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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 1,045 records · Page 58
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Si(hhm) surfaces: Templates for developing nanostructures

The fabrication of ordered low-dimensional structures on clean and metal-atom-decorated stepped Si(557) and Si(556) surfaces is discussed. The formation conditions and atomic structure of regular step systems on clean Si(557) 7 × 7 and Si(556) 7 × 7 surfaces are studied. The atomic structure of stepped Si(hhm), Ag/Si(557), and Gd/Si(557) surfaces is studied using high-resolution scanning tunneling microscopy and low-energy electron diffraction. The possibility of fabricating 1D and 2D structures of gadolinium and silver atoms on the Si(557) surface is demonstrated.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Beam current effect as a potential challenge in SEM-EBSD in situ tensile testing

Highlights: • In situ SEM-EBSD tensile tests were conducted using 304L steels with 8 and 10.4% Ni. • KAM and GROD evolution, twinning, and phase instability were investigated. • Phase transformation in 8% Ni-steel was sensitive to the electron beam current. In situ mechanical tensile tests coupled with electron backscatter diffraction (EBSD) analysis were conducted using specimens of two 304L steels with ~8 and 10.4% Ni content, respectively. Twinning was observed in steel with 10.4% Ni content, whereas steel with 8% Ni content demonstrated martensitic transformation. Testing showed that the kinetics of martensitic transformation in steel with 8% Ni content was influenced by the electron beam current used during EBSD scans. Continuous scanning using 32 nA nominal beam current led to suppression of the phase instability in the near-surface layer, but acceptable comparable-to-the-bulk results were obtained using 8 nA beam current. The exact mechanism of the beam current role is unclear, but it appears to be neutral regarding Kernel Average Misorientation behavior and deformation-induced twinning.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Thermally induced formation of 2D hexagonal BN nanoplates with tunable characteristics

We have investigated a thermally induced combustion route for preparing 2D hexagonal BN nanoplates from B{sub 2}O{sub 3}+(3+0.5k)Mg+kNH{sub 4}Cl solid system, for k=1–4 interval. Temperature–time profiles recorded by thermocouples indicated the existence of two sequential exothermic processes in the combustion wave leading to the BN nanoplates formation. The resulting BN nanoplates were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy, PL spectrometry, and Brunauer–Emmett–Teller surface area analysis. It was found that B{sub 2}O{sub 3} was converted into BN completely (by XRD) at 1450–1930 °C within tens of seconds in a single-step synthesis process. The BN prepared at a k=1–4 interval comprised well-shaped nanoplates with an average edge length ranging from 50 nm to several micrometer and thickness from 5 to 100 nm. The specific surface area of BN nanoplates was 13.7 g/m{sup 2} for k=2 and 28.4 m{sup 2}/g for k=4. - Graphical abstract: 2D hexagonal BN nanoplates with an average edge length ranging from 50 nm to several micrometer and thickness from 5 to 100 nm were prepared by combustion of B{sub 2}O{sub 3}+(3+0.5k)Mg+kNH{sub 4}Cl solid mixture in nitrogen atmosphere. - Highlights: • Thermally induced combustion route was developed for synthesizing BN nanoplates from B{sub 2}O{sub 3}. • Mg was used as reductive agent and NH{sub 4}Cl as an effective nitrogen source. • Temperature–time profiles and the combustion parameters were recorded and discussed. • BN with an average edge length from 50 nm to several micrometer and thickness from 5 to 100 nm were prepared. • Our study clarifies the formation mechanism of BN in the combustion wave.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Electrochemical behavior of β-MnO{sub 2} and MnOOH nanorods in different electrolytes

