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DOE OSTI2021

Role of Pairwise Reactions on the Synthesis of Li 0.3 La 0.57 TiO 3 and the Resulting Structure–Property Correlations

The performance of single-ion conductors is highly sensitive to the material’s defect chemistry. Tuning these defects is limited for solid-state reactions as they occur at particle–particle interfaces, which provide a complex evolving energy landscape for atomic rearrangement and product formation. In this report, we investigate the (1) order of addition and (2) lithium precursor decomposition temperature and their effect on the synthesis and grain boundary conductivity of the perovskite lithium lanthanum titanium oxide (LLTO). We use an intimately mixed sol–gel, a solid-state reaction of Li precursor + La 2 O 3 + TiO 2 , and Li precursor + amorphous La 0.57 TiO x as different chemical routes to change the way in which the elements are brought together. The results show that the perovskite can accommodate a wide range of Li deficiencies (upward of 50%) while maintaining the tetragonal LLTO structure, indicating that X-ray diffraction (XRD) is insufficient to fully characterize the chemical nature of the product (i.e., Li-deficient LLTO may behave differently than stoichiometric LLTO). Variations in the relative intensities of different reflections in XRD suggest variations in the La ordering within the crystal structure between synthesis methods. Furthermore, the choice of the precursor and the order of addition of the reactants lower the time required to form a pure phase. Density functional theory calculations of the formation energy of possible reaction intermediates support the hypothesis that a greater thermodynamic driving force to form LLTO leads to a greater LLTO yield. Here, the retention of lithium is correlated with the thermal decomposition temperature of the Li precursor and the starting material mixing strategy. Taking the results together suggests that cations that share a site with Li should be mixed early to avoid ordering. Such cation ordering inhibits Li motion, leading to higher Li ion resistance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Surface Nanostructure Control and Thermodynamic Stability Analysis of Femtosecond Laser-Ablated CuCoMn 1.75 NiFe 0.25 Nanoparticles

Surface nanostructure control is the key to functionalizing nanomaterials. This paper presents a characterization with thermodynamic stability analysis of CuCoMn 1.75 NiFe 0.25 high-entropy alloy (HEA) nanoparticles synthesized by femtosecond laser ablation in ethanol and liquid nitrogen (LN2). Using multimodal electron microscopy and spectroscopy, we examine phase, particle size, defect structure, chemical distribution, and surface composition and relate them to HEA stability. Elemental distributions are uniform in both media, but LN2 produces smaller particles with a narrower size distribution and mainly single- or few-domain interiors, whereas ethanol yields larger particles built from 2–4 nm crystallites with domain aggregation. Edge defects appear in both but energy-dispersive X-ray spectroscopy (EDS) is broadly uniform with local fluctuations in ethanol. X-ray photoelectron spectroscopy (XPS), supported by an attenuation model, indicates an ∼1 nm oxide overlayer that suppresses Mn 2p intensity; correcting for it returns Mn toward the bulk value. UV–NIR and photoluminescent spectra independently support a thin oxide shell. Composition-based thermodynamic descriptors place LN2 closer to bulk mixing parameters, while ethanol raises ΔH_mix and lowers Ω. Cooling simulations are consistent (LN2 ∼ 0.1 μs quench, ethanol ∼1 μs). In conclusion, these results connect solvent-controlled kinetics and thermodynamics to crystalline state and surface chemistry, informing surface control of HEA nanoparticles.

Femtosecond Laser Ablation↗

DOE OSTI2026

Non-equilibrium reducing flame aerosol process to create supported high-entropy alloy nanoparticles

High-entropy alloy (HEA) nanomaterials provide opportunities and property combinations for energy and electronic applications, but their practical synthesis faces challenges of elemental immiscibility, metal reducibility, and particle aggregation during their synthesis. Herein, we report a broadly applicable non-equilibrium, scalable, and in-situ reducing flame aerosol process for synthesis of supported HEA nanoparticles. This versatile process can directly load a high concentration of 2 ~ 4 nm HEA nanoparticles on various 1- to 3-dimensional supports. Notably, simultaneous formation of HEA nanoparticles and a mesoporous silica support was successfully realized in a single step. Exploration of this process demonstrates the role of kinetics and entropy on decreasing alloy particle size and altering the reducibility of elements. We propose an entropy-induced reduction mechanism to incorporate oxidizable elements into HEAs, which extends the compositional space of HEA nanoparticles. As a representative catalytic application, we present a RuPdOsIrPt/graphene electrocatalyst with high activity and stability for hydrogen oxidation reaction. Our findings open horizons for high-performance HEA design and applications in diverse fields such as catalysis, electrochemistry, and sensing.

organic↗

NASA NTRS1973

Reactions of singlet oxygen with pine pollen.

