Development and characterization of Poly(L-lactic acid) (PLLA) platforms for bone tissue engineering

The development of scaffolds based on biomaterials is a promising strategy for Tissue Engineering and cellular regeneration. This work focuses on Bone Tissue Engineering, the aim is to develop electrically tailored biomaterials with different crystalline and electric features, and study their impacts onto cell biological behavior, so as to predict the materials output in the enhancement of bone tissue regeneration. It is accepted that bone exhibits piezoelectricity, a property that has been proved to be involved in bone growth/repair mechanism regulation. In addition electrical stimulations have been proved to influence bone growth and repair. Piezoelectric materials are therefore widely investigated for a potential use in bone tissue engineering. The main goal is the development of novel strategies to produce and employ piezoelectric biomaterials, with detailed knowledge of mechanisms involved in cell-material interaction. In the current work, poly (L-lactic) acid (PLLA), a synthetic semi-crystalline polymer, exhibiting biodegradibility, biocompatibility and piezoelectricity is studied and proposed as a promoter of enhanced tissue regeneration. PLLA has already been approved for implantation in human body by the Food and Drug Administration (FDA), and at the moment it is being used in several clinical strategies. The present study consists of first preparing films with different degrees of crystallinity and characterizing these PLLA films, in terms of surface and structural properties, and subsequently assessing the behavior of cells in terms of viability, proliferation, morphology and mineralization for each PLLA configuration. PLLA films were prepared using the solvent cast technique and submitted to different thermal treatments in order to obtain different degrees of crystallinity. Those platforms were then electrically poled, positively and negatively, by corona discharge in order to tailor their electrical properties. The cellular assays were conducted by using two different osteoblast cell lines grown directly onto the PLLA films:Human osteoblast Hob, a primary cell culture and Human osteosarcoma MG-63 cell line. This thesis gives also a comprehensive introduction to the area of Bone Tissue Engineering and provides a review of the work done in this field in the past until today, in that same field, including the one related with bone’s piezoelectricity. Then the experimental part deals with the effects of the crystallinity degrees and of the polarization in terms of surface properties and cellular bio assays. Three different degrees of crystallinity, and three different polarization conditions were prepared; which results in 9 different configurations under investigation.

Fumonisina B1 em arroz: validação de método e efeito de tratamento térmico nos níveis da micotoxina

O arroz (Oryza sativa, L.), como todos os cereais, pode ser contaminado por fungos responsáveis por danos tecnológicos, nutricionais e toxicológicos, dentre eles a produção de micotoxinas. Diversas toxinas fúngicas produzidas pelo gênero Fusarium tem sido relatadas em arroz, no entanto a fumonisina B1 (FB1) é pouco estudada neste grão. As principais características da FB1 é a alta solubilidade em solventes polares, estabilidade a altas temperaturas além de efeitos neurotóxicos e carcinogênicos. Assim o objetivo deste trabalho foi avaliar o efeito do tratamento térmico e hidrotérmico nos teores de fumonisina B1 e nas características químicas de arroz comercial. Na primeira etapa do trabalho foi adaptado um método para detecção e quantificação de FB1 em arroz cru e após cocção, por HPLC-FL. O método foi avaliado quanto aos indicativos de eficiência destacando-se o LOD (30 µg.kg-1) e a recuperação ( 90% para arroz cru e 86% pra arroz cozido). Na segunda etapa realizou-se o levantamento de ocorrência de FB1 em 05 diferentes amostras comerciais de arroz integral, branco e parboilizado da cidade de Rio Grande, RS, totalizando 9 amostras. Foi detectada a presença de FB1 em 7 das 9 amostras, sendo que os maiores índices foram encontrados em amostras de arroz parboilizado e integral apresentando níveis de contaminação entre 30 e 170 µg.kg-1. A terceira etapa do trabalho consistiu no estudo do efeito de tratamentos térmicos sobre os níveis de FB1 em amostras após aplicação de calor. Foram testados tratamento hidrotérmico com evaporação, tratamento hidrotérmico com autoclavagem e tratamento térmico seco. O maior nível de redução dos teores iniciais de FB1 foi 82,8% quando se empregou tratamento térmico seco a 125 °C/3 min. Ainda foram avaliados os efeitos do t ratamento hidrotérmico com evaporação de água na composição química e na digestibilidade protéica. Esta característica proporcionou aumento de até 100% na digestibilidade in vitro das proteínas e reduziu em média 73% do teor de contaminação com FB1.