A manganese dioxide (β-MnO{sub 2}) and MnOOH nanoparticles has been synthesized by hydrothermal method. As prepared samples are analyzed by X-ray Diffraction (XRD) and Field Emission Scanning Electron Microscopy (FESEM). FESEM showed rod morphology within the diameter of 50–200 and length of few nanometers. These nanorods are immobilized on a Glassy Carbon Electrode (GCE) by drop cast method. The comparative electrochemical behavior of β-MnO{sub 2} and MnOOH rod modified GCE electrodes are analyzed by cyclic Voltammetry (CV) method in different electrolytes of 0.1M KCl, 0.1M Na{sub 2}SO{sub 4}, 0.1M NaOH, 0.1M PBS, 0.1M H{sub 2}SO{sub 4}. From the cyclic Voltammetry analysis found that in all the electrolytes both β-MnO{sub 2} and MnOOH modified GCE electrodes exhibit electrochemical behavior and KCl shows well redox properties as compared with others. There is also an observable difference in reduction potential value of both crystalline nanostructurers and concluded that β-MnO{sub 2} has high catalytic ability as compared with MnOOH rods.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Gas sensing behaviour of Cr{sub 2}O{sub 3} and W{sup 6+}: Cr{sub 2}O{sub 3} nanoparticles towards acetone

This paper reports the acetone gas sensing properties of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} nanoparticles. The simple cost-effective hydrolysis assisted co-precipitation method was adopted. Synthesized samples were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. XRD revealed that synthesized nanoparticles have corundum structure. The lattice parameters have been calculated by Rietveld refinement; and strain and crystallite size have been calculated by using the Williamson-Hall plots. For acetone gas sensing properties, the nanoparticles were applied as thick film onto alumina substrate and tested at different operating temperatures. The results showed that the optimum operating temperature of both the gas sensors is 250°C. At optimum operating temperature, the response of Cr{sub 2}O{sub 3} and 2% W{sup 6+} doped Cr{sub 2}O{sub 3} gas sensor towards 100 ppm acetone was found to be 25.5 and 35.6 respectively. The investigations revealed that the addition of W{sup 6+} as a dopant enhanced the sensing response of Cr{sub 2}O{sub 3} nanoparticles appreciably.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Selective growth of ZnO thin film nanostructures: Structure, morphology and tunable optical properties

The ZnO nanostructures (spherical, rod shape) have been successfully fabricated via a thermal evaporation followed by dip coating method. The pure, doped ZnO thin films were characterized by X-ray powder diffraction (XRD) and field emission scanning electron microscopy (FESEM) and UV-Vis spectroscopy, respectively. A possible growth mechanism of the spherical, rod shape ZnO nanostructures are discussed. XRD patterns revealed that all films consist of pure ZnO phase and were well crystallized with preferential orientation towards (002) direction. Doping by PVA, PVA+Cu has effective role in the enhancement of the crystalline quality and increases in the band gap.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Effect of carbonation temperature on CO{sub 2} adsorption capacity of CaO derived from micro/nanostructured aragonite CaCO{sub 3}

Recent years, CaO-based synthetic materials have been attracted attention as potential adsorbents for CO{sub 2} capture mainly due to their high CO{sub 2} adsorption capacity. In this study, micro/nanostructured aragonite CaCO{sub 3} was synthesized by a simple hydrothermal method with using polyacrylamide (PAM). The structural, morphological and thermal properties of the synthesized sample were investigated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and thermogravimetry analysis (TG-DTA). The XRD and FESEM results showed that the obtained sample was aragonite CaCO{sub 3} with aggregated nanorods and microspheres composed of nanorods. A TG-DTA apparatus with Thermoplus 2 software was used to investigate the effect of carbonation temperature on the CO{sub 2} adsorption capacity of CaO derived from aragonite CaCO{sub 3} sample. At 300 °C, the sample reached the CO{sub 2} adsorption capacity of 0.098 g-CO{sub 2}/g-adsorbent, whereas the sample achieved the highest capacity of 0.682 g-CO{sub 2}/g-adsorbent at 700 °C. The results showed that the carbonation temperature significantly influenced on the CO{sub 2} adsorption capacity of the CaO derived from aragonite CaCO{sub 3}.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Formation and Acid–Base Surface Properties of Highly Dispersed η-Al{sub 2}O{sub 3} Nanopowders