A study was initiated to determine whether viable atmospheric particles such as plant pollens and fungal spores containing unsaturated lipids can interact with singlet oxygen to give oxygenated products that are potentially toxic. The results obtained confirm that surface and near surface components of common viable particulate matter in the atmosphere may be subject to rapid oxidation by singlet oxygen, leading to products which are probably allylic hydroperoxides. In connection with increasing atmospheric pollution, it is important to note that materials toxic to mammalian lung tissue may be oxidatively produced on the surfaces of viable particulate matter.

Dowty, B.↗

NASA NTRS1978

Electrically-conducting thermal-control coating

Coating comprised mainly of zinc and aluminum oxides is characterized by high thermal emittance, low thermal absorption, and high electrical conductivity. Originally developed to protect spacecraft, coating can be used to prevent charge buildup on components in other applications. Mixture is stable under ultraviolet and X-ray radiation and under bombardment by ionizing particles. It can be applied to aluminum, stainless steel, epoxy/fiberglass, and other substrates. When exposed to equivalent of 1,000 Sun-hours illumination, coating remained stable and retained its optical properties.

Shai, M. C.↗

NASA NTRS1982

Plasma-sprayed self-lubricating coatings

One of the most important criterion for acceptable commercial application of a multiple phase composition is uniformity and reproducibility. This means that the performance characteristics of the coat - e.g., its lubricating properties, bond strength to the substrate, and thermal properties - can be readily predicted to give a desired performance. The improvement of uniformity and reproducibility of the coats, the oxidation behavior at three temperature ranges, the effect of bond coat and the effect of preheat treatment as measured by adhesive strength tests, coating examination procedures, and physical property measurements were studied. The following modifications improved the uniformity and reproducibility: (1) changes and closer control in the particle size range of the raw materials used, (2) increasing the binder content from 3.2% to 4.1% (dried weight), and (3) analytical processing procedures using step by step checking to assure consistency.

Nakamura, H. H.↗

NASA NTRS1995

The orbital debris detector consortium: Suppliers of instruments for in-situ measurements of small-particles in the space environment

Industry and university participants have joined together to form the IMPA:Ct consortium (In-situ Monitors of the Particulate Ambient: Circumterrestrial) which offers a broad range of flight qualified instruments for monitoring the small particle (0.1 micron to 10 cm) environment in space. Instruments are available in 12 months or less at costs ranging from 0.5 to 1.5 million dollars (US) for the total program. Detector technologies represented by these groups are: impact-induced capacitor-discharge (MOS, metal-oxide-silicon), cratering or penetration of electroactive thin film (polyvinylidene fluoride (PVDF)), impact-plasma detection, acoustic detection, CCD tracking of optical scatter of sunlight, and photodiode detection of optical scatter of laser light. The operational characteristics, general spacecraft interface and resource requirements (mass/power/telemetry), cost and delivery schedules, and points of contact for seven different instruments are presented.

Simon, C. G.↗

DOE OSTI2023

Combustion synthesis of Eu 2 O 3 nanomaterials with tunable phase composition and morphology

Combustion reactions in europium nitrate – acetylacetone – 2-methoxyethanol solutions and gels were investigated to produce europium (III) oxide (Eu 2 O 3 ) nanocrystalline materials and thin films. Thermal analyses of solutions indicated that the 2-methoxyethanol solvent also acts as a fuel in the absence of acetylacetone. Adding acetylacetone increases the overall heat of the reaction. Thermal analysis results revealed that the slow oxidation of unburned hydrocarbon residues follows the primary combustion reaction. Time-temperature profile measurements of the bulk combustion synthesis process in air and nitrogen atmospheres enabled the extraction of the maximum reaction temperature and the heating and cooling rates in the combustion zone. Several direct correlations exist between measured combustion parameters and the phase composition of the products. Combustion in air results in mixed-phase cubic and monoclinic nanocrystalline Eu 2 O 3 . Increasing the acetylacetone concentration in solutions increases the synthesis temperature and decreases the quantity of cubic Eu 2 O 3 . Here, the reaction of solutions in a nitrogen atmosphere or diluted with Eu 2 O 3 provides control of the product phase composition and reduces the quantity of the monoclinic phase. Transmission electron microscopy imaging shows that the Eu 2 O 3 end products are highly porous aggregates of nanocrystalline particles. Electrospraying of reactive solutions onto different substrates followed by short annealing makes the preparation of Eu 2 O 3 materials with diverse morphologies possible.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1978

