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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 145 records · Page 8
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Mechanisms for high creep resistance in alumina forming austenitic (AFA) alloys

Castable alumina forming austenitic (AFA) alloys have demonstrated superior creep life and oxidation resistance at temperatures exceeding 800⁰C. Despite the success in the applicability of these alloys in extreme environments, there is a limited understanding of the deformation modes and the influence of each alloying element guiding the alloy design strategies that could further enhance the creep strength of these AFA alloys, particularly at temperatures at and above 900⁰C. In this study, we reveal the mechanism underpinning the superior creep performance of castable AFA alloys that involves suppressing primary carbide formation through minor compositional modification. This approach results in a three-fold increase in creep strength at 900⁰C and 50 MPa. Here, by employing integrated characterization techniques, we analyzed the microstructures of two AFA alloys, both before and after the creep process. We discovered that the suppression of primary carbides permits the in-situ clustering of now-available interstitial elements such as C, Si, and O during high-temperature creep. This improved solid solution strengthening and reduced stacking fault energy of the alloy. Moreover, it also enabled controlled secondary carbide formation during testing, further improving the creep resistance. These findings underline the important interplay between alloy composition, microstructure, and creep properties, and offer a promising design strategy for developing economical high-temperature Fe-based alloys suitable for advanced applications.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Hydration of alumina (Al 2 O 3 ) toward advancing aluminum particles for energy generation applications

Transforming metal particle combustion may require alteration of the metal oxide passivation shell surrounding the metal core. One approach for aluminum (Al) relies on the hydrated form of the metal oxide to incite surface reactions. Here, this study explores the conditions required for hydrating alumina (Al 2 O 3 ) particles and then extends those conditions toward hydration of the Al 2 O 3 passivation layer surrounding an Al core particle. By raising the pH of the water slurry to 11 and controlling temperature and time in slurry (i.e., aging), aluminum hydroxide Al(OH) 3 formation from Al 2 O 3 particles was optimized. The procedure was then extended to Al nanoparticles (nAl). Even though heating and extended aging time in slurry proved advantageous for Al 2 O 3 particles, these conditions were discarded for nAl particles because they favored formation of AlOOH, a less desirable hydrate. Through microscopy, spectroscopy, X-ray diffraction, and thermal analyses, results indicate that for a pH range of 11.26–11.56, the original Al 2 O 3 shell on Al particles transformed into Al(OH) 3 . Results indicate a feasible path forward towards producing new shell chemistries that may result in more directed energy from metal particle combustion.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Chromium evaporation and oxidation characteristics of alumina-forming austenitic stainless steels for balance of plant applications in solid oxide fuel cells

The chromium (Cr) evaporation behavior of several different types of iron (Fe)-based AFA alloys and benchmark Cr 2 O 3 -forming Fe-based 310 and Ni-based 625 alloys was investigated for 500 h exposures at 800 °C to 900 °C in air with 10% H 2 O. The Cr evaporation rates from alumina-forming austenitic (AFA) alloys were ~5 to 35 times lower than that of the Cr 2 O 3 -forming alloys depending on alloy and temperature. The Cr evaporation behavior was correlated with extensive characterization of the chemistry and microstructure of the oxide scales, which also revealed a degree of quartz tube Si contamination during the test. As a result, long-term oxidation kinetics were also assessed at 800 to 1000 °C for up to 10,000 h in air with 10% H 2 O to provide further guidance for SOFC BOP component alloy selection.

08 HYDROGEN↗
DOE OSTI2020

Rates of levoglucosanol hydrogenolysis over Brønsted and Lewis acid sites on platinum silica-alumina catalysts synthesized by atomic layer deposition

Nanoscale coatings of AlO x were deposited onto SiO 2 using atomic layer deposition (ALD) to synthesize amorphous silica-alumina (SiAl) catalysts, and these catalysts were investigated for levoglucosanol (Lgol) hydrogenolysis. With decreasing Al 2 O 3 loading, the ratio of Brønsted to Lewis acid sites, measured by NH 3 -TPD and pyridine-FTIR, systematically increases, while the Al coordination, measured by solid state 27 Al NMR, decreases. These structural changes correspond to an increasing mass-normalized rate of Lgol hydrogenolysis. We model the mass-normalized reaction rate as the sum of independent contributions from Brønsted and Lewis sites, showing that Brønsted acid sites on ALD-AlO x /SiO 2 catalysts have a 6-times higher turnover frequency (TOF) than Lewis acid sites on these catalysts. Additionally, Lewis acid sites on ALD-AlO x /SiO 2 catalysts (potentially related to Al(V) species) have a 4-times higher TOF than Lewis acid sites on bulk γ-Al 2 O 3 . The overall mass-normalized reactivity of ALD-AlO x /SiO 2 catalysts is due to Lewis acid sites at the highest Al 2 O 3 loading, while it is predominantly due to Brønsted acid sites at the lowest Al 2 O 3 loadings. In conclusion, this work provides a new approach to synthesize amorphous SiAls with tunable Brønsted/Lewis acid site ratio and reveals differences in the reactivity of Brønsted and Lewis acid sites on these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2026

