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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.

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At least 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

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

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

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Non-destructive Quantitative Phase Analysis and Microstructural Characterization of Zirconium Coated U-10Mo Fuel Foils via Neutron Diffraction

This report uses neutron diffraction to investigate the crystal phase composition of uranium-molybdenum alloy foils (U-10Mo) for the CONVERT MP-1 Reactor Conversion Project, and determines the effect on alpha-uranium contamination following the deposition of a Zr metal diffusion layer by various methods: plasma spray deposition of Zr powders at LANL and hot co-rolling with Zr foils at BWXT. In summary, there is minimal decomposition of the gamma phase U-10Mo foil to alpha phase contamination following both plasma spraying and hot co-rolling. The average unit cell volume, i.e. lattice spacing, of the Zr layer can be mathematically extracted from the diffraction data; co-rolled Zr matches well with literature values of bulk Zr, while plasma sprayed Zr shows a slight increase in the lattice spacing, indicative of interstitial oxygen in the lattice. Neutron diffraction is a beneficial alternative to conventional methods of phase composition, i.e. x ray diffraction (XRD) and destructive metallography. XRD has minimal penetration depth in high atomic number materials, particularly uranium, and can only probe the first few microns of the fuel plate; neutrons pass completely through the foil, allowing for bulk analysis of the foil composition and no issues with addition of cladding layers, as in the final, aluminum-clad reactor fuel plates. Destructive metallography requires skilled technicians, cutting of the foil into small sections, hazardous etching conditions, long polishing and microscopy times, etc.; the neutron diffraction system has an automated sample loader and can fit larger foils, so there is minimal analysis preparation; the total spectrum acquisition time is ~ 1 hour per sample. The neutron diffraction results are limited by spectra refinement/calculation times and the availability of the neutron beam source. In the case of LANSCE at Los Alamos, the beam operates ~50% of the year. Following the lessons learned from these preliminary results, optimizations to the process and analysis can be made, and neutron diffraction can become a viable and efficient technique for gamma/alpha phase composition determination for nuclear fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Directed energy deposition of Haynes 282 nickel superalloy

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

36 - MATERIALS SCIENCE↗
DOE OSTI2025

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

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

Zhu, Zhikuan↗
DOE OSTI2026

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

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

Accelerator Physics↗
DOE OSTI2018

Analysis of Microstructure and Sliding Wear Behavior of Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} High-Entropy Alloy

Α Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} high-entropy alloy (HEA) of the well-known family of CoCrFeNiTi has been designed using empirical parameters. The aim of this design was the production of a HEA with fcc structure that gives ductile behavior and also high strength because of the solid solution effect. The VEC calculations (8.1) supported the fcc structure while the δ factor calculations (4.97) not being out of the limit values, advised a significant lattice distortion. From the other hand, the ΔΗ{sub mix} calculations (− 9.64 kJ/mol) gave strong indications that no intermetallic would be formed. In order to investigate its potential application, the Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} HEA was prepared by vacuum arc melting and a primary assessment of its surface degradation response was conducted by means of sliding wear testing using different counterbody systems for a total sliding distance of 1000 m. An effort to correlate the alloy’s wear response with the microstructural characteristics was attempted. Finally, the wear behavior of the Co{sub 1.5}CrFeNi{sub 1.5}Ti{sub 0.5} HEA was compared with that of two commercially used wear-resistant alloys. The results obtained provided some first signs of the high-entropy alloys’ better wear performance when tested under sliding conditions against a steel ball.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Fabrication, Analysis of Microstructure and Oxidation Resistance of Cemented C/C Composites by Laser

Cylindrical carbon–carbon composites have been cemented using a CO{sub 2} laser actuated by a raster scanning mirror system in a four-step sequence. Complete and homogenous surface cementation as well as thermal stability of the composites was sought after and achieved. The line of heat created from the laser beam impinged parallel to the axis of the pre-coated cylinder, while suspended from one end and slowly rotated. Four slurry compositions, all containing chloride salts from refractory elements, some combined with silicon, were pre-deposited by air spraying it over each specimen and then laser treated sequentially. Confined heat sublimed the chlorine ions resulting in silicide compounds that reacted with the carbon substrate to form a bonding layer. Microstructure characterization was performed using scanning electron microscopy, energy-dispersive spectroscopy and x-ray diffraction, immediately after the cementation was consolidated and after heat treated under argon. Preliminary oxidation weight loss tests were performed up to 1423 K under argon and air, revealing a 9.8 and 30.6% weight reduction, respectively, after 9 h of exposure. Cemented specimens were then coated with a glass overcoat layer that allowed them to perform moderately better against oxidation achieving up to a 28% weight loss after 20 h at 1273 K in air.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Weld Quality Assessment in Fiber Laser Weldments of Ti-6Al-4V Alloy

