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 1,387 records · Page 77

Synthesis of δ-Bi2O3/Bi2MoO6 composites with enhanced photocatalytic activity by hydrothermal method

Highlights: • The δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} composites were first synthesized by hydrothermal method. • The product was δ-Bi{sub 2}O{sub 3} rather than α-Bi{sub 2}O{sub 3} with the preset of Bi{sub 2}MoO{sub 6}. • The composites show enhanced photocatalytic activity compared to Bi{sub 2}MoO{sub 6}, α- and δ-Bi{sub 2}O{sub 3}. • The excellent photocatalytic performance was attributed to δ- Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} heterojunctions. - Abstract: The δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} composites were synthesized by hydrothermal method and the microstructure and photocatalytic property were characterized. The X-ray diffraction (XRD) analysis revealed that δ-Bi{sub 2}O{sub 3} was obtained with the existence of Bi{sub 2}MoO{sub 6}, while the product was α-Bi{sub 2}O{sub 3} without Bi{sub 2}MoO{sub 6} under the same experimental condition. The SEM images and the selected area electron diffraction (SAED) patterns have further verified that δ-Bi{sub 2}O{sub 3} was deposited on Bi{sub 2}MoO{sub 6}. The X-ray photoelectron spectroscopy (XPS) spectrum confirmed that the composites were composed of δ-Bi{sub 2}O{sub 3} and Bi{sub 2}MoO{sub 6}, while a fraction of Mo changed from Mo{sup 6+} to Mo{sup 5+}. The coexistence of Mo{sup 5+}/Mo{sup 6+} can be a critical factor in the formation of stable δ-Bi{sub 2}O{sub 3} on Bi{sub 2}MoO{sub 6}. Particularly, the δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} photocatalysts possess favorable photocatalytic performance under simulated sunlight illumination since the recombination of photogenerated electrons and holes was inhibited due to the p-n junction at the interface of δ-Bi{sub 2}O{sub 3} and Bi{sub 2}MoO{sub 6}, and the mechanism was discussed in detail.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Cementitious Barriers Partnership ‐ FY13 Mid‐Year Report

In FY2013, the Cementitious Barriers Partnership (CBP) is continuing in its effort to develop and enhance software tools demonstrating tangible progress toward fulfilling the objective of developing a set of tools to improve understanding and prediction of the long-term structural, hydraulic and chemical performance of cementitious barriers used in nuclear applications. In FY2012, the CBP released the initial inhouse “Beta-version” of the CBP Software Toolbox, a suite of software for simulating reactive transport in cementitious materials and important degradation phenomena. The current primary software components are LeachXS/ORCHESTRA, STADIUM, and a GoldSim interface for probabilistic analysis of selected degradation scenarios. THAMES is a planned future CBP Toolbox component (FY13/14) focused on simulation of the microstructure of cementitious materials and calculation of resultant hydraulic and constituent mass transfer parameters needed in modeling. This past November, the CBP Software Toolbox Version 1.0 was released that supports analysis of external sulfate attack (including damage mechanics), carbonation, and primary constituent leaching. The LeachXS component embodies an extensive material property measurements database along with chemical speciation and reactive mass transport simulation cases with emphasis on leaching of major, trace and radionuclide constituents from cementitious materials used in DOE facilities, such as Saltstone (Savannah River) and Cast Stone (Hanford), tank closure grouts, and barrier concretes. STADIUM focuses on the physical and structural service life of materials and components based on chemical speciation and reactive mass transport of major cement constituents and aggressive species (e.g., chloride, sulfate, etc.). The CBP issued numerous reports and other documentation that accompanied the “Version 1.0” release including a CBP Software Toolbox User Guide and Installation Guide. These documents, as well as, the presentations from the CBP Software Toolbox Demonstration and User Workshop, which are briefly described below, can be accessed from the CBP webpage at http://cementbarriers.org/. The website was recently modified to describe the CBP Software Toolbox and includes an interest form for application to use the software. The CBP FY13 program is continuing research to improve and enhance the simulation tools as well as develop new tools that model other key degradation phenomena not addressed in Version 1.0. Also efforts to continue to verify the various simulation tools thru laboratory experiments and analysis of field specimens are ongoing to quantify and reduce the uncertainty associated with performance assessments are ongoing. This mid-year report also includes both a summary on the FY13 software accomplishments in addition to the release of Version 1.0 of the CBP Software Toolbox and the various experimental programs that are providing data for calibration and validation of the CBP developed software. The focus this year for experimental studies was to measure transport in cementitious material by utilization of a leaching method and reduction capacity of saltstone field samples. Results are being used to calibrate and validate the updated carbonation model.

