The influence of the synthesis route on the final properties of SnO2-based varistors

A comparative study of two customary routes of ceramics processing applied to the synthesis of SnO2-based varistors is reported in this paper. Devices of equivalent composition were prepared through the Pechini method and through directly mixing the oxides without the addition of anti-agglomerants or binders. The microstructures of the sintered samples were characterised with X-ray diffraction and scanning and transmission electron microscopies. The electrical behaviour of the devices was studied on the basis of the current density versus electric field (J-E) characteristics and impedance spectroscopy measurements. The Pechini method ensures the homogeneity in the distribution of the additives in the tin oxide matrix but the formation of secondary phases seems to be independent of the synthesis route. Devices with similar non-linear coefficients of 18 and 21 were obtained through the mixed oxides route and the Pechini method, respectively. (C) 2007 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Síntese e caracterização de nanopartículas e filmes finos de óxidos semicondutores

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e caracterização estrutural de filmes finos Bi4Ti3O12

Pós-graduação em Ciência dos Materiais - FEIS

Cerâmica condutora à base de 'SN''O IND.2' obtida pelo método dos precursores poliméricos e sinterização por micro-ondas

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Propriedades e mecanismos de cintilação dos materiais 'GD''AL''O IND.3' e ('GD''LU')'AL''O IND.3' dopados com 'EU POT. 3+', 'TB POT. 3+' e 'PR POT. 3+'

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Preparação e caracterização de filmes finos de 'BA''BI IND.2''TA IND.2''O IND.9(BBT)' e 'BA''BI IND.2''NB IND.2''O IND.9(BBN)'

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

Síntese e caracterização de catalisadores nanométricos de LaSrNiO4 para aplicação em dessulfurização de tiofeno

The mixed metal oxides constitute an important class of catalytic materials widely investigated in different fields of applications. Studies of rare earth nickelates have been carried by several researchers in order to investigate the structural stability afforded by oxide formed and the existence of catalytic properties at room temperature. So, this study aims synthesize the nanosized catalyst of nickelate of lanthanum doped with strontium (La(1-x)SrxNiO4-d; x = 0,2 and 0,3), through the Pechini method and your characterization for subsequent application in the desulfurization of thiophene reaction. The precursor solutions were calcined at 300ºC/2h for pyrolysis of polyester and later calcinations occurred at temperatures of 500 - 1000°C. The resulting powders were characterized by thermogravimetric analysis (TG / DTG), surface area for adsorption of N2 by BET method, X-ray diffraction (XRD), scanning electron microscopy (HR_SEM) and spectrometry dispersive energy (EDS). The results of XRD had show that the perovskites obtained consist of two phases (LSN and NiO) and from 700ºC have crystalline structure. The results of SEM evidenced the obtainment of nanometric powders. The results of BET show that the powders have surface area within the range used in catalysis (5-50m2/g). The characterization of active sites was performed by reaction of desulfurization of thiophene at room temperature and 200ºC, the relation F/W equal to 0,7 mol h-1mcat -1. The products of the reaction were separated by gas chromatography and identified by the selective detection PFPD sulfur. All samples had presented conversion above 95%

Síntese de catalisadores do tipo LaNixFe1-xO3 como precursores catalíticos para reação oxidação parcial do metano

