Search NASA⌕ Search

SEARCH · Search NASA

Results for “Optical microscopy”

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 721 records · Page 40

Evaluation of the microstructure and mechanical properties of WC particle reinforced aluminum matrix composites fabricated by friction stir processing

Highlights: • FSP was used for the preparation of aluminum matrix composites reinforced with WC particle. • WC particles were uniformly distributed in the composite. • WC particles refined the grains of aluminum matrix. • WC particles enhanced the hardness and tensile strength, but decreased the ductility. - Abstract: Tungsten carbide (WC) is an attractive reinforcing material for aluminum and its alloys. However, it is technically challenging to fabricate WC particle reinforced aluminum matrix composites (AMCs) with homogeneous distribution of WC particles by liquid state processing techniques because of large density gradient. The present work aim to produce WC particle reinforced aluminum matrix composites (AMCs) through friction stir processing (FSP) and analyze the effect of its volume fraction on the microstructural features and the mechanical behavior of the developed AMCs. Microstructural evaluation was conducted on the cross-sections of the samples by optical microscopy (OM), scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). Microhardness testing was conducted across the cross-sections of FSPed samples to obtain hardness profiles and tensile test was conducted on as-received Al and FSPed samples. The fabricated AMCs exhibited the homogeneous distribution of WC particle with no obvious particle clustering in the stir zone, irrespective of position and WC particle volume fraction. Excellent WC/Al interfacial bonding was obtained in all FSPed AMCs with obviously refined grains. The average size of WC particles after FSP was slightly reduced with the increased volume fraction. It was also found that increasing the volume fraction of WC particles favored the grain refinement, improved the hardness and strength, but decreased the ductility. This improvement in the hardness and strength was attributed to the grain refinement strengthening and homogeneous distribution of WC particles. The decreased ductility resulted from the introduction of more WC particles. Increasing the volume fraction of WC particles caused the nature of fracture to move towards brittle nature.

36 MATERIALS SCIENCE↗

Pulsed laser powder bed fusion additive manufacturing of A356

Highlights: • Dense A356 specimens (98 ± 0.4%) were fabricated using a customized P-LPBF system. • Microstructure and grain morphology were examined using LOM, SEM, and EBSD. • Solidification front velocities (R) were evaluated through the KGT model. • A columnar grain structure was observed and predicted by the Hunt's criterion. - Abstract: A356 (Al7SiMg) specimens were fabricated through pulsed laser powder bed fusion (P-LPBF) additive manufacturing. Microstructural examinations and analyses were carried out through the usage of light optical microscopy (LOM), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The results revealed a fine cellular microstructure with the intercellular network consisting of Al cells and defined by a network of Si arms. The Al cells at the center of the melt pools and within the melt pool boundary bands were measured to be 423 ± 49 nm and 664 ± 76 nm, respectively. The presence of a fine columnar grain structure and epitaxial growth on partially melted grains was observed and explained by the KGT model and Hunt's criterion.

36 MATERIALS SCIENCE↗

Effect of cooling conditions on microstructure and mechanical properties of friction stir welded 7055 aluminium alloy joints

Highlights: • Water cooling improves tensile properties of friction stir welded 7055 Al alloy. • Water cooling results in smaller grains and second phase in nugget zone. • Water cooling results in finer second phase in thermos-mechanically affected zone. • Water cooling results in finer second phase in heat affected zone. • Fracture surface is flat for air-cooled joint but zig-zag for water-cooled one. - Abstract: The microstructure and mechanical properties of friction stir welded 7055 aluminium alloy under air cooling and water cooling were investigated by means of hardness and tensile testing, optical microscopy and transmission electron microscopy. Water cooling results in reduced softening in the weld zone and therefore higher tensile strength compared to air cooling. Fracture generally occurs within the thermo-mechanically affected zone (TMAZ) and heat affected zone (HAZ) on the retreating side in joints welded under air cooling but shifts towards the TMAZ and nugget zone (NZ) in the joints welded under water cooling. The fracture surfaces are generally flat for the air-cooled joint, but exhibits a zig-zag feature for the water-cooled joint. The mechanical behaviour of the weld has been discussed in light of the change in grain structure and precipitation in the NZ, TMAZ and HAZ caused by cooling conditions.