Laser welding experiments are performed on Ti-6Al-4V alloy sheets by adopting fiber laser. A special kind of workpiece fixture is designed and fabricated for providing shielding gas. After experiments, penetration depth, fusion zone width and heat-affected zone size at different locations within weld bead are measured and discussed in detail. Influence of line energies on the formation of non-uniform microstructure within weld bead is explored by conducting microstructural analysis. Various kinds of microstructural morphology of martensitic structure such as α′ martensite, blocky α, massive α and basket-weave microstructure are found in fusion zone. Experimentally, it is found that beam power is the key parameter for controlling penetration depth. Higher hardness is noticed within fusion zone due to the existence of large volume of α′ martensite. Tensile strength and hardness of welded specimens are increased with decreasing line energy. Small amount of micropores are also found in solidified weld bead. However, its sizes are in acceptable range as per BSEN:4678 standard. Most favorable welding condition is identified as a combination of beam power of 800 W and welding speed of 1000 mm/min which yields full penetration, narrower bead width, small heat-affected zone, minimal defects and acceptable mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2019

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

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

36 MATERIALS SCIENCE↗
DOE OSTI2019

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

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

36 MATERIALS SCIENCE↗
DOE OSTI2023

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

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

36 MATERIALS SCIENCE↗
DOE OSTI2015

Quantitative analysis of microstructure and deformation mechanisms during isothermal compression of Ti–5Al–5Mo–5V–1Cr–1Fe alloy

The effects of the processing parameters on the grain size and volume fraction of equiaxed α for Ti–5Al–5Mo–5V–1Cr–1Fe are quantitatively investigated using isothermal compression tests. The microstructure features, such as the morphology of equiaxed and acicular α phase, the dislocation distribution, the formation of substructure are in depth discussed with the help of transmission electron microscopy (TEM) and scanning electron microscopy (SEM) experiments so as to clarify the deformation mechanisms. The results show that few DRX α grains appear in the α + β phase region. In the β phase region, selective DRX occurs and the amount of DRX increases with increasing strain rate. DRV is main softening mechanism in the tested deformation temperature range. The elongated β grains are observed at medium deformation temperatures and lower strain rates. This phenomenon demonstrates that β phase is mainly involved in the deformation. At higher deformation temperatures and lower strain rates, acicular α is not observed for this alloy. Possible reason is that acicular α dissolves into the β matrix. - Highlights: • Few DRX α grains appear in the α + β phase region. • DRX occurs in the β phase region and raises with increasing strain rate. • α phase deforms less than β matrix at medium temperatures and lower strain rates. • Acicular α is not observed at higher temperatures and lower strain rates.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Hydrothermal corrosion studies on nitride fuels

Uranium mononitride (UN) has been identified as a candidate nuclear fuel for use in the current US light water reactor (LWR) fleet as well as in next generation nuclear plants (NGNP), largely due to its high uranium density and thermal conductivity. However, its hydrothermal corrosion performance in accident scenarios has not been thoroughly investigated. In this work, UN was synthesized using a hydride-de-hydride-nitride thermal synthesis route prior to sintering into dense compacts (> 90% TD). The compacts were corroded in a water filled autoclave up to 350 Celsius degrees and 125 atm. The kinetics of corrosion were characterized through phase analysis, mass loss, and microstructural analysis. The phases observed after hydrothermal corrosion correspond only to UN, UO{sub 2}, and UN{sub 2}; no U{sub 2}N{sub 3} was observed. Additionally, it appears that nitrogen uptake into the lattice of the solid product is a product of lattice strain and peak broadening, especially of the UN{sub 2} phase. UO{sub 2} appears to nucleate on the surface of the UN-UO{sub 2} monoliths and consumes the UN grain boundaries which suggests that in pure UN, UO{sub 2} formation proceeds from the surface and moves towards the core, but in samples with nominal concentrations of UO{sub 2}, oxidation from hydrolysis occurs throughout the bulk of the monoliths. Furthermore, it was demonstrated here that UN and UN-UO{sub 2} composites perform better than previously reported in the literature.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

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

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

42 ENGINEERING↗
DOE OSTI2020

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

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

36 MATERIALS SCIENCE↗