Orientador: Marco Antonio Bottino / Co-orientador: Cornelis Johannes Kleverlaan / Banca: Luiz Felipe Valandro Soares / Banca: Alexandre Luiz Souto Borges / Banca: Paulo Francisco César / Banca: Estevam Augusto Bonfante / Resumo: O objetivo do presente estudo foi investigar a influência de diferentes tratamentos da superfície interna de coroas e de diferentes agentes cimentantes na sobrevivência de coroas de zircônia parcialmente estabilizada por óxido de ítrio (Y-TZP) recobertas por porcelana. Inicialmente foi realizado um estudo de elementos finitos onde foram comparados os valores e a distribuição das Tensões Máxima Principal (TMP) de espécimes flat e anatômicos, com variações na anatomia dos componentes cerâmicos (coroas de Y-TZP e porcelana, com e sem ponto de contato, com e sem desenho modificado da Y-TZP para suporte da porcelana). As geometrias produzidas em software CAD (Computer-aided design) foram importadas para software de análise de elementos finitos. Foi realizado carregamento pontual e vertical de 200 N sobre o nó central dos modelos. O padrão da distribuição da TMP foi bastante similar entre os modelos estudados, com concentração importante de tensões na zona de singularidade. Considerando a dificuldade de padronização na confecção de espécimes anatômicos durante ensaios laboratoriais, a escolha do modelo simplificado (flat) pode ser justificada. Em uma segunda etapa foram usinados 90 preparos flat em resina epóxica que receberam coroas com infraestrutura em Y-TZP confeccionadas pelo sistema CAD/CAM e recobertas com porcelana pela técnica estratificada. Seis condições foram testadas (n=15): para coroas cimentadas com cimento resinoso Panavia F, quatro diferentes tratamentos foram avaliados (limpeza com álcool isopropílico [PC], aplicação de glaze [POG], jateamento com Al2O3 125 μm [POA]; jateamento com partículas de óxido de alumínio revestidas por sílica de 30 μm [PCJ]); para as coroas cimentadas com cimento de ionômero de vidro (CIV) e de fosfato de zinco (CFZ), as superfícies foram limpas com álcool isopropílico. A resistência à fadiga foi avaliada... / Abstract: The aim of this study was to investigate the influence of different treatments of the inner surface of crowns and different luting agents on the survival of crowns made of zirconia partially stabilized by yttrium oxide (YTZP) and porcelain. A first study was performed using finite element analysis, where we compared the values and the distribution of Maximum Principal Stresses (MPS) of flat and anatomical specimens, with variations in the anatomy of ceramic components (crowns composed of Y-TZP and porcelain, with and without contact point, with and without a modified design of Y-TZP supporting the porcelain). The geometries produced in CAD software (Computer-Aided-Design) were imported for a finite element analysis software. A punctual and vertical load of 200 N was carried out on the central node of the models. The MPS distribution was quite similar among the studied models with important stress concentration in the singularity zone. Considering the lack of standardization in the preparation of anatomical specimens for laboratory tests, the choice of the simplified model (flat) could be justified. In a second step, 90 flat preparations were machined in epoxy resin and received crowns with Y-TZP infrastructure made by CAD/CAM system and veneered with porcelain by the stratified technique. Six conditions were tested (n=15): for crowns cemented with Panavia F, four different treatments were evaluated (cleaning with isopropyl alcohol [PC], overglaze application [POG], sandblasting with 125 μm particles of Al2O3 [POA]; sandblasting with 30μm particles of SiO2 [PCJ]); for crowns cemented with glass ionomer cement (CIV) and zinc phosphate (CFZ), the inner surface were cleaned with isopropyl alcohol. The fatigue resistance was evaluated by the number of mechanical cycles required for fracture of the specimens through stepwise loads methodology. Samples were cycled for 5,000 cycles at 200 ... / Doutor

In recent years, sintering of powdered materials in microwaves has emerged as a manufacturing technique with many potential advantages over conventional sintering methods, including the possibility of faster processing and finer microstructure, along with the potential for vast energy savings. However, the technique remains on the level of laboratory studies and is underutilized in industry, mostly due to the difficulty of controlling the process: the intrinsically nonuniform temperature pattern that results from microwave heating routinely induces nonuniform mechanical deformation. Mathematical models and computer simulations can help to clarify the factors that influence this process and aid experimentalists in the design of efficient processing equipment. Although a number of modelling techniques have been reported to this end, they appear to inadequately represent the entire chain of related physical phenomena, which involves interaction of the electromagnetic field with the material, heat transfer, and mechanical deformation, each of which is coupled with both of the others, and all of which occur on different time scales. In this work, we present an original comprehensive mathematical formulation that accounts for the chain of physical processes comprising microwave sintering in one- and two-dimensional scenarios. We develop models for simulating the coupled electromagnetic, thermal, and mechanical phenomena at their appropriate time and spatial scales, and in addition, we account for the temperature and density dependence of the full set of thermal and dielectric properties of the material undergoing sintering. The electromagnetic and temperature fields are approximated using finite difference methods, and the mechanical problem is solved using the Master Sintering Curve representation of the density kinetics, which gives a way of accounting for the effect of microscale transport on the macroscopic property of relative density. For constant-rate sintering trials, we use the exponential integral to compute the work of sintering, which reduces computation time. The presented algorithms are all implemented and shown in MATLAB and Python. Simulation of density and temperature evolution of the sintered sample shows processing times and shrinkage rates comparable to experimental results. This work lays a theoretical and computational foundation for modelling the general three-dimensional problem and computer-aided design of efficient sintering processes.