Highly dispersed η-Al{sub 2}O{sub 3}-based nanopowders have been prepared via glycine–nitrate combustion followed by heat treatment in air. The resultant materials have been characterized by X-ray diffraction, Fourier transform IR spectroscopy, scanning electron microscopy, simultaneous thermal analysis, and other techniques. We have optimized the glycine-to-nitrate ratio (G/N = 0.2) and found heat treatment conditions for combustion products (isothermal holding at a temperature of 700°C for 6 h) that allow one to obtain single- phase nanocrystalline η-Al{sub 2}O{sub 3} powders with an average particle size of 5 ± 1 nm and specific surface area of 54 ± 5 m{sup 2}/g. The acid–base surface properties of the η-Al{sub 2}O{sub 3} nanopowder have been analyzed using pyridine sorption–desorption processes as an example. The specific concentrations of weak, intermediate, and strong Lewis acid centers on the surface of the η-Al{sub 2}O{sub 3} nanocrystals have been shown to markedly exceed those on the surface of commercially available γ-Al{sub 2}O{sub 3} (A-64). The synthesized nanopowders can thus be used as effective supports of acid catalysts.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2023

Probing the thermal decomposition of plutonium (III) oxalate with IR and Raman spectroscopy, X-ray diffraction, and electron microscopy

The thermal decomposition of Pu(III) oxalate was analyzed by Raman microspectroscopy, infrared spectroscopy, scanning electron microscopy, and powder X-ray diffraction. These data show that crystalline Pu 2 (C 2 O 4 ) 3 •9H 2 O progressively loses water and oxalate ligands as it is heated, which leads to a decrease in long-range lattice ordering, though minimal changes are observed in gross crystalline morphology. The onset of PuO 2 formation was observed between 200 - 250 °C. Thermal decomposition of oxalate ligands leads to the formation of CO 2 and plutonium oxalate-carbonate moieties, which had not been observed in previously published thermogravimetric measurements of Pu(III) oxalate. Formation of plutonium oxalate-carbonate moieties is believed to be associated with a change in the plutonium oxidation state from 3+ to 4+, which occurs prior to PuO 2 formation. The data provided herein demonstrate the rich spectroscopic nature of a rather underexplored, and technologically relevant, plutonium system. Ideally these results will further future investigations into the Pu(III) oxalate system both experimentally and computationally.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Structure-property relation and Weibull analysis of calcium aluminate cement pastes

Highlights: • Weibull distribution analysis was conducted for calcium aluminate cement pastes with 52 wt% and 71 wt% of alumina contents. • Compressive strength ranged from 10 to 45 MPa. • The hydrated phases found showed diverse polymorphisms of Gibbsite (Nordstrandite, Bayerite, Hidrogarnet and Gehlenite). - Abstract: In this investigation calcium aluminate cement (CAC) pastes with 52 wt% and 71 wt% of alumina contents were fabricated and characterized with different techniques. Samples were made with 0.4 and 0.5 water to cement (W/C) ratios. Both the raw cement powders and their corresponding samples after hydration were characterized in their microstructure by scanning electron microscopy, X-ray diffraction (with Rietveld refinement), X-ray fluorescence (XRF), Fourier Transform Infrared Spectroscopy (FTIR), density, and compression tests. With the compressive strength results, Weibull distribution analysis was conducted for 20 samples per composition. The higher compression strength obtained was about 45 MPa, which corresponds to samples with the higher W/C contents. The hydrated phases found showed diverse polymorphisms of Gibbsite (Nordstrandite, Bayerite, Hidrogarnet and Gehlenite).

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of pure Ni ultrafine/nanoparticles synthesized by electromagnetic levitational gas condensation method

Highlights: • Ni ultrafine/nanoparticles were produced using the single-step ELGC method. • Ar and He–20%Ar gas mixtures were used as the condensing gas under 1 atm. • Effects of gas type and flow rate on particle size distribution were investigated. • The nanoparticles showed both high saturation magnetization and low coercivity. - Abstract: In this work, Ni ultrafine/nanoparticles were directly produced using the one-step, relatively large-scale electromagnetic levitational gas condensation method. In this process, Ni vapors ascending from the levitated droplet were condensed by Ar and He–20%Ar gas mixtures under atmospheric pressure. Effects of type and flow rate of the condensing gas on the size, size distribution and crystallinity of Ni particles were investigated. The particles were characterized by scanning electron microscopy, X-ray diffraction and vibrating sample magnetometer (VSM). The process parameters for the synthesis of the crystalline Ni ultrafine/nanoparticles were determined.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Improving the cycle stability of LiCoPO{sub 4} nanocomposites as 4.8 V cathode: Stepwise or synchronous surface coating and Mn substitution

