Made available in DSpace on 2014-06-11T19:25:33Z (GMT). No. of bitstreams: 0 Previous issue date: 2006-12-14Bitstream added on 2014-06-13T18:53:40Z : No. of bitstreams: 1 sidel_sm_me_ilha.pdf: 1806167 bytes, checksum: 2a4e01caec0f051d6145b4716b656d11 (MD5) / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Neste trabalho foram estudados os vidros teluretos do sistema (20-x)Li2O-80TeO2- xWO3 com diferentes valores de x. Os resultados das medidas de DRX dos vidros como preparados confirmaram o comportamento amorfo das matrizes vitreas, e para os vidros tratados termicamente em diferentes temperaturas, acima de Tg, evidenciou-se a formacao das fases cristalinas durante o processo de cristalizacao. No vidro com x=0 (TL) foi observado a presenca das fases cristalinas -TeO2, -TeO2 e Li2Te2O5, e para os vidros com x=5 e 10 (TLW-5 e TLW-10) foi observado somente as duas primeiras fases cristalinas. Esse resultado sugere que o WO3 entra na estrutura como formador vitreo e inibe o crescimento da fase cristalina Li2Te2O5. Os parametros termicos, como a Tg, Tx e Tp, e o processo de cristalizacao dos vidros foram estudados por meio das medidas de DSC, e foram calculados os valores da energia de ativacao (E) e do parametro de Avrami. As curvas de DSC foram obtidas para taxas de aquecimento entre 2.5 e 12.5 K.mol-1 e particulas com tamanho 45-63 Êm. A energia de ativacao e o indice de Avrami foram calculados para cada fase cristalina e os picos de DSC foram ajustados utilizando funcoes gaussianas. As curvas de DSC das amostras tratadas termicamente apresentaram os picos de cristalizacao, referentes a cada fase cristalina, separadamente. Nas curvas de DSC do vidro TLW-5 foram observados tres picos de cristalizacao, embora as medidas de DRX tenham apresentado apenas duas fases cristalinas. Deste modo, a existencia deste terceiro pico de cristalizacao nas curvas de DSC do vidro TLW-5 confirmam o processo de transformacao da fase -TeO2 em -TeO2, conforme sugerido pelos dados de DRX e tambem pelos espectros de FT-IR. Nos espectros de infravermelho das tres matrizes vitreas foram verificadas as bandas de absorcao referentes as vibracoes das unidades tetragonais TeO4 e as bandas referentes as ligacoes W-O. / In this work the tellurite glasses of the system (20-x)Li2O-80TeO2-xWO3 with different x values were studied. The results of the XRD measurements for glasses as quenched confirmed the amorphous behavior of the glass matrix, and for the glasses thermally treated at different temperatures above Tg evidenced the phases crystalline formed during the crystallization process. In the glass with x=0 (TL) the presence of the -TeO2, -TeO2 and Li2Te2O5 crystalline phases was observed and for the glasses with x=5 and 10 (TLW-5 and TLW-10) were observed only the first two crystalline phases. This result suggests that WO3 enters in the structure as glass former and it inhibits the growth of the crystalline phase Li2Te2O5. The thermal parameters, as Tg, Tx and Tp, and the crystallization process of the glasses were studied through the DSC measurements, the values of the activation energy (E) and the Avrami s parameter were calculated. The DSC curves were obtained for heating rates between 2.5 and 12.5 K.mol-1, and 45-63 ìm particles size. The activation energy and the Avrami s parameter were calculated for each crystalline phase and the peaks of DSC were fitted using Gaussian functions. The DSC curves of the samples thermally treated showed the crystallization peaks, regarding each crystalline phase, separately. In the DSC curves of TLW- 5 glass three crystallization peaks were observed, although the measurements of XRD have presented only two crystalline phases. In this way the existence of this third crystallization peak in the DSC curves of the glass TLW-5 confirms the process of transformation of the phase -TeO2 in -TeO2, as suggested by XRD data and also for the FT-IR spectra. In the infrared spectra of the three glass matrix the absorption bands regarding the vibrations of the tetragonal units TeO4 and the bands regarding the connections W-O were observed.

