provide confidence in the ability to attain and benchmark electrical characteristics and spectral data for semiconductor radiation detectors employing complex microstructures.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2014

Resonant x-ray reflectivity study of partial decomposed boron nitride thin films using Indus-1 synchrotron

We determined the microstructural parameters and chemical composition profile of partial decomposed boron nitride thin films using x-ray reflectivity near the respective absorption edges. The elemental specificity and optical contrast variation properties of the resonant effect are utilized to combine chemical analysis with physical microstructure of thin films from x-ray scattered intensities. We demonstrated these aspects through calculations and experiments in the soft x-ray region near the boron K-absorption edge.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

The Influence of Nominal Composition on the Microstructure, Tensile Properties, and Weldability of Cast Monel Alloys

Cast Monel alloys are used in many industrial applications that require a combination of good mechanical properties and excellent resistance to corrosion. Despite relative widespread use, there has been limited prior research investigating the fundamental composition–structure–property relationships. Here in this work, microstructural characterization, thermal analysis, electron probe microanalysis, tensile testing, and Varestraint testing were used to assess the effects of variations in nominal composition on the solidification path, microstructure, mechanical properties, and solidification cracking susceptibility of cast Monel alloys. It was found that Si segregation caused the formation of silicides at the end of solidification in grades containing at least 3 wt pct Si. While increases to Si content led to significant improvements in strengthening due to the precipitation of β 1 -Ni 3 Si, the silicide eutectics acted as crack nucleation sites during tensile loading which severely reduced ductility. The solidification cracking susceptibility of low-Si Monel alloys was found to be relatively low. However, increases to Si concentration and the onset of associated eutectic reactions increased the solidification temperature range and drastically reduced cracking resistance. Increases in the Cu and Mn concentrations were found to reduce the solubility limit of Si in austenite which promoted additional eutectic formation and exacerbated the reductions in ductility and/or weldability.

36 MATERIALS SCIENCE↗
DOE OSTI2017

The α–ω phase transition in shock-loaded titanium

Here, we present a series of experiments probing the martensitic α–ω (hexagonal close-packed to simple hexagonal) transition in titanium under shock-loading to peak stresses around 15 GPa. Gas-gun plate impact techniques were used to locate the α–ω transition stress with a laser-based velocimetry diagnostic. A change in the shock-wave profile at 10.1 GPa suggests the transition begins at this stress. A second experiment shock-loaded and then soft-recovered a similar titanium sample. We then analyzed this recovered material with electron-backscatter diffraction methods, revealing on average approximately 65% retained ω phase. Furthermore, based on careful analysis of the microstructure, we propose that the titanium never reached a full ω state, and that there was no observed phase-reversion from ω to α. Texture analysis suggests that any α titanium found in the recovered sample is the original α. The data show that both the α and ω phases are stable and can coexist even though the shock-wave presents as steady-state, at these stresses.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Virtual texture analysis to investigate the deformation mechanisms in metal microstructures at the atomic scale

Understanding the deformation behavior of metallic materials at high strain rates requires the characterization of plasticity contributors such as twins, phase transformed regions, and dislocations. However, predicting the contributions from phase transformation and twinning relies on a complete understanding of the selection of variants for various loading orientations and the evolution of their volume fractions. This manuscript presents a new virtual texture (VirTex) analysis approach to characterize phase transformation and twinning variants in deformed microstructures generated using molecular dynamics (MD) simulations. Furthermore, the VirTex method involves the construction of a rotation matrix to calculate the angle/axis pairs and misorientation angles for each atom in the microstructure. Any changes in the orientation angle from angle/axis pairs and/or structure types are analyzed to determine the nucleation and evolution of variants in the microstructure. The study uses shock deformed single-crystal Fe, Ta, and Cu to analyze the variant selections for phase transformation or twinning or both in BCC and FCC systems. In addition, the VirTex analysis is able to characterize the phase transformation and twinning variants in nanocrystalline Fe and Ta microstructures. Besides characterizing variants, orientation mapping also provides an accelerated and on-the-fly approach for quantifying twin fractions in MD microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Phase transformations in a Cu−Cr alloy induced by high pressure torsion

Phase transformations induced by high pressure torsion (HPT) at room temperature in two samples of the Cu-0.86 at.% Cr alloy, pre-annealed at 550 °C and 1000 °C, were studied in order to obtain two different initial states for the HPT procedure. Observation of microstructure of the samples before HPT revealed that the sample annealed at 550 °C contained two types of Cr precipitates in the Cu matrix: large particles (size about 500 nm) and small ones (size about 70 nm). The sample annealed at 1000 °C showed only a little fraction of Cr precipitates (size about 2 μm). The subsequent HPT process resulted in the partial dissolution of Cr precipitates in the first sample and dissolution of Cr precipitates with simultaneous decomposition of the supersaturated solid solution in another. However, the resulting microstructure of the samples after HPT was very similar from the standpoint of grain size, phase composition, texture analysis and hardness measurements. - Highlights: • Cu−Cr alloy with two different initial states was deformed by HPT. • Phase transformations in the deformed materials were studied. • SEM, TEM and X-ray diffraction techniques were used for microstructure analysis. • HPT leads to formation the same microstructure independent of the initial state.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effects of CeO{sub 2} on the Microstructure and Properties of Laser Cladding 316L Coating

