R. Medeiros

Síntese de MgAl2O4 por combustão assistida por micro-ondas: influência dos parâmetros de síntese na formação e na estrutura cristalina

In recent years, microwave combustion has received special attention because it is a quick, low cost and easy method that produces materials with good chemical homogeneity. Magnesium aluminate (MgAl2O4) is one of the most well-known ceramic materials because of their excellent properties, such as high melting point, high mechanical strength at high temperatures, good resistance to thermal shock, and resistance to acids and bases. The purpose of this study was to evaluate the influence of three parameters on the formation and crystal structure of MgAl2O4: (1) fuel/oxidizer ratio (Rco), (2) calcination temperature (Tcal), and (3) microwave power (Pmic). To carry out the combustion reaction, three different power levels (450, 675 and 900 W) and three fuel/oxidant ratio (0.8:1, 1:1 and 1.2:1) were used. The materials were calcined at three different temperatures (700, 800 and 900 °C) and characterized by X-ray diffraction and scanning electron microscopy. A factorial design 23 was used to evaluate the influence of the three parameters on the crystallinity and crystallite size of the MgAl2O4 powders obtained. The results show that for MgAl2O4 synthesized with Rco larger than 1:1 and Pmic lower than 675 W small crystallite sizes between 10 and 20 nm were obtained when calcined at 700 and 800 oC. Regarding the degree of crystallinity, only the Tcal has significant influence.

Preparação de pigmentos de aluminatos de cobalto para aplicação em vidrados cerâmicos

Inorganic pigments are the most widely used in industries, since they have greater chemical and thermal stability and can be produced with high purity and uniformity. These characteristics led to the development of different intense, stable and suitable colors for use as pigments. This paper aims to synthesize ceramic materials with spinel structure for use as ceramic pigment and apply them in ceramic frits. The synthesis procedure was performed by gelatin method and the powders were studied in terms of evolution of crystalline phases by X-ray diffraction (XRD), refinement of the structures through the Rietveld method, spectroscopy in the infrared region, scanning electron microscopy, UV-visible spectroscopy and colorimetric analysis. XRD patterns showed the characteristic reflections of the spinel structure. The average crystallite size and crystallinity increased with increasing calcination temperature. The color of pigments ranged from pale blue to blue violet.

Application of Design of Experiments to the Alkaline Treatment in Mordenite Zeolite: Influence on Si/Al Ratio

This paper presents the application of Design of Experiments (DOE) to an alkaline treatment in mordenite zeolite, in order to identify the optimum settings of the variables (temperature and concentration of NaOH) that promote greater desilication. Samples of commercial mordenite with Si / Al ratio = 9 have been treated with aqueuos NaOH solution of various concentration (0,1;0,5;1,0) and temperature (30,50,70°C). Statistical analysis was carried out based on a 22 factorial design with center point replicates. Seven experiments were executed and the data of Si/Al ratio obtained. The resulting samples were characterized by x-ray difraction (XRD) and energy dispersive x-ray (EDX), to identify the structures and crystalline phases, and to determine the percentages of silicon and aluminum, respectively. In all samples, a decrease in the Si / Al ratio was observed, keeping the crystalline structure. The treatment was most effective, especially, at high temperature and NaOH concentration (experiment 4). DOE was shown to be a powerful techinique for the study of the variables, allowing determining which variables and value ranges have more influence on response, enabling optimization.

Carreadores de oxigênio a base de Ni obtidos por diferentes métodos de síntese para aplicação no processo de reforma de metano com recirculação química

Oxygen carriers containing Ni, La, Al and Mg were synthesized successfully by microwave assisted self-combustion (N6C), microwave assisted self-combustion followed by wet impregnation (N6CI) and co-precipitation (N6CP), for their application in the production of hydrogen from methane chemical recirculation systems with CO2 capture. The materials were prepared following the general formula Nix/La2O3/Al2O3/MgO, where x = 60% by weight, the remainder being related to lanthanum (8%), aluminum (30%) and magnesium (2%) oxide. The obtained solids were characterized by X-ray diffraction), temperature programmed reduction and activity through methane reforming process with chemical recirculation. Reactivity tests were conducted at 900 oC, where the sample was initially subjected to 8 cycles of OSC (oxygen storage capacity), and finally were carried out two reaction cycles, with each cycle containing 15 pulses of methane and 15 pulses of oxygen. The results of the characterizations indicate that the methods used were appropriate for obtaining different materials with different properties. Generally, the carriers showed excellent percentage of CH4 conversion, and high hydrogen production. The carrier N6CP exhibited the best performance to syngas production with H2/CO ratio equal to 2 on the 15th pulse, as well as being appointed as being the most resistant to deactivation by coke and higher oxidation potential, consuming 100% O2 up to the 12th pulse. In turn, the N6CI lost enough performance throughout the cycles and the N6C formed larger amount of coke, revealing the peculiarities of the synthesis methods employed. According to the reaction products formed in the reduction step with CH4, it can be concluded that the most frequent reactions were catalytic cracking, reforming and combustion.

Synthesis Optimization of MCM-41 for CO2 Adsorption Using Simplex-centroid Design

There is a growing concern on the relationship between anthropogenic carbon dioxide and climate changes. A promising approach is the adsorption technology using mesoporous MCM-41 materials that can be easily synthesized to depict structures adequate to the flow of gas. The aim of this study was to improve the synthesis of MCM-41 using cationic surfactant mixtures and apply the resulting materials to CO2 adsorption. To that end, the simplex-centroid design was applied to optimize CO2 adsorption from seven mesoporous MCM-41 materials synthesized by the hydrothermal method using surfactants from hydrophobic chains of different sizes. The cationic surfactants used were tetradecyltrimetylammonium bromide, cetyltrimethylammonium bromide, trimethyloctadecylammonium bromide and their mixture at ratios of 1:1 and 1:1:1. The CO2 adsorption was investigated using thegravimetric method at 298 K and pressures up to 40 bar. The resulting materials, labelled C17, C19, C21, C17C19, C19C21, C17C21 and C17C19C21, were characterized by XRD, FTIR, TG and SEM and showed significant differences in structure as well as in the mass of CO2 adsorption. The response models showed that the best combination of the surfactants resulted from C17C19 sample, which presented synergistic interactions reaching the highest value of CO2 adsorption (0.62 g CO2/g adsorbent), compared to other samples.

Influência da adição de diatomita nas propriedades de pastas geopoliméricas: volume de filtrado, tempo de espessamento e resistência à compressão

Today, the diversity of available materials for use in engineering is very large, resulting in an increasing of specific materials for each type of application. The geopolymers have been studied for various decades. They are inorganic polymers that can provide cementing characteristics that emerge as a new class of high performance materials, capable of totally or partially replace the Portland cement in various applications. In this work, we studied the influence of the addition of diatomite on geopolymeric pastes based on metakaolin. The use of a new raw material abundant in nature and low value like the diatomite is another alternative as silica source to produce geopolymers. The diatomite is an amorphous silica and in this work it was used as an additive to improve some important properties in cement pastes based in geopolymers. The effect of adding of the diatomite the geopolymeric properties of the slurries was evaluated by comparing them with the properties of the geo-polymer based on metakaolin. To analyze the effects of diatomite concentrations in geopolymeric pastes, filtrate tests were performed, thickening time and compressive strength. Also presents the results of X-ray diffraction (XRD) and scanning electron microscopy (SEM) in order to gather information for a better understanding of the geopolymers cement microstructure. The results showed that the addition of diatomite changed drastically the microstructure and mechanical properties of geopolymer pastes. With the increasing in the concentration of diatomite, the filtrate volume decreases, independent on the temperature