Stabilization of α-nickel hydoxide in the presence of organic additives: chemical route to bulk synthesis

Organic molecules such as glucose or lactose mediate the synthesis and stabilize alpha-nickel hydroxide in a simple precipitation reaction, while, in the absence of these additives, beta-nickel hydroxide is formed. The additives are not incorporated in the product phase.

Large negative magnetoresistance and metal-insulator transition observed in MnO/C composite coatings grown on ceramic alumina by metalorganic chemical vapor deposition

MnO/C composite coatings were grown by the metalorganic chemical vapor deposition process on ceramic alumina in argon ambient. Characterization by various techniques confirms that these coatings are homogeneous composites comprising nanometer-sized MnO particles embedded in a matrix of nanometer-sized graphite. Components of the MnO/C composite coating crystalline disordered, but are electrically quite conductive. Resistance vs. temperature measurements show that coating resistance increases exponentially from a few hundred ohms at room temperature to a few megaohms at 30 K. Logarithmic plots of reduced activation energy vs. temperature show that the coating material undergoes a metal-insulator transition. The reduced activation energy exponent for the film under zero magnetic field was 2.1, which is unusually high, implying that conduction is suppressed at much faster rate than the Mott or the Efros-Shklovskii hopping mechanism. Magnetoconductance us. magnetic field plots obtained at various temperatures show a high magnetoconductance (similar to 28.8%) at 100 K, which is unusually large for a disordered system, wherein magnetoresistance is attributed typically to weak localization. A plausible explanation for the unusual behavior observed in the carbonaceous disordered composite material is proposed. (C) 2010 Elsevier Ltd. All rights reserved.

Wet chemical syntheses of ultrafine multicomponent ceramic powders through gel to crystallite conversion

Coarse (BOn/2)-O-n+/xH(2)O (10

Wet chemical formation of nanoparticles of binary perovskites through isothermal gel to crystallite conversion

Coarse BO2·xH2O (2 < x < 80) gels, free of anion contaminants react with A(OH)2 under refluxing conditions at 70�100°C giving rise to crystallites of single phased, nanometer size powders of ABO3 perovskites (A = Ba, Sr, Ca, Mg, Pb; B = Zr, Ti, Sn). Solid solutions of perovskites could be prepared from compositionally modified gels or mixtures of A(OH)2. Donor doped perovskites could also be prepared from the same method so that the products after processing are often semiconducting. Faster interfacial diffusion of A2+ ions into the gel generates the crystalline regions whose composition is controllable by the A/B ratio as well as the A(OH)2 concentration.

Metal-organic chemical vapour deposition of thin films of cobalt on different substrates: study of microstructure

We have investigated the microstructure of thin films grown by metal-organic chemical vapour deposition using a beta-diketonate complex of cobalt, namely cobalt (11) acetylacetonate. Films were deposited on three different substrates: Si(100), thermally oxidised silicon [SiO2/Si(100)] and glass at the same time. As-grown films were characterised by X-ray diffraction, scanning electron microscopy, scanning tunnelling microscopy, atomic force microscopy and secondary ion mass spectrometry. Electrical resistivity was measured for all the films as a function of temperature. We found that films have very fine grains, resulting in high electrical resistivity Further, film microstructure has a strong dependence on the nature of the substrate and there is diffusion of silicon and oxygen into cobalt from the substrate. (C) 2002 Elsevier Science B.V. All rights reserved.

Phase transformation and semiconductor-metal transition in thin films of VO2 deposited by low-pressure metalorganic chemical vapor deposition