Nickel-bases catalysts have been used in several reform reactions, such as in the partial oxidation of methane to obtain H2 or syngas (H2 + CO). High levels of conversion are usually obtained using this family of catalysts, however, their deactivation resulting from carbon deposition still remains a challenge. Different approaches have been tested aiming at minimizing this difficulty, including the production of perovskites and related structures using modern synthesis methods capable of producing low cost materials with controlled microstructural characteristics at industrial scale. To establish grounds for comparison, in the present study LaNixFe1-xO3 (x=0, 0.3 or 0.7) perovskites were prepared following the Pechini method and by microwave assisted self-combustion. All samples were sub sequently calcined at 900 °C to obtain the target phase. The resulting ceramic powders were characterized by thermogravimetric analysis, infrared spectroscopy, X ray diffraction, specific area and temperature programmed reduction tests. Calcined samples were also used in the partial oxidation reaction of methane to evaluate the level of conversion, selectivity and carbon deposition. The results showed that the calcined samples were crystalline and the target phase was formed regardless of the synthesis method. According to results obtained by Rietveld refinement, we observed the formation of 70.0% of LaNi0.3Fe0.7O3 and 30.0% of La2O3 for samples LN3F7-900- P, LN3F7-900-M and 41,6% of LaNi0.7Fe0.3O3, 30.7% of La2NiO4 and 27.7% of La2O3 for samples LN7F3-900-P and LN7F3-900-M.Temperature-programmed profiles of the LaNiO3 sample revealed the presence of a peak around 510 °C, whereas the LaFeO3 sample depicted a peak above 1000°C. The highest l evel of methane conversion was obtained for LaNiO3 synthesized by the Pechini method. Overall, catalysts prepared by the Pechini method depicted better conversion levels compared to those produced by microwave assisted self-combustion

Thermogravimetric and UV-vis spectroscopic studies of chromium redox reactions in rutile pigments

In this study undoped and Cr, Sb or Mo doped TiO(2) were synthesized by polymeric precursor method and characterized by X-ray diffraction, UV-VIS spectroscopy, infrared spectroscopy and thermogravimetry (TG). The TG curves showed a continuous mass loss assigned to the hydroxyl elimination and Cr(6+) reduction. Doped TiO(2) samples showed a higher mass loss assigned to water and gas elimination at lower temperatures. In these doped materials a decrease in the anatase-rutile phase transition temperature was observed. After calcination at 1,000 A degrees C, rutile was obtained as a single phase material without the presence of Cr(6+).

Preparation and characterization of TiO2/acid leached serpentinite tailings composites and their photocatalytic reduction of Chromium(VI)

Composite TiO2/acid leached serpentine tailings (AST) were synthesized through the hydrolysis–deposition method and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energydispersive X-ray spectrometry (EDS), Fourier-transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and surface area measurement (BET). The XRD analysis showed that TiO2 coated on the surface of acid leached serpentine tailings was mixed crystal phases of rutile and anatase, the grain size of which is 10–30 nm. SEM, TEM, and EDS analysis exhibited that nano-TiO2 particles were deposited on the surface and internal cavities of acid leaching serpentine tailings. The XPS and FT-IR analysis demonstrated that the coating process of TiO2 on AST was a physical adsorption process. The large specific surface area, porous structure, and plentiful surface hydroxyl group of TiO2/AST composite resulted in the high adsorption capacity of Cr(VI). The experimental results demonstrated that initial concentration of Cr(VI), the amount of the catalyst, and pH greatly influenced the removal efficiency of Cr(VI). The removal kinetics of Cr(VI) at a relative low initial concentration was fitted well with Langmuir–Hinshelwood kinetics model with R2 value of about unity. The asprepared composites exhibited strong adsorption and photocatalytic capacity for the removal of Cr(VI), and the possible photocatalytic reduction mechanism was studied. The photodecomposition of Cr(VI) was as high as 95% within 2 h, and the reusability of the photocatalysis was proven.

La-Doped Ba2In2O5 Electrolyte: Pechini Synthesis, Microstructure, Electrical Conductivity, and Application for CO Gas Sensing

Dense (Ba1―xLax)2In2O5+x (BLIO) electrolytes with different compositions (x = 0.4, 0.5, 0.6) were fabricated using powders obtained by the Pechini method. The formation of BLIO powders was investigated by using X-ray diffraction and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy. The calcination temperature and time were optimized. The sintered (Ba1―xLax)2In2O5+x electrolytes showed a relative density greater than ∼97%, and the major phase of three electrolyte compositions was indexed as a cubic perovskite. The electrical conductivity of BLIO ceramics at elevated temperatures in air was measured by ac-impedance spectroscopy. The activation energies for conduction in BLIO were 102 kJ mol―1 between 473 and 666 K and 118 kJ mol―1 between 769 and 873 K, which are comparable to that for 8 mol % yttria-stabilized cubic zirconia. Mixed-potential gas sensors utilizing BLIO-based electrolytes exhibited good sensitivity to different CO concentrations from ∼100 to ∼500 ppm and excellent selectivity to methane at around 873 K.

