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DOE OSTI2026

Binuclear Acetoniminato Derivatives of Iron and Chromium Carbonyls: A Theoretical Study

The structures and energetics of binuclear acetoniminato metal carbonyl derivatives of the types (Me 2 C═N) 2 Fe 2 (CO) n and (Me 2 C═N) 2 Cr 2 (CO) n have been investigated by density functional theory. The (Me 2 C═N) 2 Fe 2 (CO) 6 structure, with bridging Me 2 C═N ligands using only their nitrogen atoms to bridge an Fe═Fe bond related to experimentally known species, as well as a related (Me 2 C═N) 2 Cr 2 (CO) 8 structure, appear to be energetically preferred. Among carbonyl-richer systems, the iron system energetically prefers a {Me 2 C═NC(O)} 2 Fe 2 (CO) 6 structure with bridging Me 2 C═NC(O) ligands, whereas the chromium system energetically prefers a structure with a 2,3-diazabutadiene ligand having each nitrogen atom bonded to a Cr(CO) 5 moiety. Preferred structures for systems with fewer CO groups include the tetracarbonyl (Me 2 C═N) 2 Fe 2 (CO) 4 in which one of the bridging Me 2 C═N uses its C═N double bond to bond to an iron atom, as well as (Me 2 C═N)2Cr 2 (CO) n (n = 7, 6) structures with chromium–chromium multiple bonds bridged by Me2C═N groups.

Carbonyls↗

DOE OSTI2025

Growth of Hexagonal Boron Nitride from Molten Nickel Solutions: A Reactive Molecular Dynamics Study

Metal flux methods are excellent for synthesizing high-quality hexagonal boron nitride (hBN) crystals, but the atomic mechanisms of hBN nucleation and growth in these systems are poorly understood and difficult to probe experimentally. Here, we harness classical reactive molecular dynamics (ReaxFF) to unravel the mechanisms of hBN synthesis from liquid nickel solvent over time scales up to 30 ns. These simulations mimic experimental conditions by including relatively large liquid nickel slabs containing dissolved boron and a molecular nitrogen gas phase. Overall, the reaction takes place almost exclusively on the surface of the liquid nickel, owing to the low solubility of nitrogen in bulk nickel and the intermediate species’ preference for the metal–gas interface. The formation of hBN invariably begins by reaction of dinitrogen with nickel-solvated boron atoms at the surface, forming intermediate N–N–B species, which typically evolve into B–N–B units through a short-lived intermediate where a single nitrogen atom is coordinated by one nitrogen and two boron atoms. The resulting B–N–B units, in turn, coalesce with growing hBN nuclei and carry nitrogen between hBN nanocrystals in an Ostwald ripening process. The amount of hBN produced on the tens of nanosecond time scale depends critically on the boron concentration, while having a much weaker dependence on the N 2 pressure for the regime considered (N 2 pressures of 2.5–10 MPa, Ni–B solutions with 6–12% boron by atom fraction). The highest rate of hBN formation occurs at the lowest temperature considered (1750 K, just above the melting point of nickel), while no hBN sheets are formed at 2000 K or above. An analysis of the transition pathways for nitrogen atoms shows that the final step, incorporation of small B–N motifs into larger hBN sheets, is the rate-limiting step in the regimes considered. While raising the temperature from 1750 to 2000 K has little effect on the formation of intermediates (N–N–B, B–N–B, etc.), the lack of large hBN sheets at temperatures >1900 K is explained by decreased probability of the final step and increased probability of breakup of hBN into B–N motifs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRSDate not supplied

