Superparamagnetic Ni:SiO2-C nanocomposites films synthesized by a polymeric precursor method

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

(Sr,Tm)ZrO3 powders prepared by the polymeric precursor method: Synthesis, optical properties and morphological characteristics

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Nanometric Pb1-xLaxTiO3 (x=0, 0.13 and 0.27) powders obtained by the polymeric precursor method

PLT (Pb1-xLaxTiO3, in which x = 0, 0.13 and 0.27) powders were successfully synthesized using the polymeric precursor method, based on the Pechini method. The polymeric precursors were calcined at temperatures ranging from 350 to 500 degrees C for 4 h. X-ray diffraction (XRD) showed the evolution of the crystalline phase starting from the amorphous precursor. Thermogravimetric analyses (TG) and differential thermal analyses (DTA) of the powder precursors showed the influence of the pH on the elimination of organic material. PLT powders have a tendency to form agglomerates, what can be verified by comparing the values of the average particle sizes obtained by Brunauer-Emmett-Teller method, BET (D-BET) with the values of the average crystallite sizes obtained by XRD (D-XRD). (C) 2007 Elsevier Ltd. All fights reserved.

LiNbO3 thin films prepared from a polymeric precursor method

LiNbO3 thin films were prepared from polymeric precursor method by dip coating. The precursor films, deposited on Si(111) substrates, were heat-treated from 400°C to 900°C in order to study the heat treatment influence on the crystallinity and microstructure of the final film. The X-ray diffraction patterns showed, in particular, that these films crystallize at low temperature (450°C) and present no preferential orientation. The scanning electron microscopy studies showed that the film microstructure is strongly influenced by the annealing temperature. © 1997 Trans Tech Publications.

Ferrimagnetism and spin excitation in a Ni-Mn partially inverted spinel prepared using a modified polymeric precursor method

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Very Intense Distinct Blue and Red Photoluminescence Emission in MgTiO 3 Thin Films Prepared by the Polymeric Precursor Method: An Experimental and Theoretical Approach

MgTiO3 (MTO) thin films were prepared by the polymeric precursor method with posterior spin-coating deposition. The films were deposited on Pt(111)/Ti/SiO2/Si(100) substrates and heat treated at 350 °C for 2 h and then heat treated at 400, 450, 500, 550, 600, 650 and 700 °C for 2 h. The degree of structural order−disorder, optical properties, and morphology of the MTO thin films were investigated by X-ray diffraction (XRD), micro-Raman spectroscopy (MR), ultraviolet− visible (UV−vis) absorption spectroscopy, photoluminescence (PL) measurements, and field-emission gun scanning electron microscopy (FEG-SEM) to investigate the morphology. XRD revealed that an increase in the annealing temperature resulted in a structural organization of MTO thin films. First-principles quantum mechanical calculations based on density functional theory (B3LYP level) were employed to study the electronic structure of ordered and disordered asymmetric models. The electronic properties were analyzed, and the relevance of the present theoretical and experimental results was discussed in the light of PL behavior. The presence of localized electronic levels and a charge gradient in the band gap due to a break in the symmetry are responsible for the PL in disordered MTO lattice.

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 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.

Study of electrical, chemical and structural characteristics of superconductor thin film obtained by polymeric precursors method

Superconductor films of the BSCCO system have been grown by dip coating technique with good success. The chemical method allows us to grow high temperature superconductor thin films to get better control of stoichiometry, large areas and is cheaper than other methods. There is a great technological interest in growth oriented superconductor films due anisotropic characteristics of superconductor materials of high critical temperature, specifically the cuprates, as we know that the orientation may increase the electrical transport properties. Based on this, the polymeric precursor method has been used to obtain thin films of the BSCCO system. In this work we have applied that method together with the deposition technique known as dip coating to obtain Bi-based superconductor thin films, specifically, Bi1.6Pb0.4Sr2.0C2.0Cu3.0Ox+8, also known as 2223 phase with a critical temperature around 110 K. The films with multilayers have been grown on crystalline substrates of LaAlO3 and orientated (100) after being heat treated around 790 degrees C - 820 degrees C in lapse time of 1 hour in a controlled atmosphere. XRD measurements have shown the presence of a crystalline phase 2212 with a critical temperature around 85 K with (001) orientation, as well as a small fraction of 2223 phase. SEM has shown a low uniformity and some cracks that maybe related to the applied heat treatment. WDS has also been used to study the films composition. Different heat treatments have been used with the aim to increase the percentage of 2223 phase. Measurements of resistivity confirmed the presence of at least two crystalline phases, 2212 and 2223, with T-c around 85 K and 110 K, respectively.

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.

