Preparação de espumas cerâmicas de 'TIO IND. 2' a partir do processo sol-emulsão-gel
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Data
2012-09-12
Autores
Silva, Renata Ferreira Lins da [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
O primeiro objetivo deste trabalho foi investigar os fenômenos de agregação e de gelatinização das suspensões de TiO2 obtidos através do processo sol-gel. Estas suspensões foram preparadas a partir da hidrólise do tetraisopropóxido de titânio Ti(OPri)4 em solução aquosa de ácido para-toluenossulfônico (PTSH). A evolução do tamanho das nanopartículas e o mecanismo de agregação que ocorre nos momentos iniciais da reação foram analisados através da técnica de espalhamento de raios X à baixo ângulo (SAXS). Os resultados de SAXS mostraram que as partículas de TiO2 se agregam irreversivelmente formando partículas de tamanhos maiores nos momentos iniciais da reação. Também foram realizadas medidas de SAXS e reológicas para a suspensão com razão molar [H2O/Ti] = 2,3 e [PTSH/Ti] = 0,34, preparada com diferentes tempos de envelhecimento a 60ºC (0, 12 e 21 horas). Esse estudo revelou a possibilidade de aumentar tanto o tamanho das partículas do sol quanto a temperatura de transição sol-gel com o aumento do tempo de envelhecimento. Os valores de dimensões fractais (Df), obtidos pela técnica de SAXS, indicaram que a cinética de transição sol-gel é consistente com um processo de agregação cluster-cluster limitado por difusão (DLCCA). O segundo objetivo deste trabalho foi demonstrar a viabilidade de obter espumas cerâmicas a partir de emulsões formadas pela mistura dos sóis de TiO2 com o surfactante aniônico Dodecil Sulfato de Sódio (SDS) e não-iônico Pluronic F127 (P-127), juntamente com o óleo miristato de isopropila (MI). Nesta etapa, procurou-se avaliar o papel da natureza iônica e não-iônica dos surfactantes e da razão em massa/massa (m/m) de surfactante e da fase apolar (óleo) nas propriedades estruturais das espumas cerâmicas. O comportamento térmico, as fases cristalinas e a superfície das...
The first aim of this study was to investigate the aggregation and gelatinization of TiO2 suspensions obtained by the sol-gel process. The TiO2 suspensions were achieved by hydrolysis of the titanium tetraisopropoxide Ti(OPri)4 in para-toluene sulfonic acid (PTSH) aqueous solution. The evolution of nanoparticles size and the aggregation mechanism that occurs during the first synthesis step were analyzed by using small-angle X ray scattering (SAXS) technique. SAXS results have shown that TiO2 particles form irreversible aggregates giving rise to large particles during the first synthesis step. SAXS and rheological measurements were also carried out for the suspension prepared at H2O/Ti = 2.3 and PTSH/Ti = 0.34 molar ratios aged at 60 oC for different aging times (0, 12 and 21 h). This study has revealed the possibility to increase both the sol-gel phase transition temperature as well as the particle size by increasing the aging time. The fractal dimensionality (Df) values, estimated from the SAXS analyzes, indicated that particles aggregation is characteristic of a diffusion limited cluster-cluster aggregation (DLCCA) kinetic process. Another aim of this work was to obtain ceramic foams from emulsions formed by the mixture of TiO2 suspensions, the anionic Sodium Dodecyl Sulfate (SDS),or the non-ionic Pluronic F- 127 surfactants and the isopropyl myristate (MI) oil. This study was important to evaluate the role of the ionic or non-ionic nature of these two surfactants on the structural properties of the ceramic foam by varying the weight/weight (w/w) ratio of surfactant and non-polar phase (oil). The thermal behavior, crystalline structure and surface of the ceramic foams were investigated through thermogravimentry (TG), X ray diffraction (DRX), and X-ray photoelectron spectroscopy (XPS) techniques, respectively. These foams... (Complete abstract click electronic access below)
The first aim of this study was to investigate the aggregation and gelatinization of TiO2 suspensions obtained by the sol-gel process. The TiO2 suspensions were achieved by hydrolysis of the titanium tetraisopropoxide Ti(OPri)4 in para-toluene sulfonic acid (PTSH) aqueous solution. The evolution of nanoparticles size and the aggregation mechanism that occurs during the first synthesis step were analyzed by using small-angle X ray scattering (SAXS) technique. SAXS results have shown that TiO2 particles form irreversible aggregates giving rise to large particles during the first synthesis step. SAXS and rheological measurements were also carried out for the suspension prepared at H2O/Ti = 2.3 and PTSH/Ti = 0.34 molar ratios aged at 60 oC for different aging times (0, 12 and 21 h). This study has revealed the possibility to increase both the sol-gel phase transition temperature as well as the particle size by increasing the aging time. The fractal dimensionality (Df) values, estimated from the SAXS analyzes, indicated that particles aggregation is characteristic of a diffusion limited cluster-cluster aggregation (DLCCA) kinetic process. Another aim of this work was to obtain ceramic foams from emulsions formed by the mixture of TiO2 suspensions, the anionic Sodium Dodecyl Sulfate (SDS),or the non-ionic Pluronic F- 127 surfactants and the isopropyl myristate (MI) oil. This study was important to evaluate the role of the ionic or non-ionic nature of these two surfactants on the structural properties of the ceramic foam by varying the weight/weight (w/w) ratio of surfactant and non-polar phase (oil). The thermal behavior, crystalline structure and surface of the ceramic foams were investigated through thermogravimentry (TG), X ray diffraction (DRX), and X-ray photoelectron spectroscopy (XPS) techniques, respectively. These foams... (Complete abstract click electronic access below)
Descrição
Palavras-chave
Físico-química, Agentes ativos de superficies, Dióxido de titânio, Surface active agents, Titanium dioxide
Como citar
SILVA, Renata Ferreira Lins da. Preparação de espumas cerâmicas de 'TIO IND. 2' a partir do processo sol-emulsão-gel. 2012. 122 f. Tese (doutorado) - Universidade Estadual Paulista, Instituto de Química de Araraquara, 2012.