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At least 1,495 records · Page 83
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Mechanochemical synthesis of low-fluorine doped aluminum hydroxide fluorides

Different aluminum hydroxide fluorides with varying Al/F molar ratios from 1:1.5 up to 1:0.05 were successfully synthesized by mechanochemical reactions. The characterization of the products by XRD, {sup 27}Al and {sup 19}F MAS NMR, thermal analysis, nitrogen adsorption and zeta potential techniques allows a detailed understanding of the structure and surface properties of the products. Using γ-Al(OH){sub 3} and β-AlF{sub 3}·3H{sub 2}O as OH- and F-sources, respectively, strongly disordered products were obtained with an Al: F molar ratio higher than 1:0.25. The fluorination degree has affected the amount of 4- and 5-fold coordinated Al sites, not present in the reactants. An evolution of the sub-coordinated Al-species has been detected also as a consequence of annealing processes. Obviously, these species affect the phase transition to alumina, by decreasing the transition temperature of the formation of α-Al{sub 2}O{sub 3}. Synthesis conditions (milling time, fluorination degree) play a crucial role for the product composition. - Graphical abstract: The impact of the combined action of the milling and the different fluorine doping on the structure of new aluminum hydroxide fluorides was followed by {sup 27}Al and {sup 19}F NMR and by other complementary techniques. - Highlights: • Low F-doped Al-hydroxide fluorides can be successfully prepared by mechanosynthesis. • Both F-doping and mechanochemical synthesis introduce a high number of defects in the structure. • The fluorination degree affects the amount of 4- and 5-fold coordinated Al sites as well as the transition temperature to corundum.

36 MATERIALS SCIENCE↗
DOE OSTI2017

One-step solution combustion synthesis of pure Ni nanopowders with enhanced coercivity: The fuel effect

In this paper, we report a new modified one-step combustion synthesis technique for production of Ni metal nanoparticles. The main unique feature of our approach is the use of microwave assisted foam preparation. Also, the effect of different types of fuels (urea, citric acid, glycine and hexamethylenetetramine) on the combustion process and characteristics of resultant solid products were investigated. It is observed that the combination of microwave assisted foam preparation and using of hexamethylenetetramine as a fuel allows producing pure ferromagnetic Ni metal nanoparticles with enhanced coercivity (78 Oe) and high value of saturation magnetization (52 emu/g) by one-step solution combustion synthesis under normal air atmosphere without any post-reduction processing. - Highlights: • The new approach in one-step SCS rote for Ni nanoparticles preparation is proposed. • Ni particles were synthesized with microwave-assistance and under air atmosphere. • The effect of different type of fuels on the combustion process was investigated. • Using of hexamethylenetetramine allows obtaining pure Ni nanoparticles. • Ni nanoparticles have enhanced coercivity and high saturation magnetization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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↗
DOE OSTI2013

Phase transformation during mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si alloys

Mechano-synthesis of Fe–32Mn–6Si alloy by mechanical alloying of the elemental powder mixtures was evaluated by running the ball milling process under an inert argon gas atmosphere. In order to characterize the as-milled powders, powder sampling was performed at predetermined intervals from 0.5 to 192 h. X-ray florescence analyzer, X-ray diffraction, scanning electron microscope, and high resolution transmission electron microscope were utilized to investigate the chemical composition, structural evolution, morphological changes, and microstructure of the as-milled powders, respectively. According to the results, the nanocrystalline Fe–Mn–Si alloys were completely synthesized after 48 h of milling. Moreover, the formation of a considerable amount of amorphous phase during the milling process was indicated by quantitative X-ray diffraction analysis as well as high resolution transmission electron microscopy image and its selected area diffraction pattern. It was found that the α-to-γ and subsequently the amorphous-to-crystalline (especially martensite) phase transformation occurred by milling development. - Graphical abstract: Mechano-synthesis of nanocrystalline/amorphous Fe–32Mn–6Si shape memory alloys in the powder form: amorphous phase formation, α-to-γ phase transformation, mechano-crystallization of the amorphous, and martensite phase formation during the process. Highlights: • During MA, the α-to-γ phase transformation and amorphization occurred. • Mechano-crystallization of the amorphous phase occurred at sufficient milling time. • The formation of high amount of ε-martensite was evidenced at high milling times. • The platelet, spherical, and then irregular particle shapes was extended by MA. • By MA, the particles size was increased, then reduced, and afterward re-increased.