Photocatalytic decomposition of rhodamine-B using scandium and silver-modified TiO2 Powders

Semiconductor-mediated photocatalytic oxidation is an interesting method for water decontamination and a specially modified TiO2 is said to be a promising material. This study verified that the synthesis of 1wt%Ag modified-Sc0.01Ti0.99O1.995 powder samples prepared by Polymeric Precursor Method is capable of forming a mixture of anatase-rutile phase with high photocatalytic performance. This kind of material is found to have a lower bandgap compared to the TiO2-anatase commercial powders, which can be associated to an innovative hybrid modification. The simultaneous insertion of scandium in order to generate a p-type semiconductor and a metallic silver nanophase acting as an electron trapper demonstrated being capable of enhancing the degradation of rhodamine B compared to the commercial TiO2. In spite of the different thermal treatments or phase amounts, the hybrid modified powder samples showed higher photocatalytic activity than the commercial ones.

Photocatalytic decomposition of rhodamine-b using scandium and silver-modified TiO2 powders

Semiconductor-mediated photocatalytic oxidation is an interesting method for water decontamination and a specially modified TiO2 is said to be a promising material. This study verified that the synthesis of 1wt%Ag modified-Sc0.01Ti0.99O1.995 powder samples prepared by Polymeric Precursor Method is capable of forming a mixture of anatase-rutile phase with high photocatalytic performance. This kind of material is found to have a lower bandgap compared to the TiO2-anatase commercial powders, which can be associated to an innovative hybrid modification. The simultaneous insertion of scandium in order to generate a p-type semiconductor and a metallic silver nanophase acting as an electron trapper demonstrated being capable of enhancing the degradation of rhodamine B compared to the commercial TiO2. In spite of the different thermal treatments or phase amounts, the hybrid modified powder samples showed higher photocatalytic activity than the commercial ones.

Heating rate and temperature effects on the BaTiO3 formation by thermal decomposition of (Ba,Ti) organic precursors during the Pechini process

Different thermal treatments for the synthesis of BaTiO3 powder obtained through the Pechini method were studied. The synthesis of BaTiO3 starts at 150 °C by the thermal dehydration of organic precursors. The usual inevitable formation of barium carbonate during the thermal decomposition of the precursor could be retarded at lower calcination temperatures and optimized heating rates. The organic precursors were treated at temperatures between 200 and 400 °C. Then, the samples were calcined at 700 and 800 °C for 4 and 2 h, respectively. The resulting ceramic powders were characterized by gravimetric and differential thermal analyses, X-ray powder diffraction and infrared spectroscopy. It was found that depending on the heating rate and final temperature of the thermal treatment, high amounts of BaCO3 and TiO2 could be present due to the high concentration of organics in the final calcination step. © 2007 Elsevier B.V. All rights reserved.

Effect of ceria content on the sintering of ZrO2 based ceramics synthesized from a polymeric precursor

Zirconia-ceria powders with ceria concentration varying from 0 to 12 mol% were synthesized using a polymeric precursor route based on the Pechini process. Powder characteristics were evaluated with regard to the crystallite size, BET surface area, phase distribution, nitrogen adsorption/desorption behavior, and agglomeration state. Sintering was studied considering the shrinkage rate, densification, grain size, and phase evolution. It was demonstrated that the synthesis method is effective to prepare nanosized powders of tetragonal zirconia single-phase. Sinterability mainly depended on the agglomeration state of powders and the monoclinic phase content, fully tetragonal zirconia ceramic, with grain size of 2.4 mu m, was obtained after addition of at least 9 mol% ceria and sintering at 1500 degrees C for 4 h. (C) 2000 Elsevier B.V. Ltd. All rights reserved.

Electroluminescence of zinc oxide thin-films prepared via polymeric precursor and via sol-gel methods

Zinc oxide (ZnO) is an electroluminescent (EL) material that can emit light in different regions of electromagnetic spectrum when electrically excited. Since ZnO is chemically stable, inexpensive and environmentally friendly material, its EL property can be useful to construct solid-state lamps for illumination or as UV emitter. We present here two wet chemical methods to prepare ZnO thin-films: the Pechini method and the sol-gel method, with both methods resulting in crystalline and transparent films with transmittance > 85% at 550 nm. These films were used to make thin-film electroluminescent devices (TFELD) using two different insulator layers: lithium fluoride (LiF) or silica (SiO2). All the devices exhibit at least two wide emission bands in the visible range centered at 420 nm and at 380 nm attributed to the electronic defects in the ZnO optical band gap. Besides these two bands, the device using SiO2 and ZnO film obtained via sol-gel exhibits an additional band in the UV range centered at 350 nm which can be attributed to excitonic emission. These emission bands of ZnO can transfer their energy when a proper dopant is present. For the devices produced the voltage-current characteristics were measured in a specific range of applied voltage. (C) 2007 Elsevier B.V. All rights reserved.