OBJECTIVE: The purpose of this study is to evaluate the experimental properties of zirconia-based ceramics. METHODS: Zirconia bars were veneered to 2mm total thickness. Veneering-method groups included: 1.Hand-layered feldsparthic porcelain (VM=VitaVM9,Vident) and fluorapatite glass-ceramic (CR=IPSe.maxCeram,IvoclarVivadent); 2.Pressed feldspathic porcelain (PM=VitaPM9,Vident) and fluorapatite glass-ceramic (ZP=IPSe.maxZirPress,IvoclarVivadent); 3.CAD/CAM milled feldspathic ceramic (TF=VitablocsTriluxeForte,Vident) and lithium-disilicate glass-ceramic (CAD=IPSe.maxCAD,IvoclarVivadent). CAD/CAM veneers were either cemented with resin cements (P=Panavia21,KurarayDental), (R=RelyXUltimate,3M ESPE), (M=MultilinkAutomix,IvoclarVivadent) or fused with fusion glass-ceramic (C=CrystalConnect,IvoclarVivadent). A Three-point-bending test was performed. For group VM,PM,TF-M,TF-C,CAD-M,CAD-C, ten more bars were prepared and aged with cyclic loading and thermocycling before testing. Zirconia bars (PrettauZirconia,Zirkonzahn;inCorisTZI,Sirona;ZirluxFC,PentronCeramics) specimens were prepared and polished. The specimens were divided into 3 groups: control, self-glaze fired, and glazed groups. A Three-point bending test was performed. Veneered zirconia crowns were made. Feldspathic porcelain was applied to zirconia coping. Bevel cut on porcelain was made to simulate porcelain chipping. The crowns were then divided into 4 different groups according to repair materials including: 1.Conventional-resin composite (TetricEvoCeram,IvoclarVivadent) 2.Flowable-resin composite (G-aenialUniversalFlo,GCamerica) 3.Cemented CAD/CAM milled feldspathic ceramic (VitaTriluxForte,Vident) 4.Cemented CAD/CAM milled lithium-disilicate glass-ceramic (IPSe.maxCAD,IvoclarVivadent). Each crown underwent thermocycling. The test was performed by loading force on the center of repaired part to record load-to-failure. RESULTS: There were significant differences in the failure loads of non-aged bilayered veneer-zirconia bars. Aging experiment revealed a significant difference in failure load between non-aged and aged bars in groups VM and PM, but not in the groups with CAD/CAM milled veneers. There was significant influence of surface treatments on flexural strength of zirconia specimens. Post-hoc test showed that glazed group had significant lower flexural strength than other groups. Crowns repaired with CAD/CAM ceramics showed significant higher failure load than resin composite. Repairing with lithium-disilicate glass ceramic yielded the highest load-to-failure of the specimens. CONCLUSIONS: - Veneer materials, veneering methods, and cement materials have a significant effect on the failure load of bilayered veneer- zirconia. CAD/CAM veneer-zirconia is not susceptible to aging performed in this study. - Glazing decreased the flexural strength of high translucent zirconia. - Veneered zirconia crowns repaired with CAD/CAM ceramic materials have significantly higher load-to-failure than veneered crowns repaired with resin composite. / 2018-09-28T00:00:00Z

