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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 OSTI2014

In situ synthesis of TiH{sub 2} layer on metallic titanium foil through gaseous hydrogen free acid-hydrothermal method

Graphical abstract: The reaction mechanism for in situ synthesizing TiH{sub 2} layer on titanium foil by a gaseous hydrogen free acid-hydrothermal methodology. - Highlights: • A dense TiH{sub 2} layer is synthesized by a hydrogen free acid-hydrothermal method. • Hydrogen in a TiH{sub 2} layer synthesized can release at low temperature. • During the dehydrogenation process, there is no any intermediate phase forming. • We report a method of low-cost, low-risk and convenience toward productive TiH{sub 2}. - Abstract: A novel strategy for synthesis of TiH{sub 2} layer on surface of metallic titanium by using an acid-hydrothermal method was proposed. During the synthesis process, no any elemental hydrogen was involved. X-ray powder diffraction, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscopy results confirmed that a TiH{sub 2} layer of 20 μm thickness on a Ti foil surface can be formed in situ by an interface reaction of metallic titanium with sulfuric acid solution, hydrochloric acid, or phosphoric acid, which is a hydrogen self-storage process. By tuning reaction parameters, for example, concentration of acid, composition and morphology of TiH{sub 2}-Ti hybrid materials can be adjusted. The TiH{sub 2} layer on a metallic titanium surface can be decompounded completely heated below 400 °C. This convenient, safe and low-cost method is a promising gaseous hydrogen free approach for the synthesis of hydride-based hydrogen storage materials.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Elastic and Piezoelectric Parameters of the Crystals of Histidine Phosphite L-Hist · H{sub 3}РО{sub 3} Measured by the Method of Electromechanical Resonance

Single crystals of L-histidine phosphite (L-Hist · H{sub 3}РО{sub 3}) have been grown from aqueous solution by slow cooling method. The results of elemental analysis, of X-ray-diffraction studies of the crystal structure, and the habitus of the obtained crystals are given. The elastic and piezoelectric coefficients have been measured on the plates with the (010) natural faces by the method of electromechanical resonance for stretching vibrations in the temperature range 295–340 K. Elastic compliance values s{sub 33} and s{sub 22} and the corresponding elastic-moduli values, piezoelectric coefficients d{sub 23} and d{sub 22}, coefficients of electromechanical coupling, and temperature coefficient of the resonance frequency are obtained. A comparison is given with other crystals, which are compounds of amino acids with phosphorous or phosphoric acid.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1978

Ambient cure polyimide foams

Flame and temperature resistant polyimide foams are prepared by the reaction of an aromatic dianhydride, (pyromellitic dianhydride) with an aromatic polyisocyanate, (polymethylene polyphenylisocyanate), in the presence of an inorganic acid and furfuryl alcohol. Usable acids include dilute sulfuric acid, dilute nitric acid, hydrochloric acid, polyphosphoric acid, and phosphoric acid, with the latter being preferred. The dianhydride and the isocyanate in about equimolar proportions constitute about 50% of the reaction mixture, the rest being made up with the acid and the alcohol in a ratio of about 1:10. An exothermic reaction between the acid and the alcohol provides the heat necessary for the other components to polymerize without recourse to external heat sources. The mixture can be sprayed on any surface to form polymeric foam in locations where the application of heat is not practical or possible, for instance, between walls or on mine tunnel surfaces.

Sawko, P. M.↗
NASA NTRS1980

Ambient cure polyimide foams prepared from aromatic polyisocyanates, aromatic polycarboxylic compounds, furfuryl alcohol, and a strong inorganic acid

Flame and temperature resistant polyimide foams are prepared by the reaction of an aromatic dianhydride, e.g., pyromellitic dianhydride, with an aromatic polyisocyanate, e.g., polymethylene polyphenylisocyanate (PAPI) in the presence of an inorganic acid and a lower molecular weight alcohol, e.g., dilute sulfuric acid or phosphoric acid and furfuryl alcohol. The exothermic reaction between the acid and the alcohol provides the heat necessary for the other reactants to polymerize without the application of any external heat. Such mixtures, therefore, are ideally suited for in situ foam formation, especially where the application of heat is not practical or possible.

