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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Influence of “Non-Interacting” Flux Concentration in Metallic Flux Growth Synthesis

In situ experiments probing the mechanisms of flux growth synthesis above 1100 °C, though challenging, enable direct observation of synthetic pathways, products, and metastable phases. In this study, in situ powder X-ray diffraction of flux growth synthesis up to 1200 °C was employed to investigate the role of Sn flux in the synthesis of praseodymium cobalt germanides. We demonstrate that metallic fluxes, with minimal incorporation into the target compounds, significantly influence the reaction products of flux growth synthesis of intermetallic compounds. Furthermore, the validation of in situ experiments with bulk synthesis is also presented.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Molten flux growth of single crystals of quasi-1D hexagonal chalcogenide BaTiS3

Abstract BaTiS 3 , a quasi-1D complex chalcogenide, has gathered considerable scientific and technological interest due to its giant optical anisotropy and electronic phase transitions. However, the synthesis of high-quality BaTiS 3 crystals, particularly those featuring crystal sizes of millimeters or larger, remains a challenge. Here, we investigate the growth of BaTiS 3 crystals utilizing a molten salt flux of either potassium iodide, or a mixture of barium chloride and barium iodide. The crystals obtained through this method exhibit a substantial increase in volume compared to those synthesized via the chemical vapor transport method, while preserving their intrinsic optical and electronic properties. Our flux growth method provides a promising route toward the production of high-quality, large-scale single crystals of BaTiS 3 , which will greatly facilitate advanced characterizations of BaTiS 3 and its practical applications that require large crystal dimensions. Additionally, our approach offers an alternative synthetic route for other emerging complex chalcogenides. Graphical Abstract

Materials Science↗
NASA NTRS2016

Low Temperature Flux Growth of 2H-SiC and Beta-Gallium Oxide

We present brief overview of our study on the low temperature flux growth of two very important novel wide bandgap materials 2H-SiC and Beta-gallium oxide (Beta-Ga2O3). We have synthesized and grown 5 millimeter to 1 centimeter size single crystals of Beta-gallium oxide (Beta-Ga2O3). We used a flux and semi wet method to grow transparent good quality crystals. In the semi-wet method Ga2O3 was synthesized with starting gallium nitrate solution and urea as a nucleation agent. In the flux method we used tin and other metallic flux. This crystal was placed in an alumina crucible and temperature was raised above 1050 degrees Centigrade. After a time period of thirty hours, we observed prismatic and needle shaped crystals of gallium oxide. Scanning electron microscopic studies showed step growth morphology. Crystal was polished to measure the properties. Bandgap was measured 4.7electronvolts using the optical absorption curve. Another wide bandgap hexagonal 2H-SiC was grown by using Si-Al eutectic flux in the graphite crucible. We used slight AlN also as the impurity in the flux. The temperature was raised up to 1050 degrees Centigrade and slowly cooled to 850 degrees Centigrade. Preliminary characterization results of this material are also reported.

Singh, N. B.↗
DOE OSTI2025

Synthesizing intermetallic thermoelectric materials using metal flux growth method

With zero energy poverty by 2050 goals, exploring innovative energy technologies is essential. Thermoelectric materials (TEMs) have the potential to harness waste heat and convert it to electricity (e.g., for spacecraft power, sensors, and cryogenic cooling). Two limitations of thermoelectric compounds are their low efficiency and limited pool of materials. Optimizing the efficiency of TEMs is challenging due to the interdependent relationship between electrical and thermal conductivity. A deeper understanding of electronic properties and lattice thermal conductivity is necessary to “understand, predict and ultimately control” the thermoelectric properties of TEMs. Understanding the influence of light-atom-doping and intrinsic defects on the electronic properties of the f-element containing TEMs are important questions that need to be answered to design and synthesize TEMs with optimal parameters. The purpose of this work is to understand how doping f-element based TEMs with light elements, such as carbon and boron, would impact the crystal structure, bond lengths, band gaps, and thermoelectric characteristics. High-quality f¬-element containing intermetallic single crystals are grown in metal flux media. In molten metal flux growth method, one or more low-melting metals such as aluminum, gallium, tin, and bismuth are used in excess as the reaction medium. As these are solution-state reactions, we can use lower temperatures than solid-state reactions and isolate the kinetic products instead of the thermodynamically stable compound. Then these are characterized using X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, magnetization, electrical and thermal conductivities, and thermoelectric power.

