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Autor da Dissertao: Anderson Mateus Mendona e Silva Medeiros Ttulo: Sntese e Caracterizao de Lquidos Inicos Magnticos Programa de Ps Graduao

em Qumica Data da defesa: 01/03/2012 Orientador: Prof. Dr. Joel Camargo Rubim Palavras-chave: BMI.NTf2; Lquido inico magntico; Magnetita; Maguemita; Ferrita de Cobalto. Keywords: BMI.NTf2; Ionic Liquid; Magnetite; Maghemite; Cobalt Ferrite Resumo

Lquidos Inicos Magnticos (LIM) foram obtidos a partir da disperso de nanopartculas magnticas (NPM), modificadas superficialmente, no lquido inico bis-trifluorometanosulfonilimidato de 1-n-butil-3-metilimidazlio (BMI.NTf2). As NPM do tipo -Fe2O3, Fe3O4, e CoFe2O4 foram obtidas pelo mtodo de co-precipitao qumica. A superfcie das NPM foram modificadas por silanizao com cloreto de 1-n-butil-3-3-(trimetoxipropilsilano)imidazlio. As NPM modificadas e no modificadas foram caracterizadas por difrao de raios-X (DRX), microscopia eletrnica de transmisso (MET), por espectroscopias FTIR, FTNIR e Raman, bem como por anlise termogravimtrica (TGA), calorimetria diferencial exploratria (DSC) e medidas de magnetizao (magnetizao vs campo magntico). Os difratogramas das amostras investigadas foram caractersticos das ferritas do tipo espinlio. A aplicao da equao de Scherrer aos dados de DRX mostra que as NPM de Fe3O4, CoFe2O4 e -Fe2O3 apresentam dimetros mdios correspondentes a 12,3, 11,0 e 9,9 nm,

respectivamente. Dimetros mdios similares foram obtidos por MET. Os espectros Raman das nanopartculas magnticas mostraram fnons caractersticos desses materiais e os espectros Raman dos LIM sugerem algum tipo de interao entre o lquido inico e as nanopartculas magnticas. O espectro FTNIR das amostras de Fe3O4 e CoFe2O4 mostraram absores caractersticas desses materiais. Os espectros FTIR das amostras superficialmente modificadas mostram, inequivocadamente, a presena do agente modificador na superfcie das NPM. Os resultados obtidos por TGA mostram que a superfcies das ferritas esto recobertas por pelo menos uma monocamada do modificador. As medidas de magnetizao mostram que as NPM de Fe3O4 e -Fe2O3 e os LIM corrspondentes apresentam comportamento superparamagntico com coercividades e remanncias desprezveis. Os valores de coercividade e remanncia para as NPM e LIM derivados de CoFe2O4 no foram desprezveis. A estabilidade dos LIM atribuda formao de pelo menos uma monocamada de agente modificador na superfcie das NPM a qual apresenta uma estrutura que mimetiza a estrutura do LI.

Abstract

Magnetic ionic liquids (MIL) were obtained by the dispersion of surface modified magnetic nanoparticles (MNP) in the ionic liquid (IL) 1-n-butyl 3-methylimidazolium bistrifluorometanosulfonilimide (BMI.NTf2). The MNP were made from ferrites of the type -Fe2O3, Fe3O4, and CoFe2O4 that were obtained by the co-precipitation method. The surfaces of the MNP were modified by silanization with 1-n-butyl-3-3-(trimethoxipropylsilane)imidazolium chloride. The non modified and modified MNP were characterized by x ray diffraction (XRD), transmission electron microscopy (TEM), FTIR, FTNIR, and Raman spectroscopy as well as by, TGA, DSC, and magnetization measurements (magnetization vs magnetic field). The XRD diffraction patterns of the investigated samples were characteristic of spinel ferrites and the application of Schrrers equation showed that the Fe3O4, CoFe2O4, and -Fe2O3 MNP have mean diameters of 12.3, 11.0, and 9.9 nm, respectively. Similar mean diameters were obtained by the TEM analysis. The Raman spectra of the MNP have shown the characteristic Raman phonons for these materials and the Raman spectra of the MIL suggest some kind of interaction between the IL and the MNP. The FTNIR spectra of the Fe3O4 and CoFe2O4 samples have shown the characteristic absorptions of these materials. The FTIR spectra of surface modified samples characterized unequivocally the presence of the surface modifier on the surface of the MNP. TGA results have shown that the surface of the MNP is recovered with at least one monolayer of modifier. Magnetization measurements have shown that the Fe3O4 and Fe2O3 MNP as well as their corresponding MIL present superparamagnetic behavior with negligible remanences and coercivities. The coercivities and remanences for the CoFe2O4 MNP and the corresponding MIL are not negligible. The stability of MIL is attributed to the formation of at least one monolayer of the surface modifier, which presents a structure that mimics the IL structure.