36 MATERIALS SCIENCE↗

Influence of rapid heating and cooling combined with deformation at ultrahigh strain rates on the microstructure evolution of pure titanium shaped charge liner

Highlights: • A slug prepared from pure titanium SCL was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1}. • The α → β → α phase transformation occurred in Ti SCL during the ultrahigh-strain -rate deformation. • The microstructures of the recovered slug included lamellar α grains, equiaxed α grains, and jagged α grains. - Abstract: A slug prepared from pure titanium shaped charge liners was recovered after detonation deformation at an ultrahigh strain rate over 10{sup 5} s{sup −1} and high strain over 500%. Optical microscopy, electron backscattered diffraction (EBSD), and transmission electron microscopy (TEM) were employed to investigate the microstructure of the Ti shaped charged liner before and after the detonation deformation. The microstructures of the recovered slug include lamellar α grains, equiaxed α grains within localized shear bands, and jagged α grains. EBSD results indicated that the grain orientation distribution is random and no texture was observed in the slug. TEM observation revealed that the α → β → α phase transformation occurred owing to the rapid heating and cooling combined with deformation at ultrahigh strain rates in the Ti shaped charge liner. No melting phenomenon was observed during the deformation process. The deformation process consisted of the explosive detonation stage combined with rapid heating and the subsequent penetration stage combined with rapid cooling. In the explosive detonation stage, the α → β phase transformation instantaneously occurred via a martensitic mechanism. In the penetration stage, the high-temperature slug in β state was cooled rapidly and showed different deformation behaviors in three different areas.

36 MATERIALS SCIENCE↗

Microstructure and mechanical properties development of micro channel tubes in extrusion, rolling and brazing

Highlights: • Rolling and brazing greatly affect the properties of micro-channel tubes (MCTs). • The properties of MCTs are investigated by the evolution of the microstructure. • Strength is decreased by 47% at 5%-rolling reduction ratio and 3-minute brazing. • Ductile fracture mode is observed by OM at failure of MCTs under inner pressure. - Abstract: In addition to extrusion, the post-processing of rolling and brazing has significant effect on the mechanical properties of multi-port tubes. The aluminum micro channel tubes, especially the seam welding zone in the internal webs, are investigated in terms of mechanical tests, microstructure characterization, and finite element analysis. The effect of the post-process of rolling are quantified by varying amount of rolling reduction ratios. Tensile strength and pressure bearing capacity are determined by tensile tests and burst pressure tests, respectively. The evolution of the microstructure within the seam wielding zone is characterized by Electron backscattered diffraction (EBSD) and optical microscopy (OM). The fracture profile observed by OM indicates ductile fracture mode. The pressure bearing capacity is reduced by ~47% at 5% reduction ratio of rolling followed by 3-minute brazing, where largest grains are obtained due to abnormal grain growth.

36 MATERIALS SCIENCE↗

Hydrogen induced cracking susceptibility of API 5L X70 pipeline steel in relation to microstructure and crystallographic texture developed after different thermomechanical treatments