Analysis of chromium behaviour and speciation during the electrodialytic process

The interest in chromium (Cr) arises from the widespread use of this heavy metal in various industrial processes that cause its release as liquid, solid and gaseous waste into the environment. The impact of Cr on the environment and living organisms primarily depends on its chemical form, since Cr(III) is an essential micronutrient for humans, other animals and plants, and Cr(VI) is highly toxic and a known human carcinogen. This study aimed to evaluate if the electrodialytic process (ED) is an appropriate treatment for Cr removal, through a critical overview of Cr speciation, before and after the ED experiments, to assess possible Cr(III)-Cr(VI) interconversions during the treatment. ED was the treatment technique applied to two types of matrices containing Cr: chromate copper arsenate (CCA) contaminated soil and municipal solid waste incineration (MSWI) fly ash. In order to study Cr remediation, three EDR set-ups were used: a new set-up, the combined cell (2/3C or 3/2C), with three compartments, alternating current between two anodes and different initial experimental conditions, one set-up with three compartments (3C cell) and the other set-up with two compartments (2C cell). The Cr removal rates obtained in this study were between 10-36% for the soil, and 1-13% for the fly ash. The highest Cr removal rates were achieved in the 26 days experiments: 36% for the soil, 13% for the fly ash. Regarding the 13 days experiments, the highest Cr removal rates were attained with the 2/3C set-up: 24% for the soil, 5% for the fly ash. The analysis of Cr(VI) was performed before and after ED experiments to evaluate eventual changes in Cr speciation during the treatment. This analysis was conducted by two methods: USEPA Method 3060A, for the extraction of Cr(VI); and Hach Company Method 8023, for the detection of Cr(VI). Despite the differences in Cr total concentration, both matrices presented a similar speciation, with Cr(III) being the main species found and Cr(VI) less than 3% of Cr total, before and after the treatment. For fly ash, Cr(VI) was initially below the detection limit of the method and remained that way after the treatment. For soil, Cr(VI) decreased after the treatment. Oxidation of Cr(III) to Cr(VI) did not occur during the ED process since there was no increase in Cr(VI) in the matrices after the treatment. Hence, the results of this study indicate that ED is an appropriate technique to remediate matrices containing Cr because it contributes to Cr removal, without causing Cr(III)-Cr(VI) interconversions.

Thermal and structural investigation of SnO2/Sb2O3 obtained by the polymeric precursor method

SnO2-based materials are used as sensors, catalysts and in electro-optical devices. This work aims to synthesize and characterize the SnO2/Sb2O3-based inorganic pigments, obtained by the polymeric precursor method, also known as Pechini method (based on the metallic citrate polymerization by means of ethylene glycol). The precursors were characterized by thermogravimetry (TG) and differential thermal analysis (DTA). After characterization, the precursors were heat-treated at different temperatures and characterized by X-ray diffraction. According to the TG/DTA curves basically two-step mass loss process was observed: the first one is related to the dehydration of the system; and the second one is representative to the combustion of the organic matter. Increase of the heat treatment temperature from 500 to 600 degrees C and 700 degrees C resulted higher crystallinity of the formed product.

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.

Preparation and characterization of BaBi2Nb2O9(BBN) ceramics synthetized by polymeric precursors method

Pure BBN powders and with addition of 1 and 2 wt% in excess of bismuth were obtained by Pechini Method. The powders calcined at 300°C/4h were analyzed by TG/DTA to study the temperature of organic matter decomposition. A systematic study of calcination temperature and time to the formation of the BBN phase was performed and the phase formation was accompanied by XRD. The calcined powders at 800°C during 2h were analyzed by infrared spectroscopy and by BET. The powders were isostaticaly pressed and sintered at temperatures ranging from 900°C to 1000°C. The ceramics were characterized by XRD to control the crystalline phase and by SEM to analyze the microstructure.