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Spray Pyrolysis (spray + pyrolysi)
Kinds of Spray Pyrolysis Selected AbstractsHigh-Performance Carbon-LiMnPO4 Nanocomposite Cathode for Lithium BatteriesADVANCED FUNCTIONAL MATERIALS, Issue 19 2010Seung-Min Oh Abstract A cathode material of an electrically conducting carbon-LiMnPO4 nanocomposite is synthesized by ultrasonic spray pyrolysis followed by ball milling. The effect of the carbon content on the physicochemical and electrochemical properties of this material is extensively studied. A LiMnPO4 electrode with 30 wt% acetylene black (AB) carbon exhibits an excellent rate capability and good cycle life in cell tests at 55 and 25 °C. This electrode delivers a discharge capacity of 158 mAh g,1 at 1/20 C, 126 mAh g,1 at 1 C, and 107 mAh g,1 at 2 C rate, which are the highest capacities reported so far for this type of electrode. Transmission electron microscopy and Mn dissolution results confirm that the carbon particles surrounding the LiMnPO4 protect the electrode from HF attack, and thus lead to a reduction of the Mn dissolution that usually occurs with this electrode. The improved electrochemical properties of the C-LiMnPO4 electrode are also verified by electrochemical impedance spectroscopy. [source] Time,Temperature,Transformation (TTT) Diagrams for Crystallization of Metal Oxide Thin FilmsADVANCED FUNCTIONAL MATERIALS, Issue 17 2010Jennifer L. M. Rupp Abstract Time,temperature,transformation (TTT) diagrams are proposed for the crystallization of amorphous metal oxide thin films and their specific characteristics are discussed in comparison to glass-based materials, such as glass-ceramics and metallic glasses. The films crystallize from amorphous to full crystallinity in the solid state. As an example the crystallization kinetics for a single-phase metal oxide, ceria, and its gadolinia solid solutions are reported made by the precipitation thin-film method spray pyrolysis. The crystallization of an amorphous metal oxide thin film generally follows the Lijschitz,Sletow,Wagner (LSW) Ostwald ripening theory: Below the percolation threshold of 20 vol% single grains crystallize in the amorphous phase and low crystallization rates are measured. In this state no impact of solute on crystallization is measurable. Once the grains form primary clusters above the threshold the solute slows down crystallization (and grain growth) thus shifting the TTT curves of the doped ceria films to longer times and higher temperatures in comparison to undoped ceria. Current views on crystallization of metal oxide thin films, the impact of solute dragging, and primary TTT diagrams are discussed. Finally, examples on how to use these TTT diagrams for better thermokinetic engineering of metal oxide thin films for MEMS are given, for example, for micro-Solid Oxide Fuel Cells and resistive sensors. In these examples the electrical properties depend on the degree of crystallinity and, thereby, on the TTT conditions. [source] Crystallization and Grain Growth Kinetics for Precipitation-Based Ceramics: A Case Study on Amorphous Ceria Thin Films from Spray PyrolysisADVANCED FUNCTIONAL MATERIALS, Issue 17 2009Jennifer L. M. Rupp Abstract The introductory part reviews the impact of thin film fabrication, precipitation versus vacuum-based methods, on the initial defect state of the material and microstructure evolution to amorphous, biphasic amorphous-nanocrystalline, and fully nanocrystalline metal oxides. In this study, general rules for the kinetics of nucleation, crystallization, and grain growth of a pure single-phase metal oxide thin film made by a precipitation-based technique from a precursor with one single organic solvent are discussed. For this a complete case study on the isothermal and non-isothermal microstructure evolution of dense amorphous ceria thin films fabricated by spray pyrolysis is conducted. A general model is established and comparison of these thin film microstructure evolution to kinetics of classical glass-ceramics or metallic glasses is presented. Knowledge on thermal microstructure evolution of originally amorphous precipitation-based metal oxide thin films allows for their introduction and distinctive microstructure