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Doctoral Thesis
DOI
https://doi.org/10.11606/T.76.2004.tde-11112013-150338
Document
Author
Full name
Carla Eiras
Institute/School/College
Knowledge Area
Date of Defense
Published
São Carlos, 2004
Supervisor
Committee
Goncalves, Debora (President)
Faria, Roberto Mendonça
Gobato, Yara Galvão
Nart, Francisco Carlos
Temperini, Marcia Laudelina Arruda
Title in Portuguese
Eletrossíntese e propriedades ópticas e morfológicas de filmes de poli-p-fenileno e derivados
Keywords in Portuguese
Copolímeros
Eletrossíntese
Poli-p-fenileno
Abstract in Portuguese
Nesta tese, estudamos a eletrossíntese de polímeros conjugados eletroluminescentes no azul. Filmes de poli(p-fenileno) (PPP), co-poli(p-fenileno-pirrol) (CPPI) e co-poli(p-fenileno-3-metiltiofeno) (CFMET) foram preparados por voltametria cíclica em eletrodos de vidro condutor (ITO) em uma solução não-aquosa de acetonitrila e perclorato de tetrabutilamônio contendo os monômeros e pares de co-monômeros a diferentes concentrações. Durante a síntese dos filmes de PPP, CPPI e CP3MET, a célula eletroquímica foi posicionada dentro de uma caixa seca contendo CaCl2 como agente secante e em atmosfera de N2(g) super-seco com o objetivo de reduzir a umidade do ar no meio de síntese. A baixa umidade do ar obtida durante as medidas permitiu o controle de parâmetros de crescimento dos filmes de PPP e de seus derivados (CPPI e CP3MET). A morfologia dos filmes foi correlacionada aos seus valores de espessura e de rugosidade obtidos por microscopia de força atômica (AFM). As propriedades ópticas dos filmes foram também investigadas por espectroscopia no UV-VSNIR em função do número de ciclos da varredura obtidos durante a eletrossíntese. As respostas eletroquímicas, dos filmes de FPP, CPPI e CP3MET foram obtidas por voltametria cíclica em uma solução livre de monômero. Estes filmes tiveram ainda a confirmação de suas estruturas químicas por meio de resultados obtidos por espectroscopia no infravermelho (FTIR) e por microespectroscopia e mapeamento Raman
Title in English
Electrosynthesis, optical and morphological properties of poly-p-phenylene films and derivatives
Keywords in English
Copolymers
Electrosynthesis
Poly-p-phenylene
Abstract in English
This work describes the electrochemical synthesis of poly(p-phenylene) (PPP), p-phenylene-pyrrole copolynier (GPPIC) and p-phenylene-3methylthiophene copolymer (CP3MET). The main interest in studying these materials comes from its blue-electroluminescent properties, which make them suitable for application in electroluminescent devices. The polymerization was carried out using cyclic voltammetry in an acetonitrile non-aqueous medium containing tetrabutylammonium perchlorate and different concentration of each monomer. All the films were synthesized onto indium-tin-oxide covered glass (EO) electrodes. In order to enhance the film quality, electropolymerization was carried out within a glove box containing CaCl2, which was added as a drying agent, and under N2 atmosphere. The low amount humidity during the measurements allowed us to correlate the morphological, electrochemical and optical properties of the films of PPP and derivatives (CPPI and CP3MET). The optical properties of the films were investigated by UV-VIS-NIR spectroscopy after varying the number of cyclos reached during the preparation of the films. The electrochemical response of the films was analyzed via cyclic voltammetry using a monomer-free electrolytic solution. The morphology of the films was correlated to their values of thickness and roughness as obtained by using atomic force microscopy (AFM) and the structural characterization of PPP e their derivatives were obtained by micro-Raman spectroscopy and Raman mapping.
 
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CarlaEirasD.pdf (8.15 Mbytes)
Publishing Date
2013-11-18
 
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