Made available in DSpace on 2015-04-14T13:59:09Z (GMT). No. of bitstreams: 1 460217.pdf: 1794171 bytes, checksum: 9f89fb6e90ac2a056b535eb35119531e (MD5) Previous issue date: 2014-08-01 / The growth of the polymer market leads to new application niches for these materials with present different properties when compared to the conventional ones, such as composites and nanocomposites, making key the search and the development of these products. Polyurethanes (PUs) are among the most versatile polymers in the world today. To improve the performance of a polyurethane, a common method is to incorporate fillers into the polymer, such as inorganic particles. Thus, this work proposes a study of obtaining and comparing PU nanocomposites by in situ polymerization using natural inorganic filler such as talc and synthetic talc (Ni-talc). The quantities defined Ni-talc were 0.5%, 1%, 2%, 3% and 5% on the mass of polyurethane formed during the polymerization reaction. To follow the results of the technical Infrared Spectroscopy were used Fourier transform (FTIR), differential scanning calorimetry (DSC), Thermogravimetric Analysis (TGA), Gel Permeation Chromatography (GPC), dynamic mechanical analysis (DMTA), Microscopy Scanning Electron (SEM), Analysis of X-Ray Diffraction (XRD) and Analysis of Specific Surface Area (BET). The XRD results showed that intercalation of polymer matrix in the nanocomposites structure. The Ni-talc exhibited better thermal properties when compared to natural talc. The nanocomposites with 0.5, 1 and 2% Ni-talc showed the best strain results in low deformation volues in relation to the pure PU, while the stress-strain results from natural talc nanocomposite shows higher strain values at higher deformation. / O crescimento do mercado de pol?meros surge como novos nichos de aplica??o para materiais com propriedades diferentes das existentes, tais como os comp?sitos e nanocomp?sitos, tornando fundamental a busca e o desenvolvimento destes produtos. Os poliuretanos (PU s) est?o dentre os pol?meros mais vers?teis no mundo atual. Para melhorar ainda mais o desempenho de um poliuretano, um m?todo comum ? a incorpora??o de cargas ao pol?mero, como as part?culas inorg?nicas. Desta maneira, este trabalho prop?e um estudo de obten??o e de compara??o de nanocomp?sitos de PU por polimeriza??o in situ, usando como carga inorg?nica talco natural e talco sint?tico (Ni-talco). As quantidades, definidas de Ni-talco, foram 0,5%, 1%, 2%, 3% e 5% em rela??o ? massa de poliuretano formada durante a rea??o de polimeriza??o. Na caracteriza??o dos resultados foram utilizadas as t?cnicas de Espectroscopia de Infravermelho por Transformada de Fourier (FTIR), Calorimetria Explorat?ria Diferencial (DSC), An?lise Termogravim?trica (TGA), Cromatografia de Permea??o em Gel (GPC), An?lise Din?mico Mec?nica (DMTA), Microscopia Eletr?nica de Varredura (MEV), An?lise de Difra??o de Raios-X (DRX) e An?lise da ?rea Superficial Espec?fica (BET). As an?lises de DRX mostraram que h? forma??o de uma estrutura intercalada entre a matriz polim?rica e as nanoparticulas. O Ni-talco mostrou melhores propriedades t?rmicas quando comparado com o talco natural. Os nanocomp?sitos com 0,5, 1 e 2% de Ni-talco mostraram os melhores resultados de tens?o em baixas deforma??es que o PU puro, enquanto que os resultados de tens?o-deforma??o do nanocomp?sito de talco natural mostraram valores de tens?o superiores em deforma??es mais elevadas.

Submitted by Caroline Xavier (caroline.xavier@pucrs.br) on 2017-07-27T14:12:30Z No. of bitstreams: 1 DIS_CRISTINA_LORENSKI_FERREIRA_COMPLETO.pdf: 3410093 bytes, checksum: 23798c7a6d0f4dcae08a1e2a111ebd1b (MD5) / Made available in DSpace on 2017-07-27T14:12:31Z (GMT). No. of bitstreams: 1 DIS_CRISTINA_LORENSKI_FERREIRA_COMPLETO.pdf: 3410093 bytes, checksum: 23798c7a6d0f4dcae08a1e2a111ebd1b (MD5) Previous issue date: 2017-03-27 / Peripheral nerve injury continues to be an important research topic in the scientific community as it may cause lifelong disability. Biocompatible polymers are materials potentially capable of aiding the regeneration of peripheral nerves being used for the production of biocompatible tubes. The aim of this work is to prepare and characterize polymeric nanocomposites based on polycaprolactone (PCL), poly(lactic-co-glycolic acid) (PLGA) and polypyrrole nanofibers (PPy) capable of acting as a guidewire in the regeneration of peripheral nerves. PPy was synthesized by oxidative chemical polymerization with p-toluenesulphonic acid monohydrate (PTSA) as a doping agent. PCL:PLGA blends films and PCL:PLGA:PPy nanofibers nanocomposites films were prepared by the solvent casting method, in the ratio of PCL:PLGA 100:0, 90:10, 80:20 and 70:30 (m/m); to the films with nanoload were added 10% PPy. In order to characterize the films, the following techniques were used: SEM, DSC, TGA, determination of electric conductivity and contact angle, citotoxicity test and hydrolytic degradation test, in vitro, based on ASTM F1635-11 standards. The PPy nanofibers presented electrical conductivity equal to 2.0.10-1 S.cm-1. The presence of PLGA and PPy did not change, meaningfully, the thermal properties of the films. However, in the degradation process, there was a tendency to a greater