36 MATERIALS SCIENCE↗

A comprehensive secondary ion mass spectrometry analysis of ZnO nanowalls: Correlation to photocatalytic responses

We report on the visible light induced photocatalytic responses of zinc oxide (ZnO) nanostructures in the form of nanowires and nanowalls grown on aluminum substrates. Morphological and microstructural characteristics of these nanostructures have been analyzed using scanning electron microscopy (SEM) and high resolution electron microscopy (HRTEM). The presence of surface-adsorbed H{sup +}, O{sub 2}{sup −}, and OH{sup −} species on ZnO nanostructures has been established through secondary ion mass spectrometry (SIMS). The relative change in substrate coverage under varying reaction time has also been evidenced through SIMS and is in agreement with SEM observation. Compared to nanowires, oxygen adsorption on ZnO surfaces and subsequent oxygen in-diffusion are found to be prominent for the nanowall-like structures and are seen to be highest for nanowalls grown in lower reaction time. In contrast to nanowires, nanowalls are found to exhibit higher photocatalytic activity and this can be attributed to higher adsorption of oxygen. The photocatalytic activity of the samples under visible light is originated from the native defect-states and the photocatalytic efficiency is largely influenced by the surface-adsorbants. Control of surface adsorption characteristics of the nanowalls upon tuning wall thicknesses can lead to the development of futuristic efficient photocatalytic devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Analysis of structure-property gradients in orthogonally machined chips and workpiece subsurface

Production of machined surfaces with optimized mechanical properties requires fundamental process-structure-property knowledge. In this paper, we focus on structure-property gradients in orthogonally cut OFHC Copper chips and the workpiece subsurface. We utilize orientation imaging microscopy and statistical spatial correlation metrics to quantify the microstructure. Constitutive elastic-plastic properties of the workpiece subsurface and chips are measured using spherical nanoindentation. Analysis of the data reveals significant structure and property gradients in both regions. Differences and similarities in structure and property gradients near the workpiece surface and tool-chip interface, and in the chip middle are discussed and explained.

42 ENGINEERING↗

Large area strain analysis using scanning transmission electron microscopy across multiple images

Here, we apply revolving scanning transmission electron microscopy to measure lattice strain across a sample using a single reference area. To do so, we remove image distortion introduced by sample drift, which usually restricts strain analysis to a single image. Overcoming this challenge, we show that it is possible to use strain reference areas elsewhere in the sample, thereby enabling reliable strain mapping across large areas. As a prototypical example, we determine the strain present within the microstructure of a Ni-based superalloy directly from atom column positions as well as geometric phase analysis. While maintaining atomic resolution, we quantify strain within nanoscale regions and demonstrate that large, unit-cell level strain fluctuations are present within the intermetallic phase.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Effect of Ce{sup 3+} Ion on Structural and Hyperfine Interaction Studies of Co{sub 0.5}Ni{sub 0.5}Fe{sub 2−x}Ce{sub x}O{sub 4} Ferrites: Useful for Permanent Magnet Applications

