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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Role of Modulators in Controlling the Colloidal Stability and Polydispersity of the UiO-66 Metal–Organic Framework

We report nanoscale UiO-66 Zr 6 (OH) 4 O 4 (C 8 O 4 H 4 ) 6 has been synthesized with a series of carboxylic acid modulators, R-COOH (where R = H, CH 3 , CF 3 , and CHCl 2 ). The phase purity and size of each MOF was confirmed by powder X-ray diffraction, BET surface area analysis, and scanning transmission electron microscopy (STEM). Size control of UiO-66 crystals from 20 nm to over 1 μm was achieved, and confirmed by STEM. The colloidal stability of each MOF was evaluated by dynamic light scattering and was found to be highly dependent on the modulator conditions utilized in the synthesis, with both lower pKa and higher acid concentration resulting in more stable structures. Furthermore, STEM was carried out on both colloidally stable samples and those that exhibited a large degree of aggregation, which allowed for visualization of the different degrees of dispersion of the samples. The use of modulators at higher concentrations and with lower pKas leads to the formation of more defects, as a consequence of terephthalic acid ligands being replaced by modulator molecules, thereby enhancing the colloidal stability of the UiO-66 nanoparticles. These findings could have a significant impact on nanoscale MOF material syntheses and applications, especially in the areas of catalysis and drug delivery.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Cascade Reaction of Ethanol to Butadiene over Ag-Promoted, Silica- or Zeolite-Supported Ta, Y, Pr, or La Oxide Catalysts

Ethanol converts to 1,3-butadiene in the presence of suitable multifunctional catalysts. In this work, Lewis acid cations Ta, Y, Pr, and La were dispersed on amorphous silica or beta zeolite, and after physically mixing with silica-supported Ag nanoparticles, were tested in the cascade reaction of ethanol to butadiene at 573 K. The Lewis acid catalysts were characterized by X-ray fluorescence, N 2 physisorption, scanning transmission electron microscopy (STEM), X-ray diffraction, diffuse reflectance (DR) UV-Vis and X-ray photoelectron spectroscopy. High-resolution STEM images confirmed the small oxide cluster size on the silica support. Results from DR UV-Vis spectroscopy showed zeolite-supported Ta and Pr catalysts had a smaller metal oxide cluster size, relative to their SiO 2 counterparts. X-ray photoelectron spectroscopy confirmed the oxidation state of the cations supported on the zeolite remained the same as that of their SiO 2 -supported analogues. The selectivity of the C 4 coupling products toward butadiene relative to butanol correlated with acid strength of the Lewis acid cations, as evaluated by the 2-propanol decomposition reaction to propene and acetone, with Ta being the most selective. In conclusion, the rate of C-C coupling over the zeolite-supported cations was enhanced by an order of magnitude compared to those cations supported on amorphous SiO 2 .

C-C bond formation↗
DOE OSTI2015

In situ spectroscopic characterization of Ni 1-x Zn x /ZnO catalysts and their selectivity for acetylene semihydrogenation in excess ethylene

The structures of ZnO-supported Ni catalysts were explored with in situ X-ray absorption spectroscopy, temperature-programmed reduction, X-ray diffraction, high-resolution transmission electron microscopy (HRTEM), scanning transmission electron microscopy, and electron energy loss spectroscopy. Calcination of nickel nitrate on a nanoparticulate ZnO support at 450 °C results in the formation of Zn-doped NiO (ca. N₀̣̣₈₅ Zn₀̣̣₁₅O) nanoparticles with the rock salt crystal structure. Subsequent in situ reduction monitored by X-ray absorption near-edge structure (XANES) at the Ni K edge reveals a direct transformation of the Zn-doped NiO nanoparticles to a face-centered cubic alloy, Ni 1-x Zn x , at ~400 °C with x increasing with increasing temperature. Both in situ XANES and ex situ HRTEM provide evidence for intermetallic β₁-NiZn formation at ~550 °C. In comparison to a Ni/SiO₂ catalyst, Ni/ZnO necessitates a higher temperature for the reduction of Ni II to Ni⁰, which highlights the strong interaction between Ni and the ZnO support. The catalytic activity for acetylene removal from an ethylene feed stream is decreased by a factor of 20 on Ni/ZnO in comparison to Ni/SiO₂. The decrease in catalytic activity of Ni/ZnO is accompanied by a reduced absolute selectivity to ethylene. H–D exchange measurements demonstrate a reduced ability of Ni/ZnO to dissociate hydrogen in comparison to Ni/SiO₂.These results of the catalytic experiments suggest that the catalytic properties are controlled, in part, by the zinc oxide support and stress the importance of reporting absolute ethylene selectivity for the catalytic semihydrogenation of acetylene in excess ethylene.