loss of mass for the blends with higher percentage of PLGA when submitted to longer incubation periods (150 days); when PPy was added to these blends, mass loss occurred in shorter periods (90 days). The nanocomposites films showed nontoxic and porous morphology surface, with hydrophilic intermediary character, good thermal stability and adequate degradation time for potential use in the treatment of injury in peripheral nerves. / Les?o de nervos perif?ricos continua sendo um importante tema de pesquisas no meio cient?fico, podendo causar defici?ncia no paciente por toda a vida. Pol?meros biocompat?veis s?o materiais potencialmente capazes de auxiliarem a regenera??o de nervos perif?ricos sendo utilizados para a produ??o de tubos biocompat?veis. O objetivo deste trabalho ? preparar e caracterizar nanocomp?sitos polim?ricos baseados em policaprolactona (PCL), poli(?cido l?ctico-co-glic?lico) (PLGA) e nanofibras de polipirrol (PPy) capazes de atuarem como conduto guia na regenera??o de nervos perif?ricos. PPy foi sintetizado via polimeriza??o qu?mica oxidativa com ?cido p-toluenosulf?nico monohidratado (APTS) como agente dopante. Foram preparados filmes de blendas PCL:PLGA e de nanocomp?sitos PCL:PLGA:nanofibras de PPy pelo m?todo de evapora??o de solvente, nas raz?es de PCL:PLGA 100:0, 90:10, 80:20 e 70:30 (m/m); aos filmes com a nanocarga, foram adicionados 10% de PPy. Para caracteriz?-los, foram utilizadas as t?cnicas: MEV, DSC, TGA, determina??o da condutividade el?trica e do ?ngulo de contato, teste de citotoxicidade e de degrada??o hidrol?tica, in vitro, com base na norma ASTM F1635-11. As nanofibras de PPy apresentaram condutividade el?trica igual a 2,0.10-1 S.cm-1. A presen?a de PLGA e de PPy n?o modificou, significativamente, as propriedades t?rmicas dos filmes. Por?m, no processo de degrada??o, houve uma tend?ncia ? maior perda de massa para as blendas com maior percentual de PLGA quando submetidas a maiores tempos de incuba??o (150 dias); ao adicionar PPy ?s blendas, a perda de massa ocorreu em menores tempos (90 dias). Os filmes dos nanocomp?sitos apresentaram superf?cie at?xica e de morfologia porosa, com car?ter hidrof?lico intermedi?rio, boa estabilidade t?rmica e tempo de degrada??o adequado para o potencial uso no tratamento de les?es em nervos perif?ricos.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2018-01-23T13:48:58Z No. of bitstreams: 1 ErikDosSantosSilva_TESE.pdf: 6543895 bytes, checksum: 29c9b0e4741aa669a76be6f191b18cf7 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2018-01-24T14:05:43Z (GMT) No. of bitstreams: 1 ErikDosSantosSilva_TESE.pdf: 6543895 bytes, checksum: 29c9b0e4741aa669a76be6f191b18cf7 (MD5) / Made available in DSpace on 2018-01-24T14:05:43Z (GMT). No. of bitstreams: 1 ErikDosSantosSilva_TESE.pdf: 6543895 bytes, checksum: 29c9b0e4741aa669a76be6f191b18cf7 (MD5) Previous issue date: 2017-08-30 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / A pesquisa em nanocomp?sitos de pol?meros e s?lica tornou-se foco de muitos pesquisadores nos ?ltimos anos devido ?s excelentes propriedades apresentadas quando comparadas aos componentes individuais. Neste trabalho foi realizado um tratamento de modifica??o superficial da s?lica com 3-aminopropiltriet?xisilano (APTES) para incorpora??o na blenda poli(metacrilato de metila)/poli(estireno-co-acrilonitrila) (PMMA/SAN) por meio de processamento em extrusora dupla rosca. Foi avaliado o efeito da adi??o de nanopart?culas de s?lica com e sem modifica??o superficial na estrutura e propriedades da blenda PMMA/SAN, com objetivo de promover melhores propriedades mec?nicas, sem comprometer a transpar?ncia dos materiais produzidos. Os materiais foram caracterizados por medidas de ?ndice de fluidez (MFI), ensaios mec?nicos de tra??o uniaxial, flex?o em 3 pontos, dureza Rockwell M (HRM) e Shore D, impacto Izod, reometria de placas paralelas, microscopia eletr?nica de transmiss?o (MET), ensaios de abras?o e risco. Os resultados reol?gicos indicaram que houve rea??o entre as nanopart?culas de s?lica tratadas com os pol?meros puros e com a blenda PMMA/SAN, mostrando-se uma t?cnica ?til para avaliar poss?veis rea??es durante o processo de extrus?o. Os nanocomp?sitos apresentaram um decr?scimo nas propriedades de resist?ncia m?xima ? tra??o, resist?ncia ao impacto e alongamento na ruptura, se comparado a blenda PMMA/SAN, que apresentou sinergismo nas propriedades de resist?ncia m?xima ? tra??o e alongamento na ruptura. Entretanto, as propriedades dos nanocomp?sitos com nanopart?culas de s?lica modificadas foram superiores aos nanocomp?sitos sem tratamento. A adi??o de s?lica tratada promoveu um aumento no m?dulo de elasticidade, dureza, abras?o e risco dos nanocomp?sitos produzidos. / Research on nanocomposites of polymers and silica has become the focus of many researchers in recent years because of the excellent properties presented when compared to individual components. In this work a surface modification treatment of silica with 3-aminopropyltriethoxysilane (APTES) was carried out for incorporation in the poly(methyl methacrylate)/poly(styrene-co-acrylonitrile) (PMMA/SAN) blend by processing in a twin screw extruder. The effect of the addition of silica nanoparticles with and without surface modification