Highlights: • crack propagated mainly along deformed-banded microstructure. • Lower failure strength manifested at pipeline steel surface compared to the mid-thickness. • Greater fraction of martensite/austenite constituents featured in specimen WG relative to specimen WH. • Early onset of cracking in specimen WH showed no preference to specific crystallographic orientation. • Multi-component inclusion particle was revealed along crack propagation path. - Abstract: Thermomechanical treatments offer an innovative means of controlling microstructure development and improving resistance to hydrogen induced cracking (HIC) in pipeline steel. This study was conducted on two X70 pipeline steels (labelled WG and WH) of the same chemical composition, but processed with different thermomechanical parameters. Specimen WG was hot rolled at a higher temperature range of 880–820 {sup °}C, while specimen WH was hot rolled between 830 and 760 {sup °}C before cooling at a rate of 25 {sup °}C/s. Early onset of HIC was observed in specimen WH after electrochemical hydrogen charging for 12 h in a solution of 0.2 M H{sub 2}SO{sub 4} and 3 g/l NH{sub 4}SCN, without any applied stress. Also, test pieces from the surface and mid-thickness layers of each pipeline steel were subjected to slow strain rate tensile (SSRT) test with in-situ hydrogen charging. Characterization techniques such as Optical Microscopy, Scanning Electron Microscopy, Electron Backscattered Diffraction and X-ray Diffraction were used to investigate the structure pipeline steel specimens. The role of inclusions on HIC was studied by Energy Dispersive X-ray Spectroscopy. Although the microstructure of both specimens were predominantly ferritic, more martensite/retained austenite (M/A) constituents featured in WG. Further crystallographic texture analysis indicates that grain orientation at the surfaces of both test specimens were similar with deviations towards <111> on the inverse pole figure (IPF); whereas, pole intensity at the mid-thickness deviated towards the <001> direction. Considering the increased fraction of banded-deformed grains with high stored energy, the lower HIC resistance of specimen WH in comparison to specimen WG was justified.

36 MATERIALS SCIENCE↗

Characterization of high-temperature mechanical properties of plasma-cladded coatings with thermo-mechanical coupling

High temperature mechanical properties was detected here to study the failure and strengthening mechanism of the coating-substrate (cobalt-based coatings were fabricated on FV520B substrate) integral structure with thermo-mechanical coupling effects. Microstructure, phase composition, element distribution of the coatings was characterized by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscope (TEM), electron back scattering diffraction (EBSD), X-ray diffraction (XRD), electron probe microanalysis (EPMA) and energy dispersive X-ray analysis (EDS). Results elucidate that fracture occurs in the coating for Co50 coating-substrate structure from 300 °C to 700 °C, but failure position transfer to substrate from coating at elevated temperatures with the addition of niobium and cerium oxide. Throughout, there is no crack originated from the interface. Fracture mechanism: the dislocation pile-up causes great stress concentration in the grain boundary, which results in the nucleation of the crack, and then the crack extends along the hard brittle Fe-Cr phase until the material fails. HRTEM shows the high density dislocation and the severe lattice distortion was formed during tensile deformation. On the macro level, the fracture tends to occur in the coarse dendrites region.

36 MATERIALS SCIENCE↗

Optimization of edge bead removal (EBR) process to enhance defect reduction in optical lithography

Defect reduction remains a critical objective in the integrated circuit manufacturing process, particularly within the highly re-entrant lithography modules where minimizing defects is crucial. Defects at the wafer edge can contaminate lithography modules and downstream processing equipment, leading to redistribution onto the wafer surface and adversely affecting overall device yield. A persistent challenge in the resist coating process is the formation of resist edge beads, driven by the strong Van der Waals attraction of excess photoresist (PR) to itself and the underlying substrate. The edge bead removal (EBR) process is a standard cleaning step designed to eliminate these edge beads and prevent potential contamination. Here, in this study, we identify the sources of EBR induced defects and additional EBR process encroachment toward edge patterning during the EBR cleaning process. This study provides a comprehensive study aimed at optimizing the EBR cleaning process to effectively eliminate EBR-induced defects, thereby enhancing overall device yield. Specifically, we identify three primary defects induced by the EBR cleaning process: rainbow-type, finger-shaped, and teardrop-type defects. Our experimental study reveals that in addition to EBR rinse time, PR cast time is crucial parameters contributing to the formation of these defects. By properly optimizing the PR cast time and EBR rinse time, we were able to remove nearly 100 % of dense clusters of defects that were easily visible even at low magnification optical microscopy throughout the wafer edge. We observed that shorter PR casting times shows edge defects caused by inefficient EBR process because of insufficient time for PR to fully settle causing superfluous PR to continue flowing toward wafer edge during EBR clearing step, leading to partial removal of PR at the wafer edge and the formation of rainbow defects. Proper optimization of both PR casting time and EBR chemistries dispense time is essential to resolve these defects, ensuring efficient EBR cleaning process and improved overall device yield.