Nanoparticles of Co{sub 0.5}Ni{sub 0.5}Fe{sub 2−x}Ce{sub x}O{sub 4} (where x = 0.0, 0.01, 0.015 and 0.02) ferrites are prepared by the modified solution combustion method using a mixture of fuels and are characterized to understand their structural, microstructural and magnetic properties. The X-ray diffraction is used to confirm the formation of a single-phase cubic spinel structure. The average crystallite sizes are calculated using the Scherrer formula and are found to be less than 50 nm. The microstructural features are obtained by the scanning electron microscopy, and the compositional analysis is done by using the energy-dispersive spectroscopy. The transmission electron microscopy (TEM) investigations show that the synthesized ferrites are made up of very fine spherical nanoparticles. The influence of a rare-earth element (Ce{sup 3+}) on the magnetic properties of the samples was studied using the Mössbauer spectroscopy. The Mössbauer spectroscopy reveals the formation of broadened Zeeman lines and quadrupole-split lines and the presence of the Fe{sup 3+} charge state at B sites in the samples. The quadrupole splitting shows that the orientation of the magnetic hyperfine field with respect to the principle axes of the electric field gradient was random. The magnetic hyperfine field values indicate that the A sites have more A-O-B superexchange interactions than the B sites. The coexistence of magnetic sextet and a doublet component on the room-temperature spectra suggests superparamagnetic properties of the nanoparticles. The low-temperature (15 K) Mössbauer spectroscopy explores the paramagnetic relaxation in the nanoparticles. The area under the sextet refers to Fe{sup 3+} concentrations in the tetrahedral and octahedral sites of the ferrite. This study confirms that the Ce{sup 3+} substitution of Fe{sup 3+} only for octahedron sites causes the decrease in Fe-O-Fe arrangement. The effect of Ce{sup 3+} doping on the magnetic properties of Co{sub 0.5}Ni{sub 0.5}Fe{sub 2}O{sub 4} is examined from the vibrating sample magnetometry (VSM) spectra. Saturation magnetization values are decreased initially and then increased, as result of Ce{sup 3+} doping. This can be explained by Neel’s two-sub-lattice model. Further, the value of coercivity is found to be increasing with increasing Ce{sup 3+} concentration. The obtained results of M-H loop with improved coercivity (from 851 to 1039 Oe) by Ce{sup 3+} doping of Co{sub 0.5}Ni{sub 0.5}Fe{sub 2}O{sub 4} demonstrate the usefulness for permanent magnet applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Microstructural, mechanical and weldability assessments of the dissimilar welds between γ′- and γ″-strengthened nickel-base superalloys

Dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys has been investigated to identify the relationship between the microstructure of the welds and the resultant mechanical and weldability characteristics. γ′-Strengthened nickel-base Alloy 500 and γ″-strengthened nickel-base Alloy 718 were used for dissimilar welding. Gas tungsten arc welding operations were utilized for performing the autogenous dissimilar welding. Alloy 500 and Alloy 718 base metals showed various types of phases, carbides, intermetallics and eutectics in their microstructure. The results for Alloy 500 weld metal showed severe segregation of titanium to the interdendritic regions. The Alloy 718 weld metal compositional analysis confirmed the substantial role of Nb in the formation of low-melting eutectic-type morphologies which can reduce the weldability. The microstructure of dissimilar weld metal with dilution level of 65% wt.% displayed semi-developed dendritic structure. The less segregation and less formation of low-melting eutectic structures caused to less susceptibility of the dissimilar weld metal to the solidification cracking. This result was confirmed by analytic modeling achievements. Dissolution of γ″-Ni{sub 3}Nb precipitations took place in the Alloy 718 heat-affected zone leading to sharp decline of the microhardness in this region. Remelted and resolidified regions were observed in the partially-melted zone of Alloy 500 and Alloy 718. Nevertheless, no solidification and liquation cracking happened in the dissimilar welds. Finally, this was concluded that dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys can successfully be performed. - Highlights: • Dissimilar welding of γ′- and γ″-strengthened nickel-base superalloys is studied. • Microstructural, mechanical and weldability aspects of the welds are assessed. • Microstructure of welds, bases and heat-affected zones is characterized in detail. • The type, morphology and distribution of the phases are thoroughly investigated. • Dissimilar welding is successfully performed without occurrence of any hot cracks.