3D analysis of abnormal grain growth in calcia doped alumina in the presence of large pores

Abnormal grain growth has been previously found to increase with the inclusion of large pores (∼60 µm in diameter) in 80 ppm calcium doped alumina. However, the two-dimensional analysis could not accurately describe the proximity of the abnormal grains and pores to establish a correlation. This study uses laboratory-based diffraction contrast tomography and x-ray computed tomography to spatially map the pores and abnormal grains in 3D. A preference towards the formation of abnormal grains near large pores is found when compared to all potential sites. This finding supports that the pores may be a nucleation site for complexion transitions that promote abnormal grain growth. The growth of the abnormal grains in a subsequent heat treatment at 1600°C for 16 hrs was also studied. The elongation along the principal axes is similar for both small and large grains, again supporting that abnormal grain growth was facilitated by a complexion transition.

Abnormal grain growth↗
DOE OSTI2025

Chemical interaction and compatibility of uranium mononitride and alumina forming austenitic stainless steel

Uranium mononitride (UN) and alumina forming austenitic (AFA) stainless steel are a potential fuel-cladding combination for the lead-cooled fast reactor (LFR). Chemical compatibility between UN and AFA steel needs to be verified before implementation in a nuclear reactor. Diffusion couple experiments at 823 K and 1023 K were conducted for nonirradiated UN samples in contact with as-cast (no thermally grown Al 2 O 3 ) and preoxidized (with thermally grown Al 2 O 3 ) AFA for 500 and 1000 h in an inert environment. Preoxidized AFA exhibited little to no interaction with all UN samples tested at both 823 K and 1023 K, displaying the stability and capability of the Al 2 O 3 layer to prevent chemical interaction and inter-diffusion with UN. Chemical interaction occurs between UN and as-cast AFA. At 1023 K, an aluminum and nitrogen rich phase (likely AlN) formed along the interface of as-cast AFA and UN samples. At 823 K the AlN phase was not prominently observed due to the reduced diffusivity of aluminum through AFA. The aluminum and nitrogen-enriched phase was also observed in a high temperature pressure-assisted test sample of UN and as-cast AFA thermally treated at 1373 K. Finally, in UN samples doped with a low weight percent of UO 2 (< 3 wt%), AlN was not detected along the interface at either temperatures, and an Al 2 O 3 layer likely formed along the interface and prevented further chemical interaction between UN and as-cast AFA.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Strength stability at high temperatures for additively manufactured alumina forming austenitic alloy

Several fast-spectrum nuclear reactors designed to generate high power (~450 MWe) rely on forced convection of media such as supercritical CO 2 , sodium, or liquid lead to cool the nuclear core, operating at temperatures up to 600 °C. Cost-effective, high-strength Fe-based alumina forming austenitic (AFA) alloys are a promising candidate for the fabrication of critical nuclear components. This study investigated laser powder bed fusion (LPBF) processing of an AFA alloy composition optimized for improved creep resistance. Electron microscopy revealed an elongated grain structure along the build direction with a fine sub-grain cellular structure decorated with (Cr,Fe,Nb) 23 C 6 carbide precipitates at the intercellular boundaries. Finally, at temperatures of 20–900 °C, the LPBF alloy's superior tensile properties compared to its arc-melted counterpart and other advanced steels (e.g., SS316) were attributed to the distribution of nano-sized carbide precipitates, whereas the high ductility was attributed to the LPBF alloy's elongated grain structure.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Atomically Dispersed Tin-Modified $\gamma$-alumina for Selective Propane Dehydrogenation under H 2 S Co-feed