Plant Nitrogen Uptake Responses to Elevated Carbon Dioxide

Future long-duration missions will require a sustainable supply of food to support human crews. The spaceflight cabin environment often contains very high concentrations of CO 2 due to release of CO 2 by astronauts that is not completely scrubbed from the cabin, and it is therefore crucial to understand plant responses to elevated CO 2 (eCO 2 ) environments. Much focus has been given to changes in plant photosynthetic and performance parameters in response to eCO 2 , but the effects of eCO 2 on nitrogen (N) uptake are poorly understood. Shoot nitrate reduction may be reduced at eCO 2 , likely due to less reductant available for nitrate reduction because of reduced photorespiration and increased carbon fixation 1. Relative growth rate can be reduced at eCO 2 when N is provided only as nitrate and can be unaffected when N is supplied as ammonium. However, N uptake in response to eCO 2 has, to our knowledge, not yet been studied. An increased ‘preference’ for plants to take up N as ammonium at eCO 2 could have important implications for growth in the space environment, where N is currently only supplied as nitrate. In this study, novel stable isotope approaches were used in conjunction with hydroponics and isotope ratio mass spectrometry to determine the effect of eCO 2 on N preference for ammonium or nitrate in spring barley and lettuce when both N forms are provided equally. Several varieties of spring barley displayed increased ammonium preference at eCO 2 (720 ppm) compared to ambient CO 2 (410 ppm), though this was not true for all varieties. In most cases, increases in ammonium preference were driven by increases in ammonium uptake at eCO 2 and not decreases in nitrate uptake. Current research is assessing whether similar responses are observed in the candidate space crop lettuce, at levels of CO 2 like those observed on ISS (3000 ppm), and these results will also be presented. This work will enable the development of optimized nutrient regimes for candidate crops in space environments and the selection of crop varieties adapted to eCO 2 environments. Plants adapted to ammonium nutrition may play a role in future plant-based bioregenerative life support systems with higher ammonium concentrations due to waste recycling. Moreover, this research will further our understanding of plant responses to the eCO 2 environment brought about by climate change, allowing the development of future-proof crops that will help to maintain food security.

nitrogen↗

NASA NTRS1985

Basic cryogenics and materials. Phase 1

The effects of cryogenic temperatures on the mechanical and physical properties of materials are summarized. Heat capacity and thermal conductivity are considered in the context of conservation of liquid nitrogen, thermal stability of the gas stream, and the response time for changes in operating temperature. Particular attention is given to the effects of differential expansion and failure due to thermal fatigue. Factors affecting safety are discussed, including hazards created due to the inadvertent production of liquid oxygen and the physiological effects of exposure to liquid and gaseous nitrogen, such as cold burns and asphyxiation. The preference for using f.c.c. metals at low temperatures is explained in terms of their superior toughness. The limitations on the use of ferritic steels is also considered. Nonmetallic materials are discussed, mainly in the context of their LOX compatibility and their use in the form of foams and fibers as insultants, seals, and fiber reinforced composites.

Wigley, D. A.↗

NASA NTRS1985

Basic cryogenics and materials

Wigley, D. A.↗

DOE OSTI2021

Evaluating bloom potential of the green-tide forming alga Ulva ohnoi under ocean acidification and warming

Herein we discuss the occurrence of green-tides, whose bloom potential may be increased by various human activities and biogeochemical process, results in enormous economic losses and ecosystem collapse. In this study, we investigated the ecophysiology of the subtropical green-tide forming alga, Ulva ohnoi complex (hereafter: U. ohnoi), under simulated future ocean conditions in order to predict its bloom potential using photosynthesis and growth measurements, and stable isotope analyses. Our mesocosm system included four experimental conditions that simulated the individual and combined effects of elevated CO 2 and temperature, namely control (450 μatm CO 2 & 20 °C), acidification (900 μatm CO 2 & 20 °C), warming (450 μatm CO 2 & 25 °C), and greenhouse (900 μatm CO 2 & 25 °C). Photosynthetic electron transport rates (rETR) increased significantly under acidification conditions, but net photosynthesis and growth were not affected. In contrast, rETR, net photosynthesis, and growth all decreased significantly under elevated temperature conditions (i.e. both warming and greenhouse). These results represent the imbalance of energy metabolism between electron transport and O 2 production that may be expected under ocean acidification conditions. This imbalance appears to be related to carbon and nitrogen assimilation by U. ohnoi. In particular, 13 C and 15 N discrimination data suggest U. ohnoi prefers CO 2 and NH 4 + over HCO 3 - and NO 3 - as sources of carbon and nitrogen, respectively, and this results in increased N content in the thallus under ocean acidification conditions. Together, our results suggest a trade-off in which the bloom potential of U. ohnoi could increase under ocean acidification due to greater N accumulation and through the saving of energy during carbon and nitrogen metabolism, but that elevated temperatures could decrease U. ohnoi's bloom potential through a decrease in photosynthesis and growth.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2025

Basin-Size Mapping: Prediction of Metastable Polymorph Synthesizability Across TaC–TaN Alloys