36 MATERIALS SCIENCE↗

Titanium-deposition assisted brazing of SiC ceramics using inactive AgCu filler

Highlights: • Reliable joint of SiC ceramics was achieved via Titanium-deposition assisted brazing using inactive AgCu filler metal. • Microstructure characteristic of deposited-SiC brazed joint was investigated in detail. • Ti-deposition assisted brazing inhibited the formation of numerous intermetallic compounds. - Abstract: In this study, active titanium element film was designed to deposit on SiC ceramics directly to enhance the brazability of inactive AgCu brazing alloy on ceramics. The result showed the reliable joint was successfully obtained and the deposition of titanium film on SiC directly inhibited the formation of amounts of intermetallic compounds effectively in the brazing seam. Detailed interfacial microstructure of joint investigated by scanning electron microscope equipped with energy dispersive spectrum analysis and transmission electron microscope revealed that the interfacial reactions were based on deposited Ti film. The typical joint was SiC/TiCu + Ti{sub 2}Cu/TiC/Ti{sub 5}Si{sub 3} containing TiC particles/Ag(s,s) + Cu(s,s)/Ti{sub 5}Si{sub 3} containing TiC particles/TiC/TiCu + Ti{sub 2}Cu/SiC.

36 MATERIALS SCIENCE↗

The Sliding Wear and Friction Behavior of M50-Graphene Self-Lubricating Composites Prepared by Laser Additive Manufacturing at Elevated Temperature

M50 steel is widely applied to manufacture aircraft bearings where service lives are mainly determined by the friction and wear behaviors. The main purpose of this study is to investigate the tribological behaviors and wear mechanisms of M50-1.5 wt.% graphene composites (MGC) prepared by laser additive manufacturing (LAM) (MGC-LAM) sliding against Si{sub 3}N{sub 4} ball from 25 to 550 °C at 18 N–0.2 m/s. XRD, EPMA, FESEM, and EDS mapping were conducted to understand the major mechanisms leading to the improvement in the sliding behavior of MGC-LAM. The results indicated that MGC-LAM showed the excellent friction and wear performance at 25-550 °C for the lower friction coefficient of 0.16-0.52 and less wear rate of 6.1-9.5 × 10{sup −7} mm{sup 3} N{sup −1} m{sup −1}. Especially at 350 °C, MGC-LAM obtained the best tribological performance (0.16, 6.1 × 10{sup −7}mm{sup 3} N{sup −1} m{sup −1}). It was attributed to the dense coral-like microstructure, as well as the formed surface lubricating structure which is composed of the upper uniform lubricating film with massive graphene and the underneath compacted layer.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

E-band fiber laser performance and power analysis with longitudinally averaged population modeling

To help facilitate the modeling of new fiber laser systems, such as those with complex functional microstructures, we report on a simplified modeling methodology that can accommodate the parasitic kinetic effects often present in such systems. The essence of our approach is to integrate kinetics over the length of the gain medium at the outset, thereby forfeiting longitudinally resolved information about the system but simplifying its energetics analysis. To illustrate the benefits of our new approach over more conventional coupled-rate-equation analyses, we apply our model to an Nd 3 + -doped fiber laser operating on the F 3 / 2 4 - I 4 13 / 2 transition at 1400 nm. The model produces closed-form solutions for the various output channels available to the pump power and enables projections of ultimate laser performance to be conveniently generated.

47 OTHER INSTRUMENTATION↗

In situ synchrotron tensile investigations on ultrasonic additive manufactured (UAM) zirconium

The microstructure evolution during room temperature uniaxial tensile straining of ultrasonic additive manufactured (UAM) zirconium was evaluated using the Advanced Photon Source (APS) facility. Miniature dog-bone tensile specimens of two orientations were cut from a UAM-fabricated zirconium bar for in situ synchrotron tensile tests. Wide-angle X-ray scattering (WAXS) scanning was used to unveil the changes in microstructure of the entire gauge regions throughout the straining. A series of WAXS data analysis methods were utilized to quantify both elastic and plastic deformation mechanisms within the strained specimens. Stress concentrations were identified during early stages of plastic deformation, which become candidate necking positions and eventually lead to failure. Additionally, fracture surface analysis implied that these stress concentration locations may be correlated to the fabrication defects, providing insightful guidance for future improvements of the UAM zirconium fabrication process.