Orientador: Keizo Yukimitu / Banca: Victor Ciro Solano Reynoso / Banca: Sandro Márcio Lima / Resumo: Neste trabalho foram estudados os vidros teluretos do sistema (20-x)Li2O-80TeO2- xWO3 com diferentes valores de x. Os resultados das medidas de DRX dos vidros como preparados confirmaram o comportamento amorfo das matrizes vitreas, e para os vidros tratados termicamente em diferentes temperaturas, acima de Tg, evidenciou-se a formacao das fases cristalinas durante o processo de cristalizacao. No vidro com x=0 (TL) foi observado a presenca das fases cristalinas -TeO2, -TeO2 e Li2Te2O5, e para os vidros com x=5 e 10 (TLW-5 e TLW-10) foi observado somente as duas primeiras fases cristalinas. Esse resultado sugere que o WO3 entra na estrutura como formador vitreo e inibe o crescimento da fase cristalina Li2Te2O5. Os parametros termicos, como a Tg, Tx e Tp, e o processo de cristalizacao dos vidros foram estudados por meio das medidas de DSC, e foram calculados os valores da energia de ativacao (E) e do parametro de Avrami. As curvas de DSC foram obtidas para taxas de aquecimento entre 2.5 e 12.5 K.mol-1 e particulas com tamanho 45-63 ƒÊm. A energia de ativacao e o indice de Avrami foram calculados para cada fase cristalina e os picos de DSC foram ajustados utilizando funcoes gaussianas. As curvas de DSC das amostras tratadas termicamente apresentaram os picos de cristalizacao, referentes a cada fase cristalina, separadamente. Nas curvas de DSC do vidro TLW-5 foram observados tres picos de cristalizacao, embora as medidas de DRX tenham apresentado apenas duas fases cristalinas. Deste modo, a existencia deste terceiro pico de cristalizacao nas curvas de DSC do vidro TLW-5 confirmam o processo de transformacao da fase -TeO2 em -TeO2, conforme sugerido pelos dados de DRX e tambem pelos espectros de FT-IR. Nos espectros de infravermelho das tres matrizes vitreas foram verificadas as bandas de absorcao referentes as vibracoes das unidades tetragonais TeO4 e as bandas referentes as ligacoes W-O. / Abstract: In this work the tellurite glasses of the system (20-x)Li2O-80TeO2-xWO3 with different x values were studied. The results of the XRD measurements for glasses as quenched confirmed the amorphous behavior of the glass matrix, and for the glasses thermally treated at different temperatures above Tg evidenced the phases crystalline formed during the crystallization process. In the glass with x=0 (TL) the presence of the -TeO2, -TeO2 and Li2Te2O5 crystalline phases was observed and for the glasses with x=5 and 10 (TLW-5 and TLW-10) were observed only the first two crystalline phases. This result suggests that WO3 enters in the structure as glass former and it inhibits the growth of the crystalline phase Li2Te2O5. The thermal parameters, as Tg, Tx and Tp, and the crystallization process of the glasses were studied through the DSC measurements, the values of the activation energy (E) and the Avrami’s parameter were calculated. The DSC curves were obtained for heating rates between 2.5 and 12.5 K.mol-1, and 45-63 ìm particles size. The activation energy and the Avrami’s parameter were calculated for each crystalline phase and the peaks of DSC were fitted using Gaussian functions. The DSC curves of the samples thermally treated showed the crystallization peaks, regarding each crystalline phase, separately. In the DSC curves of TLW- 5 glass three crystallization peaks were observed, although the measurements of XRD have presented only two crystalline phases. In this way the existence of this third crystallization peak in the DSC curves of the glass TLW-5 confirms the process of transformation of the phase -TeO2 in -TeO2, as suggested by XRD data and also for the FT-IR spectra. In the infrared spectra of the three glass matrix the absorption bands regarding the vibrations of the tetragonal units TeO4 and the bands regarding the connections W-O were observed. / Mestre