42 ENGINEERING↗

An experimental statistical analysis of stress projection factors in BCC tantalum

Crystallographic slip planes in body centered cubic (BCC) metals are not fully understood. In polycrystals, there are additional confounding effects from grain interactions. This paper describes an experimental investigation into the effects of grain orientation and neighbors on elastic–plastic strain accumulation. In situ strain fields were obtained by performing digital image correlation (DIC) on images from a scanning electron microscope (SEM) and from optical microscopy. These strain fields were statistically compared to the grain structure measured by electron backscatter diffraction (EBSD). Spearman rank correlations were performed between effective strain and six microstructural factors including four Schmid factors associated with the <111> slip direction, grain size, and Taylor factor. Modest correlations (~10%) were found for a polycrystal tension specimen. The influence of grain neighbors was first investigated by re-correlating the polycrystal data using clusters of similarly-oriented grains identified by low grain boundary misorientation angles. Second, the experiment was repeated on a tantalum oligocrystal, with through-thickness grains. Much larger correlation coefficients were found in this multicrystal due to the dearth of grain neighbors and subsurface microstructure. Finally, a slip trace analysis indicated (in agreement with statistical correlations) that macroscopic slip often occurs on {110}<111> slip systems and sometimes by pencil glide on maximum resolved shear stress planes (MRSSP). These results suggest that Schmid factors are suitable for room temperature, quasistatic, tensile deformation in tantalum as long as grain neighbor effects are accounted for.

36 MATERIALS SCIENCE↗

In-situ investigation of stress-induced martensitic transformation in Ti–Nb binary alloys with low Young's modulus [In-situ high-energy X-ray diffraction investigation on stress-induced martensitic transformation in Ti-Nb binary alloys]

Microstructure evolution, mechanical behaviors of cold rolled Ti-Nb alloys with different Nb contents subjected to different heat treatments were investigated. Here, optical microstructure and phase compositions of Ti-Nb alloys were characterized using optical microscopy and X-ray diffractometre, while mechanical behaviors of Ti-Nb alloys were examined by using tension tests. Stress-induced martensitic transformation in a Ti-30. at%Nb binary alloy was in-situ explored by synchrotron-based high-energy X-ray diffraction (HE-XRD). The results obtained suggested that mechanical behavior of Ti-Nb alloys, especially Young's modulus was directly dependent on chemical compositions and heat treatment process. According to the results of HE-XRD, α"-V1 martensite generated prior to the formation of α"-V2 during loading and a partial reversible transformation from α"-V1 to β phase was detected while α"-V2 tranformed to β completely during unloading.

36 MATERIALS SCIENCE↗

Biaxial creep performance of CWSR Zircaloy-4 cladding at emulated off-normal conditions of interim dry storage facility

In this study, biaxial creep behavior of hydrided Zircaloy-4 cladding was tested at 500 degrees C. Creep-life was inversely proportional to H-concentration up to 750 wppm. The weakening through hydride reorientation of hydrided specimens was not observed by optical microscopy. The power-law stress exponents and the TEM observation supported the high-temperature climb mechanism dominated the creep behavior in secondary stage.

36 MATERIALS SCIENCE↗

Creep behavior of Alloy 709 at 700 °C

Alloy 709 is an austenitic stainless steel with potential for structural applications in sodium-cooled fast reactors. In this study, creep tests on Alloy 709 specimens were performed at a temperature of 700°C under applied stresses in the range of 125 to 250 MPa. Here, the alloy exhibited a brief primary, insignificant secondary and prolonged tertiary creep stages. A Norton stress exponent (n) of ~6 was obtained from the creep plots. Microstructural analyses were carried out for both as-received and crept specimens using optical microscopy, electron backscattered diffraction, and transmission electron microscopy. The microstructures of the as-received and crept specimens were compared. The mode of fracture was transgranular as revealed by scanning electron microscopy of the creep-ruptured specimens. Thermodynamic and precipitation modeling was performed in order to obtain information on the phase types and the kinetics of precipitation for the sigma-phase and the M 23 C 6 carbide. Based on the creep data, microstructural observations and relevant modeling, creep deformation and failure mechanisms at the considered temperature are elucidated.