Spanjers, Charles S.↗
DOE OSTI2014

Spatial Control Of Functional Properties Via Octahedral Modulations In Complex Oxide Superlattices

The design of distortions and rotations of the corner-connected BO6 octahedra across interfaces has emerged as an exciting platform to control electronic or ferroic behavior in ABO3 perovskite heterostructures. Here, we investigate isovalent manganite superlattices, [(La0.7Sr0.3MnO3)n/(Eu0.7Sr0.3MnO3)n]×m, as a route to spatial control over electronic bandwidth and ferromagnetism through the creation of octahedral superstructures. Electron energy loss spectroscopy confirms a uniform Mn valence state throughout the superlattices. In contrast, the presence of modulations of the MnO6 octahedral rotations along the growth direction commensurate with the superlattice period is revealed by scanning transmission electron microscopy and x-ray diffraction. We show that the Curie temperatures of the constituent materials can be systematically engineered via the octahedral superstructures leading to a modulated magnetization in samples where the superlattice period is larger than the interfacial octahedral coupling length scale, while a single magnetic transition is observed in the short period superlattices.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2015

Visible-light-driven Bi 2 O 3 /WO 3 composites with enhanced photocatalytic activity

Semiconductor heterojunctions (composites) have been shown to be effective photocatalytic materials to overcome the drawbacks of low photocatalytic efficiency that results from electron–hole recombination and narrow photo-response range. We prepared a novel visible-light-driven Bi 2 O 3 /WO 3 composite photocatalyst by hydrothermal synthesis. The composite was characterized by scanning transmission electron microscopy (STEM), scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), X-ray photoelectron spectroscopy (XPS), Brunauer–Emmett–Teller (BET) surface area, Raman spectroscopy, photoluminescence spectroscopy (PL) and electrochemical impedance spectroscopy (EIS) to better understand the structures, compositions, morphologies and optical properties. Bi 2 O 3 /WO 3 heterojunction was found to exhibit significantly higher photocatalytic activity towards the decomposition of Rhodamine B (RhB) and 4-nitroaniline (4-NA) under visible light irradiation compared to that of Bi 2 O 3 and WO 3 . A tentative mechanism for the enhanced photocatalytic activity of the heterostructured composite is discussed based on observed activity, band position calculations, photoluminescence, and electrochemical impedance data. Our study provides a new strategy for the design of composite materials with enhanced visible light photocatalytic performance.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Stabilization and transformation of Pt nanocrystals supported on ZnAl 2 O 4 spinel

The role of interfacial interaction on the stabilization and transformation of Pt nanocrystals supported on zinc aluminate (ZnAl2O4) was systematically studied in this work. In addition to the remarkable stability of Pt nanocrystals supported on the {111} ZnAl2O4 facet under harsh oxidizing atmosphere, we also identified the phase segregation of ZnAl2O4 to ZnO and Al2O3 and the transformation of Pt to PtZn bimetallic alloy for Pt supported on other facets. High resolution scanning transmission electron microscope and X-ray diffraction analysis reveal the phase segregation is associated with a cation migration mechanism associated with replacement of Zn2+ by Al3+ in the spinel structure. This work confirms the strong interfacial interactions between precious metal nanocrystals and the spinel support is a general mechanism for stabilizing precious metal catalysts, and has important implication for the rational design of stable integrated catalysis systems

Environmental Molecular Sciences Laboratory↗
DOE OSTI2022

Electrospun porous La–Sr–Co–Ni–O nanofibers for highly sensitive non-enzymatic glucose detection

Glucose biosensors are widely used for clinical, industrial, and environmental applications. Nonenzymatic electrochemical glucose biosensors based on metal oxides with a perovskite structure have exhibited high sensitivity, excellent stability, and cost efficiency. In this work, porous La–Sr–Co–Ni–O (LSCNO) nanofibers, with an ABO 3 -type perovskite structure, were prepared through optimizing the A-site and B-site elements by electrospinning, followed with calcination at 700 °C for 5 h. Characterized by scanning and transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy, fabricated nanofibers were confirmed to be porous and nanosized polycrystalline grains with high crystallinity. A novel La 0.75 Sr 0.25 Co 0.5 Ni 0.5 O 3 -based nonenzymatic electrochemical biosensor was developed, which is sensitive to glucose because of an electrochemically catalytic mechanism, a mediated electron transfer involving Ni(II)/Ni(III) or Co(II)/Co(III), accompanying with gluconic acid complexation. The glucose biosensor presented a linear response in the range of 0.1–1.0 mM with a calibration sensitivity of 924 ± 28 μA mM –1 , a proportion of the variance of 0.9926, and a lower limit of detection of 0.083 mM, respectively, demonstrating an outstanding analytical performance. The biosensor showed no response to the most widely used anionic surfactant, sodium dodecyl sulfate, and low sensitivity to other biomolecules, such as fructose, lactose, galactose, mannose, dopamine, and ascorbic acid. A urine sample was tested by this novel nonenzymatic electrochemical biosensor by standard addition method, suggesting a potential application for clinical test.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Uptake and binding of La 3+ and Cr 3+ ions by alkali metal substituted alpha-zirconium phosphate