Sawko, Paul M.↗
DOE OSTI2016

Acid-functionalized polyolefin materials and their use in acid-promoted chemical reactions

An acid-functionalized polyolefin material that can be used as an acid catalyst in a wide range of acid-promoted chemical reactions, wherein the acid-functionalized polyolefin material includes a polyolefin backbone on which acid groups are appended. Also described is a method for the preparation of the acid catalyst in which a precursor polyolefin is subjected to ionizing radiation (e.g., electron beam irradiation) of sufficient power and the irradiated precursor polyolefin reacted with at least one vinyl monomer having an acid group thereon. Further described is a method for conducting an acid-promoted chemical reaction, wherein an acid-reactive organic precursor is contacted in liquid form with a solid heterogeneous acid catalyst comprising a polyolefin backbone of at least 1 micron in one dimension and having carboxylic acid groups and either sulfonic acid or phosphoric acid groups appended thereto.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Use of glucose as reductant to recover Co from spent lithium ions batteries

Highlights: • Glucose was innovatively used as alternative to H{sub 2}O{sub 2} in leaching of spent LiCoO{sub 2} cathode material. • Over 98% Co and nearly 100% Li are leached with 1.5 mol/L phosphoric acid and 0.02 mol/L glucose at 80 °C in 2 h. • A molecular structure diagram was made to show dissolution process of reductive of Co(III) to Co(II) with glucose oxidation. • Cobalt oxalate (purity) was obtained as the precipitating product. • There are no reports on the leaching solution of glucose and phosphate acid. - Abstract: A hydrometallurgical leaching process has been developed for recovery of Co and Li from cathode material (LiCoO{sub 2}) collected from spent LIBs using a mix solution of glucose and phosphoric acid. The spent LiCoO{sub 2} before and after leaching process are analyzed by scanning electron microscopy. A leaching rate of about 98% Co and nearly 100% Li is presented with 1.5 mol/L phosphoric acid and 0.02 mol/L glucose at 80 °C in about 2 h. During leaching process, glucose was oxidized into monocarboxylic acid with reduction of Co(III) to Co(II). Co in solution was recovered as Co-oxalate after leaching process. Using glucose as reductant to dissolve LiCoO{sub 2} with chelating agent of phosphoric acid is achieved here.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Mechanisms of proton transport in aqueous acid solutions

The fundamental understanding of proton transport, specifically the Grotthuss-like mechanism, is critical for many technological applications. The present study presents a comprehensive analysis of proton transport in aqueous solutions of sulfuric and phosphoric acids using quasielastic neutron and light scattering, broadband dielectric spectroscopy, rheology, pulsed-field gradient-NMR measurements, and ab initio molecular dynamic simulations. Results show that in all systems, proton transport occurs through short “jumps” of ~0.5 Å that are faster than structural relaxation. However, proton hopping appears to be coupled to structural relaxation in aqueous solutions of sulfuric acid, while these processes are decoupled in phosphoric acid. Neutron scattering indicates that all protons have the same fast mobility in phosphoric acid systems, while at least one proton per sulfuric molecule remains slower than other protons. Analysis reveals correlated proton jumps, but these correlations suppress conductivity, suggesting that expected Grotthuss-like enhancement of conductivity is unlikely in bulk liquids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Sapphire advanced mitigation process: wet etch to expose sub-surface damage and increase laser damage resistance and mechanical strength