36 MATERIALS SCIENCE↗
DOE OSTI2015

In-situ synthesis of Ag nanoparticles by electron beam irradiation

Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber at room temperature and the growth mechanism was explored in detail. The sizes of the Ag nanoparticles are controlled by the electron beam current density. Two nanoparticle growth stages were identified. The first growth stage was dominated by the discharging effect, while the second stage was controlled by the heating effect. The nanoparticle synthesis method should be applicable to the synthesis of other metallic nanoparticles. - Highlights: • Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber. • The sizes of the Ag nanoparticles are controlled by the electron beam current density. • The growth mechanism was studied, two growth stages were confirmed. • The first growth stage was dominated by the discharging effect, and the second stage was controlled by the heating effect.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Facile microwave synthesis and photocatalytic activity of monodispersed BaTiO{sub 3} nanocuboids

A facile microwave hydrothermal method for preparation of monodispersed barium titanate (BaTiO{sub 3}) nanocuboids with average size of 13 nm is developed, and the effects of synthesis parameters, such as molar composition of the precursor, synthesis time and temperature, on the morphology of BaTiO{sub 3} nanocrystals are systematically evaluated. The resulting products are characterized by X-ray diffraction (XRD), Raman spectrum, infrared spectrum (IR), UV–vis diffuse reflectance spectrum, water contact angle, thermogravimetry (TG), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and selected area electron diffraction (SAED). A possible formation mechanism of BaTiO{sub 3} nanocuboids is proposed. The BaTiO{sub 3} nanocuboids show high photocatalytic activity for the degradation of Rhodamin B under UV irradiation. - Highlights: • Monodispersed BaTiO{sub 3} nanocuboids are prepared by a facile microwave process. • The BaTiO{sub 3} nanocuboids have average size of 13 nm. • Oleic acid is the key factor to control the morphology of BaTiO{sub 3} nanocuboids. • BaTiO{sub 3} nanocuboids exhibit enhanced photocatalytic properties.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study of reaction sequences during MSR synthesis of TiC by controlled ball milling of titanium and graphite

Highlights: • Insights on oxygen-bonded features formed during reactive ball milling • Evolution of off-stoichiometric TiC before ignition • Growth sequence of the TiC manifested as stacks and multilayers • Dual morphology of the MSR reaction product - Abstract: During reactive ball milling of Ti and C, mechanically induced self-propagating reaction (MSR) synthesis of TiC is reported to occur via a process including initial formation of small amounts of TiC prior to exothermic ignition, followed by MSR and the formation of stiochiometric TiC (Dorofeev et al., 2011; Oghenevweta et al., 2016 [1, 2]). However, both the chemical evolution and mechanisms of reaction and growth of TiC both prior to, during and after ignition are not fully understood. This research focuses on fundamental understanding of the reaction sequences during MSR synthesis of TiC from elemental Ti and C (graphite). Magnetically controlled ball milling of stoichiometric (1:1) powder mixtures of titanium (Ti) and graphite (C) was performed under He gas with the exothermic ignition point by determined via in-situ temperature measurement. X-ray diffraction, Scanning Transmission Electron Microscopy (STEM) with electron energy loss spectroscopy (EELS), Raman Spectroscopy and X-ray Photoelectron Spectroscopy (XPS) were employed to interpret the reaction sequences. The reaction sequence involved the following: During milling prior to ignition, severely deformed Ti, spheriodised graphite and amorphous carbon forms, and minor amounts of off-stiochiometric nano-TiC{sub 1−x} crystals. In addition to the formation of TiC{sub 1−x}, XPS revealed the formation of oxide skins coating the surface regions of the milled powders. There is also an evolution towards stiochiometric TiC with increasing milling time. Immediately after ignition, a reacted product comprising a mixture of multi-layer stacks of thin TiC plates form, in addition to a matrix comprising large TiC particles which have been liquid phase sintered under the high local heat of reaction by thin layers of unreacted Ti. MSR occurs via a dual mechanism involving rapid growth of existing TiC, plus nucleation and growth of new TiC. High spatially resolved EELS combined with STEM revealed additional information about the inhomogeneous chemical environment of the milled powders.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Synthesis, densification and characterization of ultra-fine W-Al2O3 composite powder