Role of back stress in the creep behavior of particle strengthened alloys

Recent developments in the interpolation of high-temperature steady-state creep results have introduced the concept that the stress dependence of the creep rate should be in terms of the effective stress referred to as the applied stress minus a back stress. This paper reports on back stresses taken from data on a gamma-prime-strengthened wrought nickel-base superalloy, an oxide dispersion-strengthened ODS nickel-base solid solution alloy, and an ODS nickel-base superalloy. The effect of air versus vacuum environments and the effect of dynamic changes in the strengthening microstructures on the magnitude of the back stress are assessed. The role of modulus normalization and the back stress correction in determining the true creep activation energy are examined. It is shown that the high values of the apparent stress exponent 'n' of the steady-state creep equation can be easily explained through a relationship between n, the true stress exponent of steady-state creep, and the stress which when subtracted from the applied stress results in the effective driving stress acting on the mobile dislocations during creep.

Purushothaman, S.↗

NASA NTRS2001

Evolution of the Earth and Origin of Life: The Role of Gas/Fluid Interactions with Rocks

The work under the Cooperative Agreement will be centered on questions of the evolution of Life on the early Earth and possibly on Mars. It is still hotly debated whether the essential organic molecules were delivered to the early Earth from space (by comets, meteorites or interplanetary dust particles) or were generated in situ on Earth. Prior work that has shown that the matrix of igneous minerals is a medium in which progenitors of organic molecules assemble from H2O, C02 and N2 incorporated as minority "impurities" in minerals of igneous rocks during crystallization from H2O/CO2/N2-laden magmas. The underlying processes involve a redox. conversion whereby C, H, and N become chemically reduced, while 0 becomes oxidized to the peroxy state. During Year 02 the work will be divided into three tasks. Task 1: After carboxylic (fatty) acids and N-bearing compounds have been identified, other extractable organic molecules including lipids, oily substances and amino acids will be studied. Dedicated lipid analysis will be combined with gas chromatographic-mass spectroscopic (GCMS) analysis of organic compounds extracted from minerals and rocks. Task 2: Using infrared (IR) spectroscopy, C-H entities that are indicators for the organic progenitors in mineral matrices will be studied. A preliminary heating experiment with MgO single crystals has shown that the C-H entities can be pyrolyzed, causing the IR bands to disappear, but at room temperature the IR bands reappear in a matter of days to weeks. This work will be expanded, both by studying synthetic MgO crystals and olivine crystals from the Earth's upper mantle. The C-H bands will be compared to the published "organic" IR feature of dust in the interstellar medium (ISM) and interplanetary dust particles (IDP). Task 3: A paradox marks the evolution of early Life: Oxygen is highly toxic to primitive life, yet early organisms "learned" to detoxify reactive oxygen species, to utilize oxygen, and even produce it. Why would organisms on the early anaerobic Earth be under evolutionary pressure to evolve defenses against reactive oxygen species? Minerals in igneous rocks are now known to contain peroxy. When such minerals weather, the peroxy hydrolyzes to H2O2. The hypothesis will be tested whether organisms living in intimate contact with rock surfaces are subjected to a constant trickle of H202 and thus under stress to develop strategies to either detoxify the reactive oxygen species or repair the molecular damage that they cause. Understanding these processes is central to the Astrobiology mission. It opens new avenues toward understanding the evolution of early life on Earth, and the potential for aerobic life elsewhere. This Cooperative Agreement also has a strong educational and public outreach component involving high school, undergraduate students, and high school teachers.

Freund, Friedemann↗

DOE OSTI2021

Resolving Chemical and Spatial Heterogeneities at Complex Electrochemical Interfaces in Li-Ion Batteries

The high specific capacities of Ni-rich transition metal oxides have garnered immense interest for improving the energy density of Li-ion batteries (LIBs). Despite the potential of these materials, Ni-rich cathodes suffer from interfacial instabilities that lead to crystallographic rearrangement of the active material surface as well as the formation of a cathode electrolyte interphase (CEI) layer on the composite during electrochemical cycling. While changes in crystallographic structure can be detected with diffraction-based methods, probing the chemistry of the disordered, heterogeneous CEI layer is challenging. In this work, we use a combination of ex situ solid-state nuclear magnetic resonance (SSNMR) spectroscopy and X-ray photoemission electron microscopy (XPEEM) to provide chemical and spatial information, on the nanometer length scale, on the CEI deposited on LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) composite cathode films. XPEEM elemental maps offer insight into the lateral arrangement of the electrolyte decomposition products that comprise the CEI and paramagnetic interactions (assessed with electron paramagnetic resonance (EPR) and relaxation measurements) in 13 C SSNMR provide information on the radial arrangement of the CEI from the NMC811 particles outward. Using this approach, here we find that LiF, Li 2 CO 3 , and carboxy-containing structures are directly appended to NMC811 active particles, whereas soluble species detected during in situ 1 H and 19 F solution NMR experiments (e.g., alkyl carbonates, HF, and vinyl compounds) are randomly deposited on the composite surface. We show that the combined approach of ex situ SSNMR and XPEEM, in conjunction with in situ solution NMR, allows spatially-resolved, molecular-level characterization of paramagnetic surfaces and new insights into electrolyte oxidation mechanisms in porous electrode films.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Molten Salt Synthesis of Increased (100)-Facet and Polycrystalline Nickel Oxide Nanoparticles for the Oxygen Evolution Reaction: Impact of Facet and Crystallinity on Electrocatalysis

