Preparação e caracterização de pós cerâmicos de Ca(Mo,W)O4 obtidos pelo método dos precursores poliméricos
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Data
2007-03-09
Autores
Campos, Adaci Batista [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
Os molibdatos e tungstatos têm grande aplicação tecnológica devido principalmente às suas propriedades eletro ópticas e fotoluminescentes. Neste trabalho pós de molibdatos tungstatos de cálcio baseados na composição [Ca(Mo1-xWx)O4] , onde (x = 0,0; 0,2; 0,4; 0,6; 0,8, e 1,0) foram preparados e suas estruturas cristalinas identificadas. Uma conecção entre a propriedade luminescente e a desordem estrutural, na contribuição do espectro de luminescência foi realizada considerando os diferentes sistemas e as temperaturas de tratamento térmico. As propriedades estruturais e fotoluminescentes foram avaliadas tendo como referencial os compostos CaMoO4 e CaWO4. Esses sistemas foram sintetizados pelo método dos precursores poliméricos, o que possibilitou a obtenção da fase cristalina em temperaturas inferiores a 500°C. Os pós preparados por esse processo químico foram caracterizados utilizando as técnicas termogravimétricas/calorimetria TG/DSC, difração de raios X (DRX), Espectroscopia vibracional na região do infravermelho (IR), Raman, Espectroscopia na região do ultravioleta visível (UV-Vis), Fotoluminescência (FL), e Microscopia Eletrônica de Transmissão (MET). Os resultados da análise térmica TG/DSC mostraram que a temperatura de cristalização se desloca para valores mais elevados com o aumento do W. Nos difratogramas de raios X, foi observada a formação da fase em todos os sistemas preparados a partir de 450°C. Por meio da espectroscopia Raman observou se que o W induz a desordem na estrutura. A emissão da fotoluminescência à temperatura ambiente com excitação de 350.7 nm foi observada em todas as amostras tratadas de 450 até 700°C. Um mecanismo foi proposto para explicar e relacionar os resultados da FL em função das variações estruturais com a temperatura de tratamento das amostras.
The molybdates and tungstates have a great technologic potential mainly due to their electro optical and photoluminescent properties. In this work molybdate tungstate of calcium [Ca(Mo1-xWx)O4] ( x = 0,0; 0,2; 0,4; 0,6; 0,8, e 1,0) powders were prepared and their crystalline structure characterized. A connection between the luminescent properties and the crystalline structure disorder in the contribution of the luminescence spectra was discussed regarding to different amount and heat treatment temperatures. The structural and photoluminescent properties were evaluated based on CaMoO4 and CaWO4 compounds. These systems were synthesized by the polymeric precursor method which made possible the obtaining of the phase at temperatures lower than 500°C. The prepared powders by this method were characterized by thermogravimetric and differential scanning calorimetry technique (TG/DSC) X ray diffraction (XRD), Infra red (IR), Raman, UV-Visible spectroscopy, photoluminescence (PL) and finally by transmission electronic microscopy (TEM). In addition, the thermal analysis results showed that the temperature of crystallization shifts to higher values when the W concentration is increased the phase is obtained in all systems up to 450°C as evidenced by the XRD results. By the Raman results, it was observed that W promote short range disorder the PL measurements accomplished at room temperature and 350.7 were observed in all samples treated from 450 to 700°C. A mechanism was proposed to explain the results in function of the structural charges as the temperature treatment increase.
The molybdates and tungstates have a great technologic potential mainly due to their electro optical and photoluminescent properties. In this work molybdate tungstate of calcium [Ca(Mo1-xWx)O4] ( x = 0,0; 0,2; 0,4; 0,6; 0,8, e 1,0) powders were prepared and their crystalline structure characterized. A connection between the luminescent properties and the crystalline structure disorder in the contribution of the luminescence spectra was discussed regarding to different amount and heat treatment temperatures. The structural and photoluminescent properties were evaluated based on CaMoO4 and CaWO4 compounds. These systems were synthesized by the polymeric precursor method which made possible the obtaining of the phase at temperatures lower than 500°C. The prepared powders by this method were characterized by thermogravimetric and differential scanning calorimetry technique (TG/DSC) X ray diffraction (XRD), Infra red (IR), Raman, UV-Visible spectroscopy, photoluminescence (PL) and finally by transmission electronic microscopy (TEM). In addition, the thermal analysis results showed that the temperature of crystallization shifts to higher values when the W concentration is increased the phase is obtained in all systems up to 450°C as evidenced by the XRD results. By the Raman results, it was observed that W promote short range disorder the PL measurements accomplished at room temperature and 350.7 were observed in all samples treated from 450 to 700°C. A mechanism was proposed to explain the results in function of the structural charges as the temperature treatment increase.
Descrição
Palavras-chave
Luminescencia - Materiais, Molibdato de cálcio, Tungstato de cálcio
Como citar
CAMPOS, Adaci Batista. Preparação e caracterização de pós cerâmicos de Ca(Mo,W)O4 obtidos pelo método dos precursores poliméricos. 2007. 121 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química, 2007.