engineering in devices-based on microelectromechanical (MEMS) technology such as solar cells, capacitors, sensors, micro-solid oxide fuel cells, or oxygen separation membranes on Si-chips. [source] Flame-Synthesized Ceria-Supported Copper Dimers for Preferential Oxidation of COADVANCED FUNCTIONAL MATERIALS, Issue 3 2009Richard Kydd Abstract Rapid synthesis of CuCeO2 catalysts by flame spray pyrolysis produces highly active Cu dimer morphologies without the need for additional catalyst pretreatment. The active Cu component is enriched onto the CeO2 surface at concentrations higher than the nominal loading with no evidence of amorphous or crystalline CuO phase. Increasing the Cu content results in a morphological transition from isolated Cu monomers to oxygen-bridged dimers and an associated increase in oxygen vacancy concentration. Dimer-containing CuCeO2 catalysts display high levels of activity and selectivity in the low-temperature preferential oxidation of CO. Experimental measurements and simulations suggest that the geometry of the dimer presents a comparatively ionic CuO bond at the catalyst surface. Further studies indicate that these ionic dimer species promote preferential CO oxidation at lower temperatures than observed for monomeric Cu species. This is the first report to explicitly propose and demonstrate that the structural distortion associated with the formation of Cu dimers directly induces increased bond ionicity at the catalyst surface and that these changes are responsible for improved catalytic activity. [source] Transparent Nanocomposites of Radiopaque, Flame-Made Ta2O5/SiO2 Particles in an Acrylic Matrix,ADVANCED FUNCTIONAL MATERIALS, Issue 5 2005H. Schulz Abstract Mixed Ta2O5 -containing SiO2 particles, 6,14,nm in diameter, with closely controlled refractive index, transparency, and crystallinity are prepared via flame spray pyrolysis (FSP) at production rates of 6.7,100,g,h,1. The effect of precursor solution composition on product filler (particle) size, crystallinity, Ta dispersity, and transparency is studied using nitrogen adsorption, X-ray diffraction, optical microscopy, high-resolution transmission electron microscopy (HRTEM), and diffuse-reflectance infrared Fourier-transform spectroscopy (DRIFTS). Emphasis is placed on the transparency of the composite that is made with Ta2O5/SiO2 filler and dimethylacrylate. Increasing Ta2O5 crystallinity and decreasing Ta dispersity on SiO2 decreases both filler and composite transparencies. Powders with identical specific surface area (SSA), refractive index (RI), and Ta2O5 content (24,wt.-%) show a wide range of composite transparencies, 33,78,%, depending on filler crystallinity and Ta dispersity. Amorphous fillers with a high Ta dispersity and an RI matching that of the polymer matrix lead to the highest composite transparency, 86,%. The composite containing 16.5,wt.-% filler that itself contains 35,wt.-% Ta2O5 has the optimal radiopacity for dental fillings. [source] Topography Mediated Patterning of Inorganic Materials by Spray Pyrolysis,ADVANCED MATERIALS, Issue 22 2006D. Beckel Microstructured ceramic thin films are produced by spray pyrolysis of metal salt solutions onto micromachined substrates. The ceramic structures built on the substrate result from preferential assembly of particles on the edge of the initially micromachined structures, leading to smaller lateral dimensions (1,2 ,m in width) than the initial structures on the substrate (see figure). The assembly process amplifies the height of the initial structures by a factor of approximately thirty, resulting in features with an aspect ratio of three. [source] Preparation of LiMn2O4 powders via spray pyrolysis and fluidized bed hybrid systemAICHE JOURNAL, Issue 7 2006Izumi Taniguchi Abstract A novel technique has been developed to directly produce fine ceramic powders from liquid solution using a spray pyrolysis and fluidized bed hybrid system. Using this technique, the preparation of lithium manganese oxides LiMn2O4, which are the most promising cathode materials for lithium-ion batteries, has been carried out for various superficial gas velocities U0 = 0.30-0.91 m/s, static bed heights Ls = 50-150 mm, and medium particle sizes