Laser cladding was used to distribute a CeO{sub 2}-modified 316L powder coating onto a 316L stainless steel surface. The cladding layer phase composition was evaluated through x-ray diffraction. An analysis of the microstructure was conducted using an optical microscope and scanning electron microscope, while the micro-hardness was measured using a tester. The coating corrosion behavior in response to 3.5% NaCl solution was analyzed by polarization curves and electrochemical impedance spectroscopy. Finally, the overall performance of coatings with different CeO{sub 2} concentrations, 1, 2, and 3%, was compared. Results showed that adding CeO{sub 2} significantly refined the grains, reduced the coating porosity, and effectively limited the appearance of local corrosion. Also, additive CeO{sub 2} shifted the coating’s electrode potential in a positive direction, minimizing the current density of corrosion, creating a stable passivation film, and improving the coating’s corrosion resistance. The coating performance (hardness and corrosion behavior) was optimal when 2% CeO{sub 2} was employed as the powder mass.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Improved measurement of thermal effects on microstructure

The objectives were to introduce a simple methodology which could be used to replace the time-consuming and expensive conventional methods of metallographic and quantitative analysis of thermal treatment effect on microstructure. Metallurgical analysis continually calls for the evaluation of thermal treatment effects on microstructure. This commonly demands metallographic sample preparation and microscopic examination, which are time absorbing and costly. These drawbacks are burdensome when large numbers of samples must be levied fast. Mechanical testing can sometimes be substituted, but sample size and shape frequently make these methods impractical. The experiment described here is ideal for the microstructural evaluation of lamp filaments and other wire samples such as copper wire which can be conveniently coiled.

Rastani, Mansur↗
DOE OSTI2025

Generalizable Image Segmentation for Microstructure Characterization Through Integrated SEM and EBSD Analysis

We demonstrate generalizable semantic segmentation using minimal ground truth data. Correlated scanning electron microscopy (SEM) images and electron backscatter diffraction (EBSD) measurements of frictionstir processed 316L stainless steel plates were used to train deep learning models for grain boundary segmentation. Secondary electron (SE) imaging taken at an accelerating voltage of 10 keV correlated to EBSD-derived grain boundaries produced the best performing model. Notably, an ensemble of three models trained on a single SE image produced accurate segmentation over a series of BSE images of samples manufactured under different processing parameters, with a resultant mean absolute error in grain size of 0.34 µm. The striking generalizability of the models likely results from the similar escape depths of the SE training input and the EBSD training output and the reduced probability of dislocation artifacts appearing in the image. This finding highlights the importance of considering the physical principles behind imaging in the development of robust segmentation models for microstructure characterization.

Taufique, Mohammad Fuad Nur↗
DOE OSTI2024

High throughput automated characterization of enamel microstructure using synchrotron tomography and optical flow imaging

The remarkable damage-tolerance of enamel has been attributed to its hierarchical microstructure and the organized bands of decussated rods. A thorough characterization of the microscale rod evolution within the enamel is needed to elucidate this complex structure. While prior efforts in this area have made use of single particle tracking to track a single rod evolution to various degrees of success, such a process can be both computationally and labor intensive, limited to the evolution path of a single rod, and is therefore prone to error from potentially tracking outliers. Particle image velocimetry (PIV) is a well-established algorithm to derive field information from image sequences for processes that are time-dependent, such as fluid flows and structural deformation. In this work, we demonstrate the use of PIV in extracting the full-field microstructural distribution of rods within the enamel. Further, enamel samples from a wild African lion were analyzed using high-energy synchrotron X-ray micro-tomography. Results from the PIV analysis provide sufficient full-field information to reconstruct the growth of individual rods that can potentially enable rapid analysis of complex microstructures from high resolution synchrotron datasets. Such information can serve as a template for designing damage-tolerant bioinspired structures for advanced manufacturing.

36 MATERIALS SCIENCE↗
DOE OSTI2021

MOSAIC: An Effective FFT-based Numerical Method to Assess Aging Properties of Concrete

As the nuclear fleet in the United States ages and subsequent license renewal applications grow, the prediction of concrete durability at extended operation becomes more important. To address this issue, a Fast-Fourier Transform (FFT) method is utilized to simulate aging-related degradation of concrete within the Microstructure Oriented Scientific Analysis of Irradiated Concrete (MOSAIC) software. MOSAIC utilizes compositional phase maps to simulate damage from radiation-induced volumetric expansion (RIVE), applied force, creep, and thermal expansion. This compositional detail allows each mineral in the microstructure to be assigned specific material properties, allowing the simulation to be as accurate and representative as possible. The principal goal of MOSAIC is to simulate the effects of nonlinear aging mechanisms occurring in nuclear concrete on the macroscopic mechanical properties, using only the aggregate microstructure compositional information as a starting point. Here, several realistic example simulations are shown to demonstrate the utility and uniqueness of the MOSAIC software.

