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All sources NASA NTRS DOE OSTI

DOE OSTI2024

On the product phases and the reaction kinetics of carbothermic reduction of UO 2 +C at relatively low temperatures

The synthesis of UC using carbothermic reduction of UO 2 and C mixtures has been well studied at high temperatures. However, the product phase behavior of carbothermic reduction at low temperatures (≤1773 K) is not well studied. Such a study is important as low temperatures permit single phase UC synthesis without forming secondary higher carbides, and it further supports the knowledge base of the process that needs to be used for transuranic elements such as plutonium that have high vapor pressures at elevated temperatures. Therefore, a low temperature carbothermic reduction of two different C/UO 2 molar ratios under inert and reducing environments have been studied here. Two different sample holding crucibles, alumina (Al 2 O 3 ) and graphite, were also used here to differentiate the hypostoichiometric (UC 1-a ) and oxygen dissolved (UC 1-x O x ) uranium monocarbide phases adding more details on the two systems. Also, the reaction kinetics involved in the formation of UC via the carbothermic reduction of UO 2 +C using product phases instead of evolved gases such as carbon monoxide is reported here. Under inert atmospheres but with significant oxygen partial pressures, the low temperature carbothermic reduction of UO 2 +C produced up to 90 wt.% UC 1-x O x type oxycarbides as was confirmed by Xray powder diffraction. Reducing Ar-4%H 2 environments at these temperatures were not successful in synthesizing UC as it reduces the amount of C required for the carbothermic reduction, leaving UC phase at a non-equilibrium state. Inert atmospheres with low or negligible oxygen partial pressures on the other hand produced near stoichiometric UC at high phase purity, especially at 1673 – 1773 K temperature range. An activation energy of 377±75 kJmol -1 was also calculated using product phase concentrations of the carbothermic reduction of UO 2 +C under these inert Ar (g) atmospheres.

36 MATERIALS SCIENCE↗

NASA NTRS1996

Molecular Dynamics Simulation of Carbon Nanotube Based Gears

We used molecular dynamics to investigate the properties and design space of molecular gears fashioned from carbon nanotubes with teeth added via a benzyne reaction known to occur with C60. A modified, parallelized version of Brenner's potential was used to model interatomic forces within each molecule. A Leonard-Jones 6-12 potential was used for forces between molecules. One gear was powered by forcing the atoms near the end of the buckytube to rotate, and a second gear was allowed.to rotate by keeping the atoms near the end of its buckytube on a cylinder. The meshing aromatic gear teeth transfer angular momentum from the powered gear to the driven gear. A number of gear and gear/shaft configurations were simulated. Cases in vacuum and with an inert atmosphere were examined. In an extension to molecular dynamics technology, some simulations used a thermostat on the atmosphere while the hydrocarbon gear's temperature was allowed to fluctuate. This models cooling the gears with an atmosphere. Results suggest that these gears can operate at up to 50-100 gigahertz in a vacuum or inert atmosphere at room temperature. The failure mode involves tooth slip, not bond breaking, so failed gears can be returned to operation by lowering temperature and/or rotation rate. Videos and atomic trajectory files in xyz format are presented.

Han, Jie↗

DOE OSTI2025

Synthesis of Yttrium Oxide Particles for Interfacial Water Radiolysis Studies

Radiolysis of water produces hydrogen gas (H2), posing safety issues for nuclear reactors. Metal oxides can impact H2 formation when water is present on metal oxide surfaces. This presentation focuses on the development of a controllable synthesis of spherical yttrium oxide (Y2O3), that later will be tested for H2 production in water radiolysis. Y2O3 was synthesized via hydrothermal hydrolysis precipitation to form yttrium hydroxide (Y(OH)3), followed by high temperature decomposition to form Y2O3. Various synthesis conditions were tested to determine their impact on particle morphology including reaction time, cooling rate, reactant concentration, and inert atmospheres. Through short reaction times and rapid cooling rate, spherical, relatively uniform particles of 350 nm were obtained. Despite inert atmospheres, carbonate formation occurred in all particles. A calcination temperature of 800°C is necessary to remove impurities. Future work will aim to reduce carbonate formation and improve particle uniformity. The synthetic procedure will be translated to other metal ions to study their impact on interfacial radiolysis.

