Co/Al2O3 catalysts promoted with noble metals for production of hydrogen by methane steam reforming

The effect of noble metal addition on the catalytic properties of Co/Al2O3 was evaluated for the steam reforming of methane. Co/Al2O3 catalysts were prepared with addition of different noble metals (Pt, Pd, Ru and Ir 0.3 wt.%) by a wetness impregnation method and characterized by UV-vis spectroscopy, temperature programmed reduction (TPR) and temperature programmed oxidation (TPO) of the reduced catalysts. The UV-vis spectra of the samples indicate that, most likely, large amounts of the supported cobalt form Co species in which cobalt is in octahedral and tetrahedral symmetries. No peaks assigned to cobalt species from aluminate were found for the promoted and unpromoted cobalt catalysts. TPO analyses showed that the addition of the noble metals on the Co/Al2O3 catalyst leads to a more stable metallic state and less susceptible to the deactivation process during the reforming reaction. The Co/Al2O3 promoted with Pt showed higher stability and selectivity for H(2)production during the methane steam reforming. (C) 2007 Elsevier Ltd. All rights reserved.

Production of hydrogen by ethanol steam reforming on Co/Al2O3 catalysts: Effect of addition of small quantities of noble metals

The catalytic performance of Co/Al2O3 catalysts promoted with small amounts noble metals (Pt, Pd, Ru, Ir) for steam reforming of ethanol (SRE) has been investigated. The catalysts were characterized by the energy dispersive X-ray, X-ray diffraction, BET surface area, X-ray absorption fine structure and temperature reduction programmed techniques. The results showed that the promoting effect of noble metals included a marked decrease of the reduction temperatures of both Co3O4 and cobalt surface species interacting with the support due to the hydrogen spillover effect, leading to a significant increase of the reducibilities of the promoted catalysts. The better catalytic performance for the ethanol steam reforming at 400 degrees C was obtained for the CoRu/Al2O3 catalyst, which presented an effluent gaseous mixture with the highest H, selectivity and the reasonable low CO formation. (C) 2007 Published by Elsevier B.V.

Estudo das propriedades de revestimentos compósitos de níquel com Al2O3 e SiC

Neste trabalho foi avaliada a resistência à corrosão dos revestimentos compósitos de níquel, obtidos a partir de um banho de níquel químico (electroless) e um banho de níquel eletrolítico tipo Watts (com e sem tensoativo), caracterizando-os comparativamente em relação ao revestimento de níquel sem partículas. Os métodos utilizados para avaliação da resistência a corrosão foram: ensaio acelerado em névoa salina, voltametria cíclica, curva de polarização potenciodinâmica (em NaCl 0,6N) e dissolução anódica à corrente constante. Os revestimentos também foram avaliados com relação à resistência ao desgaste, rugosidade, e morfologia da camada. As partículas foram caracterizadas por difração de raio- X , dispersão granulométrica e potencial zeta. Nas condições estudadas os resultados mostraram que o revestimento compósito Ni-P-Al2O3 (Al2O3 - tamanho de grão ≅ 0,1 a 1,8µm) apresentou melhor resistência à corrosão que o revestimento de níquel químico sem incorporação de partículas (Ni-P) que por sua vez, apresentou resistência a corrosão superior ao compósito Ni-P-SiC no. 23 (SiC no. 23 - tamanho de grão ≅0,8 a 19,9µm). Já o eletrodepósito de níquel sem incorporação de partículas apresentou melhor resistência à corrosão que os revestimentos compósitos. Entre estes o compósito Ni-Al2O3 apresentou resistência a corrosão superior ao compósito Ni-SiC no. 23 A adição do tensoativo lauril sulfato de sódio reduz a quantidade de partículas incorporadas no eletrodepósito, sendo este efeito mais acentuado para o SiC com maior granulometria. Para diferentes granulometrias de carbeto de silício (SiC no. 2 - tamanho de grão ≅0,3 a 6,2µm e SiC no. 23 - tamanho de grão ≅0,8 a 19,9µm), o revestimento compósito obtido com o SiC que possui menor granulometria, apresentou maior resistência à corrosão e maior resistência ao desgaste, indicando desta forma que o tamanho da partícula incorporada no depósito de níquel exerce grande influência sobre a resistência à corrosão do revestimento, bem como sobre a resistência ao desgaste.