Highlights: • W-Al{sub 2}O{sub 3} ultrafine powder was prepared by hydrothermal synthesis. • Al{sub 2}(WO{sub 4}){sub 3} was a key process for forming nano-Al{sub 2}O{sub 3} coated W structure. • This coated structure inhibited the further growth of W particles. • Dispersed Al{sub 2}O{sub 3} particles improved obviously mechanical properties of W alloy. • Fracture mode changed into intergranular from transcrystalline with Al{sub 2}O{sub 3} addition. - Abstract: W-Al{sub 2}O{sub 3} composite powder was prepared via hydrothermal synthesis containing doping, annealing and reduction. The precursors WO{sub 3} and AlOOH were synthesized by the two sets of the hydrothermal reactions, respectively. The formation of Al{sub 2}(WO{sub 4}){sub 3} from these two precursors in an aqueous solution is a key process, which is beneficial to improve the mixing uniformity of final powder to a molecular level. During subsequent reduction, nano-Al{sub 2}O{sub 3} coated W particles were obtained, and inhibited the further deposition of reduced W atoms on the adjacent W particles, obtaining ultra-fine Al{sub 2}O{sub 3}/W composite powder. After sintering, the dense and fine-grained W-Al{sub 2}O{sub 3} alloy was obtained due to the high sintering activity of ultra-fine powder. Compared with the pure tungsten, the W-Al{sub 2}O{sub 3} alloy displays obvious higher values of both strength and plasticity especially when the Al{sub 2}O{sub 3} content is 2 wt%.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Turning “on” and “off” nucleation and growth: Microwave assisted synthesis of CdS clusters and nanoparticles

Graphical abstract: Display Omitted Highlights: ► Cadmium acetate and DMSO were employed as ion precursors. ► New approach to controlled CdS nanoparticle synthesis. ► CdS clusters and nanoparticles synthesis achieved using microwave irradiation. ► Microwave irradiation turns on and off nanoparticle growth. ► The formation of clusters, embryos and nanoparticles studied with optical spectroscopy. -- Abstract: We report here on the formation of CdS NP from the microwave assisted reaction of Cd(CH{sub 3}CO{sub 2}){sub 2} with dimethylsulfoxide (DMSO). DMSO serves as the solvent and a controlled source of sulfide ions to form (CdS){sub 1≤n≤5} clusters at the early stages of the process. The clusters grow into CdS nanoparticles, with diameters that range from 1.6 nm up to over 250 nm, with microwave heating. The time dependence of the onset of light absorption and absorbance are consistent with a concurrent nucleation and growth processes. The formation of clusters and nuclei and their subsequent reactions is controlled by turning on and off the energy supply consistent with an energy barrier to the formation of CdS nanostructures.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Effect of KCl, NaCl and CaCl{sub 2} mixture on volume combustion synthesis of TiB{sub 2} nanoparticles