Made available in DSpace on 2017-07-21T20:42:40Z (GMT). No. of bitstreams: 1 Luiza Kupchak.pdf: 1787533 bytes, checksum: ed9f8e72989aa4cdbca14d73ae5bce65 (MD5) Previous issue date: 2007-02-23 / The polycrystalline ceramics study the base of SnO2 presents great interest due to the inherent properties of emiconductor, which allows the application in some types of components, such as, protective gas sensors, varistors, protects films for different refractory uses and for glasses fusion of heavy metals. The addition of ZnO to the SnO2, makes with that these ceramics get high densification when added the low concentrations. In this work it of sintering in the initial period of training was studied kinetic, of the SnO2 with addition of 0,6% and 1,2% in mol of ZnO. The used methods of study had been the considered ones for Venkatu-Johnson, Woolfrey-Bannister, Wang-Raj and Young-Cutler. With the application of these models it was determined the energy of activation and the possible operating mechanisms in the system. The samples had been gotten by means of mixture of oxides, isostatic pressing and sintering in dilatometer, under taxes of constant heating of 2,5, 5 and 10 ºC.min- 1 until the temperature of 1350 ºC to air. The techniques used to carry through the characterization of the sintered samples had been to the ones of pycnometry of helium, diffraction of rays X and electronic microscopy of sweepings. It was verified that the addition of ZnO to the SnO2 made possible the ceramics attainment with superior relative densities 90%. The values of energy of activation gotten for the SnO2 with 0,6% in mol of ZnO, for the diverse studied models are of: 500 kJ.mol-1; 555 kJ.mol-1; 540 kJ.mol-1; 491 kJ.mol-1, respectively. For the SnO2 with 1,2% in mol of ZnO, the values of activation energy supplied by the models had been of: 444 kJ.mol-1; 555 kJ.mol-1; 424 kJ.mol-1; 491 kJ.mol-1, respectively. The results for the dominant mechanism of the sintering gotten from the used models did not allow to determine precisions from the operating diffusional mechanism in the studied compositions. / O estudo de cerâmicas policristalinas a base de SnO2 apresenta grande interesse devido às propriedades inerentes a este semicondutor, as quais permitem a aplicação em vários tipos de componentes, tais como, sensores de gás, aristores, filmes protetores para diferentes usos e refratários para fusão de vidros de metais pesados. A adição de ZnO ao SnO2, faz com que estas cerâmicas obtenham elevada densificação quando adicionadas a baixas concentrações. Neste trabalho estudou-se a cinética de sinterização no estágio inicial, do SnO2 com adição de 0,6% e 1,2% em mol de ZnO. Os étodos de estudo utilizados foram os propostos por Venkatu-Johnson, Woolfrey-Bannister, Wang-Raj e Young-Cutler. Com aplicação destes modelos foi determinada a energia de ativação e os possíveis mecanismos atuantes no sistema. As amostras foram obtidas por meio de mistura de óxidos, prensagem isostática e sinterização em dilatômetro, sob taxas de aquecimento constante de 2,5, 5 e 10 ºC.min-1 até a temperatura de 1350 oC ao ar. As técnicas utilizadas para realizar a caracterização das amostras sinterizadas foram às de picnometria de hélio, difração de raios X e microscopia eletrônica de varredura. Verificou-se que a adição de ZnO ao SnO2 possibilitou a obtenção de cerâmicas com densidades relativas superiores a 90%. Os valores de energia de ativação obtidos para o SnO2 com 0,6% em mol de ZnO, para os diversos modelos estudados são de: 500 kJ.mol-1; 555 kJ.mol-1; 540 kJ.mol-1; 491 kJ.mol-1,respectivamente. Para o SnO2 com 1,2% em mol de ZnO, os valores de energia de ativação fornecidos pelos modelos foram de: 444 kJ.mol-1; 555 kJ.mol-1; 424 kJ.mol-1; 491 kJ.mol-1, respectivamente. Os resultados para o mecanismo dominante da sinterização obtido a partir dos modelos utilizados não permitiu determinar de forma precisa o mecanismo difusional atuante nas composições estudadas.