Thin films of the semiconducting, monoclinic vanadium dioxide, VO2(M) have been prepared on ordinary glass by two methods: directly by low-pressure metalorganic chemical vapor deposition (MOCVD), and by argon-annealing films of the VO2(B) phase deposited by MOCVD. The composition and microstructure of the films have been examined by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Films made predominantly of either the B or the M phase, as deposited, can only be obtained over a narrow range of deposition temperatures. At the lower end of this temperature range, the as-deposited films are strongly oriented, although the substrate is glass. This can be understood from the drive to minimize surface energy. Films of the B phase have a platelet morphology, which leads to an unusual microstructure at the lower-deposition temperatures. Those grown at similar to370 degreesC convert to the metallic, rutile (R) phase when annealed at 550 degreesC, whereas those deposited at 420 degreesC transform to the R phase only at 580 degreesC. (When cooled to room temperature, the annealed films convert reversibly from the R phase to the M phase.) Electron microscopy shows that annealing leads to disintegration of the single crystalline VO2(B) platelets into small crystallites of VO2(R), although the platelet morphology is retained. When the annealing temperature is relatively low, these crystallites are nanometer sized. At a higher-annealing temperature, the transformation leads to well-connected and similarly oriented large grains of VO2(R), enveloped in the original platelet. The semiconductor-metal transition near 68 degreesC leads to a large jump in resistivity in all the VO2(M) films, nearly as large as in epitaxial films on single-crystal substrates. When the annealed films contain well-connected large grains, the transition is very sharp. Even when preferred orientation is present, the transition is not as sharp in as-deposited VO2(M), because the crystallites are not densely packed as in annealed VO2(B). However, the high degree of orientation in these films leads to a narrow temperature hysteresis. (C) 2002 American Institute of Physics.

Cobalt oxide thin films prepared by metalorganic chemical vapor deposition from cobalt acetylacetonate

Thin films of cobalt oxide have been deposited on various substrates, such as glass, Si(100), SrTiO3(100), and LaAlO3(100), by low pressure metalorganic chemical vapor deposition (MOCVD) using cobalt(IL), acetylacetonate as the precursor. Films obtained in the temperature range 400-600 degreesC were uniform and highly crystalline having Co3O4 phase as revealed by x-ray diffraction. Under similar conditions of growth, highly oriented thin films of cobalt oxide grow on SrTiO3(100) and LaAlO3(100). The microstructure and the surface morphology of cobalt oxide films on glass, Si(100) and single crystalline substrates, SrTiO3(100) and LaAlO3(100) were studied by scanning electron microscopy. Optical properties of the films were studied by uv-visible-near IR spectrophotometry.

Epitaxial Growth of Co3O4 Films by Low Temperature, Low Pressure Chemical Vapor Deposition

The growth of strongly oriented or epitaxial thin films of metal oxides generally requires relatively high growth temperatures or infusion of energy to the growth surface through means such as ion bombardment. We have grown high quality epitaxial thin films of Co3O4 on different substrates at a temperature as low as 450°C by low-pressure metal-organic chemical vapor deposition (MOCVD) using cobalt(II) acetylacetonate as the precursor. With oxygen as the reactant gas, polycrystalline Co3O4 films are formed on glass and Si(100) in the temperature range 350-550°C. Under similar conditions of growth, highly oriented films of Co3O4 are formed on SrTiO3(100) and LaAlO3(100). The film on LaAlO3(100) grown at 450°C show a rocking curve FWHM of 1.61°, which reduces to 1.32° when it is annealed in oxygen at 725°C. The film on SrTiO3(100) has a FWHM of 0.330 (as deposited) and 0.29° (after annealing at 725°C). The ø-scan analysis shows cube-on-cube epitaxy on both these substrates. The quality of epitaxy on SrTiO3(100) is comparable to the best of the pervoskite-based oxide thin films grown at significantly higher temperatures.

Surfactant-mediated Synthesis of Functional Metal Oxide Nanostructures via Microwave Irradiation-assisted Chemical Synthesis

