D. M. A. Melo

Evaluation of CoAl2O4 as ceramic pigments

Abstract CoAl 2 O 4 powder was obtained from a mixture of Co and Al oxalates at a ratio of 1:8 (Co:Al). The material was calcinated at different temperatures, established from TG data, and characterized using FTIR spectroscopy, X-ray diffraction, BET surface area, and thermal analysis. The dyeing characteristics of CoAl 2 O 4 were established by coating ceramic substrates with different concentrations of the powder.

Characterization and comparative study of pyrolysis kinetics of the rice husk and the elephant grass

A comparative evaluation of different biomasses allows the choice that presents the best potential as fuel for energy production. The knowledge of the thermal and kinetics parameters of the biomass in the process of thermal conversion is fundamental as their chemical and physical characterization. Various methodologies have been developed for the determination of kinetic parameters as apparent activation energy and reaction order from the thermogravimetric analysis. In this work, the apparent activation energy needed to break the bonds of hemicelluloses and cellulose of rice husk and elephant grass during the thermal conversion was evaluated according to the kinetics models of Flynn and Wall and Model Free Kinetics developed by Vyazovkin. The biomass elephant grass and rice husk were characterized for moisture, ash and volatile matter by ASTM E871, ASTM E1755, ASTM E872, respectively, and fixed carbon by difference. The percentage of carbon, hydrogen, nitrogen, and oxygen were determined by ultimate analysis. The elephant grass showed to be more suitable for production of bio-oil through pyrolysis due to the higher percentage of volatile, less ash content and less energy required to break the bonds of hemicellulose and cellulose than rice husk in the thermal conversion process.

Low-temperature synthesis of single-phase crystalline LaNiO3 perovskite via Pechini method

Abstract LaNiO 3 powders were prepared from polymeric precursors. The material was calcinated either under flowing oxygen or in air at temperatures ranging from 300 to 800 °C. The formation of new phases upon calcination was investigated using X-ray diffraction, thermal gravimetric analysis, Fourier-transform infrared spectroscopy and CHN analysis. The results revealed the formation of a single-phase powder having the perovskite structure at temperatures as low as 600 °C. The atmosphere did not significantly affect the final product.

Effect of the Order and Disorder of BaMoO4 Powders in Photoluminescent Properties

The study of the photoluminescent properties affected by order and disorder of the BaMoO4 powders is the principal objective in this work. BaMoO4 compounds were prepared using soft chemical process called Complex Polymerization Method. In this work, different deagglomeration types and different heating rates were used to promote different disorder degrees. Scheelite type phase (BaMoO4) was determined by X-ray Diffraction (XRD), Fourier Transformed Infra-Red (FTIR) and Raman spectroscopy after heat treating the sample at 400°C. The room temperature luminescence spectra revealed an intense single-emission band in the visible region. Based on XRD and Raman data it was observed that the transition between the completely disordered structure to completely ordered structure is a good condition for photoluminescence (PL) emission. The best PL emission is obtained when the material possesses short range disorder, i.e., is periodically ordered (XRD), but some disorder as measured by Raman spectroscopy. The excellent optical properties observed for disordered BaMoO4 suggested that this material is a highly promising candidate for optical applications.

Pechini synthesis and microstructure of nickel-doped copper chromites

Spinel-type solid solutions were synthesized by the Pechini method and calcined between 500 and 900 °C for 4 hours and at 900 °C for 8 hours to produce ceramic pigments. The resulting powders were characterized by thermogravimetric analysis, Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), particle size analysis and BET surface area measurements. The formation of spinel took place upon calcination at 700 °C. IR spectroscopy revealed the presence of n1 and n2 bands, typical of spinel structures, broadened by the presence of more than one cationic species in the structure. The specific area of the resulting powder decreased from 24.7 to 1.4 m2 g-1 as the calcination temperature increased from 700 to 900 °C. Microstructural analyses revealed the presence of crystalline spinel as the only phase present in powders calcined at 900 °C. Colorimetric analyses using L*a*b* coordinates and UV-visible spectroscopy revealed that the pigment was predominantly black.