Revestimentos a base de Ta/Al2O3 produzidos por aspersão térmica sobre substrato metálico

Metal substrates were coated by thermal spraying plasma torch, they were positioned at a distance of 4 and 5 cm from the nozzle exit of the plasma jet. The starting materials were used for deposition of tantalum oxide powder and aluminium. These two materials were mixed and ground into high-energy mill, then immersed in the torch for the production of alumina coating infused with particles of tantalum with nano and micrometric size. The spraying equipment used is a plasma torch arc not transferred, which operating in the range of 250 A and 80 V, was able to produce enough heat to ignite aluminothermic between Ta2O5 and aluminum. Upon reaching the plasma jet, the mixing powders react with the heat of the blaze, which provides sufficient energy for melting aluminum particles. This energy is transferred through mechanisms of self-propagating to the oxide, beginning a reduction reaction, which then hits on the surface of the substrate and forms a coating on which a composite is formed by a junction metal - ceramic (Ta +Al2O3). The phases and quantification of each were obtained respectively by X-ray diffraction and the Rietveld method. Morphology by scanning electron microscopy and chemical analysis by energy dispersive spectroscopy EDS. It was also performed measurements of the substrate roughness, Vickers microhardness measurements in sprays and determination of the electron temperature of the plasma jet by optical emission spectroscopy EEO. The results confirmed the expectation generated around the end product of spraying the mixture Ta2O5 + Al, both in the formation of nano-sized particles and in their final form. The electron excitation temperature was consistent with the purpose of work, in addition, the thermodynamic temperature was efficient for the reduction process of Ta2O5. The electron excitation temperature showed values of 3000, 4500 and 8000 K for flows10, 20 and 30 l / min respectively, these values were taken at the nozzle exit of the plasma jet. The thermodynamic temperature around 1200 ° C, was effective in the reduction process of Ta2O5

Síntese e caracterização de catalisadores de LaNiO3 não suportados e suportados em Al2O3 e ZrO2 para a reforma a vapor do metano

Ionic oxides with ABO3 structure, where A represents a rare earth element or an alkaline metal and B is a transition metal from group VIII of the periodic table are potential catalysts for oxidation and good candidates for steam reforming reaction. Different methods have been considered for the synthesis of the oxide materials with perovskite structure to produce a high homogeneous material with low amount of impurities and low calcination temperatures. In the current work, oxides with the LaNiO3 formula had been synthesized using the method of the polymeric precursors. The thermal treatment of the materials took place at 300 ºC for 2h. The material supported in alumina and/or zirconia was calcined at 800 ºC temperature for 4h. The samples had been characterized by the following techniques: thermogravimetry; infrared spectroscopy; X-ray diffraction; specific surface area; distribution of particle size; scanning electron microscopy and thermo-programmed reduction. The steam reforming reaction was carried out in a pilot plant using reducing atmosphere in the reactor with a mixture of 10% H2-Argon, a mass about 5g of catalyst, flowing at 50 mL.min-1. The temperature range used was 50 - 1000 oC with a heating rate of 10 oC.min-1. A thermal conductivity detector was used to analyze the gas after the water trapping, in order to permit to quantify the consumption of hydrogen for the lanthanum nickelates (LaNiO3). The results showed that lanthanum nickelate were more efficient when supported in alumina than when supported in zirconia. It was observed that the methane conversion was approximately 100% and the selectivity to hydrogen was about 70%. In all cases were verified low selectivity to CO and CO2

Obtenção de compósitos cerâmicos baseados em Al2O3/TiC através dos precursores poliméricos