08 - HYDROGEN↗

DOE OSTI2021

Development of a Nitrogen and Magnesium Oxide based Class A, B & D Suffocating Fire System (SFSS) for Gloveboxes

Testing related to the development and performance of a “Proof of Concept” Nitrogen/Magnesium Oxide Suffocating Fire System (SFSS) was conducted at Fire and Pump Service Group (FPSG) located in Rancho Dominguez, California. The SFSS Engineering Team (SFSSET), consisting of FPSG and Los Alamos National Laboratory (LANL) personnel researched, developed a prototype, and conducted testing to determine effective means to deliver magnesium oxide (MgO) sand into a glovebox (GB) in a class D fire event. The prototypes development also established the effective coverage area of a magnesium oxide suppression system as well as demonstrated that the GB inert atmosphere could be maintained during and after the release of the MgO sand to control Class A, B and D fires. Previous testing conducted on nitrogen based SFSS provided evidence that the nitrogen based SFSS controlled Class A and B fires (Ralph Clayton, Los Alamos National Laboratory, Brandon Troc and Frank Broidy, Fire and Pump Service Group 2020).Final testing was conducted within a mock GB capable of simulating an inert glovebox atmosphere. Testing demonstrated that the inert atmosphere can be maintained during and after discharge of the MgO sand over a coverage area.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2022

Production of graphene-structured products from coal using thermal molten salt process

The invention provides a method for the production of graphene-structured products. The method generally comprises contacting at a conversion temperature ranging from about 850° C. to about 1100° C. in an inert atmosphere coal with a molten salt to produce a graphene-structured product. In an alternate embodiment, the method comprises contacting at a conversion temperature ranging from about 850° C. to about 1100° C. in an inert atmosphere coal with a molten salt to produce a graphene-structured product; and, separating a rare earth element from the graphene-structured product.

Shi, Fan↗

DOE OSTI2020

Surface-Activated Corrosion in Tin–Lead Halide Perovskite Solar Cells

Mixed tin–lead halide perovskite solar cells have promising power conversion efficiencies, but long-term stability is still a challenge. Here, we examine the stability of a 60:40 tin–lead perovskite to better understand diminished device performance upon thermal treatment, both in ambient and inert atmosphere. Operando X-ray diffraction shows a stable bulk structure of the perovskite absorber, leading to the hypothesis that surface chemistry dominates the degradation mechanism. X-ray photoelectron spectroscopy reveals two new observations post-thermal annealing that accompany previously reported Sn 4+ evolution: (i) the formation of I 3 – intermediates preceding I 2 loss at the surface and (ii) evidence of under-coordinated tin and lead surface sites (Sn δ<2+ and Pb δ<2+ , respectively) in inert and ambient conditions. These two species indicate an activated corrosion (i.e., both oxidation and reduction) process at the surface as a possible chemical pathway for degradation, which is expected to be accelerated under operando voltage and light biases.

14 SOLAR ENERGY↗

NASA NTRS1970

The Varestraint test for refractory metals, task 2

The principles of the Varestraint test were applied to the evaluation of refractory metal alloys. This required development of a special test apparatus employing a modest specimen size for improved economy and compatible with the high purity inert atmosphere required for welding these alloys. Minimum specimen size is desirable because of the high cost of these alloys and also to permit timely testing of limited production developmental alloys. The Varestraint apparatus satisfies these requirements by providing a timely and economic test for hot crack sensitivity. This test can be used both for alloy development and production surveillance. The test apparatus was designed for use in vacuum purged dry boxes and is completely compatible with high purity inert atmosphere. Augmented strain can be varied continuously from 1/4% thru 4%. In addition to varying the augmented strain, the primary Varestraint variable, the effect on hot cracking of varying other weld parameters such as unit weld length heat input have also been studied. Test reproducibility, in terms of bending or strain rate, was demonstrated using high speed photography.

Lessmann, G. G.↗

NASA NTRS1987

Inerting and atmospheres

It is argued that fires are dependent primarily on the concentration of oxygen, whereas life is dependent on the partial pressure of oxygen. It follows that in an inhabited capsule it should be possible to exercise a certain amount of willful control over fire and still maintain habitability by proper selection of the composition of the atmosphere. This leads to two concepts in the control of fires in confined spaces by controlling atmospheric composition: the first, to lower the overall potential hazard by maintaining the percent of oxygen in the capsule below that of air, and second, to provide for the emergency extinguishment of a fire by sudden flooding with nitrogen. Several relevant charts and graphs are presented.

Carhart, Homer W.↗

NASA NTRS1991

Method for the determination of lignin content of a sample by flash pyrolysis in an atmosphere of hydrogen or helium and method therefor

The lignin content of wood, paper pulp or other material containing lignin (such as filter paper soaked in black liquor) is more readily determined by flash pyrolysis of the sample at approximately 550.degree. C. in a reducing atmosphere of hydrogen or in an inert atmosphere of helium followed by a rapid analysis of the product gas by a mass spectrometer. The heated pyrolysis unit as fabricated comprises a small platinum cup welded to an electrically-heated stainless steel ribbon with control means for programmed short duration (1.5 sec, approximately) heating and means for continuous flow of hydrogen or helium. The pyrolysis products enter an electron-ionization mode mass spectrometer for spectral evaluation. Lignin content is obtained from certain ratios of integrated ion currents of many mass spectral lines, the ratios being linearly related to the Kappa number of Klason lignin.