36 MATERIALS SCIENCE↗

Build orientation, surface roughness, and scan path influence on the microstructure, mechanical properties, and flexural fatigue behavior of Ti–6Al–4V fabricated by electron beam melting

In the present work, microstructure and fatigue behavior of Electron Beam Melted (EBM) Ti–6Al–4V have been systematically studied. Fatigue behavior was investigated using four-point bend tests of rectangular bars with internal features fabricated with different build orientations, scan paths, and surface conditions. Microstructural variations were evaluated by optical microscopy and Vickers micro-hardness indentations, both of which were found to be consistent throughout the build and within ranges reported in the literature. The fatigue performance of the EBM material was comparable to wrought Ti–6Al–4V when the loading direction was parallel to the build direction, but severely limited when loaded perpendicular to the build direction or if surface roughness defects were present. Scanning electron microscopy and interrupted fatigue tests were utilized to characterize fracture surfaces, failure mechanisms, crack initiation, and propagation behavior. Crack initiation sites in the vertically-oriented specimens were identified to be melt-related defects formed by insufficient melting.

36 MATERIALS SCIENCE↗

Prediction of softening kinetics and recrystallization texture in non-isothermally annealed bulged tubes using CPFEM and CA models

A hierarchically coupled cellular automata (CA) model, crystal plasticity finite element method (CPFEM), and thermal finite element (FE) model is developed to predict the softening kinetics of the bulged steel tube during non-isothermal annealing. Through the developed model, the kinetics of softening mechanisms including static recovery (SRV) and static recrystallization (SRX), as well as the recrystallization texture are predicted. Later, the Johnson-Mehl-Avrami-Kohnogorov (JMAK) model based on the predicted SRX data is developed to interpret the recrystallization behavior of the material. To perform this study, diverse experimental tests including tube hydroforming (THF), annealing, uniaxial tensile test, hardness test, as well as microstructure observations through optical microscopy and Electron Backscatter Diffraction (EBSD) tests on steel tube are performed. The obtained experimental data are utilized to calibrate and verify the implemented CPFEM model for simulation of THF process, thermal FE model for prediction of the local temperature over annealing time, and CA algorithm for modeling of the softening kinetics and texture evolution throughout the annealing process. The study shows that the predicted deformation characteristics, softening kinetics, recrystallization texture and temperature profile during non-isothermal annealing are in good agreement with experimental data. During the annealing process, a total of four stages for the kinetics of softening mechanisms is observed: No softening; SRV only; SRV dominant; and SRX dominant. During the progress of SRX, the behavior of recrystallization is abruptly changed, confirming that two different mechanisms are controlling the kinetics of transformation.

36 MATERIALS SCIENCE↗

Spall damage mechanisms in laser powder bed fabricated stainless steel 316L

This paper reports on spall damage mechanisms in laser powder bed fusion (LPBF) fabricated stainless steel 316L (SS316L) subjected to uniaxial, strain plate-impact loading and explores failure evolution with increasing impact velocity and peak pressure. Analysis of velocimetry profiles reveals a heterogeneous failure response with several different failure mechanisms activated during impact and resulting spall. The analysis is supported by optical microscopy and electron backscattered diffraction (EBSD) observation of soft recovered impacted samples, which show evidence of localized nano-twinning, twin growth, severe grain rotation, and grain refinement along the spall plane, in addition to pore nucleation, coalescence, and growth. Furthermore, the observed failure mechanisms, including crack formation and propagation along high angle grain boundaries (HAGBs), are not consistently indicative of ductile fracture typical of wrought stainless steel.

36 MATERIALS SCIENCE↗

Hydrogen embrittlement of Zircaloy-4 fabricated by ultrasonic additive manufacturing