The conversion of alpha-zirconium phosphate, Zr(HPO 4 ) 2 ·H 2 O, to the K-, Rb-, and Cs-phases and the subsequent ion exchange behavior of these alkali metal phases, A-ZrP, with La 3+ and Cr 3+ have been investigated. The conversion to the A-ZrP phases was achieved by reaction with metal chloride, metal hydroxide solution, and confirmed through various techniques, including X-ray powder diffraction, thermogravimetry analysis, IR spectroscopy, scanning and transmission electron microscopy, and X-ray photoelectron spectroscopy. The effect of material hydration, which increased the interlayer distance, was also examined. The ion exchange behavior of the A-ZrP showed strong affinity for both La 3+ , a representative for trivalent lanthanide metals, and Cr 3+ , a representative for the trivalent transition metals, with a rapid, near quantitative removal of the M 3+ ions at a pH of 3 when the ion concentration was ≤25% of the ion exchange capacity of the materials. Additionally, the ion affinity was shown to be pH and concentration-dependent, decreasing with a decrease in pH or an increase in ion concentration. Lastly, the binding strength of La- and Cr-loaded ZrP materials was examined through a series of leaching experiments in a carbonate buffer, phosphate buffer, HEPES buffer, and a series of EDTA solutions at various concentrations. No observable leaching occurred in the carbonate buffer, phosphate buffer, HEPES buffer, or when the EDTA concentration was below 0.1 mM. These results highlight the potential for the A-ZrP materials to provide a platform for trivalent transition metal and trivalent lanthanide radionuclide capture for various applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Improving lithium-ion battery performances by adding fly ash from coal combustion on cathode film

A lithium battery is composed of anode, cathode and a separator. The performance of lithium battery is also influenced by the conductive material of cathode film. In this research, the use of fly ash from coal combustion as conductive enhancer for increasing the performances of lithium battery was investigated. Lithium iron phosphate (LiFePO{sub 4}) was used as the active material of cathode. The dry fly ash passed through 200 mesh screen, LiFePO{sub 4} and acethylene black (AB), polyvinylidene fluoride (PVDF) as a binder and N-methyl-2-pyrrolidone (NMP) as a solvent were mixed to form slurry. The slurry was then coated, dried and hot pressed to obtain the cathode film. The ratio of fly ash and AB were varied at the values of 1%, 2%, 3%, 4% and 5% while the other components were at constant. The anode film was casted with certain thickness and composition. The performance of battery lithium was examined by Eight Channel Battery Analyzer, the composition of the cathode film was examined by XRD (X-Ray Diffraction), and the structure and morphology of the anode film was analyzed by SEM (Scanning Electron Microscope). The composition, structure and morphology of cathode film was only different when fly ash added was 4% of AB or more. The addition of 2% of AB on cathode film gave the best performance of 81.712 mAh/g on charging and 79.412 mAh/g on discharging.

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

Properties of different LLM-105 preparations

LLM-105 (2,6-diamino-3,5-dinitropyrazine-1-oxide) has been prepared at several different size quantities (~10–70 Kg) and not subjected to further purification, such as recrystallization. Chemical and physical properties were compared—small-scale safety testing (impact, friction, ESD), thermal (chemical reactivity, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), one-dimensional time-to-explosion (ODTX)), morphological (particle-size distribution (PSD), scanning electron microscopy (SEM), powder x-ray diffraction (PXRD), skeletal density). Each preparation had similar properties to the other preparations except for PSD and PXRD. For PSD, all preparations exhibited a mono-modal distribution with a variation in median values from ~ 40 μm to over 80 μm. All PXRD values indicated the same morphology with minor variations in crystal orientations. Possible polymorphism was also observed in a few cases. SEM images and PXRD indicate all preparations to be diamond-type and X-type crystals with some twinning. Impact, friction, and ESD and thermal sensitivities values are consistent with these type of crystal habits as seen in vast literature studies.