Shakkottai, Parthasarathy↗

DOE OSTI2022

Synthesis of high-density olivine LiFePO 4 from paleozoic siderite FeCO 3 and its electrochemical performance in lithium batteries

The lithium-ion cathode material olivine LiFePO 4 (LFP) has been synthesized for the first time from natural paleozoic iron carbonate (FeCO 3 ). The ferrous carbonate starting material consists of the mineral siderite at about 92 wt. % purity. Because FeCO 3 has divalent iron, the reaction with lithium dihydrogen phosphate (LiH 2 PO 4 ) provides a unique method to develop iron-(II) containing LFP in an inert atmosphere. Since siderite FeCO 3 is a common mineral that can be directly mined, it may, therefore, provide an inexpensive route for the production of LFP. After carbon-coating, the LFP yields a capacity in the range of 80–110 mAh g -1 LFP (in one chosen specimen sample), which is lower than commercially available LiFePO 4 (150–160 mAh g -1 LFP ). However, the tap density of LFP derived from siderite is noticeably high at 1.65 g cm -3 . The material is likely to be improved with powder purification, nanosized processing, and more complete carbon-coating coverage with increased optimization.

36 MATERIALS SCIENCE↗

NASA NTRS1995

Safety-Enclosure System For MOCVD Process Chamber

Safety-enclosure system filled with nitrogen surrounds reaction chamber in which metallo-organic chemical vapor deposition (MOCVD) performed. Designed to protect against explosions and/or escaping toxic gases and particulates. Gas-purification subsystem ensures during loading and unloading of process materials, interior of MOCVD chamber exposed to less than 1 ppm of oxygen and less than 5 ppm of water in nitrogen atmosphere. Toxic byproducts of MOCVD process collected within inert atmosphere. Enclosure strong enough to contain any fragments in unlikely event of explosion.

Singletery, James, Jr.↗

DOE OSTI2022

Container Evaluation: Analysis of the Swagelok Knuckle with Viewport as an Approved Hermetically Sealed Inner Container

This report outlines the results from the water ingress test, helium leak test and additional atmosphere testing for the Swagelok knuckle with viewport container further referred to as the SKV. This container is constructed from a standard union vacuum fitting, 1.33” conflat to 0.5” male VCR, a 1.33” conflat fused silica lensed viewport fitting, and a 0.5 inch VCR cap. The primary intended use of this container is to store Pu metal samples in the vault for a time interval exceeding 40 years. The samples need to be contained in an air free environment to ensure that the material does not oxidize over time. The container viewport is a critical design feature that will help the operators visually inspect and evaluate the state of the metal samples prior to opening the container. These containers are advertised as leak tight, but experimental tests were performed to test the water resistant criteria and the gas leaking criteria set forth by the TA-55 Criticality Safety Program. The results of the water ingress test show that the container is water-tight, with no signs of water penetrating the container within the required guidelines outlined in TA55-AP-522. The preliminary He leak test performed demonstrate that the conflat window port and VCR cap are able to maintain a hermetic seal. Additionally, all containers will be He leak tested independently by the manufacturer prior to shipping to LANL. A third voluntary test was added to assess the container’s ability to hold atmosphere, with successful results indicating the container is able to hold inert atmosphere to prevent lanthanum metal oxidation. It is the conclusion of the authorsthat there is enough evidence through the test conducted and outlined within this document that the proposed container meets the definition of a water-tight container, and it is able to provide a hermetic seal.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1958

The Thermal Stability of Unsymmetrical Dimethylhydrazine

The thermal stability of unsymmetrical dimethylhydrazine was investigated in a static system simulating conditions in an almost-empty fuel tank. The self-ignition temperature and spontaneous decomposition temperature of the pure fuel were determined at atmospheric pressure to be 454 and 740 F. respectively, with the larger (740 F) value, obtained in an inert atmosphere of nitrogen, representing the minimum temperature that would cause a rapid exothermic reaction. The addition of 40 weight percent dimethylenetriamine to unsymmetrical dimethylhydrazine did not significantly affect these properties.

Spakowski, Adolph E.↗

DOE OSTI2025

Continuous manufacturing of carbon foam structures at atmospheric pressure

A method of manufacturing essentially crack-free carbon foam structures and carbon foam structures made in single-piece flow through a continuous kiln under inert atmosphere at atmospheric pressure. This process greatly reduces the cost to manufacture by reducing manufacturing time and increasing the ability to integrate automation equipment.

