Synthesis of nanocrystalline tetragonal zirconia by a polymeric organometallic method

A polymeric precursor method based on the Pechini process was successfully used to synthesize zirconia-12 mol% ceria ceramic powders, the influence of the main process variables (citric acid-ethylene glycol ratio, citric acid-total oxides ratio and calcination temperature) on phase formation and powder morphology (surface area and crystallite size) were investigated. The thermal decomposition behavior of the precursor is presented. X-ray diffraction (XRD) patterns of powders revealed a crystalline tetragonal zirconia single-phase, with crystallite diameter ranging from 6 to 15 nm. The BET surface areas were relatively high, reaching 95 m(2) g(-1) Nitrogen adsorption/desorption on the powders suggested that nonaggregated powders could be attained, depending on the synthesis conditions. Copyright (C) 1999 John Wiley & Sons, Ltd.

Microstructural and optical characterization of CaWO4 and SrWO4 thin films prepared by a chemical solution method

Stoichiometric CaWO4 and SrWO4 thin films were synthesized using a chemical solution processing, the so-called polymeric precursor method. In this soft chemical method, soluble precursors such as strontium carbonate, calcium carbonate and tungstic acid, as starting materials, were mixed in an aqueous solution. The thin films were deposited on glass substrates by means of the spinning technique. The surface morphology and crystal structure of the thin films were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Nucleation stages and surface morphology evolution of the thin films on glass substrates were studied by atomic force microscopy. The films nucleate at 300 degreesC, after the coalescence of small nuclei into larger grains yielding a homogeneous dense surface. XRD characterization of these films showed that the CaWO4 and SrWO4 phases crystallize at 400 degreesC from an inorganic amorphous phase. No intermediate crystalline phase was identified. The optical properties were also studied. It was found that CaWO4 and SrWO4 thin films have an optical band gap, E-gap=5.27 and 5.78 eV, respectively, of a direct transition nature. The excellent microstructural quality and chemical homogeneity confirmed that this soft solution processing provides an inexpensive and environmentally friendly route for the preparation of CaWO4 and SrWO4 thin films. (C) 2003 Elsevier B.V. All rights reserved.

Development of metal oxide nanoparticles by soft chemical method

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Particle growth during calcination of polycation oxides synthesized by the polymeric precursors method

The particle-growth kinetics of sodium niobate and zirconium titanate powders that were processed by the polymeric precursors method were studied. The growth kinetics that were studied for the particle, in the final stage of crystallization, showed that the growth process occurs in two different stages. For temperatures <800°C, the particle-growth mechanism is associated with surface diffusion, with an activation energy in the range of 40-80 KJ/mol. For temprratures >800°C, particle growth is controlled by densification of the nanometric particle cluster and by a neck-size-controlled particle-growth mechanism. The results suggest that this behavior was typical of the synthesis method, because two different polycation oxides presented the same behavior.

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.

Obtenção e caracterização de filmes finos de Bi3NbO7 pelo método dos precursores poliméricos

Pós-graduação em Engenharia Mecânica - FEG

Desenvolvimento de recobrimento submicrométrico de óxido de nióbio para aplicação em tubulações de prospecção de petróleo

Pós-graduação em Engenharia Mecânica - FEG

Effect of the iron doping on the thermal decomposition of the polymeric precursor for the titanium dioxide powder synthesis

The Polymeric Precursor Method has proved suitable for synthesizing reactive powders using low temperatures of calcination, especially when compared with conventional methods. However, during the thermal decomposition of the polymeric precursor the combustion event can be releases an additional heat that raises the temperature of the sample in several tens of degrees Celsius above the set temperature of the oven. This event may be detrimental to some material types, such as the titanium dioxide semiconductor. This ceramic material has a phase transition at around 600 ° C, which involves the irreversible structural rearrangement, characterized by the phase transition from anatase to rutile TiO2 phase. The control of the calcination step then becomes very important because the efficiency of the photocatalyst is dependent on the amount of anatase phase in the material. Furthermore, use of dopant in the material aims to improve various properties, such as increasing the absorption of radiation and in the time of the excited state, shifting of the absorption edge to the visible region, and increasing of the thermal stability of anatase. In this work, samples of titanium dioxide were synthesized by the Polymeric Precursor Method in order to investigate the effect of Fe (III) doping on the calcination stages. Thermal analysis has demonstrated that the Fe (III) insertion at 1 mol% anticipates the organic decomposition, reducing the combustion event in the final calcination. Furthermore, FTIR-PAS, XRD and SEM results showed that organic matter amount was reduced in the Fe (III)-doped TiO2 sample, which reduced the rutile phase amount and increased the reactivity and crystallinity of the powder samples.