Synthesis and characterization of La1-xSr xMnO3±δ powders obtained by the polymeric precursor route

Polycrystalline strontium-doped lanthanum manganite (LSM) powders with 0.15, 0.22, and 0.30 mol % Sr were synthesized by the polymeric precursor route using a molar ratio of 3:1 citric acid and metal cations. The powders were characterized by Fourier transform infrared spectroscopy, thermal analysis, high-temperature X-ray diffraction to determine the crystalline perovskite phase and crystallite sizes, scanning electron microscopy for the morphological analysis, nitrogen adsorption to determine the specific surface area, and laser scattering to evaluate the particle size distribution. The LSM perovskite-type oxides containing intermediate 0.22 mol % Sr were found to exhibit a tendency to decrease in crystallite size and increase in specific surface area and, when calcined at 700-900 oC exhibited a pure phase of perovskite, had a crystallite size of about 17-20 nm and a specific surface area for 900 oC of 34.3 m2.g-1.

Determination of Total Acid in Palygorskite Chemically Modified by N-Butylamine Thermodesorption

The acid properties of palygorskite clay (R1) were studied using n-butylamine as probe molecule. A comparison was made of these properties in palygorskite clay (R1), in an acidified palygorskite (R2) and in acid palygorskite loaded with 2% of lanthanum (R3). The total acid properties were determined by FTIR (Fourier Transform Infrared) and TG-DTA (thermogravimetry). The acidity increased as follows: R3>R2>R1. The acid strength sites were classified as physisorbed, weak, medium and strong. The acid treatment did not change the site distribution, apparently only removing channel impurities. The introduction of lanthanum created many more acid sites and increased the specific area. Both weak and strong sites, which increased significantly, were considered new active acid sites produced by the lanthanum.

Synthesis of high value-added zeolitic materials using glass powder residue as a silica source

In this work, zeolite A was obtained using alkaline fusion followed by a hydrothermal treatment of glass powder residue derived from the manufacturing of glass. The following parameters were evaluated: leaching of the stock material (silica source), mineralizing agent, alumina source, and the alkaline fusion and crystallization temperatures. The synthesized materials were characterized by chemical analysis using energy dispersive X-ray analysis (EDX), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD and SEM results showed that zeolite A was obtained under almost all of the evaluated parameters. The use of pseudoboehmite as an aluminum source led to the formation of zeolite X as a secondary phase and a change in the temperature of fusion, which at 500 °C, there was formation of zeolite A, hydrated sodalite and zeolite X.

Caracterização e uso de xisto para adsorção de chumbo (II) em solução

Existe um grande interesse no uso de materiais de baixo custo para remocao de metais pesados em aguas residuais. Novas tecnicas de processamento e adsorventes incluindo argilas, resinas sinteticas, turfa e quitosana tem sido estudados objetivando substituir o carvao ativado. No presente trabalho, xisto retortado (XR), um rejeito solido da transformacao termica do xisto oleigeno, foi caracterizado com o objetivo de utiliza-lo como adsorventes para remocao de metais pesados. O aproveitamento desse rejeito e de grande interesse, uma vez que o Brasil possui a segunda maior reserva mundial de xisto oleigeno. Os rejeitos foram caracterizados por diferentes tecnicas de caracterizacao, incluindo tamanho de particula, analise termogravimetrica, fluorescencia de raios X, espectroscopia na regiao do infravermelho, difracao de raios X, e microscopia eletronica de varredura-EDS. As caracteristicas dos pos foram adequadas para os experimentos de adsorcao. Estudos de adsorcao de Pb2+ pelo metodo de banho finito foram realizados. A remocao do Pb2+ foi superior a 85%.

Kinetic Parameters of Polyethylene Degradation by the Natural Zeolite Chabazite

High-density polyethylene (PE) was subjected to thermal degradation alone and in the presence of an ammonium-exchanged zeolite chabazite (CHA/PE). The processes were carried out in a reactor connected online to a gas chromatograph/mass spectrometer in order to analyse the evolved products. Polymer degradation was also evaluated by thermogravimetry, from room temperature up to 800°C, under a dynamic nitrogen atmosphere, with multiple heating rates. From the TG curves, the activation energy relating to the degradation process was calculated by using the Flynn and Wall multiple heating rate kinetic model for pure PE and for CHA/PE. The exchanged chabazite exhibited good selectivity for the catalytic degradation of PE to low molecular mass hydrocarbons.