In this study, a novel, to the best of our knowledge, method of wet chemical etching of sapphire workpieces (such as optics, wafers, windows, and cones), called the sapphire advanced mitigation process (or sapphire AMP), has been developed that exposes sub-surface mechanical damage created during the optical fabrication process and significantly enhances the surface laser damage resistance (> 2×) and mechanical strength (up to ~ 2.6×). Sapphire AMP involves first treating the workpiece with a mixture of sulfuric and phosphoric acid ([H 2 SO 4 ]:[H 3 PO 4 ]= 1 : 3) at 220°C, followed with phosphoric acid at 160°C, then with sodium hydroxide base (NaOH) and surfactant at 40°C, and finally with a high-pressure deionized water spray rinse. Sapphire AMP has been demonstrated on both A- and C-plane sapphire workpieces. The mechanism of this etch process involves the reaction of the sapphire (Al 2 O 3 ) surface with sulfuric acid (H 2 SO 4 ) forming aluminum sulfate [Al2(SO4)3], which has low solubility. The high phosphoric acid content in the first and second steps of sapphire AMP results in the efficient conversion of Al 2 (SO 4 ) 3 to aluminum phosphate (AlPO 4 ), which is very soluble, greatly reducing reaction product redeposition on the workpiece surface. Sapphire AMP is shown to expose sub-surface mechanical damage on the sapphire surface created during the grinding and polishing processes, whose etched morphology has either isotropic or anisotropic evolution depending on the nature of the initial surface damage. Sapphire AMP was also designed to remove the key known surface, laser absorbing precursors (namely, foreign chemical impurities, the fracture surface layer of preexisting sub-surface damage, and reaction product or foreign species redeposition or precipitation). Static and sliding indention induced surface microfractures on sapphire are shown after sapphire AMP to have a significant decrease in the fast photoluminescence intensity (a known metric for measuring the degree of laser damaging absorbing precursors). In addition, the onset of laser damage (at 351 nm 3 ns) on sapphire AMP treated workpieces was shown to increase in fluence from ~ 4 to >9.5J/cm 2 . Finally, biaxial ball-on-ring mechanical tests on sapphire disks showed an increase in the failure stress from 340 MPa (with pre-existing 28 µm flaws) to ~ 900MPa after sapphire AMP, which is attributed to the blunting of the surface microfractures.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Electrocatalysis of fuel cell reactions: Investigation of alternate electrolytes

Oxygen reduction and transport properties of the electrolyte in the phosphoric acid fuel cell are studied. A theoretical expression for the rotating ring-disk electrode technique; the intermediate reaction rate constants for oxygen reduction on platinum in phosphoric acid electrolyte; oxygen reduction mechanism in trifluoromethanesulfonic acid (TFMSA), considered as an alternate electrolyte for the acid fuel cells; and transport properties of the phosphoric acid electrolyte at high concentrations and temperatures are covered.

Chin, D. T.↗
DOE OSTI2022

Designing Porous Ion Emitters for Thermal Ionization Mass Spectrometry: Evaluating Metal-Organic Frameworks

In this work we describe the first exploration of metal-organic frameworks (MOFs) as ‘next generation’ ion emitters for thermal ionization mass spectrometry (TIMS). MOFs were identified as promising candidates for this application given the synthetic control over their desired structural properties. This tunability results in well-ordered, high surface area, high porosity frameworks with targeted sorption affinities. Here we explored an aluminum-based, bipyridine-containing MOF (MOF-253) with and without incorporating the high work function metal, rhenium (Re). After analysis of a Nd-bearing MOF, we hypothesized that the well-dispersed, sponge-like interconnected network of the degraded structure would enhance Nd ionization more than traditional TIMS loading activators (i.e., phosphoric acid). Compared to filaments loaded with phosphoric acid that require an additional benzene carburization step, the Nd ionization efficiencies (atoms detected relative to atoms loaded) for heated filaments loaded with MOF-253 were similar (~1%). Electron microscopy after TIMS analysis demonstrated that the MOF was retained on the filament and, as hypothesized, preserved sub-micron porosity post analysis. While these results are preliminary, they demonstrate that MOFs have potential to enhance ionization and exceed the performance of traditional loading techniques by forming nano-porous ion emitters (nano-PIEs). Thus, further experimentation is likely to exceed this performance through more specific selection of the base MOF structure and modifications to porosity and composition. This work represents a novel application of MOFs and a next step in the pursuit of advanced thermal ionization with potential to expand across the periodic table.