Nickel oxide nanocubes with increased (100) surface facet presence (NiO(100)) were synthesized through a molten salt synthesis procedure to probe their oxygen evolution reaction (OER) activity in order to investigate the relationship between the surface facet and OER performance. While altering the synthesis parameters to decrease NiO(100) particle sizes and agglomeration, a polycrystalline NiO nanoparticle system formed from using Li2O as a Lux-Flood base (labelled Li2O-MSS NiO, where MSS stands for molten salt synthesis). This novel synthesis was further elaborated and the obtained materials were also tested for OER activity. After thorough structural characterization to determine crystallinity, lattice spacings, and elemental distribution, their OER activity was compared versus high surface area NiO(111) nanosheets in a three-electrode rotating disk electrode (RDE) system. The activity trend of (111) > Li2O-MSS > (100) was observed. This decrease in activity of the nanocube and polycrystalline samples was explained by differences between theoretical and experimental conditions, differences in ink rheology and resulting catalyst layer properties, and significant agglomeration seen in the imaging of the sample. Methods for improving the OER activity of these samples are discussed in the conclusion of this study.

08 HYDROGEN↗

DOE OSTI2022

Preliminary benchmarks and analysis of boundary conditions in a trenched microstructured silicon radiation detector

Microstructured neutron detectors have the benefit of enhanced neutron detection efficiency as compared to planar devices, achieved by etching 6 LiF-filled trenches on the top surface of a silicon PIN diode. This sensor geometry results in a complex electric field distribution and depletion characteristics within the diode under reverse bias. For the first time on record, the effects of a fixed oxide charge on the microstructured device depletion characteristics and mobile carrier transport is investigated. Prototype detectors were fabricated with non-conformal surface doping. Capacitance voltage and current voltage measurements were performed for these prototypes and compared with COMSOL Multiphysics simulations. A spectral response from an 241Am alpha particle source was acquired and analyzed. It was found that monoenergetic alpha particles produce three prominent peaks in the pulse height spectrum output by the device. The peaks were confirmed by simulations to correlate with dead layers and incident trajectories into the microstructure. It was also found that significant differences in pulse rise time result, corresponding with events arriving in a low-field region in the fins and a high-field region in the bulk. Geant4 was utilized for radiation transport, interaction modeling, and benchmarking the spectral data. The results of this simulation work provide confidence in the ability to attain and benchmark electrical characteristics and spectral data for semiconductor radiation detectors employing complex microstructures.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

NASA NTRS1973

An ERTS multispectral scanner experiment for mapping iron compounds.

An experiment is described which is designed to produce visible-reflective infrared ratio images from ERTS satellite data. The ERTS-A multispectral scanner has two channels in the visible-reflective infrared wavelength region which should be capable of duplicating aircraft scanner results. The average reflectances in the four ERTS-A MSS spectral bands for a few minerals and some vegetation are tabulated. The mineral laboratory samples were granular, with a particle diameter range of 250 to 1200 micrometer. If there were no spectral atmospheric or illumination variation effects, the ratio of energies in band 1 to band 4 would permit discrimination of pyroxenes (found in basic and ultrabasic rocks), quartz (found in acidic rocks), limonite and hematite (iron oxides), and green vegetation, on the basis of their respective ratio magnitudes.