dpm,g = 294-498 ,m. The resulting powders had spherical nanostructured particles that comprised primary particles with a few tens of nanometer in size, and they exhibited a pure cubic spinel structure without any impurities in the XRD patterns. Moreover, the as-prepared powders showed better crystallinity and smaller specific surface area than those by conventional spray pyrolysis. The effects of process parameters on powder properties, such as specific surface area and crystallinity, were investigated for a wide range of superficial gas velocities and static bed heights. An as-prepared sample was used as cathode active materials for lithium-ion batteries and the cell performance has been investigated. Test experiments in the electrochemical cell Li/1M LiClO4 in PC/LiMn2O4 demonstrated that the sample prepared by the present technique was superior to that by the conventional spray pyrolysis and solid-state reaction method. © 2006 American Institute of Chemical Engineers AIChE J, 2006 [source] Pressureless Sintering t -zirconia@,-Al2O3 (54 mol%) Core,Shell Nanopowders at 1120°C Provides Dense t -Zirconia-Toughened ,-Al2O3 NanocompositesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 3 2010Min Kim Zirconia-toughened alumina (ZTA) is of growing importance in a wide variety of fields exemplified by ZTA prosthetic implants. Unfortunately, ZTA composites are generally difficult to process because of the need to preserve the tetragonal zirconia phase in the final dense ceramic, coincident with the need to fully densify the ,-Al2O3 component. We report here that liquid-feed flame spray pyrolysis of mixtures of metalloorganic precursors of alumina and zirconia at varying compositional ratios provide access in one step to core,shell nanoparticles, wherein the shell is ,-Al2O3 and the core is a perfect single crystal of tetragonal (t -) zirconia. Pressureless sintering studies provided parameters whereby these nanopowder compacts could be sintered to full density (>99%) at temperatures just above 1100°C converting the shell component to ,-Al2O3 but preserving the t -ZrO2 without the need for any dopants. The final average grain sizes of these sintered compacts are ,200 nm. The resulting materials exhibit the expected response to mechanical deformation with the subsequent production of monoclinic ZrO2. These materials appear to offer a low-temperature, low-cost route to fine-grained ZTA with varied Al2O3:t -ZrO2 compositions. [source] Synthesis and Characterization of Nanostructured Cerium Dioxide Thin Films Deposited by Ultrasonic Spray PyrolysisJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 1 2010Mario F. García-Sánchez Nanostructured thin films of cerium dioxide have been prepared on single-crystalline silicon substrates by ultrasonic spray pyrolysis using cerium acetylacetonate as a metal,organic precursor dissolved in anhydrous methanol and acetic acid as an additive. The morphology, structure, optical index, and electrical properties were studied by X-ray diffraction, scanning electron microscopy, atomic force microscopy, ellipsometry, and impedance spectroscopy. The use of additives is very important to obtain crack-free films. The substrate temperature and flow rate was optimized for obtaining smooth (Ra<0.4 nm), dense (n>2), and homogeneous nanocrystalline films with grain sizes as small as 10 nm. The influence of thermal annealing on the structural properties of films was studied. The low activation energy calculated for total conductivity (0.133 eV) is attributed to the nanometric size of the grains. [source] Structure of Disodium Dimolybdate Synthesized Using Thermodynamically Stable Molybdenum (VI) Oxide Clusters as PrecursorsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 10 2009Dragana J. Jovanovi The structure of disodium dimolybdate (Na2Mo2O7) synthesized by a low-temperature method in the process of ultrasonic spray pyrolysis using acidified aqueous solutions of thermodynamically stable molybdenum (VI) oxide clusters as a precursor was refined down to an R -factor of 7%. The refinement of the diffraction data showed that Na2Mo2O7 powder synthesized at 300°C belongs to the base-centered orthorhombic type of structure with a space group of