The obtaining of ceramic materials from polymeric precursors is subject of numerous studies due to lower energy costs compared to conventional processing. The aim of this study is to investigate and improve the mechanism for obtaining ceramic matrix composite (CMC) based on SiOC/Al2O3/TiC by pyrolysis of polysiloxane in the presence of an active filler and inert filler in the pyrolysis temperature lower than the usually adopted for this technique, with greater strength. It also investigates the influence of pyrolysis temperature, the content of Alas active filler, the presence of infiltrating agents (Al, glass and polymer) after pyrolysis, temperature and infiltration time on some physical and mechanical properties. Alumina is used as inert filler and Al and Ti as active filler in the pyrolysis. Aluminum, glass and polysiloxane are used as agents infiltrating the post-pyrolysis. The results are analyzed with respect to porosity and bulk density by the Archimedes method, the presence of crystalline phases by X-ray diffraction (XRD) and microstructure by scanning electron microscopy (SEM). The ceramic pyrolyzed between 850 °C 1400 °C contain porosity 15% to 33%, density 2.34 g/cm3 and flexural strength at 4 points from 30 to 42 MPa. The microstructure features are porous, with an array of Al2O3 reinforced by TiC particles and AlTi3. The infiltration post-pyrolysis reveals decrease in porosity and increase density and strength. The composites have potential applications where thermal stability is the main requirement

Growth of Al2O3 thin film by oxidation of resistively evaporated Al on top of SnO2, and electrical properties of the heterojunction SnO2/Al2O3

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Preparation of Al2TiO5-Al2O3 and Al2TiO5-Al2O3-TiO2 Ceramics by High-Energy Ball Milling and Sintering

The present work reports on the preparation of Al2O3-TiO2 ceramics by high-energy ball milling and sintering, varying the molar fraction in 1:1 and 3:1. The powder mixtures were processed in a planetary Fritsch P-5 ball mill using silicon nitride balls (10 mm diameter) and vials (225 mL), rotary speed of 250 rpm and a ball-to-powder weight ratio of 5:1. Samples were collected into the vial after different milling times. The milled powders were uniaxially compacted and sintered at 1300 and 1500 degrees C for 4h. The milled and sintered materials were characterized by X-ray diffraction and electron scanning microscopy (SEM). Results indicated that the intensity of Al2O3 and TiO2 peaks were reduced for longer milling times, suggesting that nanosized particles can be achieved. The densification of Al2O3-TiO2 ceramics was higher than 98% over the relative density in samples sintered at 1500 degrees C for 4h, which presented the formation of Al2TiO5.

Obtenção de biodiesel através da transesterificação do óleo de farelo de arroz utilizando KI/Al2O3

This study proposes to find a biodiesel through transesterification of rice bran oil with KI/Al2O3 checking the influence of two types of alumina (Amorphous and Crystalline) for conversion into methyl esters. The catalyst was synthesized by the wet impregnation method. Adding 30 mL of 35% KI(aq.) in 10 g of alumina, under stirring at 80 °C for 3 hours. The reaction conditions used in this study were optimized, with a molar ratio methanol:oil of 15:1, 8 h of reaction time and reflux temperature. The catalyst amount was varied in the range of 1 to 5 % wt. The solid catalysts materials were analyzed by: x-ray diffraction (XRD), thermogravimetry (TG), N2 adsorption/desorption, scanning electron microscopy (SEM) and basicity, for the identification of its structure and composition, verifying the presence of basic sites. The results showed that Al2O3(A) presents an amorphous structure, high surface area and a better catalytic activity, in relation to the catalyst synthesized with Al2O3(C) support that proved to have a more crystalline structure, having as well, a lesser surface area, enabling difficulties for the incorporation of active sites. The obtained biodiesel with 5% wt. KI/Al2O3(A) presented physicochemical properties within the standards specified by the Resolution No 7/2008 ANP and obtained the best reaction yield with 95.2%, according to quantitative measurement from the TG, which showed 96.2% conversion into methyl esters. It was furthermore found that with the increasing amount of the quantity of the catalyst in the reaction, there was also an increase in the ester content obtained. The specific mass and the kinematic viscosity were reduced with the increase of the amount of quantity of the catalyst, indicating an increase in the conversion of triglycerides