Highlights: {yields} A low melting diluent lowers the ignition temperature in combustion synthesis. {yields} Deagglomerated synthesized products are formed as the result of diluent addition. {yields} Addition of 45% salt mixture resulted in formation of 70 nm TiB{sub 2} nanoparticles. {yields} Thermodynamically unstable Mg{sub 2}TiO{sub 4} and Mg{sub 3}B{sub 2}O{sub 6} by-products were formed. {yields} Small change in particle size was observed with addition of salt mixture. -- Abstract: Preparation of titanium diboride (TiB{sub 2}) nanoparticles was carried out by volume combustion synthesis. TiO{sub 2}, B{sub 2}O{sub 3} and elemental Mg were mixed with 0-60% salt mixture of KCl, NaCl and CaCl{sub 2} with increment of 15% as a low melting temperature diluent. Compressed samples were synthesized in a tubular furnace at a constant heating rate under argon atmosphere. Thermal analysis of the process showed that the addition of the low melting temperature salts mixture led to a significant decrease in ignition and combustion temperatures. Synthesized samples were then leached by nitric and hydrochloric acids to remove impurities. The samples were examined by XRD, SEM and DLS analysis. The results showed the formation of fine deagglomerated particles with the addition of the salts mixture. The results revealed that 45% salts mixture had the smallest average particle size of about 90 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Facile synthesis of mesoporous core-shell TiO{sub 2} nanostructures from TiCl{sub 3}

Highlights: {yields} Stable TiCl{sub 3} solution is adopted as Ti sources. {yields} Low-cost glucose assisted facile solvothermal reactions. {yields} Exquisite core-shell morphology and mesoporous structure of TiO{sub 2} nanostructures. {yields} Superior photocatalytic activity of TiO{sub 2} nanostructures in UV light irradiation. -- Abstract: The present study reports the synthesis and formation process of mesoporous core-shell TiO{sub 2} nanostructures by employing a glucose-assisted solvothermal process using water-ethanol mixture as solvent and subsequent calcination process at 550 {sup o}C for 4 h. X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy and nitrogen adsorption-desorption analysis were used to investigate the structural properties of these nanostructures. By optimizing the preparation conditions, especially the contents of water and ethanol in the mixture solvent, mesoporous core-shell TiO{sub 2} nanostructures were obtained. These mesoporous nanostructures have anatase phase and exhibit the superior photocatalytic activity. This synthesis route is facile due to the usage of stable and low-cost Ti precursor such as TiCl{sub 3} and is thus applicable for large-scale production.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Extracellular synthesis of silver nanoparticles using the leaf extract of Coleus amboinicus Lour

Highlights: {yields} Synthesis of AgNPs using the leaf extract of Coleus amboinicus L. was described. {yields} UV-vis absorption spectra showed the formation of isotrophic AgNPs at 437 nm in 6 h. {yields} XRD analysis showed intense peaks corresponding to fcc structure of AgNPs. {yields} HR-TEM analysis revealed the formation of stable anisotrophic and isotrophic AgNPs. -- Abstract: In the present investigation, Coleus amboinicus Lour. leaf extract-mediated green chemistry approach for the synthesis of silver nanoparticles was described. The nanoparticles were characterized by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The influence of leaf extract on the control of size and shape of silver nanoparticles is reported. Upon an increase in the concentration of leaf extract, there was a shift in the shape of nanoparticles from anisotrophic nanostructures like triangle, decahedral and hexagonal to isotrophic spherical nanoparticles. Crystalline nature of fcc structured nanoparticles was confirmed by XRD spectrum with peaks corresponding to (1 1 1), (2 0 0), (2 2 0) and (3 1 1) planes and bright circular spots in the selected-area electron diffraction (SAED). Such environment friendly and sustainable methods are non-toxic, cheap and alternative to hazardous chemical procedures.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Morphology-controlled hydrothermal synthesis of MnCO{sub 3} hierarchical superstructures with Schiff base as stabilizer