36 MATERIALS SCIENCE↗
DOE OSTI2025

In-situ synchrotron X-ray study on microstructure and stress evolutions of electroplated copper upon self-annealing

Background: The self-annealing behavior of electroplated copper (Cu) at room temperature is gaining attention in the microelectronics industry due to its significant impact on reliability issues such as substrate warpage and electrical resistivity. Methods: In this study, in-situ analysis of the microstructure transition and stress relaxation of the electroplated copper upon self-annealing was conducted via synchrotron white X-ray nanodiffraction (beamline 21A, Taiwan Photon Source) and grazing-incidence X-ray diffraction (beamline 17B1, Taiwan Light Source). Significant Findings: Remarkable relaxations of deviatoric stress and absolute strain component along the [002] direction were closely related to the Cu grain growth and crystallographic reorientation at the early stage of selfannealing, and a complete stress/strain relaxation can be achieved with the cessation of microstructure transition. In conclusion, the in-situ synchrotron X-ray studies provided an insight into Cu self-annealing mechanism, offering valuable information for improving Cu interconnect reliability.

Cu Self-annealing↗
DOE OSTI2023

Anisotropic spall failure of additively manufactured 316L stainless steel

The dynamic high strain rate tensile (spall) failure of additively manufactured (AM) materials is an area of great interest but much less understood than material failure under other loading regimes. The research presented here examines the effects of microstructure anisotropy in 316L stainless steel fabricated by laser powder bed fusion (LPBF) on its spall failure and properties. In this work, plate-on-plate impact experiments were performed using an 80-mm gas gun to investigate the spall behavior of AM fabricated sample discs with impact along the perpendicular and parallel orientations relative to build directions. Experiments were also performed on wrought 316L stainless steel as baseline material with uniform equiaxed grain microstructure for comparison with the AM material of same composition. The spall experiments involved free-surface velocity profiles measured using Photon Doppler Velocimetry (PDV) to capture the spall pull-back signals, combined with post-mortem analysis of the microstructure of soft-recovered impacted samples. In the case of AM samples, spall failure initiated preferentially at melt pool boundaries in both impact directions. The spall plane location and spall strength, however, were both heavily influenced by the orientation of the impact direction relative to the build direction in the AM samples. The spall behavior is also observed to be more complex in the samples impacted perpendicular to the build (through-thickness) direction, due in large part to the orientation of the microstructural features such as melt pool boundaries, laser scan tracks, and general grain morphology.

36 MATERIALS SCIENCE↗
NASA NTRS2004

Brazing SiC/SiC Composites to Metals

Experiments have shown that active brazing alloys (ABAs) can be used to join SiC/SiC composite materials to metals, with bond strengths sufficient for some structural applications. The SiC/SiC composite coupons used in the experiments were made from polymerbased SiC fiber preforms that were chemical-vapor-infiltrated with SiC to form SiC matrices. Some of the metal coupons used in the experiments were made from 304 stainless steel; others were made from oxygen-free, high-conductivity copper. Three ABAs were chosen for the experiments: two were chosen randomly from among a number of ABAs that were on hand at the time; the third ABA was chosen because its titanium content (1.25 percent) is less than those of the other two ABAs (1.75 and 4.5 percent, respectively) and it was desired to evaluate the effect of reducing the titanium content, as described below. The characteristics of ABAs that are considered to be beneficial for the purpose of joining SiC/SiC to metal include wettability, reactivity, and adhesion to SiC-based ceramics. Prior to further development, it was verified that the three chosen ABAs have these characteristics. For each ABA, suitable vacuum brazing process conditions were established empirically by producing a series of (SiC/SiC)/ABA wetting samples. These samples were then sectioned and subjected to scanning electron microscopy (SEM) and energy-dispersive x-ray spectrometry (EDS) for analysis of their microstructures and compositions. Specimens for destructive mechanical tests were fabricated by brazing of lap joints between SiC/SiC coupons 1/8-in. (.3.2- mm) thick and, variously, stainless steel or copper tabs. The results of destructive mechanical tests and the SEM/EDS analysis were used to guide the development of a viable method of brazing the affected materials.

Steffier, Wayne S.↗
DOE OSTI2016

Understanding to Hierarchical Microstructures of Crab (Chinese hairy) Shell as a Natural Architecture

This work was done to better understand the microstructures, composition and mechanical properties of Chinese hairy crab shell. For fully revealing its hierarchical microstructure, the crab shell was observed with electron microscope under different magnifications from different facets. XRD, EDS, FTIR and TGA techniques have been used to characterize the untreated and chemically-treated crab shells, which provided enough information to determine the species and relative content of components in this biomaterial. Combined the microstructures with constituents analysis, the structural principles of crab shell was detailedly realized from different structural levels beyond former reports. To explore the relationship between structure and function, the mechanical properties of shell have been measured through performing tensile tests. The contributions of organics and minerals in shell to the mechanical properties were also discussed by measuring the tensile strength of de-calcification samples treated with HCl solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2017

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Ceramics↗