Developing an earth-abundant catalyst that is sulfur-tolerant, active, and highly selective is of great interest for valorizing natural gas streams containing sour gas. Here, a tin-modified alumina catalyst is reported that is stable and selective for propane dehydrogenation in the presence of percent quantities of H 2 S in the feed. In particular, Sn/Al 2 O 3 –S catalysts with 1.5–5% Sn content exhibit 98% selectivity with up to 16% conversion at 560 °C during the fourth cycle. Experimental and computational characterization shows that the active sites are the defect tricoordinated Al atoms. H 2 S pretreatment further modifies a portion of these sites via exchanging a neighboring oxygen atom with sulfur, thereby rendering them more active and selective. At low loadings, Sn is atomically dispersed and selectively binds to hydroxyl groups or oxygen atoms on Al 2 O 3 . This prevents the formation of original (unmodified) defect sites on Al 2 O 3 and improves overall selectivity. The activity and selectivity of the catalyst are heavily dependent on the chemical potential of sulfur and hydrogen because they influence both the relative concentration of the two types of sites and the overall reaction mechanism. Finally, the catalyst can be regenerated fully under a pure H 2 S stream, thereby precluding treatment under oxygen, which can lead to sintering.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Thermal shock resistance of additively manufactured alumina

The mechanical behavior and cracking patterns of thermally-shocked additively manufactured alumina were investigated. The flexural strength of test specimens that had been heated to temperatures ranging from 200°C to 1000°C and then rapidly quenched in water was determined at ambient temperature by four-point bending. Results indicated that the surface cracking patterns had a multifractal structure and that an increase in the thermal shock temperature led to an increase in the density and uniformity of the crack network. Further, the flexural strength results were analyzed with Weibull statistics, where the Weibull moduli for most of the thermal shock conditions tested were found to be statistically indistinguishable. It was also found that a significant decrease (~50%) in flexural strength occurred for heating temperatures ≥300°C. The effect of the manufacturing method on cracking patterns is discussed, as well as the implication of the material behavior for practical applications of these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Evaluating Pretreatment Strategies with Modeling for Reducing Scaling Potential of Reverse Osmosis Concentrate: Insights from Ion Exchange and Activated Alumina

Reverse osmosis concentrate (ROC) treatment is critical for enhancing water recovery and minimizing concentrate volume for disposal, especially in regions facing water scarcity. This study investigates the application of ion exchange (IX) resins and activated alumina (AA) as pretreatment strategies to mitigate scaling in ROC due to high concentrations of total dissolved solids, hardness (Ca 2+ and Mg 2+ ), and silica. Through a series of Langmuir isotherms, continuous column experiments, and model simulation, two types of strong acid cation IX resins and three types of strong base anion IX resins alongside three types of AA were evaluated. Results indicate that AA exhibits superior performance in silica removal, achieving up to a 65% reduction and maintaining performance for up to 800 bed volume without reaching saturation. Model simulation of a secondary reverse osmosis treating ROC after the IX and AA pretreatment indicated an additional water recovery of ~70% using antiscalants. This study demonstrates the potential for achieving higher water recovery while also identifying opportunities for pretreatment improvement. Challenges such as the limited IX capacity treating ROC, which requires frequent regeneration and increases operational costs, along with the restricted regeneration capacity of AA, underscore the importance of innovation. These findings emphasize the critical need for developing advanced materials and optimized strategies to further enhance the efficiency of ROC treatment processes.

activated alumina↗
NASA NTRS2000

Life Studies of Metal Films on Beta-Alumina at High Temperature

Applications of metallic films on sodium beta-alumina solid electrolyte (BASE) ceramic in technology for the alkali metal thermal to electric converter (AMTEC) include both electrode and metallization functions.

AMTEC beta-alumina Thermal-to-Electric Energy Conv↗
DOE OSTI2022

Ultra‐Thin Single‐Particle‐Layer Sodium Beta‐Alumina‐Based Composite Polymer Electrolyte Membrane for Sodium‐Metal Batteries

Inorganic/organic composite polymer electrolytes (CPEs) with good flexibility and electrode contact have been pursued for solid-state sodium-metal batteries. However, the application of CPEs for high energy density solid-state sodium-metal batteries is still limited by the low Na + conductivity, large thickness, and low ion transference number. Herein, an ultra-thin single-particle-layer (UTSPL) composite polymer electrolyte membrane with a thickness of ≈20 µm straddled by a sodium beta-alumina ceramic electrolyte (SBACE) is presented. A ceramic Na + -ion electrolyte that bridges or percolates across an ultra-thin and flexible polymer membrane provides: 1) the strength and flexibility from the polymer membrane, 2) excellent electrolyte/electrode interfacial contact, and 3) a percolation path for Na + -ion transfer. Owing to this novel design, the obtained UTSPL-35SBACE membrane exhibits a high Na+-ion conductivity of 0.19 mS cm -1 and a transference number of 0.91 at room temperature, contributing to long-term cycling stability of symmetric sodium cells with a small overpotential. The assembled quasi-solid-state cell with the as-prepared UTSPL-35SBACE membrane displays superior cycling performance with a discharge capacity of 105 mAh g -1 at 0.5 °C rate after 100 cycles and excellent rate performance (82 mAh g -1 at 5 °C rate) at room temperature with the potassium manganese hexacyanoferrate (KMHCF)@CNTs/CNFs cathode, where KMHCF refers to potassium manganese hexacyanoferrate.

