Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2015-11-27T13:08:55Z No. of bitstreams: 1 AseneteFrutuosoDaCosta_TESE.pdf: 4115238 bytes, checksum: 72a04780a21fa7344d83533cdbdd3d36 (MD5) / Approved for entry into archive by Elisangela Moura (lilaalves@gmail.com) on 2015-11-27T14:44:06Z (GMT) No. of bitstreams: 1 AseneteFrutuosoDaCosta_TESE.pdf: 4115238 bytes, checksum: 72a04780a21fa7344d83533cdbdd3d36 (MD5) / Made available in DSpace on 2015-11-27T14:44:06Z (GMT). No. of bitstreams: 1 AseneteFrutuosoDaCosta_TESE.pdf: 4115238 bytes, checksum: 72a04780a21fa7344d83533cdbdd3d36 (MD5) Previous issue date: 2014-08-18 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior - CAPES / Dentre os principais pigmentos, os materiais cer?micos que possuem a estrutura espin?lio AB2O4 v?m se tornando objeto de grande interesse cient?fico e tecnol?gico devido ? capacidade em acomodar diferentes c?tions em sua estrutura, permitindo diferentes tipos dopagens e, consequentemente, a obten??o de diferentes cores. Estudos sobre pigmentos cer?micos, atualmente, v?m sendo direcionados para o desenvolvimento de pigmentos est?veis e obtidos a baixas temperaturas e com maior reprodutibilidade. O objetivo do seguinte estudo ? a utiliza??o de pigmentos inorg?nicos para aplica??es em revestimentos cer?micos, tentando compreender quais par?metros influenciam na colora??o do pigmento nos esmaltes cer?micos. Pigmentos a base de CoCr2O4, CoAl2O4, Co0,8Zn0,2Cr2O4 e Co0,8Zn0,2Al2O4Co/Cr, foram sintetizados por uma rota qu?mica usando gelatina como precursor org?nico. Tais pigmentos foram caracterizados por An?lise termogravim?trica, Difra??o de raios X (DRX), Espectroscopia na regi?o do Infravermelho, Microscopia eletr?nica de varredura (MEV) Espectroscopia na regi?o do UV-Vis?vel e Colorimetria. Os resultados confirmaram a viabilidade da rota de s?ntese utilizada; com rela??o aos p?s sintetizados, Os pigmentos mostraram-se cristalinos e as fases desejadas foram obtidas a partir de 500oC, com um aumento da cristalinidade, assim como o tamanho m?dio de cristalito. Os pigmentos possuem tonalidades que v?o do verde ao violeta de acordo com as dopagens e suas temperaturas de calcina??o. / Ceramic pigments that own mainly the spinel structure AB2O4 are becoming a matter of great scientific and technological interest due to the ability of accommodate different cations in its structure, allowing different dopings and thus obtaining different colors. Studies on ceramic pigments currently are being directed to the development of stable and pigments obtained at low temperatures and with greater reproducibility. This work aims at the use of inorganic pigments for applications in ceramic tiles, investigating the influence of doping and calcination temperature on the coloring pigments and ceramic glazes. the based pigments of CoCr2O4, CoAl2O4, Co0,8Zn0,2Cr2O4 and Co0,8Zn0,2Al2O4 were synthesized by a chemical route using commercial gelatin as organic precursor. The materials were characterized by thermogravimetric analysis (TG), X-ray diffraction (XRD), infrared spectroscopy (FTIR) spectroscopy scanning electron microscopy (SEM) in the UVVisible region and colorimetry. The results confirmed the feasibility of synthesis used, the route presented pigments crystal structures and the desired phases were obtained from 500 ?C with increased crystallinity and the crystallite size. The pigments have hues ranging from green to violet according to their doping and calcination temperatures.

Made available in DSpace on 2015-03-03T15:15:27Z (GMT). No. of bitstreams: 1 MateusBB_DISSERT.pdf: 4491805 bytes, checksum: 6567583b83544d78b05fe6787b44a3ce (MD5) Previous issue date: 2012-03-27 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / In this experimental study sintetic samples of Jacobsites (MnFe2O4) were synthesized by the Pechini method and calcined within ambient atmosphere and afterwards in the vacuum from 400 to 700?C, the range of calcination temperatures. The X-Ray Diffraction (XRD) and the Scanning Electronic Microscopy (SEM) analysis have shown that the samples treated at 400?C temperature are composed by a simple type of spinel phase, with a crystallite size of 8:8nm for the sample calcined in ambient atmosphere and 20; 1nm for the sample treated in the vacuum, showing that the cristallite average size can be manipulated by the atmosphere control. The hysteresis loops for the sample calcined at 400?C in ambient atmosphere reveal features of superparamagnetic behavior with magnetization 29:3emu=g at the maximum field of 1:2T. The sample calcined in 400oC under vacuum show magnetization = 67emu=g at the maximum field of 1:5T. The sample treated at 500oC, under ambient atmosphere, has shown besides the spinel phase, secondary phases of hematite (Fe2O3) and bixbyite (FeMnO3). The hysteresis loops demonstrate a sharp drop of the magnetization compared to the previous sample. The analysis has revealed that for the samples treated in higher temperatures (600?C and 700?C) its observed the absence of the spinel phase and the maintenance of the bixbyite and hematite. The hysteresis loops for those samples in accordance to the external magnetic field are straight lines crossing the origin, consistent with the antiferromagnetic behavior of the phases.The M?ssbauer espectroscopy show to the sample calcined at 400?C within ambiente atmosphere two sextet and one