Synthesis, structure and magnetic properties of Y3Fe5-xAlxO12 garnets prepared by the soft chemical method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Synthesis of imines from amines in aliphatic alcohols on Pd/ZrO2 catalyst under ambient conditions

Synthesis of imines from amines and aliphatic alcohols (C1–C6) in the presence of base on supported palladium nanoparticles has been achieved for the first time. The catalytic system shows high activity and selectivity in open air at room temperature. As an example of the isostructural Ln3Sb3Co2O14 (Ln: La, Pr, Nd, Sm—Ho) series with an ordered pyrochlore structure, the La variant is prepared by a citrate complex method employing stoichiometric amounts of La(NO3)3, Co(NO3)2, and Sb tartrate together with citric acid with a metal/citrate molar ratio of 1:2

Low-temperature preparation of fine-particle cobaltites

A novel solid-solution precursor method for the preparation of fine-particle cobaltites at low temperatures has been described. The precursors, hydrazinium metal hydrazine carboxylate hydrates, N2H5M1/3Co2/3(N2H3COO)3 · H2O, where M = Mg, Mn, Fe, Co, Ni, and Zn, decompose in air <250°C to yield corresponding metal cobaltites, MCo2O4. Formation of cobaltites has been confirmed by thermogravimetry (TG) weight loss, IR, and X-ray diffraction. Combustion of the precursor in air yields fine-particle cobaltites with surface areas in the range of 12–115 m2g−1 and particle sizes of 1–40 μm. Low decomposition temperatures of the precursors accompanied by the evolution of large amounts of gases appear to control the particle size of the cobaltites.

Preparative solid state chemistry. Recent developments

A survey of recent developments in preparative solid state chemistry shows that, with a knowledge of structural chemistry and reactivity patterns of solids, it is possible to synthesize a variety of new solids possessing novel structures. A distinction is made between synthesis ofnew solids and synthesis of solids bynew methods. Three new routes to solid state synthesis are recognized: the precursor method, and topochemical methods involving redox and ion-exchange reactions. The low-temperature topochemical methods enable synthesis of metastable phases that are inaccessible by the high temperature route. Several illustrative examples of solid state synthesis from the recent literature are presented.

Low temperature fabrication and impedance spectroscopy of PMN-PT ceramics

Single phase perovskite 0.9Pb(Mg1/3Nb2/3)O-3-0.1(PbTiO3) ceramics were prepared using the columbite precursor method after optimizing the synthesis conditions. X-ray diffraction (XRD) studies were carried out to verify the phase formation at each processing step. Scanning electron microscopy (SEM) was employed to observe the microstructure of the sintered ceramics. Impedance and modulus spectroscopic data were used to gain an insight into the electrical properties of the samples and with a view to observing the relaxations in them. (C) 1999 Elsevier Science Ltd.

Structural, dielectric relaxation and piezoelectric characterization of Sr2+ substituted modified PMS-PZT ceramic

Pyrochlore phase free [Pb0.94Sr0.06] [(Mn1/3Sb2/3)(0.05)(Zr0.53Ti0.47)(0.95)] O-3 ceramics has been synthesized with pure Perovskite phase by semi-wet route using the columbite precursor method. The field dependences of the dielectric response and the conductivity have been measured in a frequency range from 50 Hz to 1 MHz and in a temperature range from 303 K to 773 K. An analysis of the real and imaginary parts of the dielectric permittivity with frequency has been performed, assuming a distribution of relaxation times. The scaling behavior of the dielectric loss spectra suggests that the distribution of the relaxation times is temperature independent. The SEM photographs of the sintered specimens present the homogenous structures and well-grown grains with a sharp grain boundary. The material exhibits tetragonal structure. When measured at frequency (100 Hz), the polarization shows a strong field dependence. Different piezoelectric figures of merit (k(p), d(33) and Q(m)) of the material have also been measured obtaining their values as 0.53, 271 pC/N and 1115, respectively, which are even higher than those of pure PZT with morphotropic phase boundary (MPB) composition. Thus the present ceramics have the optimal overall performance and are promising candidates for the various high power piezoelectric applications. (C) 2011 Elsevier B.V. All rights reserved.