Nanostructured materials have attracted considerable interest in recent years due to their properties which differ strongly from their bulk phase and potential applications in nanoscale electronic and optoelectronic devices. Metal oxide nanostructures can be synthesized by variety of different synthesis techniques developed in recent years such as thermal decomposition, sol-gel technique, chemical coprecipitation, hydrothermal process, solvothermal process, spray pyrolysis, polyol process etc. All the above processes go through a tedious synthesis procedure followed by prolonged heat treatment at elevated temperature and are time consuming. In the present work we describe a rapid microwave irradiation-assisted chemical synthesis technique for the growth of nanoparticles, nanorods, and nanotubes of a variety of metal oxides in the presence of an appropriate surfactant, without the use of any templates The method is simple, inexpensive, and helps one to prepare nanostructures in a very simple way, and in a very short time, measured in minutes. The synthesis procedure employs high quality metalorganic complexes (typically -diketonates) featuring a direct metal-to-oxygen bond in its molecular structure. The complex is dissolved in a suitable solvent, often with a surfactant added, and the solution then subjected to microwave irradiation in a domestic microwave oven operating at 2.45 GHz frequency with power varying from 160-800 W, from a few seconds to a few minutes, leading to the formation of corresponding metal oxides. This method has been used successfully to synthesize nanostructures of a variety of binary and ternary metal oxides such as ZnO, CdO, Fe2O3, CuO, Ga2O3, Gd2O3, ZnFe2O4, etc. There is an observed variation in the morphology of the nanostructures with the change of different parameters such as microwave power, irradiation time, appropriate solvent, surfactant type and concentration. Cationic, anionic, nonionic and polymeric surfactants have been used to generate a variety of nanostructures. Even so, to remove the surfactant, there is either no need of heat treatment or a very brief exposure to heat suffices, to yield highly pure and crystalline oxide materials as prepared. By adducting the metal complexes, the shape of the nanostructures can be controlled further. In this manner, very well formed, single-crystalline, hexagonal nanorods and nanotubes of ZnO have been formed. Adducting the zinc complex leads to the formation of tapered ZnO nanorods with a very fine tip, suitable for electron emission applications. Particle size and their monodispersity can be controlled by a suitable choice of a precursor complex, the surfactant, and its concentration. The resulting metal oxide nanostructures have been characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, FTIR spectroscopy, photoluminescence, and electron emission measurements.

Growth of nanowires of beta-NaxV2O5 by metalorganic chemical vapor deposition

Films comprised of nanowires of beta-NaxV2O5 measuring 20-200 nm in diameter and 10-30 mum in length have been prepared on glass substrates by metalorganic chemical vapor deposition using the beta-diketonate complex, vanadyl acetyl acetonate, as precursor, but without the use of either templates or catalysts. Films consisting of nanowires of monophasic beta-NaxV2O5 with a preferred orientation along (h0l) are formed only at 550 degreesC, whereas those deposited at 540 degreesC comprise a mixture of nanowires (beta-NaxV2O5) and platelets (V2O5). The films deposited at lower temperatures are less crystalline and comprise a mixture of vanadium oxide phases. From the observations that nanowires are formed only in the narrow temperature range of 540-550 degreesC, and from the critical dependence of the formation of nanowires on the balance between the CVD growth rate and the evaporation rate of the film, it is inferred that the formation of nanowires of beta-NaxV2O5 is due to chemical vapor transport.

Photoluminescence of Sr(2-x)Ln(x)CeO(4+x/2) (Ln = Eu, Sm or Yb) prepared by a wet chemical method

A wet chemical route is developed for the preparation of Sr2CeO4 denoted the carbonate-gel composite technique. This involves the coprecipitation of strontium as fine particles of carbonates within hydrated gels of ceria (CeO2.xH(2)O, 40

Studies on the structural and ionic transport properties at elevated temperatures of La1-xMnO3 +/-delta synthesized by a wet chemical method

Structural transformation and ionic transport properties are investigated on wet-chemically synthesized La1-xMnO3 (X=0.0-0.18) compositions. Powders annealed in oxygen/air at 1000-1080 K exhibit cubic symmetry and transform to rhombohedral on annealing at 1173-1573 K in air/oxygen. Annealing above 1773 K in air or in argon/helium at 1473 K stabilized distorted rhombohedral or orthorhombic symmetry. Structural transformations are confirmed from XRD and TEM studies. The total conductivity of sintered disks, measured by four-probe technique, ranges from 5 S cm(-1) at 298 K to 105 S cm(-1) at 1273 K. The ionic conductivity measured by blocking electrode technique ranges from 1.0X10(-6) S cm(-1) at 700 K to 2.0X10(-3) S cm(-1) at 1273 K. The ionic transference number of these compositions ranges from 3.0X10(-5) to 5.0X10(-5) at 1273 K. The activation energy deduced from experimental data for ionic conduction and ionic migration is 1.03-1.10 and 0.80-1.00 eV, respectively. The activation energy of formation, association and migration of vacancies ranges from 1.07 to 1.44 eV. (C) 2002 Elsevier Science B.V. All rights reserved.