Desenvolvimento de indicadores enzimáticos inteligentes para monitoramento da qualidade de alimentos

A dificuldade em conhecer o histórico de temperatura de um alimento, desde sua produção até o consumo, torna difícil prever sua verdadeira vida-útil. O uso de indicadores de tempo e temperatura (ITT) pode ser uma alternativa inovadora empregada para garantir a validade de produtos de forma dinâmica. Assim, este trabalho visa desenvolver novos indicadores enzimáticos de tempo e temperatura para monitorar a qualidade de alimentos perecíveis durante o seu processamento e armazenamento, baseados na reação de complexação entre o amido e o iodo (azul), e na posterior atuação de uma enzima amilase sobre esse complexo, para causar uma redução da intensidade da cor azul a uma taxa dependente do tempo e da temperatura de armazenagem. Os sistemas inteligentes propostos possuem versatilidade de atuação em função do tipo e quantidade de amilase empregada. Desta forma, foi utilizada uma amilase termoestável para a formulação de um indicador inteligente de processamento, utilizado para o controle de tratamentos térmicos industriais (pasteurização);e uma amilase termosensível na formulação de um indicador de armazenamento, empregada para o controle das condições de temperatura durante a cadeia de frio de produtos perecíveis. Na elaboração dos ITT de processamento foram realizadas simulações em laboratório e testes em planta fabril, os quais avaliaram diferentes concentrações de amilase termoestável nos protótipos de ITT quando submetidos as condições de tempo e temperatura de pasteurização. Os resultados evidenciaram que a resposta de cor dos indicadores foi visualmente interpretada, como adaptável à medição usando equipamentos, apresentando boa reprodutibilidade em todas as condições estudadas. O ITT contendo 6,5 % de amilase termoestável (penzima/pamido) foi aquele cujo resultado melhor se adequou à utilização na validação de cozimento de presunto. Nesta condição, o protótipo anexado à embalagem primária do produto indicou o processo de pasteurização de forma fácil, precisa e não destrutiva. Já durante o desenvolvimento do ITT de armazenamento foram realizadas simulações em laboratório, testes em planta fabril e ponto de venda, os quais avaliaram o uso de diferentes concentrações de amilase termosensível nos protótipos de ITT quando submetidos a diversas condições de cadeia de frio. Os resultados evidenciaram que devido à possibilidade de definir a vida-útil destes protótipos variando as concentrações de enzima termosensível, os indicadores podem ser facilmente adaptados para controlar as condições de temperatura durante a cadeia de diversos alimentos perecíveis. O protótipo contendo 60 % de amilase termosensível (penzima/pamido) foi aquele cujo resultado melhor se adequou à utilização no controle da cadeia avícola. Assim, o ITT indicou visualmente o histórico de tempo e temperatura de produtos à base de frango de forma fácil e precisa. Os resultados obtidos na avaliação das percepções dos consumidores frente ao emprego de indicadores inteligentes em embalagens alimentícias mostraram que o uso de ITT é uma inovação receptiva, com consequente aceitação e intenção de compra elevada pela população brasileira. Assim, com este trabalho espera-se contribuir efetivamente para que o conceito de embalagens inteligentes possa ser aceito comercialmente e que sejam estabelecidas no Brasil normas que regulamentem seu uso, conferindo benefícios à conservação de grande variedade de alimentos.