Olson, III, Rudolph Andrew↗

DOE OSTI2026

Balancing moisture and oxygen can match the crystallization dynamics of inert halide perovskite processing

Understanding crystallization in ambient environments is essential for scaling the fabrication of halide perovskite solar cells. Antisolvent-free perovskite deposition offers improved compatibility with high-throughput processing but introduces distinct crystallization dynamics relative to the more ubiquitous use of antisolvents in lab-scale perovskite fabrication. These dynamics are driven by interactions between solutes, solvent and the deposition environment. Using in situ wide-angle X-ray scattering during spin-coating and annealing, we demonstrate how relative humidity (RH) and oxygen, can be tuned to drive polytype evolution during ambient crystallization of formamidinium lead iodide to match that of inert synthesis and achieve comparable film and device quality. In an inert (N 2 ) environment, we find that perovskite films follow a well-established 2H → 3C phase transformation with a short period of coexistence of the 4H and 6H phase during heating. During crystallization in dry air (RH 0%), the added presence of oxygen leads to the dominance of 4H intermediate for an extended duration, establishing a 2H → 4H → 3C pathway. Introducing low humidity (RH 10%) suppresses the 4H phase to a short-lived intermediate above 100 °C, facilitating a more direct transition to the desired 3C phase and almost replicating the crystallization behavior observed under inert conditions. Interestingly, films crystallized under RH 10% show a lower onset temperature for the perovskite 3C phase than under N 2 . At higher humidity (RH 40%), the strong interaction of oxygen and moisture with iodoplumbates appears to stabilize higher order polytypes (4H and 6H). Devices fabricated under RH 10% achieve higher efficiency and enhanced stability compared to those produced under inert atmosphere. These findings provide mechanistic insight into crystallization pathways in different environments and provide a framework to transfer processes from inert to ambient conditions. The results highlight the critical role of controlled humidity in tuning antisolvent-free perovskite crystallization for scalable processing.

Hossain, Maimur [Univ. of California, San Diego, C↗

NASA NTRS1994

A high temperature testing system for ceramic composites

Ceramic composites are presently being developed for high temperature use in heat engine and space power system applications. The operating temperature range is expected to be 1090 to 1650 C (2000 F to 3000 F). Very little material data is available at these temperatures and, therefore, it is desirable to thoroughly characterize the basic unidirectional fiber reinforced ceramic composite. This includes testing mainly for mechanical material properties at high temperatures. The proper conduct of such characterization tests requires the development of a tensile testing system includes unique gripping, heating, and strain measuring devices which require special considerations. The system also requires an optimized specimen shape. The purpose of this paper is to review various techniques for measuring displacements or strains, preferably at elevated temperatures. Due to current equipment limitations it is assumed that the specimen is to be tested at a temperature of 1430 C (2600F) in an oxidizing atmosphere. For the most part, previous high temperature material characterization tests, such as flexure and tensile tests, have been performed in inert atmospheres. Due to the harsh environment in which the ceramic specimen is to be tested, many conventional strain measuring techniques can not be applied. Initially a brief description of the more commonly used mechanical strain measuring techniques is given. Major advantages and disadvantages with their application to high temperature tensile testing of ceramic composites are discussed. Next, a general overview is given for various optical techniques. Advantages and disadvantages which are common to these techniques are noted. The optical methods for measuring strain or displacement are categorized into two sections. These include real-time techniques. Finally, an optical technique which offers optimum performance with the high temperature tensile testing of ceramic composites is recommended.

Hemann, John↗

NASA NTRS1992

Elevated temperature envelope forming

Elevated temperature envelope forming includes enclosing a part blank and form tool within an envelope sealed against the atmosphere, heat treating the combination while forming pressure holds the envelope and part against the form tool, and allowing part cool down to occur in an inert atmosphere with forming pressure removed. The forming pressure is provided by evacuating the envelope and may be aided by differential force applied between the envelope and the form tool.

Burg, Bruce M.↗

NASA NTRS1974

2200 C oxidizing atmosphere furnace for space manufacturing

The design of a high temperature furnace is presented which uses electrically conducting ceramic oxide heating elements. The heating elements are made of either thoria or stabilized zirconia which become conductive when preheated to 700 to 1000 C. These heater elements can be operated to 2200 C in oxidizing or inert atmospheres. The furnace is being designed to have a temperature which can be controlled to within 11 C. By a replacement of the heater element, the working cavity can be changed from isothermal to a cavity with a selected specific axial temperature gradient of up to 200 C per centimeter. This furnace concept is appropriate for the growth of crystals which might be grown best in an oxidizing atmosphere such as sapphire (melting point 2040 C), yttrium aluminum garnet (1970 C) or yttrium orthoaluminate (1875 C).

Halbach, C. R.↗