Graphical abstract: MnCO3 microcrystals with hierarchical superstructures were synthesized by using the CO2 in atmosphere as carbonate ions source and Schiff base as shape guiding-agent in water/ethanol system under hydrothermal condition. Highlights: {yields} The most interesting in this work is the use of the greenhouse gases CO{sub 2} in atmosphere as carbonate ions source to precipitate with Mn{sup 2+} for producing MnCO{sub 3} crystals. {yields} This work is the first report related to the small organic molecule Schiff base as shape guiding-agent to produce different MnCO{sub 3} hierarchical superstructures. {yields} We are controllable synthesis of the MnCO{sub 3} hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like microcrystals. {yields} The as-prepared MnCO{sub 3} could be used precursor to fabricate the Mn{sub 2}O{sub 3} hierarchical superstructures after thermal decomposition at high temperature. -- Abstract: MnCO{sub 3} with hierarchical superstructures such as chrysanthemum, straw-bundle, dumbbell and sphere-like were synthesized in water/ethanol system under environment-friendly hydrothermal condition. In the synthesis process, the CO{sub 2} in atmosphere was used as the source of carbonate ions and Schiff base was used as shape guiding-agent. The different superstructures of MnCO{sub 3} could be obtained by controlling the hydrothermal temperature, the molar ratio of manganous ions to the Schiff base, or the volume ratio of water to ethanol. A tentative growth mechanism for the generation of MnCO{sub 3} superstructures was proposed based on the rod-dumbbell-sphere model. Furthermore, the MnCO{sub 3} as precursor could be further successfully transferred to Mn{sub 2}O{sub 3} microstructure after heating in the atmosphere at 500 {sup o}C, and the morphology of the Mn{sub 2}O{sub 3} was directly determined by that of the MnCO{sub 3} precursor.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Microwave-hydrothermal synthesis of perovskite bismuth ferrite nanoparticles

Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-ray analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Solvothermal synthesis of carbon-coated tin nanorods for superior reversible lithium ion storage

Highlights: Black-Right-Pointing-Pointer Large-scale synthesis of Sn-C core-shell nanorods. Black-Right-Pointing-Pointer Facile template-engaged solvothermal approach. Black-Right-Pointing-Pointer The combination of tin with high specific capacity and carbon with good cycle life. Black-Right-Pointing-Pointer Relatively higher initial Coulombic efficiency and lithium storage capacities. -- Abstract: This paper reports the large-scale synthesis of carbon-coated tin (Sn-C) nanorods through a facile solvothermal carbonization approach by using Sn nanorods as templates and ethanol as a solvent. The as-synthesized Sn-C nanorods have been applied as anode materials for lithium-ion batteries. The Sn-C anode, which exhibits relatively higher initial Coulombic efficiency and lithium storage capacities, is more attractive than the previously reported tin oxide or sulfide anodes. The superior performance of the Sn-C nanorods makes it a promising anode material in high-energy density batteries.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Low temperature synthesis of LnOF rare-earth oxyfluorides through reaction of the oxides with PTFE

Highlights: Black-Right-Pointing-Pointer Low temperature synthesis of LnOF rare-earth oxyfluorides from Ln{sub 2}O{sub 3} and PTFE (CF{sub 2}). Black-Right-Pointing-Pointer Rhombohedral LnOF is the major phase and forms as nanocrystals, 29-103 nm. Black-Right-Pointing-Pointer Expected lanthanide contraction observed in lattice parameters and bond lengths. Black-Right-Pointing-Pointer TbOF orders antiferromagnetically at 10 K and has a metamagnetic transition at 1.8 T. Black-Right-Pointing-Pointer GdOF orders antiferromagnetically at 5 K, other LnOF are paramagnetic. -- Abstract: A low temperature solid-state synthesis route, employing polytetrafluoroethylene (PTFE) and the rare-earth oxides, for the formation of the LnOF rare-earth oxyfluorides (Ln = Y, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er), is reported. With the exception of LaOF, which forms in a tetragonal variant, rhomobohedral LnOF is found to be the major product of the reaction. In the case of PrOF, a transition from the rhombohedral to the cubic fluorite phase is observed on heating in air to 500 Degree-Sign C. X-ray diffraction shows the expected lanthanide contraction in the lattice parameters and bond lengths. Magnetic susceptibility measurements show antiferromagnetic-like ordering in TbOF, T{sub m} = 10 K, with a metamagnetic transition at a field {mu}{sub 0}H{sub t} = 1.8 T at 2 K. An antiferromagnetic transition, T{sub N} = 4 K, is observed in GdOF. Paramagnetic behavior is observed above 2 K in PrOF, NdOF, DyOF, HoOF and ErOF. The magnetic susceptibility of EuOF is characteristic of Van Vleck paramagnetism.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Nanoparticles synthesis of tungsten disulfide via AOT-based microemulsions