on the structure and properties of the PMMA/SAN blend was evaluated, aiming to promote better mechanical properties without compromising the transparency of the materials produced. The materials were characterized by flow index measures (MFI), mechanical tests of uniaxial traction, 3-point flexure, Rockwell M hardness (HRM) and Shore D, Izod impact, parallel plate rheometry, transmission electron microscopy (TEM), abrasion and scratch tests. The rheological results indicated that there was a reaction between the silica nanoparticles treated with the pure polymers and with the PMMA/SAN blend, showing a useful technique to evaluate possible reactions during the extrusion process. The nanocomposites showed a decrease in the properties of maximum tensile strength, impact strength and elongation at break when compared to PMMA/SAN blends, which showed synergism in the properties of maximum tensile strength and elongation at break. However, the properties of the nanocomposites with modified silica nanoparticles were superior to the nanocomposites without treatment. The addition of treated silica promoted an increase in the modulus of elasticity, hardness, abrasion and scratch of the nanocomposites produced.

Made available in DSpace on 2014-12-17T14:06:57Z (GMT). No. of bitstreams: 1 AntonioMM_DISSERT.pdf: 3167534 bytes, checksum: a8247e394e6c3656375c3f16b429e065 (MD5) Previous issue date: 2010-10-15 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Poly(methyl methacrylate)/clay nanocomposites were prepared by melt mixing using a montmorillonite-rich clay (MMT). The clay in natura was treated with acrylic acid to facilitate the dispersion in the polymer matrix. A masterbatch of PMMA/clay was prepared and combined with the pure PMMA and then subjected to extrusion process using singlescrew and twin-screw extruders followed by injection. Nanocomposites were processed with clay contents of 1, 3, 5 and 8 wt.%. The effect of shear processing on the morphology of the nanocomposites was evaluated by XRD, SEM and TEM. Thermal and mechanical properties of the nanocomposites were investigated through TGA, DSC, HDT, VICAT, tensile and impact tests, to evaluate the effect of the addition of clay to the PMMA matrix. Flammability tests were also conducted to investigate the effect of the addition of clay on the flame retardation properties. SEM images of the nanocomposites indicated the presence of clay agglomerates, which resulted in the reduction of properties such as thermal stability, mechanical strength and impact resistance, and increased the rate of burning for materials processed by both extrusion routes / Nanocomp?sitos de poli(metacrilato de metila) (PMMA) foram preparados a partir da t?cnica de mistura no estado fundido com argila rica em montmorilonita (MMT). A argila in natura foi inicialmente tratada com ?cido acr?lico para facilitar a dispers?o na matriz polim?rica. Depois, foi preparado um concentrado de PMMA e argila que foi combinado com o PMMA puro e submetido ao processo de extrus?o realizado em extrusoras monorosca e dupla rosca com posterior inje??o. Nanocomp?sitos foram processados com 1, 3, 5 e 8% em massa de argila. O efeito do cisalhamento sobre a morfologia dos nanocomp?sitos foi avaliado por DRX, MEV e MET. Para avaliar o efeito da adi??o de argila na matriz de PMMA foram investigadas propriedades t?rmicas e mec?nicas, atrav?s de an?lises de TG, DSC, HDT, VICAT, tra??o e impacto. Ensaios de inflamabilidade foram tamb?m realizados para investigar o efeito da adi??o de argila sobre as propriedades de retardo de chama. As an?lises morfol?gicas mostraram a presen?a de aglomerados de argila distribu?dos na matriz de PMMA, o que resultou na redu??o de propriedades como estabilidade t?rmica, resist?ncia mec?nica e ao impacto, e elevou a taxa de queima para os materiais processados por ambas as rotas de extrus?o

Made available in DSpace on 2014-12-17T14:07:15Z (GMT). No. of bitstreams: 1 MaraTST_DISSERT.pdf: 2071273 bytes, checksum: 9636b6602dd1a469f78b17d077ba757f (MD5) Previous issue date: 2013-03-04 / In recent decades have seen a sharp growth in the study area of nanoscience and nanotechnology and is included in this area, the study of nanocomposites with self-cleaning properties. Since titanium dioxide (TiO2) has high photocatalytic activity and also antimicrobial, self-cleaning surfaces in your application has been explored. In this study a comparison was made between two synthesis routes to obtain TiO2 nanoparticles by hydrothermal method assisted by microwave. And after analysis of XRD and SEM was considered the best material for use in nanocomposites. It was deposited nanocomposite film of poly (dimethyl siloxane) (PDMS) with 0.5, 1, 1.5 and 2% by weight of nanoparticles of titanium dioxide (TiO2) by the spraying method. The nanocomposite was diluted with hexane and the suspension was deposited onto glass substrate, followed by curing in an oven with forced air circulation. The photocatalytic activity of the nanocomposite impregnated with methylene blue was evaluated by UV- vis spectroscopy from the intensity variation of absorption main peak at 660nm with time of exposure to the UV chamber. Changes in the contact angle and microhardness were analyzed before and