Explosive characterization↗
DOE OSTI2023

Cr silicate as a prototype for engineering magnetic phases in air-stable two-dimensional transition-metal silicates

Abstract Identifying environmentally inert, ferromagnetic two-dimensional (2D) materials with high Curie temperatures ( T c ) down to the single layer limit has been an obstacle to fundamental studies of 2D magnetism and application of 2D heterostructures to spin-polarized devices. To address this challenge, the growth, structure and magnetic properties of a 2D Cr-silicate single layer on Pt(111) was investigated experimentally and theoretically. The layer was grown by sequentially depositing SiO and Cr followed by annealing in O 2 . Scanning tunneling microscopy (STM), low-energy electron diffraction (LEED), and low energy electron microscopy all indicated a well-ordered layer that uniformly covered the surface, with STM and LEED indicating that the silicate relaxed to its favored lattice constant. Further experimental characterizations demonstrated that the Cr was nominally 3+ but with a lower electron density than typical trivalent Cr compounds. Comparison with theory identified a Cr 2 Si 2 O 9 structure that resembles a single layer of a dehydrogenated dioctahedral silicate. Magnetic circular dichroism in x-ray absorption spectroscopy revealed a ferromagnetically ordered state up to at least 80 K. Theoretical analysis revealed that the Cr in a dehydrogenated Cr-silicate/Pt(111) is more oxidized than Cr in freestanding Cr 2 Si 2 O 9 H 4 layers. This greater oxidation was found to enhance ferromagnetic coupling and suggests that the magnetism may be tuned by doping. The 2D Cr-silicate is the first member of a broad series of possible layered first-row transition metal silicates with magnetic order; thus, this paper introduces a new platform for investigating 2D ferromagnetism and the development of magnetoelectronic and spintronic devices by stacking 2D atomic layers.

2D materials↗
DOE OSTI2016

Prediction of two-dimensional topological insulator by forming a surface alloy on Au/Si(111) substrate

Two-dimensional (2D) topological insulators (TIs), which can be integrated into the modern silicon industry, are highly desirable for spintronics applications. Here, using first-principles electronic structure calculations, we show that the Au/Si(111)- 3 substrate can provide a platform for hosting 2D TIs obtained through the formation of surface alloys with a honeycomb pattern of adsorbed atoms. We systematically examined elements from groups III to VI of the periodic table at 2/3 monolayer coverage on Au/Si(111)- 3 , and found that In, Tl, Ge, and Sn adsorbates result in topologically nontrivial phases with band gaps varying from 0 to 50 meV. Our scanning tunneling microscopy and low-energy electron diffraction experiments confirm the presence of the honeycomb pattern when Bi atoms are deposited on Au/Si(111)- 3 , in accord with our theoretical predictions. Our findings pave the way for using surface alloys as a potential route for obtaining viable 2D TI platforms.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

In situ characterization of foreign object damage (FOD) in environmental-barrier-coated silicon carbide (SiC) ceramic

Environmental barrier coatings (EBCs) protect advanced ceramics and ceramic matrix composites (CMCs) from oxidation and corrosion in gas turbine engine environments. Foreign object damage (FOD), where debris impact the protective coatings, is a critical hazard which limits the turbine durability. Despite previous efforts to understand FOD in EBCs, a detailed understanding of the fundamental transient damage mechanisms is still lacking. In the current work, the real-time FOD behavior of a Mullite / Silicon EBC was visualized via a dynamic synchrotron X-ray source in phase contrast imaging (PCI) configuration. Prior to the in situ FOD experiments, the microstructure and composition of the coating were respectively characterized using a scanning electron microscope (SEM) and X-ray diffraction (XRD). The variation in the properties of the debris was modeled by ~ 1.5 mm diameter Partially Stabilized Zirconia (PSZ) and Silicon Nitride (Si 3 N 4 ) spheres. A modified light-gas gun setup, synchronized with the X-ray beam, was used to propel the projectiles at velocities ranging between 300 and 355 m·s -1 . Coated samples were impacted under a fully backed support configuration and at normal incidence. Coating penetration and delamination, as well as projectile deformation at the bond coat resulted for FOD by PSZ spheres. Comparatively, projectile fracture, with subsequent rebound of fragments, as well as complete coating penetration and delamination at the substrate interface occurred for FOD by Si 3 N 4 spheres. It should be noted that only cone cracking was observed for FOD by PSZ spheres while back surface cracking was present for both projectile types. Qualitative understanding of the driving forces for the observed damage mechanisms were provided.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Temperature, Time, Concentration, Annealing, and Substrates on ZnO Nanorod Arrays Growth by Hydrothermal Process on Hot Plate