The sizes of the basins of attraction on the potential energy surface are helpful indicators in determining the experimental synthesizability of metastable phases. In principle, these basins can be controlled with changes in thermodynamic conditions such as composition, pressure, and surface energy. Herein, we use random structure sampling to computationally study how alloying smoothly perturbs basin of attraction sizes. The TaC 1-x N x pseudobinary is an ideal test system given the structural and polymorphic contrast of its parent compounds and their technological relevance as epitaxial substrates for Al 1-x Ga x N. While we find limited thermodynamic stability across all computationally observed phases, random structure sampling shows a significant composition region where the rocksalt basin dominates. As such, we predict the potential for the nonequilibrium synthesis of metastable rocksalt TaC 1-x N x alloys as substrates for Al 1-x Ga x N. At higher nitrogen concentrations, other low-energy metastable polymorphs emerge that continue to retain the hexagonal close packing suitable for III-N growth. Confidence in these trends was established through uncertainty quantification of the basin sizes and energy distributions; such analysis utilized the Beta and Dirichlet distributions. In conclusion, we also find (a) polymorph basin sizes can be rationalized in terms of energetic preferences for different coordination environments; and (b) basin sizes universally shrink with increasing nitrogen content, making the system more prone to amorphous growth.

36 MATERIALS SCIENCE↗

NASA NTRS1983

Method of carbonizing polyacrylonitrile fibers

This invention relates to a method of carbonizing polyacrylonitrile fibers by exposing the fibers at an elevated temperature to an oxidizing atmosphere; then exposing the oxidized fibers to an atmosphere of an inert gas such as nitrogen containing a carbonaceous material such as acetylene. The fibers are preferably treated with an organic compound, for example benzoic acid, before the exposure to an oxidizing atmosphere. The invention also relates to the resulting fibers. The treated fibers have enhanced tensile strength.

Cagliostro, D. E.↗

NASA NTRS2001

Solar-Thermal Engine Testing

A solar-thermal engine serves as a high-temperature solar-radiation absorber, heat exchanger, and rocket nozzle. collecting concentrated solar radiation into an absorber cavity and transferring this energy to a propellant as heat. Propellant gas can be heated to temperatures approaching 4,500 F and expanded in a rocket nozzle, creating low thrust with a high specific impulse (I(sub sp)). The Shooting Star Experiment (SSE) solar-thermal engine is made of 100 percent chemical vapor deposited (CVD) rhenium. The engine 'module' consists of an engine assembly, propellant feedline, engine support structure, thermal insulation, and instrumentation. Engine thermal performance tests consist of a series of high-temperature thermal cycles intended to characterize the propulsive performance of the engines and the thermal effectiveness of the engine support structure and insulation system. A silicone-carbide electrical resistance heater, placed inside the inner shell, substitutes for solar radiation and heats the engine. Although the preferred propellant is hydrogen, the propellant used in these tests is gaseous nitrogen. Because rhenium oxidizes at elevated temperatures, the tests are performed in a vacuum chamber. Test data will include transient and steady state temperatures on selected engine surfaces, propellant pressures and flow rates, and engine thrust levels. The engine propellant-feed system is designed to Supply GN2 to the engine at a constant inlet pressure of 60 psia, producing a near-constant thrust of 1.0 lb. Gaseous hydrogen will be used in subsequent tests. The propellant flow rate decreases with increasing propellant temperature, while maintaining constant thrust, increasing engine I(sub sp). In conjunction with analytical models of the heat exchanger, the temperature data will provide insight into the effectiveness of the insulation system, the structural support system, and the overall engine performance. These tests also provide experience on operational aspects of the engine and associated subsystems, and will include independent variation of both steady slate heat-exchanger temperature prior to thrust operation and nitrogen inlet pressure (flow rate) during thrust operation. Although the Shooting Star engines were designed as thermal-storage engines to accommodate mission parameters, they are fully capable of operating as scalable, direct-gain engines. Tests are conducted in both operational modes. Engine thrust and propellant flow rate will be measured and thereby I(sub sp). The objective of these tests is to investigate the effectiveness of the solar engine as a heat exchanger and a rocket. Of particular interest is the effectiveness of the support structure as a thermal insulator, the integrity of both the insulation system and the insulation containment system, the overall temperature distribution throughout the engine module, and the thermal power required to sustain steady state fluid temperatures at various flow rates.