Nanostructured LiCo{sub 1−x}Mn{sub x}PO{sub 4}/C (x = 0 and 0.05) materials were successfully produced as superior quality cathodes by combined sol-gel and carbothermal reduction methods. X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), high-resolution transmission electron microscopy (HR-TEM), energy dispersive spectroscopy (EDS), fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma (ICP), cyclic voltammetry (CV) and galvanostatic measurements were applied to determine the phase purity, morphology and electrochemical qualifications. HR-TEM analysis reveals that the thickness of the surface carbon layer of 5 to 10 nm range with the uniform distribution. LiCo{sub 0·95}Mn{sub 0·05}PO{sub 4}/C particles were between 40 and 80 nm and the same material exhibits a higher and stable reversible capacity (140 mA h g{sup −1}) with the long voltage plateau (4.76 V). Substitution of Co{sup 2+} with Mn{sup 2+} in LiCoPO{sub 4}/C has an influence on the initial discharge capacity and excellent cycling behaviour. The obtained results have attributed that production dynamics in nano-synthesis, the coating process with proper carbon source and an effective doping represent three parameters to prepare favorable cathode materials. - Highlights: • Structural, morphological and electrochemical effects of Mn doped LiCo{sub 1−x}Mn{sub x}PO{sub 4}–C electrodes are investigated. • Cheap, effective and simple sol-gel assisted carbothermal reduction approach is used. • After 60th cycle, capacity retention is almost 92% for LiCo{sub 0·95}Mn{sub 0.05}PO{sub 4}–C electrode. • Mn-doped sample exhibits distinctive oxidation (4.76 V and 4.12 V) peaks.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structure, magnetic, and dielectric properties of Ti-doped LaFeO{sub 3} ceramics synthesized by polymer pyrolysis method

Highlights: • The LaFe{sub 1−x}Ti{sub x}O{sub 3} samples can be successfully prepared by polymer pyrolysis method. • XANES spectra confirmed the mixed valence states of Fe{sup 3+} and Fe{sup 4+} for Fe ions and valence states of Ti{sup 4+} for Ti ions. • The ferromagnetism (FM) at room temperature (RT) can be observed in all LaFe{sub 1−x}Ti{sub x}O{sub 3} nanoparticles and ceramics. • The uncompensated spins at the surface played an important role in the magnetism of LaFe{sub 1−x}Ti{sub x}O{sub 3} nanoparticles. • The giant dielectric behavior of the ceramic samples can be easily found by substitution at B site. - Abstract: Perovskite Ti-doped LaFeO{sub 3} (LaFe{sub 1−x}Ti{sub x}O{sub 3}, x = 0, 0.1, and 0.2) nanoparticles synthesized by the polymer pyrolysis method were investigated. X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray absorption near edge spectroscopy (XANES), and vibrating sample magnetometry (VSM) were used to characterize phase, morphology, valence states and magnetic properties of the samples. The samples had a phase of the orthorhombic structure with crystallite sizes of 25 ± 2–47 ± 2 nm for nanoparticles, while ceramic samples had the grain sizes of 0.9 ± 0.3–6.0 ± 2.3 μm. The result of XANES spectra showed that the Fe{sup 3+}/Fe{sup 4+} and Ti{sup 4+} exist in the samples. The weak ferromagnetic behavior at room temperature is observed for all LaFe{sub 1−x}Ti{sub x}O{sub 3} samples with a maximum magnetization of 0.32 emu/g for x = 0.2. Additionally, larger hysteresis loops induced significantly in ceramic samples with no saturation up to 10 kOe. The dielectric properties as a function of frequency at low temperatures suggest the presence of polarization in the samples due to the electron hopping between Fe{sup 3+} and Fe{sup 4+} ions.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Controlled synthesis of α-MnO{sub 2} nanowires and their catalytic performance for toluene combustion