after UV aging test. The effect of ultraviolet radiation on the chemical structure of the PDMS matrix was evaluated by spectrophotometry Fourier transform infrared (FTIR).The results indicated that the addition of TiO2 nanoparticles in the coating PDMS gave high photocatalytic activity in the decomposition of methylene blue, an important characteristic for the development of self-cleaning coatings / Nas ?ltimas d?cadas tem-se observado um crescimento acentuado no estudo da ?rea de nanoci?ncia e nanotecnologia em que inclui-se nessa ?rea, o estudo de nanocomp?sitos com propriedades autolimpantes. Desde que o di?xido de tit?nio (TiO2) apresenta alta atividade fotocatal?tica e tamb?m, atividade antimicrobiana, sua aplica??o em superf?cies autolimpantes tem sido amplamente explorada. Neste trabalho foi feito uma compara??o entre duas rotas de s?ntese para obten??o de nanopart?culas de TiO2 pelo m?todo hidrot?rmico assistido por micro-ondas. Ap?s an?lise de DRX e MEV foi analisado o melhor material para aplica??o em nanocomp?sitos. Foram depositados filmes de nanocomp?sito de poli(dimetil siloxano) (PDMS) com 0,5, 1, 1,5 e 2% em massa de nanopart?culas de di?xido de tit?nio (TiO2) pelo m?todo de aspers?o. O nanocomp?sito foi dilu?do em hexano e a suspens?o foi depositada sobre l?minas de vidro, seguida de cura em estufa com circula??o for?ada de ar. A atividade fotocatal?tica do nanocomp?sito impregnado com azul de metileno foi avaliada pela t?cnica de espectroscopia de UV-V?sivel, a partir da varia??o da intensidade de absor??o do pico principal a 660 nm com o tempo de exposi??o em c?mara UV. Altera??es no ?ngulo de contato e na microdureza foram analisadas antes e ap?s o ensaio de envelhecimento UV. O efeito da radia??o ultravioleta na estrutura qu?mica da matriz de PDMS foi avaliado por espectrofotometria no infravermelho por transformada de Fourier (FTIR). Os resultados indicaram que a adi??o das nanopart?culas de TiO2 em PDMS conferiram ao revestimento boa atividade fotocatal?tica na decomposi??o do azul de metileno, caracter?stica importante para o desenvolvimento de revestimentos autolimpantes

Made available in DSpace on 2014-12-17T14:07:18Z (GMT). No. of bitstreams: 1 LourdesARR_TESE.pdf: 12458480 bytes, checksum: 0efd4ff8bfb0c0bf6bcd3c18e449a690 (MD5) Previous issue date: 2013-05-17 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Nacomposites of polymers and lamellar clayminerals, has generated high scientific and technological interest, for having mechanical properties and gas barriers differentiated of polymers and conventional composites. In this work, it was developed nanocomposites by single screw extruder and injection, utilizing commercial raw material, with the goal to investigate the quality of new developed materials. It was evaluated the influence of the content and the kind of clay in the structure and in the nanocomposites properties. It was used regular and elastomeric poly (methyl methacrylate) (Acrigel LEP 100 and Acrigel ECP800) and six montmorillonites (Cloisite 10A, 11B, 15A, 20A, 25A e 30B) at the concentration of 1% e 3% in weight. The nanocomposites were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA), transmission electron microscopy (TEM), colorimetric, optical transparency, flexural and tensile tests, Rockwell hardness and esclerometry. It was founded that is possible to obtain intercalated and exfoliated nanocomposites PMMA/MMT, and the top results was obtained in the materials with 1%in clay weight organophilizated with 2M2HT (Cloisite 15A and 20A) presented intercalate and hybrid morphology (exfoliated and flocullated). The ones that was produced with organophilizated clay with 2MHTL8 (Cloisite 30B) had excellent visual quality, but the majority presented hybrid morphology. In the materials processed with organophilizated clay with MT2ETOH (Cloisite 30B), there were color change and loss of transparency. It occurs improvement in a few mechanical properties, mainly in the materials produced with PMMA elastomeric (Acrigel ECP800), being more significant, the increase in the resistance to stripping in those nanocomposites / Nanocomp?sitos de pol?meros e argilominerais lamelares t?m gerado alto interesse cient?fico e tecnol?gico por possu?rem propriedades mec?nicas e de barreira ? g?s diferenciadas de pol?meros e de comp?sitos convencionais. Neste trabalho, foram desenvolvidos nanocomp?sitos por meio de extrusora monorosca e injetora, utilizando mat?rias-primas comerciais, com a finalidade de investigar a qualidade dos novos materiais desenvolvidos. Foi avaliada a influ?ncia do teor e do tipo de argila na estrutura e nas propriedades dos nanocomp?sitos. Foram usados PMMA comum e elastom?rico (Acrigel? LEP100 e Acrigel? ECP800) e seis argilas montmorilonitas (Cloisite? 10A, 11B, 15A, 20A, 25A e 30B) nas concentra??es de 1% e 3% em peso. Os nanocomp?sitos foram caracterizados por difra??o de raios X (DRX), termogravimetria (TGA), microscopia eletr?nica de transmiss?o (MET), colorimetria, transpar?ncia ?ptica, ensaios de tra??o uniaxial, flex?o, dureza Rockwell e esclerometria. Constatou-se que ? poss?vel obter nanocomp?sitos PMMA/MMT intercalados e esfoliados, sendo os melhores resultados obtidos nos materiais processados com 1% em peso de argilas organofilizadas com 2MBHT (Cloisite? 10A e 11B). Materiais produzidos com argilas organofilizadas com 2M2HT (Cloisite? 15A e 20A) apresentaram morfologia intercalada e h?brida (esfoliada e floculada). J? os produzidos com argilas organofilizadas com 2MHTL8 (Cloisite? 25A) tiveram excelente qualidade visual, por?m a maioria apresentou morfologia h?brida. Nos materiais processados com argilas organofilizadas com MT2ETOH (Cloisite? 30B) houve altera??o na cor e perda da transpar?ncia. Houve melhoria em algumas propriedades mec?nicas, principalmente nos materiais produzidos com PMMA elastom?rico (Acrigel? ECP800), sendo mais significativo, o aumento na resist?ncia ao riscamento nesses nanocomp?sitos