Tucker, Stephen↗

DOE OSTI2023

Stable ammonia absorbents

The present disclosure relates to systems and methods of making ammonia using stable ammonia absorbents. The system and method for producing ammonia, comprises a reactor comprising a catalyst that converts at least a portion of nitrogen feed gas and at least a portion of hydrogen feed gas to ammonia (NH3) forming a reaction mixture comprising the ammonia, unreacted nitrogen, and unreacted hydrogen. An absorber configured to selectively absorb ammonia from the reaction mixture at a temperature of about 180 deg. C. to 330 deg. C. and a pressure of about 1-20 bar, the absorber comprising a solid absorbent. Preferably the solid absorbent is at least one metal halide and a solid support. The unabsorbed ammonium, the unreacted nitrogen, and unreacted hydrogen gas are recycled to the reactor.

Cussler, Edward↗

NASA NTRS1998

Flexible Ceramic-Metal Insulation Composite and Method of Making

A method for joining a woven flexible ceramic fabric and a thin metal sheet creating an integral metal surfaced flexible thermal protection article, which methods compress: placing multiple dots of high temperature metallic or fabric and the thin metal sheet in a random or organized pattern, with the proviso that the brazing material covers about 10% or less of the surface of one flat side of the metal sheet; heating the flexible ceramic fabric, brazing material and thin metal sheet for a predetermined period of time to integrally connect the same; and cooling the formed flexible article to ambient temperature. Preferably the flexible ceramic is selected from fibers comprising atoms of silicon, carbon, nitrogen, boron, oxygen or combinations thereof. The flexible thermal protection article produced is also part of the present invention. The thin metal sheet is comprised of titanium, aluminum, chromium, niobium or alloys or combinations thereof. The brazing material is selected from copper/silver or copper/gold or is a ceramic brazing or adhesive material.

Rasky, Daniel J.↗

NASA NTRS1983

Method of increasing minority carrier lifetime in silicon web or the like

A silicon dendrite is grown as a ribbon forming two silicon crystal layers which are separated by an interface layer which contains a large number of defects. Significant increase of minority carrier lifetime with homogeneous distribution at the outer surfaces of the two silicon crystal layers is achieved by processing the web in an atmosphere of a selected gas, e.g., oxygen, nitrogen or an inert gas, for about 30 minutes to several hours at a temperature preferably on the order of 900 to 1200 C.

Liu, J. K.↗

NASA NTRS2003

Sooting Limits Of Diffusion Flames With Oxygen-Enriched Air And Diluted Fuel

Oxygen-enhanced combustion permits certain benefits and flexibility that are not otherwise available in the design of practical combustors, as discussed by Baukal. The cost of pure and enriched oxygen has declined to the point that oxygen-enhanced combustion is preferable to combustion in air for many applications. Carbon sequestration is greatly facilitated by oxygen enrichment because nitrogen can be eliminated from the product stream. For example, when natural gas (or natural gas diluted with CO2) is burned in pure oxygen, the only significant products are water and CO2. Oxygen-enhanced combustion also has important implications for soot formation, as explored in this work. We propose that soot inception in nonpremixed flames requires a region where C/O ratio, temperature, and residence time are above certain critical values. Soot does not form at low temperatures, with the threshold in nonpremixed flames ranging from about 1250-1650 K, a temperature referred to here as the critical temperature for soot inception, Tc. Soot inception also can be suppressed when residence time is short (equivalently, when the strain rate in counterflow flames is high). Soot induction times of 0.8-15 ms were reported by Tesner and Shurupov for acetylene/nitrogen mixtures at 1473 K. Burner stabilized spherical microgravity flames are employed in this work for two main reasons. First, this configuration offers unrestricted control over convection direction. Second, in steady state these flames are strain-free and thus can yield intrinsic sooting limits in diffusion flames, similar to the way past work in premixed flames has provided intrinsic values of C/O ratio associated with soot inception limits.

Sunderland, P. B.↗

NASA NTRS1980

Kinetic and photochemical data for atmospheric chemistry reactions of the nitrogen oxides

Data sheets for thermal and photochemical reactions of importance in the atmospheric chemistry of the nitrogen oxides are presented. For each reaction the available experimental data are summarized and critically evaluated, and a preferred value of the rate coefficient is given. The selection of the preferred value is discussed and an estimate of its accuracy is given. For the photochemical process, the data are summarized, and preferred for the photoabsorption cross section and primary quantum yields are given.