Orientador: Estevão Tomomitsu Kimpara / Coorientador: Marina Amaral / Banca: Lourenço Correr Sobrinho / Banca: Fabiola Pessôa Pereira Leite / Banca: Guilherme de Siqueira Ferreira Anzaloni Saavedra / Banca: Carolina Machado Martinelli Lobo / Resumo: Essa pesquisa avaliou o comportamento mecânico e físico das repetidas queimas provenientes das técnicas de caracterização extrínseca do dissilicato de lítio (DL). Duzentos e setenta discos de DL foram fabricados de acordo com a ISO 6872/2008 e distribuídos nos diferentes grupos (n=30). Controles (CO), nos quais não foram realizados caracterização extrínseca. Caracterizados nos quais as queimas de cristalização e do glaze foram realizadas em passo único com IPS e.max CAD Crystall e Glaze Paste (Ivoclar Vivadent) (CR). E caracterizados nos quais as cerâmicas foram primeiramente cristalizadas, seguido da aplicação do IPS e.max Ceram Shades e do Glaze Paste (Ivoclar Vivadent) (CE). Cada tipo de caracterização teve suas amostras submetidas a duas, quatro ou seis queimas: COII, COIV, COVI, CRII, CRIV, CRVI, CEII, CEIV e CEVI. Análises de cor e translucidez foram realizadas com espectrofotômetro colorimétrico após as diversas queimas (n=20). Espectroscopia de raios X por dispersão em energia (EDS), difração de raios-X (DRX) e Raman foram utilizadas para análise de elementos químicos. A rugosidade Ra e a nanodureza Vickers também foram aferidas. Testes de flexão biaxial (n = 10, 1000 kgf, 1 mm/min) e de fadiga - staircase (n = 20, 5x104 ciclos, 5Hz, tensão inicial - 50% e incremento 5% da carga inicial de fadiga) foram realizados. Análises microscópicas da superfície das amostras (estereomicroscopia, mapping e MEV) também foram feitas. ANOVA um fator e Tukey foram os testes estatísti... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract : The objective of this research was to evaluate the mechanical and physical behavior of repeated firings from the aesthetic characterization of lithium disilicate (LD). Two hundred and seventy LD discs were manufactured according to ISO 6872/2008 and distributed in different groups (n = 30): controls (CO), in which no aesthetic characterization was made; characterized in which the crystallization and glaze firings were performed in a single step with IPS e.max CAD Crystall and Glaze Paste (Ivoclar Vivadent) (CR); and characterized in which the ceramics were first crystallized, followed by the IPS e.max Ceram Shade and Glaze Paste (Ivoclar Vivadent) application (CE). Each type of characterization had samples submitted to two, four or six firings: COII, COIV, COVI, CRII, CRIV, CRVI, CEII, CEIV and CEVI. Color and translucency analyzes were performed with a colorimetric spectrophotometer after the burnings (n = 20). X-ray dispersive energy spectroscopy (EDS), X-ray diffraction (XRD) and Raman spectroscopy were used to analyze chemical elements. Roughness (Ra) and Vickers nano-hardness were also measured. Biaxial flexion tests (n = 10, 1000 kgf, 1 mm/min) and fatigue - staircase (n = 20, 5x104 cycles, 5 Hz, initial tension - 50% and 5% increment of initial fatigue load) . Microscopic analysis of sample surfaces (stereomicroscopy, mapping and scanning electron microscope - SEM) were also performed. One-way ANOVA and Tukey were the statistical tests used (α = 0.05). For CE and CO6X-2X, values of ΔE00 were demonstrative of unacceptable color changes (ΔE00> 1.8). Group CO showed significant changes of translucency (p = 0.02); for CE (p = 0.09) and CR (p = 0.26) the values increased significantly. The values of nano-hardness among the nine groups were statistically similar (p> 0.05). However, Ra values indicated significant differences due to the type of characterization .....(Complete abstract click electronic access below) / Doutor

Orientador: Edson Alves de Campos / Resumo: A cerâmica é uma opção que preenche as exigências estéticas, biológicas, mecânicas e funcionais de um material restaurador. O sistema CAD/CAM empregado na Odontologia permite confeccionar restaurações indiretas, em um curto período de tempo, cimentá-las na mesma sessão clínica, sem a intermediação do laboratório de prótese. Qualquer material restaurador está sujeito a desgastes por ação da mastigação e a escovação diária. Protocolos de higienização profissional devem ser estabelecidos de maneira a não afetarem a rugosidade superficial das restaurações. O objetivo deste estudo foi avaliar a rugosidade superficial (Ra) de materiais restauradores CAD/CAM após diferentes métodos de higienização. Trata-se de um estudo in vitro que utilizou espécimes (n=144) dos seguintes materiais: Cerâmica Feldspática (Cerec Blocs, Dentsply Sirona); Cerâmica Feldspática reforçada por Leucita (IPS Empress CAD, Ivoclar Vivadent); Cerâmica Di-silicato de lítio (IPS e-max CAD, Ivoclar Vivadent) e Compósito nano híbrido (Grandio Blocs, Voco), sendo que dois materiais, Cerâmica Feldspática e Cerâmica Feldspática reforçada por Leucita foram avaliados com e sem glaze. Os espécimes foram submetidos a três diferentes métodos de higienização (escovação simulada; jato de bicarbonato de sódio e profilaxia com taça de borracha e pasta profilática). A rugosidade superficial foi mensurada antes e após os diferentes métodos de higienização por meio do rugosímetro de contato. A análise de variância foi feita para ... