Desenvolvimento de revestimentos híbridos do sistema siloxano-PMMA com aplicações anticorrosivas
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Data
2009-08-13
Autores
Schiavetto, Mateus Geraldo [UNESP]
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Editor
Universidade Estadual Paulista (Unesp)
Resumo
Revestimentos híbridos orgânico-inorgânicos preparados pelo processo sol-gel são considerados como uma boa alternativa para a passivação da superfície do aço, em substituição a compostos a base de cromo que apresentam problemas ambientais devido a sua alta toxicidade. Filmes híbridos a base de polisiloxano foram depositados em substratos de aço inoxidável 316L por dip-coating a partir de um sol preparado via catálise ácida com a hidrólise e co-policondensação do tetraetoxi silano (TEOS) e 3- metacriloxipropril trimetoxi silano (MPTS), seguido da polimerização radicalar dos grupos metacrilato. Características estruturais do híbrido a base de polisiloxano foram estudadas por ressonância magnética nuclear (RMN) de 13C e 29Si, espectroscopia de fotoelétrons induzida por raios X (XPS), calorimetria exploratória diferencial (DSC) e análise termogravimétrica (TG) em função da razão TEOS/MPTS, que variou entre 0 e 2. Os resultados de RMN e TG mostraram para a amostra com razão TEOS/MPTS = 2 um alto grau de polimerização e policondesação maior que 85% e uma estabilidade térmica de até 415 °C. Todos os filmes apresentaram boa adesão e a morfologia foi analisada por microscopia de força atômica (AFM) e microscopia óptica. A eficiência contra a corrosão dos filmes depositados sobre o aço inoxidável foi investigada por XPS, espectroscopia de impedância eletroquímica (EIS) e curvas potenciodinâmicas de polarização, após a imersão das amostras em meio salino neutro e acidificado. Os resultados mostraram uma eficiente proteção do aço no meio salino. Os efeitos anticorrosivos da incorporação de íons cério IV no híbrido a base de siloxano foram estudados por XPS e testes eletroquímicos que mostraram melhorias na proteção contra a corrosão dos filmes modificados por Ce4+.
Organic-inorganic hybrid coatings prepared by the sol-gel process are considered as a good alternative for the passivation of steel surfaces, substituting chromium compounds, which present environmental problems due to their high toxicity. Polysiloxane-based hybrid were deposited on 316L stainless steel substrates by dip-coating in a sol prepared by acid-catalyzed hydrolytic co-polycondensation of tetraethoxysilane (TEOS) and 3-methacryloxy propyltrimethoxysilane (MPTS), followed by radical polymerization of methacrylic moieties. Structural features of the polysiloxane-based hybrids were studied using 13C and 29Si nuclear magnetic resonance (NMR), X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), as a function of the TEOS/MPTS ratio, which ranged between 0 and 2. The NMR and TGA results indicated for the hybrid film with a TEOS/MPTS ratio of 2 a high degree of polymerization and polycondensation, of up to 85% and elevated thermal stability up to 415 °C. All films presented good adhesion and morphological analyses were performed by atomic force microscopy (AFM) and optical microscopy. The efficiency of the corrosion protection of hybrid-coated stainless steel was investigated by XPS, electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves, after immersion of the samples in a neutral saline and acidified environment. The results have shown an efficient protection of the steel surface in saline solution. The effects of the incorporation of cerium IV ions in polysiloxane-based hybrid were studied by XPS and electrochemical tests and the results indicate the improvement on the protective properties against corrosion of the films modified by Ce4+.
Organic-inorganic hybrid coatings prepared by the sol-gel process are considered as a good alternative for the passivation of steel surfaces, substituting chromium compounds, which present environmental problems due to their high toxicity. Polysiloxane-based hybrid were deposited on 316L stainless steel substrates by dip-coating in a sol prepared by acid-catalyzed hydrolytic co-polycondensation of tetraethoxysilane (TEOS) and 3-methacryloxy propyltrimethoxysilane (MPTS), followed by radical polymerization of methacrylic moieties. Structural features of the polysiloxane-based hybrids were studied using 13C and 29Si nuclear magnetic resonance (NMR), X-ray photoelectron spectroscopy (XPS), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), as a function of the TEOS/MPTS ratio, which ranged between 0 and 2. The NMR and TGA results indicated for the hybrid film with a TEOS/MPTS ratio of 2 a high degree of polymerization and polycondensation, of up to 85% and elevated thermal stability up to 415 °C. All films presented good adhesion and morphological analyses were performed by atomic force microscopy (AFM) and optical microscopy. The efficiency of the corrosion protection of hybrid-coated stainless steel was investigated by XPS, electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves, after immersion of the samples in a neutral saline and acidified environment. The results have shown an efficient protection of the steel surface in saline solution. The effects of the incorporation of cerium IV ions in polysiloxane-based hybrid were studied by XPS and electrochemical tests and the results indicate the improvement on the protective properties against corrosion of the films modified by Ce4+.
Descrição
Palavras-chave
Físico-química, Aço inoxidavel, Proteção contra a corrosão, Physical chemistry
Como citar
SCHIAVETTO, Mateus Geraldo. Desenvolvimento de revestimentos híbridos do sistema siloxano-PMMA com aplicações anticorrosivas. 2009. 109 f. Dissertação (mestrado) - Universidade Estadual Paulista, Instituto de Química, 2009.