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-04-22T21:40:21Z No. of bitstreams: 1 EvansPaivaDaCostaFerreira_TESE.pdf: 4808121 bytes, checksum: 445ac97bb5a954c9963c5839ef4da0e9 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-04-22T21:56:58Z (GMT) No. of bitstreams: 1 EvansPaivaDaCostaFerreira_TESE.pdf: 4808121 bytes, checksum: 445ac97bb5a954c9963c5839ef4da0e9 (MD5) / Made available in DSpace on 2016-04-22T21:56:58Z (GMT). No. of bitstreams: 1 EvansPaivaDaCostaFerreira_TESE.pdf: 4808121 bytes, checksum: 445ac97bb5a954c9963c5839ef4da0e9 (MD5) Previous issue date: 2015-07-03 / Comparados aos comp?sitos convencionais, os nanocomp?sitos de matriz polim?rica apresentam tipicamente ganhos de propriedades com uma fra??o de volume de fase dispersa significativamente menor. Estudos publicados na literatura indicam que a adi??o de nanosilicatos pode aumentar a resist?ncia ? propaga??o de chamas de pol?meros. Neste trabalho, um processo de tratamento de argila nanom?trica do tipo montmorilonita (MMT) e o efeito da sua adi??o na propaga??o de chamas da resina estervin?lica foram estudados. A pesquisa foi desenvolvida em duas etapas. A primeira consistiu na purifica??o e ativa??o da argila coletada de uma jazida natural para permitir a sua compatibiliza??o com a resina polim?rica. Uma modifica??o da argila com acetato de s?dio foi tamb?m estudada para melhorar a dispers?o do particulado no pol?mero. A etapa seguinte focou no estudo do efeito da adi??o da argila tratada nas propriedades dos nanocomp?sitos. Nanocomp?sitos com percentuais de argila de 1%, 2%, 4% em massa foram processados. Na caracteriza??o da argila utilizaram-se as t?cnicas de fluoresc?ncia de raios X (FRX), difra??o de raios X (DRX), termogravimetria (TG), calorimetria explorat?ria diferencial (DSC), an?lise de ?rea superficial (BET) e espectroscopia de infravermelho por transformada de Fourier (FTIR). Na caracteriza??o dos nanocomp?sitos foram utilizadas as t?cnicas de termogravimetria (TG), calorimetria explorat?ria diferencial (DSC), espectroscopia de infravermelho (FTIR), microscopia eletr?nica de varredura (MEV), microscopia eletr?nica de transmiss?o (MET), al?m da determina??o da resist?ncia ? tra??o, m?dulo de elasticidade e resist?ncia ? propaga??o de chamas. De acordo com os resultados obtidos, o tratamento de purifica??o e ativa??o da montmorilonita desenvolvido neste trabalho com secagem da argila por liofiliza??o mostrou-se eficiente para promover sua compatibiliza??o e dispers?o na matriz polim?rica como comprovado pela caracteriza??o dos nanocomp?sitos. Observou-se ainda que a modifica??o da argila por meio de acetato de s?dio n?o produziu impacto significativo como compatibilizante da argila com o pol?mero. A adi??o da MMT tratada resultou em uma redu??o de at? 53% na velocidade de propaga??o de chama do pol?mero e n?o produziu altera??o na resist?ncia mec?nica ? tra??o e m?dulo de elasticidade do pol?mero, o que indica compatibiliza??o entre argila e pol?mero. A efici?ncia na redu??o de velocidade de propaga??o de chamas atingiu um pico para os nanocomp?sitos com 2% de argila, indicando ser este o valor ?timo de concentra??o de argila para esta propriedade. Em resumo, o tratamento de argila montmorilon?tica desenvolvido neste trabalho permite a produ??o de nanocomp?sitos de matriz estervin?lica com propriedade de retardo de propaga??o de chamas sem comprometimento de suas propriedades mec?nicas / Compared to conventional composites, polymer matrix nanocomposites typically exhibit enhanced properties at a significantly lower filler volume fraction. Studies published in the literature indicate t hat the addition of nanosilicate s can increase the resistance to flame propagation in polymers. In this work, a treatment of montmorillonite (MMT) nano clay and the effect of its ad dition o n flame propagation characteristics of vinyl ester were studied. The resea rch was conducted in two stages. The first stage focused on the purification and activation of the MMT clay collected from a natural deposit to improve compatibility with the polymer matrix . Clay modification with sodium acetate was also studied to improve particle dispersion in the polymer. The second step was focused on the effect of the addition of the treated clay on nanocomposites ? properties. Nanocomposites with clay con tents of 1, 2, 4 wt. % were processed. T he techniques for the characterization of the clay included X - ray fluorescence (XRF), X - r ay d iffraction (XRD), thermogravimetric a nalysis (TGA), d ifferential scanning