doublet. The two sextets are assigned to the hyperfine fields related to the magnetic deployment in the nuclei of Fe3+ ions, at the tetraedric and octaedric sites. The doublet is assigned to superparamagnetic behavior of the particles with smaller diameter than dc . Now the sample calcined at 400?C under vacuum only show two sextet / ?Neste estudo experimental, amostras sint?ticas de Jacobsitas (MnF e2O4) foram sintetizadas pelo m?todo Pechini e calcinadas em atmosfera ambiente e em v?cuo de 400 at? 700?C. An?lises de difra??o de raio-x (DRX) e microscopia eletr?nica de varredura (MEV) revelaram que a amostra calcinada em 400?C ? composta por uma fase simples tipo espin?lio, com tamanho m?dio do cristalito de 8,8nm para amostra calcinada em atmosfera ambiente, e 20,1nm para amostra calcinada em v?cuo, indicando que o tamanho m?dio do cristalito pode ser manipulado pelo controle da atmosfera. A curva de magnetiza??o para amostra calcinada a 400?C em atmosfera ambiente revela caracter?sticas de comportamento superparamagn?tico, com magnetiza??o de 29:3emu=g num campo m?ximo de 1.2T . J? a amostra calcinada em 400?C sob v?cuo apresentou magnetiza??o = 67emu/g no campo m?ximo de 1.5T . A amostra tratada em 500 ]C, em atmosfera ambiente, acusa al?m da fase espin?lio, fases secund?rias de hematita (Fe2O3) e bixbyita (FeMnO3). A curva de magnetiza??o mostra uma queda abrupta na magnetiza??o comparada com as amostras anteriores. A an?lise mostra que, para mais altas temperaturas (600?C and 700?C), observou-se apenas a continua??o das fases hematita e bixbyita. A curva de magnetiza??o dessas amostras s?o linhas retas cortando a origem, consistente com o comportamento antiferromagn?tico dessas fases. A espectroscopia M?ssbauer revelou que para a amostra calcinada em 400?C em atmosfera ambiente h? dois sextetos e um dubleto. Os dois sextetos s?o atribu?dos aos campos hiperfinos referentes ao desdobramento magn?tico no n?cleo dos ?ons Fe3+, nos s?tios tetra?dricos e octa?dricos. O dubleto ? atribu?do ao comportamento superparamagn?tico das part?culas com di?metro menor que dc. J? a amostra calcinada em 400?C sob v?cuo apresenta apenas dois sextetos.

Made available in DSpace on 2014-12-17T14:06:56Z (GMT). No. of bitstreams: 1 AseneteFC_DISSERT.pdf: 1219908 bytes, checksum: bebef255f66d82cd8504a8398fd23379 (MD5) Previous issue date: 2010-12-10 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Inorganic pigment comprises a host lattice, which is part of the chromophore component (usually a transition metal cation) and possible components modifiers, which stabilize, add or restate the properties pigments. Among the materials with spinel, ferrites, and the chromite stand out, because they have broad technological importance in the area of materials, applicability, pigments, catalytic hydrogenation, thin film, ceramic tiles, among others. The present work, pigments containing CuFe2O4, CuCr2O4,e CuFeCrO4, were synthesized by a method that makes use of gelatin as organic precursor using their application to ceramic pigments. The pigments were characterized by X-ray diffraction (XRD), Infrared spectroscopy, scanning electron microscopy (SEM) spectroscopy in the UV-visible and Colorimetry. The results confirmed the feasibility of the synthetic route used, with respect to powders synthesized, there is the formation of spinel phase from 500?C, with an increase in crystallinity and the formation of other phases. The pigments were shown to be crystalline and the desired phases were obtained. The copper chromite have hues ranging from green to black according to the calcination temperature, while the copper chromite doped with iron had brownish. The ferrites showed copper color and darker brown to black, which may indicate an interesting factor because of the importance of black pigment / Pigmento inorg?nico ? formado por uma rede hospedeira, na qual se integra o componente crom?foro (normalmente um c?tion de metal de transi??o) e os poss?veis componentes modificadores, que estabilizam, conferem ou reafirmam as propriedades pigmentantes. Dentre os pigmentos, as estruturas tipo espin?lio se destacam por possuir ampla import?ncia tecnol?gica na ?rea de materiais, com aplica??o em pigmentos, cat?lise de hidrogena??o, filmes finos, revestimentos cer?micos, dentre outros. No presente trabalho, pigmentos contendo CuFe2O4, CuCr2O4,e CuFeCrO4 foram sintetizados por uma nova rota qu?mica usando gelatina como precursor org?nico visando sua aplica??o para pigmentos cer?micos. Os pigmentos foram caracterizados por difra??o de raios X (DRX), espectroscopia na regi?o do Infravermelho, Microscopia eletr?nica de varredura (MEV) espectroscopia na regi?o do UV-Vis?vel e Colorimetria. Os resultados confirmaram a viabilidade da rota de s?ntese utilizada; Com rela??o aos p?s-sintetizados, observase a forma??o da fase espin?lio a partir de 500oC, com um aumento da cristalinidade, bem como a forma??o de outras fases. Os pigmentos se mostraram cristalinos e as fases desejadas foram obtidas. As cromitas de cobre possuem tonalidades que v?o do verde ao preto, de acordo com a temperatura de calcina??o, enquanto que as cromitas de cobre dopadas com ferro obtiveram colora??o marrom. As ferritas de cobre apresentaram cores bem mais escuras, do marrom ao preto, o que ? uma caracter?stica interessante devido ? grande import?ncia dos pigmentos pretos na ind?stria cer?mica