Sintering and mass transport features of (Sn,Ti)O2 polycrystalline ceramics

Different (Sn,Ti)O2 compositions were sintered at 1450 °C for 2 h with the purpose of investigating their sintering and mass transport properties. Highly dense ceramics were obtained and their structural properties studied by X-ray diffraction and scanning electron microscopy. The changes in lattice parameters were analyzed by the Rietveld method and two mass transport mechanisms were observed during sintering in different temperature ranges, evidenced by the linear shrinkage rate as a function of temperature. The effect of the concentration of TiO2 on mass transport and densiffication during sintering was analyzed by considering the intrinsic defects. System densiffication was attributed to a mass transport mechanism in the SnO2 matrix, caused by the presence of TiO2, which formed a solid solution phase. The change in the mass transport mechanism was attributed to chemical bonding between SnO2 and TiO2, which improves ionic difusion as the concentration of TiO2 increased in (Sn,Ti)O2 compositions. © 2002 Elsevier Science Ltd. All rights reserved.

Rietveld refinements of SnO(2) ceramic powders doped with ZnO, WO(3), CoO, Nb(2)O(5) and MoO(3)

Polycrystalline materials of SnO(2) doped with ZnO, WO(3), CoO, Nb(2)O(5), and MoO(3). were synthesized by solid state reaction. X-ray powder diffraction data were collected with Cu K(alpha) radiation from a Rigaku-Rint 2000 rotating anode source. The structural and profile parameters were refined by the Rietveld method using GSAS [2]. The obtained residual parameters are R(wp) = 11,93% and R(Bragg) = 4,19%. The refined profile parameters indicate no anisotropic crystallite microstrain. The refinement results and Fourier differences calculations indicate that the dopants do not occupy interstitial sites in the crystal structure of SnO(2).

Effect of atmosphere and dopants on sintering of SnO2

Tin oxide is an n-type semiconductor material with a high covalent behavior. Mass transport in this oxide depends on the surface state promoted by atmosphere or by the solid solution of a non-isovalent oxide doping The sintering and grain growth of this type of oxide powder is then controlled by atmosphere and by extrinsic oxygen vacancy formation. For pure SnO2 powder the surface state depends only on the interaction of atmosphere molecules with the SnO2 surface. Inert atmosphere like argon or helium promotes oxygen vacancy formation at the surface due to reduction of SnO2 to SnO at the surface and liberation of oxygen molecules forming oxygen vacancies. As consequence surface diffusion is enhanced leading to grain coarsening but no densification. Oxygen atmosphere inhibits the SnO2 reduction decreasing the surface oxygen vacancy concentration. Addition of dopants with lower valence at sintering temperature creates extrinsic charged oxygen vacancies that promote mass transport at grain boundary leading to densification and grain growth of this polycrystalline oxide.

Study of KCl + x% in and KCl + y% TlCl thin films

The present work reports the study of KCl thin films doped with In+ or Tl+. Both systems show optical absorption bands similar to single crystals. As the impurity concentration increases, so does the absorption as also the half band width, unlike in KCl: Cu+ films. Further experimental techniques such as X-ray diffraction, scanning electron micrographs and energy dispersive X-ray observations were used and comparative analysis with KCl : Cu+ films reveals new conditions for better crystallinity of the samples.

The influence of crystallization route on the SrBi2Nb2O9 thin films

Polycrystalline SrBi2Nb2O9-layered ferroelectric thin films were synthesized on Pt/Ti/SiO2/Si substrate using the polymeric precursors solution. The dip-coated films were specular and crack-free and crystallized during firing at 700 °C. Single-, double-, and triple-layered films were obtained by several dips in the deposition solution, and the influence of crystallization between each dip was studied. Microstructure and morphological evaluation were followed by grazing incident x-ray diffraction (GIXRD), scanning electron microscopy (SEM), and atomic force microscopy (AFM). Multilayered films obtained using the intermediate-crystallized layer route present a dense microstructure with spherical grains, with a preferential orientation in the 〈215〉 direction; films obtained using the intermediate-amorphous layer route are polycrystalline and present elongated grains around 250 nm in size.

Metal-insulator transition in Nd1-xEuxNiO 3 compounds

Polycrystalline Nd1-xEuxNiO3 (0≤x≤0.5) compounds were synthesized in order to investigate the character of the metal-insulator (MI) phase transition in this series. Samples were prepared through the sol-gel route and subjected to heat treatments at ∼1000 °C under oxygen pressures as high as 80bar. X-ray diffraction (XRD) and neutron powder diffraction (NPD), electrical resistivity ρ(T), and magnetization M(T) measurements were performed on these compounds. The NPD and XRD results indicated that the samples crystallize in an orthorhombic distorted perovskite structure, space group Pbnm. The analysis of the structural parameters revealed a sudden and small expansion of ∼0.2% of the unit cell volume when electronic localization occurs. This expansion was attributed to a small increase of ∼0.003 of the average Ni-O distance and a simultaneous decrease of ∼-0.5° of the Ni-O-Ni superexchange angle. The ρ(T) measurements revealed a MI transition occurring at temperatures ranging from TMI∼193 to 336K for samples with x ≤ 0 and 0.50, respectively. These measurements also show a large thermal hysteresis in NdNiO3 during heating and cooling processes, suggesting a first-order character of the phase transition at TMI. The width of this thermal hysteresis was found to decrease appreciably for the sample Nd 0.7Eu0.3NiO3. The results indicate that cation disorder associated with increasing substitution of Nd by Eu is responsible for changing the first-order character of the transition in NdNiO3. © 2006 IOP Publishing Ltd.