c alorimetry (DSC) , s urface area (BET) and Fourier transform infrared spectroscopy (FTIR). For t he characterization of the nanocomposites , the techniques used were thermogravimetric a nalysis (TGA) , differential scanning c alorimetry (DSC), Fourier transform infrared spectroscopy (FTIR) , scanning electron mi croscopy (SEM), transmission electron m icroscopy (TEM), and the determination of tensile strength, modulus of elasticity and resistance to flame propagation. According to the results, the purification and activation treatment with freeze - drying used in thi s work for the montmorillonite clay was efficient to promote compatibility and dispersion in the polymer matrix as evidenced by the characterization of the nanocomposite s . It was also observed that the clay modifica tion using sodium acetate did not produce any significant effect to improve compatibilization of the clay with the polymer. The addition of the treated MMT resulted in a reduction of up to 53% in the polymer flame propagation speed and did not affect the mechanical tensile strength and modulus o f elas ticity of the polymer, indicating compatibility between the clay and polymer. The effectiveness in reducing flame propagation speed peaked for nanocomposites with 2 wt. % clay, indicating that this is the optimum clay concentration for this property. T he clay treatment used in this work enables the production of vinylester matrix nanocomposites with flame - retardancy properties .

Submitted by Setor de Tratamento da Informa??o - BC/PUCRS (tede2@pucrs.br) on 2015-06-19T11:25:03Z No. of bitstreams: 1 470698 - Texto Completo.pdf: 3211899 bytes, checksum: 304adc552bbe30591d967a6721608b0c (MD5) / Made available in DSpace on 2015-06-19T11:25:03Z (GMT). No. of bitstreams: 1 470698 - Texto Completo.pdf: 3211899 bytes, checksum: 304adc552bbe30591d967a6721608b0c (MD5) Previous issue date: 2015-03-23 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior - CAPES / The research work is related to the preparation of polymer composites based on polyaniline (PAni) and graphite. Polyaniline nanofibers were synthesized by the method of rapid mixing. Hybrid load (PAni/NLG) was synthesized by polymerizing aniline in the presence of graphite nanosheets (NLG). Polymer composites were prepared using differents methodologies: melt blending and in situ polymerization. In preparing polymer composites of polyethylene (PE)/PAni, PE/NLG and PE/PAni/NLG by in situ polymerization, the catalyst system was used Cp2ZrCl2/MAO. Polymeric composites by melt blending with the melt PE and conductive load were prepared in the melting chamber. The conductive loads as well as those produced composites were characterized by Scanning Electron Microscopy (SEM), TGA (Thermogravimetric Analysis), DSC (Differential Scanning Calorimetry) and electrical properties (Probe Two Tips). Rapid mixing, nanofiber synthesis methodology was efficient, as were prepared nanofibers with a diameter of approximately 50-80 nm and with yield of the synthesis reaction of 23%. From the results it was found that the in situ polymerization was the most suitable method to produce polymeric composites in the presence of polyaniline, as the composite exhibited good load dispersion inducing the formation of the conductive network. The presence of graphite in hybrid material improves electrical conductivity of composites and the quality of nanofibers is affected positively. The methodology of the mixture by melting was not efficient to disperse the nanofiber Pani in PE matrix. / O trabalho de pesquisa est? relacionado com a prepara??o de comp?sitos de polietileno (PE) contendo carga condutiva baseadas na polianilina (PAni) e grafite. Nanofibras de PAni foram sintetizadas atrav?s do m?todo da mistura r?pida. Carga h?brida (PAni/NLG) foi sintetizada por meio da polimeriza??o da anilina na presen?a de nanol?minas de grafite (NLG). Comp?sitos foram preparados utilizando-se diferentes metodologias: mistura por fus?o e polimeriza??o in situ. Na prepara??o de comp?sitos polim?ricos de polietileno (PE)/PAni, PE/NLG e PE/PAni/NLG, por meio da polimeriza??o in situ, foi utilizado sistema catal?tico Cp2ZrCl2/MAO. As cargas condutivas assim como os comp?sitos produzidos foram caracterizados por MEV (Microscopia Eletr?nica de varredura), TGA (An?lise Termogravim?trica), DSC (Calorimetria Diferencial de Varredura) e propriedades el?tricas (Sonda de Duas Pontas). A intera??o entre a PAni e o sistema catal?tico Cp2ZrCl2/MAO foi investigada atrav?s da T?cnica da Voltametria C?clica e de Pulso Diferencial. A mistura r?pida, metodologia de s?ntese de nanofibras mostrou-se eficiente, pois foram preparadas nanofibras com di?metro de aproximadamente 50-80 nm e com rendimento de rea??o de 23%. A partir dos resultados constatou-se que a polimeriza?ao in situ foi a metodologia mais adequada para produzir comp?sitos polim?ricos na presen?a de PAni, visto que os comp?sitos apresentaram boa dispers?o da carga induzindo ? forma??o da rede condutiva. A presen?a de grafite no material h?brido melhora a condutividade el?trica dos comp?sitos e a qualidade das nanofibras ? afetada positivamente. A metodologia da mistura por fus?o n?o foi eficiente para dispersar as nanofibras de Pani na matriz de PE.