Efeito do tratamento térmico do titânio sobre a proliferação de células pré-osteoblásticas

Titanium is a biomaterial widely employed in biomedical applications (implants, prostheses, valves, stents). Several heat treatments are usually used in order to obtain physical properties required to different applications. This work studied the influence of the heat treatment on microstructure of commercial pure titanium, and their consequences in growth and proliferation of MC3T3-E1 cells. Discs of titanium were treated in different temperatures, and characterized by optical microscopy, image analysis, wettabillity, roughness, hardness and X-ray diffraction. After the heat treatment, significant modifications in these properties were observed. Pattern images of titanium, before and after the cell culture, were compared by overlapping to analyze the influence of microstructure in microstructure and preferences guidance cells. However, in general, titanium discs that showed a higher residual strength also presented an increase of cells numbers on surface

Estudo da sinterização do aço inox 316L reforçado com 3% Carbeto de Tântalo - TaC

The present work shows a contribution to the studies of development and solid sinterization of a metallic matrix composite MMC that has as starter materials 316L stainless steel atomized with water, and two different Tantalum Carbide TaC powders, with averages crystallite sizes of 13.78 nm and 40.66 nm. Aiming the metallic matrix s density and hardness increase was added different nanometric sizes of TaC by dispersion. The 316L stainless steel is an alloy largely used because it s high resistance to corrosion property. Although, its application is limited by the low wear resistance, consequence of its low hardness. Besides this, it shows low sinterability and it cannot be hardened by thermal treatments traditional methods because of the austenitic structure, face centered cubic, stabilized mainly in nickel presence. Steel samples added with TaC 3% wt (each sample with different type of carbide), following a mechanical milling route using conventional mill for 24 hours. Each one of the resulted samples, as well as the pure steel sample, were compacted at 700 MPa, room temperature, without any addictive, uniaxial tension, using a 5 mm diameter cylindrical mold, and quantity calculated to obtain compacted final average height of 5 mm. Subsequently, were sintered in vacuum atmosphere, temperature of 1290ºC, heating rate of 20ºC/min, using different soaking times of 30 and 60 min and cooled at room temperature. The sintered samples were submitted to density and micro-hardness analysis. The TaC reforced samples showed higher density values and an expressive hardness increase. The complementary analysis in optical microscope, scanning electronic microscope and X ray diffractometer, showed that the TaC, processed form, contributed with the hardness increase, by densification, itself hardness and grains growth control at the metallic matrix, segregating itself to the grain boarders

Obtenção e caracterização de nanopartículas de argilominerais

Natural nanoclays are of great interest particularly for the production of polymer-based nanocomposites. In this work, kaolinite clays from two natural deposits in the State of the Rio Grande do Norte and Paraiba were purified with thermal treatment and chemical treatments, and characterized. Front to the gotten data, had been proposals methodologies for elimination or reduction of coarse particle texts, oxide of iron and organic substance. These methodologies had consisted of the combination of operations with thermal treatments, carried through in electric oven, and acid chemical attacks with and hydrogen peroxide. The Analyzers Thermogravimetric was used to examine the thermal stability of the nanoclays. The analysis indicated weight losses at temperatures under 110 ºC and over the temperature range of 350 to 550 ºC. Based on the thermal analysis data, the samples were submitted to a thermal treatment at 500 °C, for 8 h, to remove organic components. The X-ray diffraction patterns indicated that thermal treatment under 500 °C affect the basic structure of kaolinite. The BET surface area measurements ranged from 32 to 38 m2/g for clay samples with thermal treatment and from 36 to 53 m2/g for chemically treated samples. Thus, although the thermal treatment increased the surface area, through the removal of organic components, the effect was not significant and chemical treatment is more efficient, not affect the basic structure of kaolinite, to improve particle dispersion. SEM analysis confirms that the clay is agglomerated forming micron-size particles

Sinterização de aço inoxidável reforçado com partículas nanométricas dispersas de carbeto de nióbio - NbC