Er3+-doped Y2O3 obtained by polymeric precursor: Synthesis, structure and upconversion emission properties

The relentless pursuit for materials containing rare earth ions with photoluminescent properties has led to several studies with applications in the development of new technologies. The main focus of this work is the preparation of Er3+-doped polycrystalline Y2O3 with photoluminescent properties using PEG as an organic precursor and heat-treated at different temperatures. The methodology used in this synthesis is highly attractive due to its high feasibility for improved technology and low cost for preparing materials. The behavior of the viscous resin has been evaluated and the final compounds exhibited the formation of a cubic polycrystalline phase, which is able to support variations in Er3+ doping concentrations up to 10 mol%, without significant changes in the polycrystalline parameters. The values of the nanocrystallite size calculated by Scherrer's equation showed direct dependence on the heat-treatment temperature as well as the Er3+ concentration. Intense emission in the visible region under excitation at 980 nm was attributed to an upconversion phenomenon assigned to the intraconfigurational f-f transitions of Er3+ ions. The upconversion mechanism was investigated and it was demonstrated that the higher intense emission in the red region in comparison to the emission in the green region is related to the crystallite size. The studies about the intensity showed the dependence of upconversion emission of power source, indicating that two-photon are responsible for the green and red photoluminescence. These polycrystalline materials exhibit properties that make them promising for use in solar energy systems, C-telecom band or solid-state laser devices. (C) 2014 Elsevier B.V. All rights reserved.

Método para controle da qualidade de medicamentos sólidos por difração de raios X

Pós-graduação em Química - IQ

Structural and optical properties of CaTiO3 perovskite-based materials obtained by microwave-assisted hydrothermal synthesis: An experimental and theoretical insight

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of thermal annealing treatment in oxygen atmosphere on grain boundary chemistry and non-ohmic properties of SnO2 center dot MnO polycrystalline semiconductors

The present work studied the influence of thermal treatment in oxygen rich atmosphere on heterogenous junctions in Mn-doped SnO2 polycrystalline system presenting varistor behavior. The samples were prepared by conventional oxide mixture methodology, and were submitted to heat treatment in oxygen rich atmosphere at 900 degrees C for 2h. The samples were characterized by X-ray diffraction, scanning electron microscopy, dc and ac electrical measurements. The results showed that there is an evident relationship between the microstructure heterogeneity and non-ohmic electrical properties. It was found that for this SnO2 center dot MnO-based varistor system the heat treatment in oxygen rich atmosphere does not necessarily increase the varistors properties, which was related to the decrease in the grain boundary resistance. The results are compared with Co-doped SnO2 varistors and ZnO based varistors. (C) 2008 WILEY-VCH Verlay GmbH & Co. KGaA, Weinheim.

Nature of potential barrier in (Ca-1/4,Cu-3/4)TiO3 polycrystalline perovskite

The nonohmic electrical features of (Ca-1/4,Cu-3/4)TiO3 perovskite ceramics, which have very strong gigantic dielectric is believed originate from potential barriers at the grain boundaries. In the present study, we used the admittance and impedance spectroscopy technique to investigate (Ca-1/4,Cu-3/4)TiO3 perovskite ceramics with low nonohmic electrical properties. The study was conducted under two different conditions: on as-sintered ceramics and on ceramics thermally treated in an oxygen-rich atmosphere. The results confirm that thermal treatment in oxygen-rich atmospheres influence the nonohmic properties. Annealing at oxygen-rich atmospheres improve the nonohmic behavior and annealing at oxygen-poor atmospheres decrease the nonohmic properties, a behavior already reported for common metal oxide nonohmic devices and here firstly evidenced for the (Ca-1/4,Cu-3/4)TiO3 perovskite related materials. The results show that oxygen also influences the capacitance values at low frequencies, a behavior that is indicative of the Schottky-type nature of the potential barrier. (c) 2006 Elsevier Ltd. All rights reserved.

Resistive-Switching Behavior in Polycrystalline CaCu3Ti4O12 Nanorods

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

Size effects of polycrystalline lanthanum modified Bi4Ti3O12 thin films

The film thickness dependence on the ferroelectric properties of lanthanum modified bismuth titanate Bi3.25La0.75Ti3O12 was investigated. Films with thicknesses ranging from 230 to 404 nut were grown on platinum-coated silicon substrates by the polymeric precursor method. The internal strain is strongly influenced by the film thickness. The morphology of the film changes as the number of layers increases indicating a thickness dependent grain size. The leakage current, remanent polarization and drive voltage were also affected by the film thickness. (c) 2007 Elsevier Ltd. All rights reserved.

Relationship between grain-boundary capacitance and bulk shallow donors in SnO2 polycrystalline semiconductor

The relationship between grain-boundary capacitance and extrinsic shallow donors caused by Nb addition to SnO2 center dot COO binary polycrystalline system has been investigated by means of combined techniques such as I-V characteristic response, complex impedance and capacitance analysis and electrostatic force microscopy. The estimated role of the Nb doping is to increase the concentration of shallow donors that are capable of enhancing the electronic donation to grain-boundary acceptors. This effect leads to the formation of potential barriers at grain boundaries with a simultaneous increase of grain-boundary capacitance and non-Ohmic features of the polycrystalline device doped with Nb atoms.

Electronic ceramics based on polycrystalline SnO2, TiO2 and (Sn xTi1-x)O2 solid solution

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