Made available in DSpace on 2014-12-17T14:07:16Z (GMT). No. of bitstreams: 1 AntonioCAM_DISSERT.pdf: 2526278 bytes, checksum: 858d8dc4858eb48a9d6ce6faab8763d4 (MD5) Previous issue date: 2014-02-26 / Universidade Federal do Rio Grande do Norte / Epoxy based nanocomposites with 1 wt % and 3 wt % of nanographite were processed by high shear mixing. The nanographite was obtained by chemical (acid intercalation), thermal (microwave expansion) and mechanical (ultrasonic exfoliation) treatments. The mechanical, electrical and thermal behavior of the nanocomposites was determined and evaluated as a function of the percentage of reinforcement. According to the experimental results, the electrical conductivity of epoxy was not altered by the addition of nanographite in the contents evaluated. However, based on the mechanical tests, nanocomposites with addition of 1 wt.% and 3 wt.% of nanographite showed increase in tensile strength of 16,62 % and 3,20 %, respectively, compared to the neat polymer. The smaller increase in mechanical strength of the nanocomposite with 3 wt.% of nanographite was related to the formation of agglomerates. The addition of 1 wt.% and 3 wt.% of nanographite also resulted in a decrease of 6,25 % and 17,60 %, respectively, in the relative density of the material. Thus, the specific strength of the nanocomposites was approximately 33,33 % greater when compared to the neat polymer. The addition of 1 wt.% and 3 wt.% of nanographite in the material increased the mean values of thermal conductivity in 28,33 % and 132,62 %, respectively, combined with a reduction of 26,11 % and 49,80 % in volumetric thermal capacity, respectively. In summary, it has been determined that an addition of nanographite of the order of 1 wt.% and 3 wt.% produced notable elevations in specific strength and thermal conductivity of epoxy / Nanocomp?sitos a base de resina ep?xi e nanografite foram processados por mistura de alto cisalhamento, com concentra??es de 1 % e 3 % p/p de refor?o. O nanografite foi obtido atrav?s de tratamentos: qu?mico (intercala??o ?cida), t?rmico (expans?o por microondas) e mec?nico (esfolia??o por ultrassom). Os comportamentos mec?nico, el?trico e t?rmico dos materiais obtidos foram analisados em fun??o da porcentagem de refor?o. De acordo com os resultados obtidos, n?o foram verificadas altera??es na condutividade el?trica do ep?xi com a adi??o de nanografite, nos percentuais estudados. Entretanto, com base nos ensaios mec?nicos observou-se que os nanocomp?sitos com adi??o de 1 % p/p e 3 % p/p de grafite expandido apresentaram aumento na resist?ncia ? tra??o de 16,62 % e 3,20 % respectivamente, em rela??o ao pol?mero puro. O menor aumento de resist?ncia mec?nica para os nanocomp?sitos com 3 % p/p de nanografite foi relacionado com a forma??o de aglomerados. A adi??o de 1 % p/p e 3% p/p de nanografite tamb?m resultou em uma diminui??o de 6,25 % e 17,60 %, respectivamente, na densidade relativa do pol?mero. Portanto, a eleva??o da resist?ncia espec?fica dos nanocomp?sitos foi de aproximadamente 33,33% para os dois nanocomp?sitos, em rela??o ao pol?mero puro. A adi??o de 1 % p/p e 3 % p/p de nanografite no material aumentou os valores m?dios de condutividade t?rmica em 28,33 % e 132,62 %, respectivamente, combinado com uma redu??o de 26,11 % e 49,80 %, respectivamente, na capacidade t?rmica volum?trica. Em resumo, verificou-se que uma adi??o de nanografite da ordem de 1 % e 3 % p/p produziram eleva??es not?veis na resist?ncia mec?nica espec?fica e condutividade t?rmica do ep?xi

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-03-31T22:25:53Z No. of bitstreams: 1 JoaoPauloDeFreitasGrilo_DISSERT.pdf: 2371966 bytes, checksum: df286c50ea1a146c8169f0dc3c57c7f5 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-04-01T23:19:59Z (GMT) No. of bitstreams: 1 JoaoPauloDeFreitasGrilo_DISSERT.pdf: 2371966 bytes, checksum: df286c50ea1a146c8169f0dc3c57c7f5 (MD5) / Made available in DSpace on 2016-04-01T23:19:59Z (GMT). No. of bitstreams: 1 JoaoPauloDeFreitasGrilo_DISSERT.pdf: 2371966 bytes, checksum: df286c50ea1a146c8169f0dc3c57c7f5 (MD5) Previous issue date: 2015-06-25 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior - CAPES / Comp?sitos NiO-C0.9Gd0.1O1.95 (NiO-CGO), um dos materiais mais utilizado para fabrica??o de anodos de C?lulas a