36 MATERIALS SCIENCE↗

Strain rate sensitivity, microstructure variations, and stress-assisted β → α" phase transformation investigation on the mechanical behavior of dual-phase titanium alloys

In this study, the microstructures of three widely used dual-phase titanium alloys: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo, and Ti-6Al-2Sn-4Zr-6Mo are characterized using backscatter electron imaging and the deformation behaviors in their individual α and β phases are investigated using in situ high-energy X-ray diffraction during uniaxial tension experiments. This is accompanied by calculation of the strain rate sensitivity (SRS) in these alloys, as a function of applied loading. The results of the calculated SRS and the mechanical response (in terms of lattice strains and hardening behaviors) are rationalized based on the local microstructure, composition, and texture of the alloy. A stress-induced β (BCC) to α" (orthorhombic) phase transformation is observed during the in-situ diffraction experiment, which permitted analysis of the lattice strain evolution during the phase transformation. Results from this study provide insights into the relationship between microstructure, composition, applied loading, and the deformation behavior, including effects on loading with time holds. Specifically, the results show that the microstructure, and not necessarily the chemical composition (Mo content), along with the applied loading have a dominant role in the observed SRS variation in titanium alloys. Further, the evolution of the α" (orthorhombic) phase is observed for the first time during deformation of an industrially relevant titanium alloy, Ti-6246.

36 MATERIALS SCIENCE↗

Detailed Analysis of RUS Insertion Experiment and Scoping Studies for Performing Next Experiment using an Enriched Fuel Sample

Microstructure evolution due to irradiation in a nuclear reactor can have a dramatic effect on material properties. A better understanding of this evolution is necessary for developing improved nuclear fuels and materials. The ability to measure such changes in real time is extremely challenging due to high temperatures, high radiation fields, and limited access of the reactor environment. Through carefully designed experiments, measurement of elastic properties can be tied directly to microstructure. We present an instrument that has been developed to monitor in-pile changes in grain microstructure. The measurement approach involves optically exciting and detecting flexural waves in a thin cantilever beam. An instrument capsule based on this technique was fabricated and underwent an irradiation test in the TREAT reactor in May 2019. Analyses of the test results are presented in this report. Scoping studies on the expected impact of radiation on similar tests are also presented.

36 MATERIALS SCIENCE↗

Creep-rupture and fractographic analysis of Stirling engine superalloys tested in air and 15 MPa hydrogen

A brief comparative analytical and microstructural evaluation of creep-rupture performance of two iron-base superalloys in air and 15 MPa of hydrogen, is presented. Creep rupture data are presented for the sheet alloy 19-9DL and the cast alloy XF-818, including temperature, initial stress, rupture life, minimum creep rate, time to reach one percent creep strain, and total elongation. In 19-9DL, both rupture life and minimum creep rate are more sharply dependent on small stress changes than in XF-818 in the given environment, and 19-9DL appears to become a more creep-resistant material with increasing Q (apparent activation energy) while the opposite is noted for XF-818. There appears to be no environmental effect on minimum creep rate for 19-9DL, whereas Q becomes less negative for XF-818 for 15 MPa of H2. Multiple cracks leading to rupture are observed on the fracture surfaces, with sheet specimens showing many more cracks close to the fracture surface than cast specimens.