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

Tracking Molecular Transport Across Oil/Aqueous Interfaces: Insight into “Antagonistic” Binding in Solvent Extraction

Liquid/liquid (L/L) interfaces play a key, yet poorly understood, role in a range of complex chemical phenomena where time-evolving interfacial structures and transient supramolecular assemblies act as gatekeepers to function. Here, for this study, we employ surface-specific vibrational sum frequency generation combined with neutron and X-ray scattering methods to track the transport of dioctyl phosphoric acid (DOP) and di-(2-ethylhexyl) phosphoric acid (DEHPA) ligands used in solvent extraction at buried oil/aqueous interfaces away from equilibrium. Our results show evidence for a dynamic interfacial restructuring at low ligand concentrations in contrast to expectation. These time-varying interfaces arise from the transport of sparingly soluble interfacial ligands into the neighboring aqueous phase. These results support a proposed “antagonistic” role of ligand complexation in the aqueous phase that could serve as a holdback mechanism in kinetic liquid extractions. These findings provide new insights into interfacially controlled chemical transport at L/L interfaces and how these interfaces vary chemically, structurally, and temporally in a concentration-dependent manner and present potential avenues to design selective kinetic separations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Bio- and mineral acid leaching of rare earth elements from synthetic phosphogypsum

Leaching of six individual rare earth (yttrium, cerium, neodymium, samarium, europium, and ytterbium) doped synthetic phosphogypsum samples using a suite of lixiviants was conducted. The lixiviants chosen for this study were phosphoric acid, sulfuric acid, gluconic acid, and a “biolixiviant” consisting of spent medium containing organic acids from the growth of the bacterium Gluconobacter oxydans on glucose. The biolixiviant had a pH of 2.1 and the dominant organic acid was determined to be gluconic acid, present at a concentration of 220 mM. The leaching behaviors of the studied lixiviants were compared and rationalized by thermodynamic simulations. The results suggest that at equivalent molar concentrations of 220 mM the biolixiviant was more efficient at rare earth element (REE) extraction than gluconic acid and phosphoric acid but less efficient than sulfuric acid. Unlike the organic acids, at pH 2.1 the mineral acids failed to extract REE, likely due to different complexation and kinetic effects.

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

DEHP− extractant binding to trivalent lanthanide Er3+: Fast binding accompanied by concerted angular motions of hydration water

Solvent extraction of trivalent rare earth metal ions by organophosphorus extractants proceeds via binding of phosphoric acid headgroups to the metal ion. Water molecules in the tightly bound first hydration shell of the metal ions must be displaced by oxygen atoms from phosphoric acid headgroups. Here, we use classical molecular dynamics simulations to explore the event in which a fully hydrated Er3+ binds to its first phosphoric acid headgroup. Approach of the headgroup into the region between the first and second hydration shells leads to a fast ejection of a water molecule that is accompanied by reordering of the hydration water molecules, including discretization of their angular positions and collective rotation about the metal ion. The water molecule ejected from the first shell is located diametrically opposite from the binding oxygen. Headgroup binding places a headgroup oxygen closer to Er3+ than its first hydration shell and creates a loosely bound water that subsequently exchanges between the first shell and its environment. This second exchange of water also occurs at discrete angular positions. This geometrical aspect of binding may be of relevance to understanding the binding and transport of ion–extractant complexes that are expected to occur at the organic–aqueous liquid–liquid interface used in solvent extraction processes.

Chemistry↗
NASA NTRS1984

Electrocatalysis of fuel cell reactions: Investigation of alternate electrolytes

Oxygen reduction and transport properties of the electrolyte in the phosphoric acid fuel cell are studied. The areas covered were: (1) development of a theoretical expression for the rotating ring disk electrode technique; (2) determination of the intermediate reaction rate constants for oxygen reduction on platinum in phosphoric acid electrolyte; (3) determination of oxygen reduction mechanism in trifluoreomethanesulfonic acid (TFMSA) which was considered as an alternate electrolyte for the acid fuel cells; and (4) the measurement of transport properties of the phosphoric acid electrolyte at high concentrations and temperatures.