Combust?veis de ?xido S?lido (CCOS) atualmente, foram obtidos por uma rota qu?mica que consiste na mistura das solu??es precursoras das fases NiO e CGO previamente obtidas pelo m?todo Pechini, com percentual m?ssico da fase NiO variando entre 0 e 100 %. Os nanop?s como obtidos foram caracterizados por t?cnicas de an?lise t?rmica (termogravimetria e Calorimetria Diferencial Explorat?ria) e os materiais calcinados foram estudados por difratometria de raios X (DRX). Amostras sinterizadas entre 1400 e 1500 ?C por 4 h foram caracterizadas pelo m?todo de Arquimedes. Os efeitos da composi??o relativa na microestrutura e propriedades el?tricas (condutividade e energia de ativa??o) de comp?sitos sinterizados a 1500 ?C foram investigados por microscopia eletr?nica e espectroscopia de imped?ncia (entre 300 e 650 ?C em ar). O refinamento dos dados de DRX indicaram que os p?s s?o ultrafinos e que o tamanho do cristalito da fase CGO tende a diminuir com o aumento de teor de NiO. De maneira semelhante, o cristalito da fase NiO tende a diminuir com o aumento da concentra??o de CGO, principalmente acima de 50% em massa de CGO. A an?lise por Arquimedes evidencia uma varia??o na densidade relativa em fun??o do teor de NiO. Densidades relativas acima de 95% foram obtidas em comp?sitos contendo a partir de 50 % em massa de NiO e sinterizados entre 1450 e 1500 ?C. Os resultados de microscopia e espectroscopia de imped?ncia indicam que a partir de 30 - 40 % de NiO h? aumento do n?mero de contatos NiO-NiO, ativando o mecanismo de condu??o eletr?nica que governa o processo de condu??o a baixas temperaturas (300-500 ?C). Por outro lado, com o aumento da temperatura de medida a mobilidade das vac?ncias de oxig?nio torna-se maior que a dos buracos eletr?nicos do NiO, como resultado, a condutividade de alta temperatura (550 - 650 ?C) em comp?sitos contendo at? 30-40% de NiO ? inferior ? do CGO. Varia??es na energia de ativa??o confirmam mudan?a do mecanismo de condu??o com o aumento do teor de NiO. O comp?sito contendo 50 % em massa de cada fase apresenta condutividade de 19 mS/cm a 650 ?C (pouco superior a 13 mS/cm encontrada para o CGO) e energia de ativa??o 0,49 eV. / Composite NiO-C0.9Gd0.1O1.95 (NiO-GDC), one of the materials most used for the manufacture of anodes of Cells Solid Oxide Fuel (SOFC) currently, were obtained by a chemical route which consists in mixing the precursor solution of NiO and CGO phases obtained previously by the Pechini method. The nanopowders as-obtained were characterized by thermal analysis techniques (thermogravimetry and Differential Scanning Calorimetry) and calcined materials were evaluated by X-ray diffraction (XRD). Samples sintered between 1400 and 1500 ? C for 4 h were characterized by Archimedes method. The effects of the composition on the microstructure and electrical properties (conductivity and activation energy) of the composites sintered at 1500 ? C were investigated by electron microscopy and impedance spectroscopy (between 300 and 650 ? C in air). The refinement of the XRD data indicated that the powders are ultrafine and the crystallite size of the CGO phase decreases with increasing content of NiO. Similarly, the crystallite of the NiO phase tends to decrease with increasing concentration of CGO, especially above 50 wt % CGO. Analysis by Archimedes shows a variation in relative density due to the NiO content. Densities above 95% were obtained in samples containing from 50 wt % NiO and sintered between 1450 and 1500 ?C. The results of microscopy and impedance spectroscopy indicate that from 30-40 wt.% NiO there is an increase in the number of contacts NiO - NiO, activating the electronic conduction mechanism which governs the process of conducting at low temperatures (300 - 500 ?C). On the other hand, with increasing the measuring temperature the mobility of oxygen vacancies becomes larger than that of the electronic holes of NiO, as a result, the high temperature conductivity (500-650 ? C) in composites containing up to 30-40 wt.% of NiO is lower than that of CGO. Variations in activation energy confirm change of conduction mechanism with the increase of the NiO content. The composite containing 50 wt. % of each phase shows conductivity of 19 mS/cm at 650 ?C (slightly higher than 13 mS/cm found for CGO) and activation energy of 0.49 eV.