Cmca (no. 64). It was found that the basic units of the octahedral MoO6 precursor complexes exist in the structure of Na2Mo2O7. Tetrahedral MoO4 building units that coexist together with octahedral units in the structure of Na2Mo2O7 are most likely developed by the termination of weak octahedral bonds and by the placement of the molybdenum atom in the center of the tetrahedra. [source] Spray Pyrolysis of Fe3O4,BaTiO3 Composite ParticlesJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 2009Tomoyuki Adachi Fe3O4,BaTiO3 composite particles were successfully prepared by ultrasonic spray pyrolysis. A mixture of iron(III) nitrate, barium acetate and titanium tetrachloride aqueous solution were atomized into the mist, and the mist was dried and pyrolyzed in N2 (90%) and H2 (10%) atmosphere. Fe3O4,BaTiO3 composite particle was obtained between 900° and 950°C while the coexistence of FeO was detected at 1000°C. Transmission electron microscope observation revealed that the composite particle is consisted of nanocrystalline having primary particle size of 35 nm. Lattice parameter of the Fe3O4,BaTiO3 nanocomposite particle was 0.8404 nm that is larger than that of pure Fe3O4. Coercivity of the nanocomposite particle (390 Oe) was much larger than that of pure Fe3O4 (140 Oe). These results suggest that slight diffusion of Ba into Fe3O4 occurred. [source] Nanocomposite Formation Through Thermal Decomposition of Mixed Samarium and Magnesium Citrate-Derived Gels Formed by Spray PyrolysisJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2008Thorsten Enz Metal citrate gels of samarium and magnesium were used as precursors for the generation of hollow sphere particles by spray pyrolysis under mild thermal conditions. Six mixtures with different Sm/Mg ratios as well as pure Sm and Mg samples were prepared. As a result of the low synthesis temperature the particles consist of amorphous metal carboxylate networks. The texture of the shells is governed by microporosity yielding the major part of the total surface area. A detailed investigation of thermal decomposition, crystallization, and grain growth behavior was carried out under constant heating rate conditions. The decomposition products are nanocrystalline Sm2O3 and MgO and corresponding two-phase nanocomposites. The pure samarium carboxylate gel features considerably higher thermal stability compared with the one comprised of only magnesium. Accordingly the decomposition behavior of mixed samples is dependent on the Sm/Mg ratio. Furthermore it is shown that small amounts of MgO are able to slow down the kinetics of grain growth of Sm2O3 whereas high amounts are necessary to significantly reduce the final grain size at 1000°C. [source] Preparation of Matrix-Type Nickel Oxide/Samarium-Doped Ceria Composite Particles by Spray PyrolysisJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 4 2007Seiichi Suda Matrix-type nickel oxide (NiO)/samarium-doped ceria (SDC) composite particles, in which NiO and SDC nano-particles were homogeneously dispersed, were synthesized by spray pyrolysis (SP) for an anode precursor of intermediate-temperature solid oxide fuel cells (IT-SOFCs). SP of an aqueous solution containing Ni, Ce, and Sm salts resulted in capsule-type composite particles that had NiO enveloped with SDC. The capsule-type composite particles actually prevent Ni aggregation between particles, but they cannot have a large contact area between nickel (Ni) and SDC. A matrix-type composite particle is expected to have a large contact area because the matrix-type composite is comprised of nanometer-sized Ni and SDC particles. An adequate addition of ethylene glycol successfully resulted in matrix-type NiO/SDC composite particles. The matrix-type composite particles also showed higher anode performance than the capsule-type composite particles in these experiments and they were effective as precursors of high-performance IT-SOFC anodes. [source] Synthesis and Characterization of Mixed-Metal Oxide Nanopowders Along the CoOx,Al2O3 Tie Line Using Liquid-Feed Flame Spray PyrolysisJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2006Jose Azurdia We report here the use of liquid-feed flame spray pyrolysis (LF-FSP) to produce a series