Transformações mineralógicas causadas por queima são estudadas pelo método semiquantitativo de difração de raios X. O desaparecimento do mineral original e o neomineral foram avaliados quantitativamente. Além disso, a quantificação de fase não cristalina foi alcançada acima de 1000 ºC, sendo usado quartzo como padrão. Este estudo descreve um calcário branco argentino comercial, o qual é submetido a uma queima cerâmica tradicional, com base na sua importância tecnológica, ele atua como modelo para outras argilas com base cerâmica. Os materiais foram submetidos a tratamento térmico entre 700 ºC e 1000 ºC. Uma caracterização preliminar da sinterização foi avaliar a evolução da retração e da porosidade. Análise simultânea termogravimétrica e térmica diferencial foi realizada para determinar as temperaturas em que ocorrem mudanças químicas. Finalmente, foi feita uma analise quantitativa com base no refinamento Rietveld dos padrões de difração de raios X, para caracterizar as fases cristalinas na argila e nos materiais obtidos após os tratamentos térmicos. As reações químicas que ocorrem são propostas. As fases identificadas após a queima na temperatura tradicional de trabalho (1040 ºC) são quartzo, plagioclásio, e o espinélio tipo aluminio-silicato, juntamente com metacaulim não detetado e algum teor de fase vítrea. Foi também determinada gehlenita em temperaturas intermediarias (900 ºC). A presença e a decomposição de carbonatos (calcita e dolomita) foram também avaliadas e demonstrada sua atuação nas características da sinterização.

Mineralogical transformations caused by firing are usually studied by XRD methods only semi-quantitatively. In this work the original mineral disappearance and the neo-mineralization were evaluated quantitatively. Furthermore an indirect non crystalline phase quantification was performed under 1100 ºC was also carried out using the quartz content as internal standard. This study specifically discusses the behavior of an Argentinean white calcareous earthenware commercial when subjected to traditional ceramic firing, besides the technological importance of this particular material, it acts as a model for other clay based ceramic materials. Materials were subjected to thermal treatments between 700 ºC and 1100 ºC. A preliminary sintering characterization was carried out by contraction and porosity evolution. Simultaneous thermogravimetric and differential thermal analysis (TG-DTA) was carried out to elucidate the actual temperature at which the chemical changes occur. Finally, a quantitative analysis based on the Rietveld refinement of the X-ray diffraction patterns was performed to characterize the crystalline phases present in both the clay and in the materials obtained after different thermal treatments. The actual chemical reactions are proposed. The phases identified after firing at traditional working temperature (1040 ºC) are quartz, plagioclase, and the Spinel type alumino-silicate, accompanied by the non-diffracting un-reacted metakaolin and some amount of amorphous glassy phase. At intermediate temperatures (900 ºC) the presence of gehlenite was also detected. The carbonates (calcite and dolomite) presence and decomposition were also evaluated and demonstrated to determine the sintering characteristics of this material.

The metals of the group IV B (Ti, Zr, Hf) present a series of carbides and oxicarbides with scientific and technological interest. Many of these compounds belong to the subsystem "MO - MC" of the pseudoternary "MO - MN - MC" system (where M = Ti, Zr or Hf). In this work carboreduction reactions of TiO2 and ZrO2 were performed in argon atmosphere, using temperatures from 1250° to 1650° and reaction times of 120 min. The oxicarbides obtained were in the range TiC0.16O0.84 to TiC0.73O0.27 and ZrC0.46O0.54 to ZrC0.90O0.10. respectively. The reaction products were characterized by X-ray diffraction (XRD), with the calculation of their cell constants by means of the Rietveld method. Scanning Electron Microscopy (SEM) was used in the characterization of powdered materials. Additionally, the carborreduction reaction was followed by weight loss.

Zirconium compounds are of great interest for ceramic application due to their excellent thermal and mechanical properties. Zirconium phases of the system Zr-O-C-N were obtained using carbonitriding reactions of zircon mineral (ZrO2.SiO2), under different reaction conditions. The reaction products were studied by X-ray diffraction (XRD) using the Rietveld method. Silicon was employed as internal standard. Zirconium compounds formed were m-ZrO2 (monoclinic), beta"-zirconium oxynitride and a cubic Zr(C,N,O) phase whose lattice parameter a o depends on the composition. The crystallite sizes of the three zirconium phases were determined also by XRD. The minority phases present are the ones of the Si-O-N-C system. The reaction conditions employed allows to obtain reaction products with low or without silicon content.