37 - INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL C↗
DOE OSTI2023

High pO2 Flux Growth and Characterization of NdNiO3 Crystals

Single crystals of the perovskite nickelate NdNiO3 with dimensions of up to 50 μm on edge have been successfully grown using the flux method at a temperature of 400 °C and oxygen pressure of 200 bar. The crystals were investigated by a combination of techniques, including high-resolution synchrotron X-ray single-crystal and powder diffraction and physical property measurements such as magnetic susceptibility and resistivity. Resistivity measurements revealed a metal-insulator transition (MIT) at TMIT~180 K with apparent thermal hysteresis; however, no superlattice peaks or peak splitting below TMIT, which corresponds to a structural transition from Pbnm to P21/n, was observed. The successful growth of NdNiO3 crystals at relatively low temperatures and oxygen pressure provides an alternative approach for preparing single crystals of interesting perovskites such as RNiO3 (R = Sm-Lu) and parent phases of superconducting square planar nickelates.

Wang, Xiaoli↗
DOE OSTI2022

Flux Growth of Cerium Nickel Gallides Studied by In Situ Neutron Diffraction

In this work, reactions of cerium and nickel in excess molten gallium were monitored by neutron diffraction during heating and cooling. The formation of binary intermediates CeGa 2 and Ni 2 Ga 3 was observed during heating. During cooling of the molten mixture from 900 °C, precipitation of BaAl 4 -type CeNi 0.74 Ga 3.26 occurred at 850 °C. Upon cooling to 650 °C, this compound reacted in the flux to form Ce 2 NiGa 10 and then Ce 2 NiGa 12 , the latter of which persisted to room temperature. Making use of this information, subsequent reactions were quenched at 750 °C to isolate crystals of CeNi 0.74 Ga 3.26 for further study. Similar reactions replacing Ce with La and quenching above 750 °C yielded LaNi 0.35 Ga 3.65 crystals. Magnetic susceptibility studies on CeNi 0.74 Ga 3.26 indicate that the cerium is trivalent; the Ce 3+ moments undergo a strongly anisotropic ferromagnetic ordering with moment perpendicular to the c axis below 7 K. Heat capacity data show little evidence of heavy fermion behavior. Resistivity measurements show that both LaNi0.35Ga3.65 and CeNi 0.74 Ga 3.26 exhibit metallic behavior. Density of states calculations support this and indicate that Ni/Ga mixing in the compound stabilizes the structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Warming and elevated CO 2 alter tamarack C fluxes, growth and mortality: evidence for heat stress-related C starvation in the absence of water stress

Climate warming is increasing the frequency of climate-induced tree mortality events. While drought combined with heat is considered the primary cause of this mortality, little is known about whether moderately high temperatures alone can induce mortality, or whether rising CO 2 would prevent mortality at high growth temperatures. In this study, we grew tamarack ( Larix laricina ) under ambient (400 p.p.m.) and elevated (750 p.p.m.) CO 2 concentrations combined with ambient, ambient +4 °C and ambient +8 °C growth temperatures to investigate whether high growth temperatures lead to carbon (C) limitations and mortality. Growth at +8 °C led to 40% mortality in the ambient CO 2 (8TAC) treatment, but no mortality in the elevated CO 2 treatment. Thermal acclimation of respiration led to similar leaf C balances across the warming treatments, despite a lack of photosynthetic acclimation. Photosynthesis was stimulated under elevated CO 2 , increasing seedling growth, but not leaf C concentrations. However, growth and foliar C concentrations were lowest in the +8 °C treatments, even with elevated CO 2 . Dying 8TAC seedlings had lower needle C concentrations and lower ratios of photosynthesis to respiration than healthy 8TAC seedlings, indicating that C limitations were likely the cause of seedling mortality under high growth temperatures.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2025

Investigation of Americium-Containing Phosphates, Silicates, Borates, Molybdates, and Fluorides Synthesized via High-Temperature Flux Crystal Growth

