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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

Obtaining NiFe2O4 superparamagnetic nanoparticles by hydrothermal synthesis assisted by microwave / ObtenÃÃo de NanopartÃculas SuperparamagnÃticas de NiFe2O4 por SÃntese HidrotÃrmica Assistida por Micro-Ondas

Wesley dos Santos GalvÃo 21 February 2014 (has links)
Universidade Federal do Cearà / NanopartÃculas de NiFe2O4, foram sintetizadas pelo mÃtodo da co-precipitaÃÃo, assistida por aquecimento de micro-ondas. Em seguida, estudou-se o efeito do tempo de aquecimento sobre as propriedades estruturais e magnÃticas da ferrita de NÃquel. O precipitado coloidal foi submetido ao aquecimento, mantida a temperatura constante em 160 ÂC, em trÃs tempos diferentes 7, 12 e 17 minutos, a fim de se determinar a melhor temperatura para sÃntese e que resultasse em materiais com boa morfologia e pequeno tamanho de cristalito. Os difratogramas das amostras confirmaram a formaÃÃo das nanopartÃculas, que apresentaram estrutura cÃbica do tipo espinelio inverso e boa cristalinidade. O tamanho do cristalito foi calculado usando a equaÃÃo de Scherrer. A variaÃÃo da magnetizaÃÃo como uma funÃÃo do campo magnÃtico aplicado à temperatura ambiente foi estudada usando o MagnetÃmetro de Amostra Vibrante (VSM), obtendo valores de magnetizaÃÃo remanescente e coercividade igual à zero, sugerindo comportamento superparamagnÃtico. O aumento do tempo de aquecimento (7, 12 e 17 minutos) produziu um aumento no tamanho do cristalito (8,9 â 14 nm) e um aumento na magnetizaÃÃo de saturaÃÃo (31 â 45 emu/g) para a amostra. A temperatura de bloqueio foi encontrada traÃando um grÃfico de magnetizaÃÃo remanescente versus temperatura. A amostra de magnetita sofreu modificaÃÃo de sua superfÃcie pelo polÃmero APTES (3-aminopropil)-trietoxisilano, utilizando o aquecimento por micro-ondas. Os dados obtidos do VSM, termogravimetria (TG) e Infravermelho (FT-IR), confirmaram a adsorÃÃo. A partir dos experimentos realizados, foi possÃvel construir uma rampa de aquecimento eficiente para a produÃÃo de nanomateriais. / NiFe2O4 nanoparticles were synthesized by co-precipitation method, assisted by microwave heating. The colloidal precipitate was subjected to heating at various temperatures in order to determine the optimal temperature for the synthesis and resulted in materials with good morphology and small size of crystal. Next, we studied the effect of heating time on the structural and magnetic properties of nickel ferrite. The colloidal precipitate was subjected to microwave heating, keeping the temperature constant at 160  C at three different times 7 , 12 and 17 minutes. The XRD patterns of the samples confirmed the formation of nanoparticles, which showed cubic structure of the inverse spinel type and good crystallinity. The crystallite size was calculated using the Scherrer equation. The variation of the magnetization as a function of applied magnetic field at room temperature was studied using a vibrating sample magnetometer (VSM), obtaining values of remanent magnetization and coercivity equal to zero , suggesting superparamagnetic behavior. Increasing the heating time (7, 12 and 17 minutes) produced an increase in the size of the crystallite (9 â 27 nm) and an increase in the saturation magnetization (31 â 45 emu/g) to the sample. Blocking temperature was found by tracing graphic of remanent magnetization versus temperature. A sample of magnetite, courtesy of Advanced Materials Group â GQMAT, suffered modification of its surface by the polymer APTES (3-aminopropil)trietoxisilano, using microwave heating. Data obtained from the (VSM), thermogravimetry (TG) and Infrared (FT-IR) confirmed the adsorption from the experiments, it was possible to construct a heating ramp efficient for the production of nanomaterials to lower synthesis temperature and shorter heating time.

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