Chin, D. T.↗
NASA NTRS1983

Advanced coal gasifier-fuel cell power plant systems design

Two advanced, high efficiency coal-fired power plants were designed, one utilizing a phosphoric acid fuel cell and one utilizing a molten carbonate fuel cell. Both incorporate a TRW Catalytic Hydrogen Process gasifier and regenerator. Both plants operate without an oxygen plant and without requiring water feed; they, instead, require makeup dolomite. Neither plant requires a shift converter; neither plant has heat exchangers operating above 1250 F. Both plants have attractive efficiencies and costs. While the molten carbonate version has a higher (52%) efficiency than the phosphoric acid version (48%), it also has a higher ($0.078/kWh versus $0.072/kWh) ten-year levelized cost of electricity. The phosphoric acid fuel cell power plant is probably feasible to build in the near term: questions about the TRW process need to be answered experimentally, such as weather it can operate on caking coals, and how effective the catalyzed carbon-dioxide acceptor will be at pilot scale, both in removing carbon dioxide and in removing sulfur from the gasifier.

Heller, M. E.↗
NASA NTRS1980

Cathode catalyst for primary phosphoric fuel cells

Alkylation of Vulcan XC-72 provided the most stable bond type for linking CoTAA to the surface of the carbon; this result is based on data obtained by cyclic voltammetry, pulse voltammetry and by release of 14C from bonded CoTAA. Half-cell tests at 100 C in 85% phosphoric acid showed that CoTAA bonded to the surface of carbon (Vulcan XC-72) via an alkylation procedure is a more active catalyst than is platinum based on a factor of two improvement in Tafel slope; dimeric CoTAA has catalytic activity equal to platinum. Half-cell tests also showed that bonded CoTAA catalysts do not suffer a loss in potential when air is used as a fuel rather than oxygen. Commercially available PTFE was shown to be stable for four months in 200 C 85% phosphoric acid based on lack of change in surface wetting properties, IR and physical characteristics. When stressed electrochemically in 150 C 85% phosphoric acid, PTFE also showed no changes after one month.

Walsh, F.↗
DOE OSTI2014

High power density fuel cell comprising an array of microchannels

A phosphoric acid fuel cell according to one embodiment includes an array of microchannels defined by a porous electrolyte support structure extending between bottom and upper support layers, the microchannels including fuel and oxidant microchannels; fuel electrodes formed along some of the microchannels; and air electrodes formed along other of the microchannels. A method of making a phosphoric acid fuel cell according to one embodiment includes etching an array of microchannels in a substrate, thereby forming walls between the microchannels; processing the walls to make the walls porous, thereby forming a porous electrolyte support structure; forming anode electrodes along some of the walls; forming cathode electrodes along other of the walls; and filling the porous electrolyte support structure with a phosphoric acid electrolyte. Additional embodiments are also disclosed.

25 ENERGY STORAGE↗
NASA NTRS1981

Applications study of advanced power generation systems utilizing coal-derived fuels. Volume 1: Executive summary

The technology status of phosphoric acid and molten carbon fuel cells, combined gas and steam turbine cycles, and magnetohydrodynamic energy conversion systems was assessed and the power performance of these systems when operating with medium-Btu fuel gas whether delivered by pipeline to the power plant or in an integrated mode in which the coal gasification process and power system are closely coupled as an overall power plant was evaluated. Commercially available combined-cycle gas turbine systems can reach projected required performance levels for advanced systems using currently available technology. The phosphoric acid fuel cell appears to be the next most likely candidate for commercialization. On pipeline delivery, the systems efficiency ranges from 40.9% for the phosphoric acid fuel cell to 63% for the molten carbonate fuel cell system. The efficiencies of the integrated power plants vary from approximately 39-40% for the combined cycle to 46-47% for the molden carbonate fuel cell systems. Conventional coal-fired steam stations with flue-gas desulfurization have only 33-35% efficiency.

Robson, F. L.↗