Ultrasonic additive manufacturing (UAM) was successfully applied to the zirconium material system to create a planar geometry. Following fabrication, SS-J3 type tensile specimens of the UAM and wrought Zircaloy-4 with a nominal gage section of 5×1.2×0.75 mm were machined for hydriding studies and mechanical testing. The SS-J3 type tensile specimens were gas-charged with hydrogen using a custom system that precisely controls hydrogen gas flow rate, hydrogen partial pressure, and temperature. To avoid altering the UAM material, the maximum process temperature was limited to 550°C. Using different initial hydrogen gas pressures and flow rates, various hydrogen contents (70–1755 wppm) were achieved for Zircaloy-4 specimens. Tensile testing shows that, regardless of hydrogen content, all UAM specimens measured yield strengths in the range of 557±16 MPa and ultimate tensile strengths of 660±4MPa. However, total elongation clearly decreased as a function of increasing hydrogen content. Further, at the lowest hydrogen content, the total plastic elongation measured 21.5%, and this value decreased to less than 2% when the hydrogen content was increased to 1000 wppm. Cross-sectional optical microscopy images revealed that the hydride distributions are randomly oriented. For the low hydrogen content specimen, these randomly distributed hydrides are isolated from each other. A sandwiched structure, consisting of high-density and low-density layers, was also observed for the specimens with hydrogen content between 200 and 400 wppm. As the hydrogen content increases, the hydrides diffuse into the low-density hydride layers to form a network across the whole specimen. Although the tensile properties of UAM and wrought Zircaloy-4 exhibit the same behavior with increasing hydrogen content, the distinctions in grain orientations led to differences in the hydride orientations at low and intermediate hydrogen concentrations.

36 MATERIALS SCIENCE↗

Integration of layered group IV selenides: From SnSe–SnSe 2-x S x core-shell crystals to complex (SnSe–SnSe 2-x S x )-GeSe van der waals heterostructures

The layered semiconductor tin selenide (SnSe) has received extensive interest due to its promising thermoelectric and ferroelectric properties. Integrating SnSe with other layered crystals in heterostructures can enable the modification of charge- and thermal transport, electrical polarization, and other properties such as chemical stability, optoelectronics, and photonics. Here, we demonstrate the vapor transport synthesis of single-crystalline SnSe monochalcogenide flakes that are spontaneously encapsulated in a thin layered SnSe 2-x S x dichalcogenide shell. In a second growth step, such SnSe-SnSe 2-x S x heterostructures are integrated with the monochalcogenide GeSe, which is laterally stitched to the SnSe side facets while preserving the dichalcogenide shell across the basal facets. This architecture is confirmed by optical microscopy, electron microscopy and diffraction, energy dispersive X-ray and Raman spectroscopies, as well as cathodoluminescence spectroscopy. Furthermore, the results extend our capabilities for materials integration by forming complex heterostructures with both vertical van der Waals interfaces and covalent lateral interfaces between layered semiconductors.

2D layered crystals↗

Microscopic analysis of irradiated AGR-1 coated particle fuel compacts

The AGR-1 experiment involved irradiation of 72 TRISO-coated particle fuel compacts to a peak compact-average burnup of 19.5% FIMA with no in-pile failures observed out of 3 x 105 total particles. Irradiated AGR-1 fuel compacts have been cross-sectioned and analyzed with optical microscopy to characterize kernel, buffer, and coating behavior. Six compacts have been examined, spanning a range of irradiation conditions (burnup, fast fluence, and irradiation temperature) and including all four TRISO coating variations irradiated in the AGR-1 experiment. The cylindrical specimens were sectioned both transversely and longitudinally, then polished to expose from 36 to 79 individual particles near midplane on each mount. The analysis focused primarily on kernel swelling and porosity, buffer densification and fracturing, buffer–IPyC debonding, and fractures in the IPyC and SiC layers. Characteristic morphologies have been identified, 981 particles have been classified, and spatial distributions of particle types have been mapped. No significant spatial patterns were discovered in these cross sections. However, some trends were found between morphological types and certain behavioral aspects. Buffer fractures were found in 23% of the particles, and these fractures often resulted in unconstrained kernel protrusion into the open cavities. Fractured buffers and buffers that stayed bonded to IPyC layers appear related to larger pore size in kernels. Buffer–IPyC interface integrity evidently factored into initiation of rare IPyC fractures. Fractures through part of the SiC layer were found in only four classified particles, all in conjunction with IPyC–SiC debonding. Compiled results suggest that the deliberate coating fabrication variations influenced the frequencies of IPyC fractures and IPyC–SiC debonds.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