of nanopowders along the CoOx,Al2O3 tie line. The process is a general aerosol combustion synthesis route to a wide range of lightly agglomerated oxide nanopowders. The materials reported here were produced by aerosolizing ethanol solutions of alumatrane [Al(OCH2CH2)3N] and a cobalt precursor, made by reacting Co(NO3)2·6H2O crystals with propionic acid. The compositions of the as-produced nanopowders were controlled by selecting the appropriate ratios of the precursors. Nine samples with compositions (CoO)y(Al2O3)1,y, y=0,1 along the CoOx,Al2O3 tie line were prepared and studied. The resulting nanopowders were characterized by X-ray fluorescence, BET, scanning electron microscopy, high-resolution transmission electron micrographs, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and FTIR. The powders typically consist of single-crystal particles <40 nm diameter and specific surface areas (SSAs) of 20,60 m2/g. XRD studies show a gradual change in powder patterns from ,-Al2O3 to Co3O4. The cobalt aluminate spinel phase is observed at stoichiometries (21 and 37 mol%) not seen in published phase diagrams, likely because LF-FSP processing involves a quench of >1000°C in microseconds frequently leading to kinetic rather than thermodynamic products. Likewise, the appearance of Co3O4 rather than CoO as the end member in the tie line is thought to be a consequence of the process conditions. TGA studies combined with diffuse reflectance FTIR spectroscopic studies indicate that both physi- and chemi-sorbed H2O are the principal surface species present in the as-processed nanopowders. The only sample that differs is Co3O4, which has some carbonate species present that are detected and confirmed by a sharp mass loss event at ,250°C. The thermal behavior of the high cobalt content samples differs greatly from the low cobalt content samples. The latter behave like most LF-FSP-derived nanopowders exhibiting typical 1%,4% mass losses over the 1400°C range due mostly to loss of water and some CO2. The high cobalt content samples exhibit a sharp mass loss event that can be attributed to the decomposition of Co3O4 to CoO. [source] Improved electrical, optical, and structural properties of undoped ZnO thin films grown by water-mist-assisted spray pyrolysisPHYSICA STATUS SOLIDI (A) APPLICATIONS AND MATERIALS SCIENCE, Issue 10 2006L. Martínez Pérez Abstract Undoped ZnO thin films were prepared using the ultrasonic spray pyrolysis deposition technique with zinc acetylacetonate dissolved in N,N-dimethylformamide as the source materials solution. The addition of water mist in a parallel flux to the spray solution stream was also used during deposition of the films. The addition of water mist improved the electrical characteristics of the ZnO films. Fresh ZnO samples were then thermally annealed in a H2 reducing atmosphere. X-ray diffraction patterns show mainly the wurzite crystalline ZnO phase in the films. An electrical resistivity (, ) of around 2.7 × 10,2 , cm was measured at room temperature for the best undoped ZnO film. , is approximately one order of magnitude lower than the resistivities found in undoped ZnO films obtained by means of similar non-vacuum deposition techniques. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Optical properties of TiO2 thin films prepared by chemical spray pyrolysis from aqueous solutionsPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 3-4 2010R. Ayouchi Abstract Titanium dioxide (TiO2) is known to have three different kinds of polymorphous crystalline forms: rutile, anatase, and brookite. The rutile phase is always formed at higher temperatures, while the anatase phase is formed at lower temperatures and transformed into rutile phase above 800 ºC. Various deposition techniques have been developed for depositing TiO2 thin films, including evaporation, sputtering, chemical vapour deposition and thermal oxidation of titanium. Among them, the Chemical Spray Pyrolysis (CSP) technique has many advantages, such as good conformal coverage, the possibility of epitaxial growth and the application to large area deposition. Also, this method is low cost and it is easy to control the deposition growth parameters. In the present work, TiO2 thin films