Vincent, R. K.↗

NASA NTRS1979

Photographic combustion characterization of LOX/hydrocarbon type propellants

Single element injectors and two fuels were tested with the aim of photographically characterizing observed combustion phenomena. The three injectors tested were the O-F-O triplet, the transverse like on like (TLOL), and the rectangular unlike doublet (RUD). The fuels tested were RP-1 and propane. The hot firings were conducted in a specifically constructed chamber fitted with quartz windows for photographically viewing the impingement spray field. All LOX/HC testing demonstrated coking with the RP-1 fuel leaving far more soot than the propane fuel. No fuel freezing or popping was experienced under the test conditions evaluated. Carbon particle emission and combustion light brilliance increased with Pc for both fuels although RP-1 was far more energetic in this respect. The RSS phenomena appear to be present in the high Pc tests as evidenced by striations in the spray pattern and by separate fuel rich and oxidizer rich areas. The RUD element was also tested as a fuel rich gas generator element by switching the propellant circuits. Excessive sooting occurred at this low mixture ratio (0.55), precluding photographic data.

Judd, D. C.↗

NASA NTRS1992

Upper-atmosphere Aerosols: Properties and Natural Cycles

The middle atmosphere is rich in its variety of particulate matter, which ranges from meteorite debris, to sulfate aerosols, to polar stratospheric ice clouds. Volcanic eruptions strongly perturb the stratospheric sulfate (Junge) layer. High-altitude 'noctilucent' ice clouds condense at the summer mesopause. The properties of these particles, including their composition, sizes, and geographical distribution, are discussed, and their global effects, including chemical, radiative, and climatic roles, are reviewed. Polar stratospheric clouds (PSCs) are composed of water and nitric acid in the form of micron-sized ice crystals. These particles catalyze reactions of chlorine compounds that 'activate' otherwise inert chlorine reservoirs, leading to severe ozone depletions in the southern polar stratosphere during austral spring. PSCs also modify the composition of the polar stratosphere through complex physiocochemical processes, including dehydration and denitrification, and the conversion of reactive nitrogen oxides into nitric acid. If water vapor and nitric acid concentrations are enhanced by high-altitude aircraft activity, the frequency, geographical range, and duration of PSCs might increase accordingly, thus enhancing the destruction of the ozone layer (which would be naturally limited in geographical extent by the same factors that confine the ozone hole to high latitudes in winter). The stratospheric sulfate aerosol layer reflects solar radiation and increases the planetary albedo, thereby cooling the surface and possibly altering the climate. Major volcanic eruptions, which increase the sulfate aerosol burden by a factor of 100 or more, may cause significant global climate anomalies. Sulfate aerosols might also be capable of activating stratospheric chlorine reservoirs on a global scale (unlike PCSs, which represent a localized polar winter phenomenon), although existing evidence suggests relatively minor perturbations in chlorine chemistry. Nevertheless, if atmospheric concentrations of chlorine (associated with anthropogenic use of chlorofluorocarbons) continue to increase by a factor of two or more in future decades, aircraft emissions of sulfur dioxide and water vapor may take on greater significance.

Turco, Richard P.↗

NASA NTRS2011

High temperature strain gages

A ceramic strain gage based on reactively sputtered indium-tin-oxide (ITO) thin films is used to monitor the structural integrity of components employed in aerospace propulsion systems operating at temperatures in excess of 1500.degree. C. A scanning electron microscopy (SEM) of the thick ITO sensors reveals a partially sintered microstructure comprising a contiguous network of submicron ITO particles with well defined necks and isolated nanoporosity. Densification of the ITO particles was retarded during high temperature exposure with nitrogen thus stabilizing the nanoporosity. ITO strain sensors were prepared by reactive sputtering in various nitrogen/oxygen/argon partial pressures to incorporate more nitrogen into the films. Under these conditions, sintering and densification of the ITO particles containing these nitrogen rich grain boundaries was retarded and a contiguous network of nano-sized ITO particles was established.

Gregory, Otto J.↗

DOE OSTI2020

Point defects in Ga 2 O 3

In the field of high-power electronics, gallium oxide (Ga 2 O 3 ) is attracting attention due to its wide band gap and ability to be doped n-type. Point defects, including vacancies, impurities, and dopants, play important roles in optimizing device performance. This tutorial discusses the fundamental properties of point defects in monoclinic β-Ga 2 O 3 and the methods employed to study them. Oxygen vacancies are deep donors that do not cause n-type conductivity but may compensate acceptors. Gallium vacancies are deep acceptors that can be partially passivated by hydrogen. Substitutional magnesium is a promising acceptor that produces semi-insulating material and also forms a complex with hydrogen. Calcium and iron also have deep acceptor levels. Iridium deep donors are introduced into crystals grown from a melt in an Ir crucible. Here, other defects are introduced by irradiation with energetic particles such as neutrons or protons. In addition to altering the electronic properties, defects give rise to UV/visible emission bands in photoluminescence and cathodoluminescence spectra.

36 MATERIALS SCIENCE↗