Bhattacharyya, S.↗

Microstructural investigation of plastically deformed Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy by X-ray diffraction and transmission electron microscopy

The microstructure evolution in body-centered cubic (bcc) Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy during quasi-static compression test was studied by X-ray line profile analysis (XLPA) and transmission electron microscopy (TEM). The average lattice constant and other important parameters of the microstructure such as the mean crystallite size, the dislocation density and the edge/screw character of dislocations were determined by XLPA. The elastic anisotropy factor required for XLPA procedure was determined by nanoindentation. XLPA shows that the crystallite size decreased while the dislocation density increased with strain during compression, and their values reached about 39 nm and 15 × 10{sup 14} m{sup −2}, respectively, at a plastic strain of ~ 20%. It was revealed that with increasing strain the dislocation character became more screw. This can be explained by the reduced mobility of screw dislocations compared to edge dislocations in bcc structures. These observations are in line with TEM investigations. The development of dislocation density during compression was related to the yield strength evolution. - Highlights: • Ti{sub 20}Zr{sub 20}Hf{sub 20}Nb{sub 20}Ta{sub 20} high entropy alloy was processed by arc-melting. • The mechanical was evaluated by RT compression test. • The microstructure evolution was studied by XLPA and TEM. • With increasing strain the dislocation character became more screw. • The yield strength was related to the development of the dislocation density.

36 MATERIALS SCIENCE↗

CVD of silicon carbide on structural fibers: Microstructure and composition

Structural fibers are currently being considered as reinforcements for intermetallic and ceramic materials. Some of these fibers, however, are easily degraded in a high temperature oxidative environment. Therefore, coatings are needed to protect the fibers from environmental attack. Silicon carbide (SiC) was chemically vapor deposited (CVD) on Textron's SCS6 fibers. Fiber temperatures ranging from 1350 to 1500 C were studied. Silane (SiH4) and propane (C2H8) were used for the source gases and different concentrations of these source gases were studied. Deposition rates were determined for each group of fibers at different temperatures. Less variation in deposition rates were observed for the dilute source gas experiments than the concentrated source gas experiments. A careful analysis was performed on the stoichiometry of the CVD SiC coating using electron microprobe. Microstructures for the different conditions were compared. At 1350 C, the microstructures were similar; however, at higher temperatures, the microstructure for the more concentrated source gas group were porous and columnar in comparison to the cross sections taken from the same area for the dilute source gas group.

Veitch, Lisa C.↗

CVD of silicon carbide on structural fibers - Microstructure and composition

Structural fibers are currently being considered as reinforcements for intermetallic and ceramic materials. Some of these fibers, however, are easily degraded in a high temperature oxidative environment. Therefore, coatings are needed to protect the fibers from environmental attack. Silicon carbide (SiC) was chemically vapor deposited (CVD) on Textron's SCS6 fibers. Fiber temperatures ranging from 1350 to 1500 C were studied. Silane (SiH4) and propane (C2H8) were used for the source gases and different concentrations of these source gases were studied. Deposition rates were determined for each group of fibers at different temperatures. Less variation in deposition rates were observed for the dilute source gas experiments than the concentrated source gas experiments. A careful analysis was performed on the stoichiometry of the CVD SiC coating using electron microprobe. Microstructures for the different conditions were compared. At 1350 C, the microstructures were similar; however, at higher temperatures, the microstructure for the more concentrated source gas group were porous and columnar in comparison to the cross sections taken from the same area for the dilute source gas group.

Veitch, Lisa C.↗

Failure Analysis and Magnetic Evaluation of Tertiary Superheater Tube Used in Gas-Fired Boiler

Failure analysis was carried out on a prematurely failed tertiary superheater tube used in gas-fired boiler. The analysis includes a comparative study of visual examination, chemical composition, hardness and microstructure at failed region, adjacent and far to failure as well as on fresh tube. The chemistry was found matching to the standard specification, whereas the hardness was low in failed tube compared to the fish mouth opening region and the fresh tube. Microscopic examination of failed sample revealed the presence of spheroidal carbides of Cr and Mo predominantly along the grain boundaries. The primary cause of failure is found to be localized heating. Magnetic hysteresis loop (MHL) measurements were carried out to correlate the magnetic parameters with microstructure and mechanical properties to establish a possible non-destructive evaluation (NDE) for health monitoring of the tubes. The coercivity of the MHL showed a very good correlation with microstructure and mechanical properties deterioration enabling a possible NDE technique for the health monitoring of the tubes.

36 MATERIALS SCIENCE↗