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Dental ceramic has been a restorative material option that may provide the aesthetic, biological, mechanical and functional requirements. CAD/CAM (computer aided design/computer aided manufacturing) system used in Dentistry allows to perform indirect restorations in a short period of time and proceed the cementation in the same clinical session without the intermediation of prosthesis laboratory. However, any restorative material can wear due to chewing and daily toothbrushing action. Thus, hygiene protocols should be stated in order to not affect the surface roughness of restorations. This study aimed to evaluate the surface roughness (Ra) of CAD/CAM restorative materials after different hygiene protocols. This in vitro study used the following materials (n=144): Feldspathic ceramic (Cerec Blocs, Dentsply Sirona); Leucite-reinforced feldspathic ceramic (IPS Empress CAD, Ivoclar Vivadent); Lithium disilicate ceramic (IPS e-max CAD, Ivoclar Vivadent) and Nanohybrid resin-based composite (Grandio Blocs, Voco). For Feldspathic ceramic and Leucite-reinforced feldspathic ceramic it was performed the evaluations with and without glaze. The samples were submitted to three different hygiene protocols (simulated brushing, sodium bicarbonate jet and prophylaxis with rubber cup and prophylactic paste). Surface roughness was measured before and after the hygiene protocols by a contact rugosimeter. ANOVA test was applied to evaluate the initial roughness among materials, followed by Games... (Complete abstract click electronic access below) / Mestre

Thesis (M.S.)--Massachusetts Institute of Technology, Dept. of Materials Science and Engineering, 1982. / MICROFICHE COPY AVAILABLE IN ARCHIVES AND SCIENCE / Vita. / Includes bibliographical references. / by Normand Denis Corbin. / M.S.

Orientador: Renata Garcia Fonseca / Resumo: Pouco se sabe sobre o efeito do jateamento pré-sinterização da zircônia na sua resistência mecânica, sob condições de envelhecimento. Este estudo avaliou a influência do tamanho da partícula, do momento do jateamento e do envelhecimento na resistência mecânica de uma zircônia estabilizada por ítria. Quatrocentos discos de uma zircônia estabilizada por ítria pré-sinterizados foram alocados como segue: sem jateamento; jateamento com partículas de óxido de alumínio (Al2O3) de 50 µm ou 120 µm antes (50/PRÉ ou 120/PRÉ) ou após (50/PÓS ou 120/PÓS) sua sinterização. Os discos foram não envelhecidos (24h) ou envelhecidos por: ciclagem mecânica (CM); envelhecimento hidrotérmico (EH) ou CM+EH, totalizando 20 grupos (n=20). Os espécimes foram submetidos ao teste de resistência à flexão biaxial (RFB) e, posteriormente, foram analisados fractograficamente. A análise de difração de raios-X (DRX) foi realizada em determinadas condições para caracterizar cristalograficamente o efeito do jateamento na zircônia. Os dados de RFB (MPa) foram analisados por ANOVA a 3 fatores e pós teste de Games Howell (α=0,05). Também foi realizada análise de Weibull. A RFB e a resistência característica (σ0) dos grupos 120/PÓS, envelhecidos ou não, foram significativamente maiores que as dos demais grupos jateados, e estatisticamente similares ou maiores que as dos respectivos grupos sem jateamento. Em contrapartida, o grupo 120/PRÉ/não envelhecido e todos os grupos 50/PRÉ apresentaram os menores valores. Em to... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Little is known about the effect of air-abrasion before zirconia sintering on its strength, under aging challenge. This study aimed to verify the influence of the airabrasion moment (before or after zirconia sintering), particle size (50 or 120 µm) and aging on the mechanical strength of a Y-TZP ceramic. Four hundred pre-sintered zirconia discs were allocated as follows: non-air-abraded; air-abraded with 50 µm or 120 µm Al2O3 particles before (50/BS or 120/BS) or after sintering (50/AS or 120/AS). The discs were non-aged (24h) or aged by: mechanical cycling (MC); hydrothermal aging (HA) or by both methods (MC+HA), totaling 20 groups (n=20). Specimens were subjected to biaxial flexural strength test (BFS). Fractographic analysis was performed to identify the fracture origin. The X-ray diffraction analysis (XRD) was performed under certain conditions to characterize the crystallographic effect of airabrasion on the zirconia. The BFS data (MPa) were analyzed by ANOVA and Games Howell post hoc test (α=.05). Weibull statistics was also applied. The BFS and the characteristic resistance (σ0) of the 120/AS groups, aged or not, were significantly higher than those of the other air-abraded groups, and statistically similar or higher than the respective groups without air-abrasion. In contrast, the 120/BS/non-aged group and all those 50/BS presented the lowest values. In all groups, the initial defect had its origin on the tensile stress side. Neither air-abrasion nor aging (except for 50/AS/MC+HA) reduced the zirconia reliability compared with the respective controls. Air-abrasion promotes an increase in the monoclinic phase content, while sintering zeroed this phase. Air-abrasion before zirconia sintering yields worse performance for BFS than after sintering, under aging challenges. The BFS and σ0 were strongly determined by the particle size and air-abrasion moment / Doutor

A arqueometria é uma área consolidada, com ampla utilização de métodos analíticos nucleares destrutivos e não destrutivos para caracterização, proteção e restauração de peças arqueológicas. O presente projeto teve como objetivo estudar a composição química elementar de amostras de fragmentos cerâmicos encontradas no sítio arqueológico São Paulo II localizado na calha do rio Solimões, próximo ao município de Coari na Amazônia Brasileira. Realizou-se a caracterização das amostras pela determinação de Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Na, Nd, Sb, Sm, Rb, Sc, Ta, Tb, Th, U, Yb and Zn por meio da análise por ativação com nêutrons (NAA). A partir da composição química da cerâmica, foi possível definir o agrupamento de amostras em função da similaridade/dissimilaridade da composição química presente no material cerâmico. O agrupamento foi interpretado por métodos estatísticos multivariados como análise de cluster, análise de componentes principais e análise de discriminante. Foram selecionadas, a partir da formação dos grupos, 7 cerâmicas com o objetivo de elaborar o horizonte temporal do sítio, realizado por termoluminescência (TL) e ressonância paramagnética eletrônica (EPR). A temperatura de queima da cerâmica foi determinada em 6 fragmentos por meio da técnica de EPR. Os resultados apresentados neste trabalho podem contribuir com os estudos arqueológicos sobre a dinâmica da ocupação da Amazônia Central anterior à colonização Brasileira. / Archaeometry is currently a well established field in the archaeological sciences. The nuclear method for analysis of chemical elements is one of the important instruments for the characterization of the archaeological materials and has influences on the preservation and restoration. From the chemical and physical analyses it is possible to infer technical processes in ceramics manufacture and tools used by ancient people. Therefore, it contributes to the typology and to understand the roles of materials available in the archaeological sites, such as clays and lythic sources. Evidently, all the archaeological materials and sites are related to people that lived there a long time ago, and studies, as outlined above, reconstruct at least partially the history of such a population. This project aimed at studying the elementary chemical composition of 70 ceramic fragments samples from São Paulo II archaeological site, located along the Solimões River channel, next to Coari city, in Brazilian Amazon. The characterization of samples was performed by neutron activation analysis (NAA). By the determination of 22 elements in the ceramic fragments ( Ce, Co, Cr, Cs, Eu, Fe, Hf, K, La, Lu, Na, Nd, Sb, Sm, Rb, Sc, Ta, Tb, Th, U, Yb and Zn), it was possible to define groups of samples regarding the similarity/dissimilarity in elementary chemical composition. For such a task, the multivariate statistical methods employed were cluster analysis (CA), principal component analysis (PCA) and discriminant analysis (DA). Afterwards, seven ceramic fragments have been selected to elaborate the site temporal horizon using thermoluminescence (TL) and electron paramagnetic resonance (EPR) dating results. The EPR technique was also used to find the average firing temperature to produce the ceramics. The results of this research may contribute to the study on the occupation dynamics in the pre-colonial Brazilian Amazon.