Well aligned 1D ZnO nanostructures are important for optoelectronic and nanoscale electronic devices. In this report, 1D ZnO nanorods were synthesized by very simple, low cost, low temperature hydrothermal process. An effect of concentration, growth time, growth temperature, seed layer annealing, and seed layer thickness was investigated. The synthesized ZnO nanorods were characterized by scanning and transmission electron microscopies, X-ray diffraction, Raman and ultraviolet–visible spectroscopies. Growth parameters were found to influence strongly on the morphology, orientation, diameter, length, and density of the ZnO nanorod arrays. The growth temperature 80–90°C, seed layer annealing at 300–400°C, growth time 3 h, 0.025 M precursor concentration, and 0.2–0.3 M seed layer solution concentrations are more favorable conditions for better orientation and excellent crystallinity of the ZnO nanorods.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Effect of CMAS composition on hot corrosion behavior of gadolinium zirconate thermal barrier coating materials

The resistance of synthesized pyrochlore-type Gd 2 Zr 2 O 7 bulk specimens to four calcium-magnesium aluminosilicate (CMAS) compositions at different temperatures was investigated. The reaction products were identified by x-ray diffraction and penetration depths were examined using scanning electron microscopy. A dense reaction layer is comprised mainly of Ca 2 Gd 8 (SiO 4 ) 6 O 2 and a cubic fluorite phase formed during the CMAS attack, and some unreacted CMAS was found in a transition layer below the reaction layer. The overall infiltration depth changed slightly with temperature, however, the thickness of the reaction layer and the morphology of the transition layer varied distinctly with temperature. The sintered sample underwent the most severe degradation by the CaO-lean CMAS, whereas the effect of CaSO 4 and CaCO 3 was not significant. Furthermore, the Gd content of the ZrO 2 -based cubic fluorite phase depends on the temperature and the molar ratio of Ca:Si in the CMAS.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Chemical weathering of layered Ni-rich oxide electrode materials: Evidence for cation exchange

Lithiated ternary oxides containing nickel, cobalt, and manganese are intercalation compounds that are used as positive electrodes in high-energy lithium-ion batteries. These materials undergo compositional changes that adversely affect their cycling performance when they are stored in humid air or exposed to moisture. There is a new urgency to better understanding of these “weathering” processes as manufacturing moves towards a more environmentally benign aqueous processing of the positive electrode. Delithiation in the oxide subsurface regions and the formation of lithium salts (such as hydroxides and carbonates) coating the surface, have been suggested as chemical drivers for these processes, but the mechanistic details remain poorly known. The redox reactions which follow oxide delithiation are believed to cause all of the observed transformations. In this article we suggest another possibility: namely, the proton – lithium exchange. We argue that this hypothesis provides a simple, comprehensive rationale for our observations from X-ray diffraction, X-ray photoelectron spectroscopy, scanning transmission electron microscopy, and electrochemical measurements. These observations include contraction of the c-axis (unit cell) lattice parameter, strain in the crystalline oxide bulk, directionality of the chemical damage, formation of amorphous surface films, and the partial recovery of capacity loss by electrochemical relithiation of the material. Lastly, these effects need to be mitigated before aqueous processing of the positive electrode can find widespread adoption during cell manufacturing.

25 ENERGY STORAGE↗
DOE OSTI2018

An alkali-free method to manufacture ramie fiber

Ramie is one of the most significant fiber resources and it needs the degumming process to produce fibers. The traditional manufacturing process of ramie fibers requires a large amount of alkali, which causes serious environmental issues. This paper presents a novel path to manufacture ramie fibers without alkali. In this study, ramie bast was pretreated by steam explosion and then treated with deep eutectic solvent. The properties of ramie fibers prepared by the novel alkali-free method, including physical properties, Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and X-ray diffraction (XRD), were compared with that produced by the traditional alkali process. Results showed that the fiber qualities, including residual gum content (4.68%), average fiber fineness (1419.99 N m ) and breaking tenacity (5.98 cN/dtex), were comparable with the traditional alkali process, which all meet the requirement of the relevant Chinese National Standards. The FTIR, SEM and XRD results all confirmed the degumming ability of the novel method to manufacture ramie fibers. Furthermore, the novel method was proved to be eco-friendly. Taken together, these data indicate that the novel alkali-free method is green and effective in manufacturing ramie fibers.

42 ENGINEERING↗