Highlights: • One-dimensional α-MnO{sub 2} nanowires were prepared by a facile hydrothermal route. • Shape and crystal phase of the products were controlled by tuning reaction conditions. • A possible formation mechanism of the α-MnO{sub 2} nanowires was discussed. • The α-MnO{sub 2} nanowires showed great catalytic activity for toluene combustion. - Abstract: α-MnO{sub 2} nanowires with a length about 6–10 μm and an average diameter of 20 nm were synthesized through a facile hydrothermal process without any templates or surfactants. The products were characterized by X-ray powder diffraction, Raman spectroscopy, field emission scanning electron microscopy, transmission electron microscopy, hydrogen temperature-programmed reduction techniques, X-ray photoelectron spectroscopy and surface area analysis. The effects of the hydrothermal temperature and the concentration of CH{sub 3}COOH on the crystal phase and morphology of the final products were studied in detail. The hydrothermal temperature and the concentration of CH{sub 3}COOH play crucial roles in determining the crystal phase and morphology of the products. The possible formation mechanism of the α-MnO{sub 2} nanowires was investigated and discussed. Additionally, the as-prepared α-MnO{sub 2} nanowires showed higher catalytic activity for toluene combustion than the commercial MnO{sub 2}, suggesting their potential applications in the elimination of volatile organic compounds.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Mechanism of Ball Milling Effect on Carbothermic Reduction of Industrial Magnesia by Coke

Mechanical milling always improves the chemical reaction rate in the metallurgy process. The experiment proved that ball milling treatment on raw materials, including industrial magnesia, metallurgical coke, and fluoride calcium, could increase greatly the reaction rate of magnesia. The reaction samples and residues were analyzed by particle size measurement, X-ray diffraction (XRD) analysis, Raman spectroscopy analysis, scanning electron microscope (SEM), and transmission electron microscope (TEM). The results suggested that the positive effect of ball milling on the reaction rate came from three aspects. Ball milling could decrease magnesia particle size and peel coke into graphite sheets to enlarge their contact surface. Meanwhile, ball milling could slightly destroy the crystal grain surface of magnesia and decrease the crystallization of graphite. The nanometer-scale magnesia particles and graphite sheets would stably and strongly attract together after a longer time ball milling. The possible evolution of the particles during ball milling was given, which explained the mechanism of the ball milling effect on the carbothermic reduction of industrial magnesia by coke.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Correlative characterization of primary particles formed in as-cast Al-Mg alloy containing a high level of Sc

Primary particles formed in as-cast Al-5Mg-0.6Sc alloy and their role in microstructure and mechanical properties of the alloy were investigated using optical microscopy (OM), scanning electron microscopy (SEM), electron back-scatter diffraction (EBSD) and tensile testing. It was found that primary particles due to a close orientation to matrix could serve as the potent heterogeneous nucleation sites for α-Al during solidification and thus impose a remarkable grain refinement effect. Eutectic structure consisted of layer by layer of ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ and cellular-dendritic substructure were simultaneously observed at the particles inside, indicating that these particles could be identified as the eutectics rather than individual Al{sub 3}Sc phase. A calculating method, based on EBSD results, was introduced for the spatial distribution of these particles in matrix. The results showed that these eutectic particles randomly distributed in matrix. In addition, the formation of primary eutectic particles significant improved the strength of the Al-Mg alloy in as-cast condition, which is ascribed to the structural evolution from coarse dendrites to prefect fine equiaxed grains. On the other hand, these large-sized particles due to the tendency to act as the microcrack sources could cause a harmful effect in the ductility of Al-Mg-Sc alloy. - Highlights: •Primary particles exhibit an ‘Al{sub 3}Sc + α-Al + Al{sub 3}Sc + ⋯’ multilayer feature with a cellular-dendritic mode of growth. •EBSD analyses the mechanism of grain refinement and the distribution of primary particles in α-Al matrix. •A computational method was presented to calculate the habit planes of primary particles.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Influence of fuel on phase formation of ZnFe{sub 2}O{sub 4} prepared by self-propagated combustion route

Zinc iron oxide (ZnFe{sub 2}O{sub 4}) nanoparticles were prepared by self-propagated combustion route.The fuel plays a major role on the formation of structure and particle size. Here three different fuels like alanine, glycine and proline were used to synthesis the zinc iron oxide nanoparticle. Influence of combustion nature through the fuel, the phase formation, particle size, band gap and surface morphology has been modified. The prepared powder was characterized by powder X-ray diffraction method (PXRD), field-emission scanning electron microscopy (FE-SEM) and the composition of the material was analysed by X-ray energy dispersive spectroscopy (EDAX).The elemental mapping was confirmed the uniform distribution of Zn, Fe and O elements in the prepared material of ZnFe{sub 2}O{sub 4}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