Orientador: José Roberto Ribeiro Bortoleto / Banca: Sonia Regina Homem de Mello Castanho / Banca: Sidney Domingues / Banca: Elidiane Cipriano Rangel / Banca: Sandro Donnini Mancini / O Programa de Pós Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi / Resumo: Esta tese teve como finalidade realizar a síntese e a caracterização de óxido de zinco dopado com alumínio (AZO) para a confecção de alvos cerâmicos para serem utilizados na deposição de filmes finos condutivos (TCO) pela técnica de pulverização catódica. O óxido de zinco dopado com alumínio foi obtido pelo Método Pechini. A estruturação do material, através de seu precursor, deu-se pelo tratamento térmico em ar. A caracterização do material obtido foi realizada mediante as técnicas de Análises Térmicas Simultâneas (TG, DTG, DTA), Difração de Raios-X (DRX), Refinamento Estrutural pelo Método de Rietveld (REMR), Microscopia Eletrônica de Varredura (EDS) e Análise Semi-qualitativa por Energia de Raios-X (MEV). Os resultados mostraram que a ~600ºC, o material na forma de pó nanoestruturado, teve a eliminação majoritária de orgânicos dos precursores como indicado pelas análises térmicas TG, DTG, DTA. Por volta desta temperatura pode-se notar, também, o início da estruturação da fase cristalina confirmado pela análise de difração de Raios-X. Por fim, tratamentos acima de 1000ºC permitiram a obtenção de óxidos com alta cristalinidade, ausência de fases resistivas, além da eliminação de orgânicos. Acima de 1200ºC houve aumento da concentração de alumínio devido a volatização do zinco. O alvo foi confeccionado a partir de uma suspensão de pó de AZO em etilenoglicol que foi depositada em demarcação por máscara sobre disco de alumina, recebendo tratamento térmico para sinterização dos grãos. Este alvo foi utilizado para a síntese de filmes finos sobre substratos de vidro pela técnica da Pulverização Cotódica. Com o alvo obtido, foi possível realizara deposição de filmes finos de tipo TCO. Os filmes finos foram caracterizados por medidas de transmitância óptica na região do espectro visível, DRX, e teste de condutividade elétrica. Os resultados de caracterização... / Abstract: This thesis had intended to perform the synthesis and characterization of aluminum-doped zinc oxide (AZO) for making ceramic targets for use in conductive thin film deposition (TCO) by sputtering technique. The aluminium-doped zinc oxide was obtained by Pechini Method. The structuring of the material, through its precursor, by heat treatment in air. The characterization of the material obtained was performed by Simultaneous Thermal Analysis techniques (TG, DTG, DTA), X-Ray Diffraction (XRD), Structural Refinement by the Rietveld method (REMR), scanning electron microscopy (EDS) and Semi-quantitative Analysis by X-Ray Energy (MEV). The results showed that the ~600ºC, the material in the form of nanostructured powder, had the majority of organic disposal of precursors as indicated by thermal analysis TG, DTG, DTA. Around this temperature can be noted, too, the beginning of the structure of the crystalline phase confirmed by X-Ray Diffraction Analysis. Finally, above 1000ºC treatments allowed the obtaining of oxides with high crystallinity, absence of resistive phases, in addition to the complete elimination of organics. Up to 1200ºC aluminum concentration increased due to volatilization of zinc. The target was made from a powder suspension of AZO in ethyleneglycol that was deposited in demarcation for mask over alumina getting disk heat treatment for sintering of grain. This target was used for the synthesis of thin films on glass substrates by Cathodic spraying technique. With the target, it was possible to accomplish the thin film deposition of type TCO. The thin films were characterization by optical transmittance measurements in the visible spectrum, DRX, and electrical conductivity test. The results of characterization showed that the ceramic target, obtained by Pechini Method, made possible the growth of thin films with low electrical resistitivity with values near the 1.10-3 cm, plus a high transmittance (90%) characterized as... / Doutor