Hampson, R. F., Jr.↗

NASA NTRS2011

Hybrid Composite Cryogenic Tank Structure

A hybrid lightweight composite tank has been created using specially designed materials and manufacturing processes. The tank is produced by using a hybrid structure consisting of at least two reinforced composite material systems. The inner composite layer comprises a distinct fiber and resin matrix suitable for cryogenic use that is a braided-sleeve (and/or a filamentwound layer) aramid fiber preform that is placed on a removable mandrel (outfitted with metallic end fittings) and is infused (vacuum-assisted resin transfer molded) with a polyurethane resin matrix with a high ductility at low temperatures. This inner layer is allowed to cure and is encapsulated with a filamentwound outer composite layer of a distinct fiber resin system. Both inner and outer layer are in intimate contact, and can also be cured at the same time. The outer layer is a material that performs well for low temperature pressure vessels, and it can rely on the inner layer to act as a liner to contain the fluids. The outer layer can be a variety of materials, but the best embodiment may be the use of a continuous tow of carbon fiber (T-1000 carbon, or others), or other high-strength fibers combined with a high ductility epoxy resin matrix, or a polyurethane matrix, which performs well at low temperatures. After curing, the mandrel can be removed from the outer layer. While the hybrid structure is not limited to two particular materials, a preferred version of the tank has been demonstrated on an actual test tank article cycled at high pressures with liquid nitrogen and liquid hydrogen, and the best version is an inner layer of PBO (poly-pphenylenebenzobisoxazole) fibers with a polyurethane matrix and an outer layer of T-1000 carbon with a high elongation epoxy matrix suitable for cryogenic temperatures. A polyurethane matrix has also been used for the outer layer. The construction method is ideal because the fiber and resin of the inner layer has a high strain to failure at cryogenic temperatures, and will not crack or produce leaks. The outer layer serves as more of a high-performance structural unit for the inner layer, and can handle external environments.

DeLay, Thomas↗

NASA NTRS2001

A Quadrupole Ion Trap Mass Spectrometer for Quantitative Analysis of Nitrogen-Purged Compartments within the Space Shuttle

To enter orbit, the Space Shuttle burns 1.8 million liters of liquid hydrogen combined with 0.8 million liters of liquid oxygen through three rocket engines mounted in the aft. NASA monitors the nitrogen-purged aft compartment for increased levels of hydrogen or oxygen in order to detect and determine the severity of a cryogenic fuel leak. Current monitoring is accomplished with a group of mass spectrometer systems located as much as 400 feet away from the Shuttle. It can take up to 45 seconds for gas to reach the mass spectrometer, which precludes monitoring for leaks in the final moments before liftoff (the orbiter engines are started at T-00:06 seconds). To remedy the situation, NASA is developing a small rugged mass spectrometer to be used as point-sensors around the Space Shuttle. As part of this project, numerous mass analyzer technologies are being investigated. Presented here are the preliminary results for one such technology, quadrupole ion trap mass spectrometry (QITMS). A compact QITMS system has been developed in-house at the University of Florida for monitoring trace levels of four primary gases, hydrogen, helium, oxygen, and argon, all in a nitrogen background. Since commercially available QITMS systems are incapable of mass analysis at m/z(exp 2), the home-built system is preferred for the evaluation of QITMS technology.

Ottens, Andrew K.↗

NASA NTRS2010

Hydrogen peroxide catalytic decomposition

Nitric oxide in a gaseous stream is converted to nitrogen dioxide using oxidizing species generated through the use of concentrated hydrogen peroxide fed as a monopropellant into a catalyzed thruster assembly. The hydrogen peroxide is preferably stored at stable concentration levels, i.e., approximately 50%-70% by volume, and may be increased in concentration in a continuous process preceding decomposition in the thruster assembly. The exhaust of the thruster assembly, rich in hydroxyl and/or hydroperoxy radicals, may be fed into a stream containing oxidizable components, such as nitric oxide, to facilitate their oxidation.

Parrish, Clyde F.↗

NASA NTRS1995

Microstructure and properties of cryomilled nickel aluminide extruded with chromium or molybdenum

Previous results from high energy, attrition milled NiAl in liquid nitrogen (cryomilled) indicate that this process can produce high temperature, creep resistant AlN particulate reinforced materials. However, the low temperature toughness of such materials is below that preferred for structural applications in aerospace engines. In order to improve the toughness of these materials, prealloyed nickel aluminide (Ni-53 atomic percent Al) powder was cryomilled and mixed with chromium or molybdenum powders. The resulting materials were hot extruded and tested for room temperature toughness and 1300 K compressive strength.

Aikin, Beverly J. M.↗