Graphical abstract: A controlled synthesis of WS2 nanoparticles (most probably inorganic fullerene (IF)) via microemulsion was applied for the first time to prepare WS2 (7–12 nm) by acidification of the water cores of the AOT reverse microemulsion. Highlights: ► An innovative reverse microemulsion technique was developed for WS{sub 2} synthesis. ► WS{sub 2} nanoparticles were obtained with narrow size distribution in range of 7–12 nm. ► Operating cost of microemulsion was lower in contrast to quartz reactor method. ► WS{sub 2} morphology could be controlled to obtain highly active and selective catalysts. ► Lower size of WS{sub 2} in this study overcomes the shortcoming of quartz reactor method. -- Abstract: The tungsten disulfide (WS{sub 2}) nanoparticles (most probably inorganic fullerene (IF)) with a narrow size distribution were synthesized by a reverse micelle technique for the first time. The particle size was controlled by varying water-to-surfactant molar ratio (W{sub 0}), aging time and reagent concentration. The synthesized WS{sub 2} nanoparticles were characterized by zetasizer, UV–visible spectrophotometers and transmission electron microscopy (TEM). The WS{sub 2} nanoparticles with particle diameter size of 7–12 nm were obtained via 24 h aging time. The particle size was controlled by changing the aging time and molar ratio of water/surfactant. Doubling W{sub 0} increased the amount and particle size of WS{sub 2} by 22 and 26%, respectively. The effect of aging time in the range of 6–24 h was investigated and the complete disappearance of yellowish color at 24 h resulted in an optically clear solution, which was the indication of WS{sub 2} formation with 100% conversion of reactant ((NH{sub 4}){sub 2}WS{sub 4}) in the batch reactor.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Template-directed preparation of two-layer porous NiO film via hydrothermal synthesis for lithium ion batteries

Graphical abstract: A two-layer porous NiO film is prepared via hydrothermal synthesis method based on monolayer polystyrene sphere template and shows noticeable Li battery performance with good cycle life and high capacity. Highlights: ► Two-layer porous NiO film is prepared via monolayer polystyrene spheres template. ► NiO film with high capacity as anode material for lithium ion batteries. ► Two-layer porous structure is favorable for fast lithium ion and electron transfer. -- Abstract: A two-layer porous NiO film is prepared by hydrothermal synthesis method through self-assembled monolayer polystyrene spheres template. The substructure of the NiO film is composed of ordered close-packed hollow-sphere array and the superstructure is made up of randomly NiO nanoflakes. The electrochemical properties are measured by galvanostatic charge/discharge tests and cyclic voltammetric analysis (CV). As anode material for lithium ion batteries, the two-layer porous NiO film exhibits high initial coulombic efficiency of 75%, high reversible capacity and rather good cycling performance. The discharge capacity of the two-layer porous NiO film is 501 mAh g{sup −1} at 0.5 C after 50 cycles. The two-layer porous architecture is responsible for the enhancement of electrochemical properties.

36 MATERIALS SCIENCE↗