25 ENERGY STORAGE↗
DOE OSTI2025

In Situ/Operando Probing of Dynamic Phase Structures of Alumina‐Supported Ultrasmall Copper‐Gold Alloy Nanoparticles Under Reaction Conditions

Abstract The ability to control phase structures and surface sites of ultrasmall alloy nanoparticles under reaction conditions is essential for preparing catalysts by design. This is, however, challenging due to limited understanding of the atomic‐scale phases and their correlation with the ensemble‐averaged structures and activities of catalysts during catalytic reactions. We reveal here a dynamic structural stability of alumina‐supported ultrasmall and equiatomic copper‐gold alloy nanoparticles under reaction conditions as a model system in the in situ/operando study. In situ atomic‐scale morphological tracking under oxygen reveals temperature‐dependent dynamic crystalline‐amorphous dual‐phase structures, showing dynamic stability over an elevated temperature range. This atomic‐scale dynamic phase stability coincides with a “conversion plateau” observed for carbon monoxide oxidation on the catalyst. It is substantiated by the stable lattice ordering/disordering structures and surface sites with oscillatory characteristics shown by operando ensemble‐average structural tracking of the catalyst during the oxidation reaction. The understanding of the atomic‐scale dynamic phase structures in correlation with the ensemble‐average dynamic ordering/disordering phase structures and surface sites provides fresh insights into the unique synergy of the supported alloy nanoparticles. This understanding has implications for the design and structural tuning of active and stable ultrasmall alloy catalysts under elevated temperatures.

Chemistry↗
DOE OSTI2021

Indirectly Detected DNP-Enhanced 17 O NMR Spectroscopy: Observation of Non-Protonated Near-Surface Oxygen at Naturally Abundant Silica and Silica-Alumina

Recent studies have shown that dynamic nuclear polarization (DNP) can be used to detect 17 O solid-state NMR spectra of naturally abundant samples within a reasonable experimental time. Observations using indirect DNP, which relies on 1 H mediation in transferring electron hyperpolarization to 17 O, are currently limited mostly to hydroxyls. Direct DNP schemes can hyperpolarize non-protonated oxygen near the radicals; however, they generally offer much lower signal enhancements. In this study, we demonstrate the detection of signals from non-protonated 17 O in materials containing silicon. The sensitivity boost that made the experiment possible originates from three sources: indirect DNP excitation of 29 Si via protons, indirect detection of 17 O through 29 Si nuclei using two-dimensional 29 Si{ 17 O} D-HMQC, and Carr-Purcell-Meiboom-Gill refocusing of 29 Si magnetization during acquisition. This 29 Si-detected scheme enabled, for the first time, 2D 17 O– 29 Si heteronuclear correlation spectroscopy in mesoporous silica and silica-alumina surfaces at natural abundance. In contrast to the silanols showing motion-averaged 17 O signals, the framework oxygens exhibit unperturbed powder patterns as unambiguous fingerprints of surface sites. Furthermore, along with hydroxyl oxygens, detection of these moieties will help in gaining more atomistic-scale insights into surface chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Revisiting Wagner’s Criteria to Predict Establishment and Retention of Alumina Scales on Ternary NiCrAl Alloys

Despite the advent of numerical modeling approaches and high-performance computing infrastructure, the design and development of corrosion-resistant high temperature alloys (> 500 °C) continue to be largely empirical and typically involve extensive experimentation. This is mainly due to the lack of a single unified physics-based model that can address the impact of multiple competing factors such as time, environment, alloy composition, microstructure, and geometry. The classical Wagner’s criteria have been foundational to estimate the minimum concentrations required of an oxide-forming element to establish and sustain a protective oxide scale. However, the formulation is primarily limited to lower-order alloy systems (binary alloys) and ignores the time dependence of subsurface compositional changes in the alloy. The lack of key data on the temperature and composition dependence of the solubility and transport of oxidants in multicomponent-multiphase alloys further exacerbates the problem. In the present work, a few of these limitations were addressed using a flux-based approach (FLAP) which tracks the spatiotemporal evolution of the fundamental flux balance between oxygen and the oxide-forming elements to enable the prediction of the formation of an external alumina scale in ternary NiCrAl alloys. In conclusion, the modeling results were validated with the literature findings and additional experimental work conducted in the present work.

36 MATERIALS SCIENCE↗