The crystal chemistry of americium-containing extended structures was investigated, and several classes of americium-containing solid-state oxide materials were obtained in single-crystal form via high-temperature flux crystal growth. This enabled the structural characterization of rare examples of ternary, quaternary, and penternary americium-containing silicates K 3 Am (Si 2 O 7 ) and Cs 6 Am 2 Si 21 O 48 , phosphates Na 3 Am (PO 4 ) 2 and K 3 Am (PO 4 ) 2 , borates Ba 3 Am 2 (BO 3 ) 4 and AmBO 3 , borate halides Ca 5 Am(BO 3 ) 4 Cl, molybdates Li 0.5 Am 0.5 MoO 4 , and fluorides CsAm 2 F 7 . Using these crystallographic data, the ionic radii of Am 3+ with coordination numbers of six (0.975 Å), seven (1.052 Å), and nine (1.162 Å) were established. A maximum entropy method (MEM) analysis was performed on the single-crystal X-ray diffraction data that were collected for K 3 Nd(PO 4 ) 2 /K 3 Am(PO 4 ) 2 , K 3 NdSi 2 O 7 /K 3 AmSi 2 O 7 , and NdBO 3 /AmBO 3 , to qualitatively compare the ionicities of the Nd–O and Am–O bonds. In conclusion, Raman spectroscopy data were collected on single crystals of K 3 Am(PO 4 ) 2 and compared to the calculated Raman spectrum of K 3 Am(PO 4 ) 2 obtained from DFT calculations.

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

Probing Phosphorus Solubility and Its Effect on Critical Temperature ( T c ) in the Helical Superconducting Magnet RbEuFe 4 As 4– x P x

RbEuFe 4 As 4 exhibits a rare combination of high-temperature superconductivity and noncollinear magnetism, originating from the FeAs and Eu layers, respectively. In order to fine-tune its superconducting and magnetic properties, we studied P-doped RbEuFe 4 As 4–x P x . To determine the value of x for which RbEuFe 4 As 4–x P x exists, members of the series have been synthesized in the form of relatively large-sized single crystals by a high-temperature flux growth technique using RbAs flux as well as polycrystalline powder by direct combination reactions between RbFe 2 As 2 and EuFe 2 As 2–x P x . The flux crystal growth reactions indicate that RbEuFe 4 As 4–x P x forms with the values of x ≤ 0.12, which is corroborated by the Rietveld refinement analysis on the products obtained from direct combination reactions. The solubility limit exists primarily due to the preferential site As(2) occupation by P in the RbEuFe 4 As 4 crystal structure. Finally, as x increases in RbEuFe 4 As 4–x P x , magnetization measurements reveal that the superconducting critical transition temperature (T c ) decreases, while the magnetic ordering temperature (T N ) remains almost unchanged in comparison to undoped RbEuFe 4 As 4 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Identifying the connections between grain growth and flux expulsion in low RRR niobium SRF cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2025

Identifying the Connections between Grain Growth and Flux Expulsion in Low RRR Niobium SRF Cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, Katrina N. [Chicago U.] (ORCID:00000003256↗
DOE OSTI2025

Identifying the Connections between Grain Growth and Flux Expulsion in Low RRR Niobium SRF Cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, Katrina [Chicago U.] (ORCID:00000003256133↗
DOE OSTI2026

Identifying the connections between grain growth and flux expulsion in low RRR niobium SRF cavities

The SRF community has shown that high temperature annealing can improve the flux expulsion of niobium cavities during cooldown. The required temperature will vary between cavities and different batches of material, typically around 800 C and up to 1000 C. However, for niobium with a low residual resistance ratio (RRR), even 1000 C is not enough to improve its poor flux expulsion. The purpose of this study is to observe the grain growth behavior of low RRR niobium coupons subjected to high temperature annealing to identify the mechanism for improving flux expulsion. We observe that low RRR material experiences less grain growth than high RRR when annealed at the same temperature. We search for the limitations to grain growth in low RRR material and develop a diagnostic based on grain structure to determine the appropriate recipe for good flux expulsion. The results of this study have the potential to unlock a new understanding on SRF materials and enable the next generation of high Q/high gradient surface treatments.

Howard, K. [Chicago U.] (ORCID:0000000325613308)↗