Eficiência do processo de obtenção do biodiesel de girassol usando o catalisador KNO3/Al2O3

It is known that the head office world energetics is leaning in the fossil fuels. However, the world panorama is changing quickly, for linked reasons to three of the humanity's great concerns in that century beginning: environment, global economy and energy. The biodiesel production is based on the transesterificação of vegetable oils or animal fats, using catalysts homogeneous or heterogeneous. The process of heterogeneous transesterificação presents lower conversions in comparison with the homogeneous, however, it doesn't present corrosion problems and it reduces to the occurrence of parallel reactions as saponification. In this sense, this work has for purpose the synthesis of a heterogeneous catalyst, KNO3/Al2O3, that soon afterwards was used in the reaction of transesterificação of the oil of the Helianthus annuus L. (sunflower). The solid materials (it supports and catalyst) they were analyzed by diffraction of ray-X (XRD) and electronic microscope of sweeping (MEV). After the analysis of Al2O3, a structure monophase amorphous tetragonal was verified, with characteristic patterns of that material, what could not be visualized in the difratograma of the catalyst. The biodiesel obtained with 4% wt. of KNO3/Al2O3 it was what obtained a better cinematic viscosity 8,3 mm2/s, comparing with the norms of ANP, and it also presented the best conversion tax in ethyl ésteres, in accordance with the quantitative measure starting from TG, that was of 60%. While the biodiesel with 6% wt. and with 8% wt. of KNO3/Al2O3 it was it that no transesterificou, because it was observed in the analysis termogravimétrica of those two materials, a single thermal event, that it corresponds the decomposition or volatilization of the triglycerides

Structural characterization of phase transition of Al2O3 nanopowders obtained by polymeric precursor method

Nanocrystalline Al(2)O(3)powders have been synthesized by the polymeric precursor method. A study of the evolution of crystalline phases of obtained powders was accomplished through X-ray diffraction, micro-Raman spectroscopy and refinement of the structures through the Rietveld method. The results obtained allow the identification of three steps on the gamma-Al2O3 to alpha-Al2O3 phase transition. The single-phase alpha-Al2O3 Powder was obtained after heat-treatment at 1050 degrees C for 2 h. A study of the morphology of the particles was accomplished through measures of crystallite size, specific surface area and transmission electronic microscopy. The particle size is closely related to gamma-Al2O3 to alpha-Al2O3 phase transition. (c) 2007 Elsevier B.V. All rights reserved.

Compósitos de Al2O3/ZrO2 recobertos com hidroxiapatita dopada com íons Ag

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

Si3N4 ceramic cutting tool sintered with CeO2 and Al2O3 additives with AlCrN coating

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

Structural and spectroscopic analysis of gamma-Al2O3 to alpha-Al2O3-CoAl2O4 phase transition

Co-doped alumina powders were synthesized by means of the polymeric precursor method to obtain ceramic pigments. The effect of different contents of Co2+ on phase transition gamma to alpha-Al2O3 and appearing of CoAl2O4 spinel were studied by means of X-ray diffraction. A partial phase diagram of the system CoAl2O3 was proposed from these data by means of determination of the percentages of these phases according to the calcining temperature. Critical particle size to phase transition was determined by means of calculations of crystallite size and determination of superficial area through the BET method. UV-vis spectroscopy of the samples allow to compare the band shift with the phase transition. Besides, a study of thermal stability and intensity of the blue coloration of the synthesized powders with the presence of cobalt in relation to the calcining temperature was accomplished and compared to the phase transition. The results show that the higher blue color intensity was obtained for the powders with Co-doped gamma-Al2O3 closest of phase transition to alpha-Al2O3 + CoAl2O4. (c) 2005 Elsevier B.V. All rights reserved.