Crystallization kinetics parameters of a stoichiometric glass with the composition Li1.5Al0.5Ge1.5(PO4)3 were investigated by subjecting parallelepipedonal samples (3 × 3 × 1.5 mm) to heat treatment in a differential scanning calorimeter at different heating rates (3, 5, 8 and 10 °C/min). The data were analyzed using Ligero's and Kissinger's methods to determine the activation energy (E) of crystallization, which yielded, respectively, E = 415 ± 37 kJ/mol and 378 ± 19 kJ/mol. Ligero's method was also employed to calculate the Avrami coefficient (n), which was found to be n = 3.0. A second set of samples were heat-treated in a tubular furnace at temperatures above the glass transition temperature, Tg, to induce crystallization. The X-ray diffraction analysis of these samples indicated the presence of LiGe2(PO4)3 which displays a NASICON-type structure. An analysis by optical microscopy revealed the presence of spheric crystals located primarily in the volume, in agreement with the crystallization mechanism predicted by the Avrami coefficient.

A fase Li1,5[Al0,5Ge1,5(PO4) 3] foi obtida via vitrocerâmica. Com o objetivo de se obter amostras com diferentes microestruturas, o vidro precursor do sistema Li2O-Al2O3-GeO2-P 2O5 foi submetido a tratamentos térmicos duplos. As amostras foram primeiramente nucleadas na temperatura de transição vítrea por diferentes tempos, e posteriormente cristalizados a 571 ºC. Foi também obtida uma vitrocerâmica por tratamento térmico simples a 618 ºC por 30 min. A caracterização por difração de raios X revela que a fase NASICON é a única fase presente após a cristalização. A caracterização elétrica foi realizada por espectroscopia de impedância, no intervalo de temperatura entre a ambiente e 120 ºC. Para algumas das amostras obtidas, os espectros de impedância mostram dois semicírculos evidenciando a presença de duas contribuições diferentes na condutividade elétrica, sempre próxima a 10-5 S/cm à temperatura ambiente. A energia de ativação de condução variou de H" 0,36 a 0,49 eV. A análise por microscopia eletrônica de varredura revela que tratamentos térmicos com tempos menores de nucleação geram amostras com grão maiores. Por outro lado, os resultados de condutividade elétrica indicam que as amostras com grãos maiores são mais condutoras.

The highly conductive Li1.5[Al0.5Ge1.5(PO4) 3] phase was obtained by a glass-ceramic route. To achieve different microstructures, the parent Li2O-Al2O3-GeO2-P 2O5 glass was submitted to double heat treatments. Glasses were first nucleated for different periods of time at the temperature of glass transition and then subsequently fully crystallized at 571 ºC. A glass-ceramic was also obtained by simple heat treatment at 618 ºC for 30 min. X-Ray diffraction analyses show that, after crystallization, the NASICON phase is the unique phase present. Electrical characterization was carried out by impedance spectroscopy, from room temperature to 120 ºC. Impedance complex plane plots of some samples reveal two semicircles, enabling the identification of two contributions to the total electrical conductivity, which was close to 10-5 S/cm at room temperature. Activation energy varied from 0.36 eV to 0.49 eV. Scanning electron microscopy analysis confirms that heat treatments with shorter nucleation time lead to samples with higher grain size. Moreover, electrical measurements show that samples with larger grain size present a higher ionic conductivity.

As linhas de pesquisa do grupo de cerâmicas eletrônicas do DEMa-UFSCar e sua estrutura de apoio são apresentadas juntamente com as teses e dissertações concluídas e os principais resultados obtidos nos últimos anos. Um pequeno resumo dos trabalhos em andamento também é apresentado.

The research lines of the group on electronic ceramics of DEMa-UFSCar and research facilities are presented together with theses, dissertations and the main research results that was done in the last years. A short summary of the nature of the work in progress is also presented.