have been deposited on p-Si (001) and fused silica substrates by Chemical Spray Pyrolysis (CSP) method from aqueous solution containing titanium (IV) isopropoxide (Ti[OCH(CH3)2]4. As-deposited thin films show anatase polycrystalline structure, and rutile phase formed for films annealed at 750ºC. SEM images have confirmed a smooth and crack-free surface with low surface roughness. X-ray photoelectron spectroscopy (XPS) combined with 4 keV Ar+ depth profiling has shown that crystallized films correspond to TiO2. Residual carbon coming from the organic precursor solution is only detected at the surface of the film. Thin films deposited on fused silica were highly transparent (more than 85%), with an indirect optical band gap of 3,43 and 3,33 eV for as-deposited and annealed films, respectively, and refractive indexes in the range between 2.01,2.29. Spectroscopic Ellipsometry (SE) also has been used to extract optical parameters. SE data fitted to triple-layer physical model revealed the same tendency to increase refractive index in annealed films. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Surface morphology engineering of metal-oxide films by chemical spray pyrolysisPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 11 2007J. Rodriguez Abstract The Chemical Spray Pyrolysis technique and a combination of sol-gel and spray pyrolysis techniques have been used in order to monitor the morphology of metal-oxide-based thin films to be used as functional materials. We can obtain surfaces from specular to rough-porous according to the physico-chemical conditions of the precursor/spraying solution. We have produced coatings of ZnO-based and NiOx -based coatings from alcoholic and aqueous solutions. A single glass, ITO-precoated glass or alumina was used as the substrate. Porous materials of WO3, WO3 -SnO2 and SnO2 have been produced by spraying either inorganic or metal alkoxide gels over a hot substrate. The morphologies of coatings were evaluated by either SEM or optical measurements. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Structural and optical properties of polycrystalline MgxZn1,xO and ZnO:Mn films prepared by chemical spray pyrolysisPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue 8 2006Tomoaki Terasako Abstract Polycrystalline MgxZn1,xO (0.00 , x , 0.21) and ZnO:Mn films prepared by chemical spray pyrolysis were characterized by X-ray diffraction, optical transmittance, photoacoustic (PA) spectroscopy and photoluminescence (PL). Successful growth of the MgxZn1,xO (0.00 , x , 0.21) films was confirmed by the blue shift of both the near-band-edge PL peak and absorption edge with increasing the alloy composition x. However, the influence of the tail states caused by the deviation from stoichiometric compsosition and/or the spatial fluctuation of the alloy composition x was observed on the PA and PL spectra. Both the transmittance and PA spectra for the ZnO:Mn films showed the absorption band due to the d-d transitions in Mn2+ ion. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Thin films of Co3O4, MnCo2O4 and their solid solution as electrocatalyst: study of their magnetic propertiesPHYSICA STATUS SOLIDI (C) - CURRENT TOPICS IN SOLID STATE PHYSICS, Issue S1 2004E. Ríos Abstract We present magnetic measurements performed on the MnxCo3,xO4 (0 , x , 1) solid solution, prepared by spray pyrolysis. Thin films of about 20 ,m thickness were obtained after depositing aqueous metal nitrates precursors on Ti or conducting glass substrates. Powder material scratched from the substrate's surface was used for physico-chemical characterization. Presence of two oxidation states for each metal ion (Mn3+,Mn4+; Co2+,Co3+) triggers specific conduction mechanisms and double-exchange magnetic interactions. The ferromagnetic components are enhanced when x(Mn) increases, in detriment of the antiferromagnetic interactions. The ordering temperature Tc changes with x (from 22 K up to room temperature, for x = 0 up to x = 1). Based in the paramagnetic moment ,eff obtained at T > Tc, we propose a cationic distribution which can be nicely compared to the one obtained from crystallographic analyses. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] | |||||||||||||