Metal powder sintering appears to be promising option to achieve new physical and mechanical properties combining raw material with new processing improvements. It interest over many years and continue to gain wide industrial application. Stainless steel is a widely accepted material because high corrosion resistance. However stainless steels have poor sinterability and poor wear resistance due to their low hardness. Metal matrix composite (MMC) combining soft metallic matrix reinforced with carbides or oxides has attracted considerable attention for researchers to improve density and hardness in the bulk material. This thesis focuses on processing 316L stainless steel by addition of 3% wt niobium carbide to control grain growth and improve densification and hardness. The starting powder were water atomized stainless steel manufactured for Höganäs (D 50 = 95.0 μm) and NbC produced in the UFRN and supplied by Aesar Alpha Johnson Matthey Company with medium crystallite size 16.39 nm and 80.35 nm respectively. Samples with addition up to 3% of each NbC were mixed and mechanically milled by 3 routes. The route1 (R1) milled in planetary by 2 hours. The routes 2 (R2) and 3 (R3) milled in a conventional mill by 24 and 48 hours. Each milled samples and pure sample were cold compacted uniaxially in a cylindrical steel die (Ø 5 .0 mm) at 700 MPa, carried out in a vacuum furnace, heated at 1290°C, heating rate 20°C stand by 30 and 60 minutes. The samples containing NbC present higher densities and hardness than those without reinforcement. The results show that nanosized NbC particles precipitate on grain boundary. Thus, promote densification eliminating pores, control grain growth and increase the hardness values

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Mesoestruturas porosas a partir de materiais naturais

The MCM-41 mesoporous synthesis was done using rice hulls ash and chrysotile as natural alternative silica sources. For the using of these sources, chemical and thermic treatments were done in both materials. After chemical and thermic treatments, these materials were employed on the MCM-41 mesoctructures synthesis. The natural materials treated and employed in the synthesis were characterized by several techniques such as X-ray diffraction, N2 adsorption and desorption, scanning electronic microscopy and thermogravimetric analysis. MCM-41 standart samples synthetized with aerosil 200 commercial sílica were used to evaluation. The formed material from rice hulls ash showed values from BET specific area about 468 m².g-1, N2 adsorption and desorption isotherms and loss mass similar to reference materials. The silica from chrysotile calcined and leached was employed to mesoporous materials synthesis. The BET specific area showed values about 700 m².g-1, N2 adsorption and desorption isotherms type IV and loss mass similar to mesoporous materials. The formed material from calcined and leached chrysotile, without calcination, applied to phenol remotion carried high performance liquid chromatography and evaluated with organophilic clays with different treatments. By the characterization techniques were proved that mesoporous materials with lesser order that reference samples. The material formed from rice hulls ash without the calcination step achieved better adsorption results than organophilic clays

Tratamento térmico do titânio e suas consequências sobre as propriedades físico-químicas e de biocompatibilidade

The titanium and titanium alloys are widely used as biomaterial in biomedical device and so research have been developed aiming to improve and/or better to understand interaction biomaterial/biological environment. The process for manufacturing of this titanium implants usually involves a series of thermal and mechanical processes which have consequence on the final product. The heat treatments are usually used to obtain different properties for each application. In order to understand the influence of these treatments on the biological response of the surface, it was done, in this work, different heat treatments in titanium and analyzed their influence on the morphology, adhesion and proliferation of the pre-osteoblastic cells (MC3T3-E1). For such heat-treated titanium disks were characterized by optical microscopy, contact angle, surface energy, roughness, microhardness, X-ray diffraction and scanning through the techniques (BSE, EDS and EBSD). For the analysis of biological response were tested by MTT proliferation, adhesion by crystal violet and β1 integrin expression by flow cytometry. It was found that the presence of a microstructure very orderly, defined by a chemical attack, cells tend to stretch in the same direction of orientation of the material microstructure. When this order does not happen, the most important factor influencing cell proliferation is the residual stress, indicated by the hardness of the material. This way the disks with the highest level state of residual stress also showed increased cell proliferation

Membrana de alumina anódica: comportamento da microestrutura e estudo das propriedades ópticas após tratamento térmico

Thin commercial aluminum electrolytic and passed through reactions was obtained with anodic alumina membranes nanopores. These materials have applications in areas recognized electronic, biomedical, chemical and biological weapons, especially in obtaining nanostructures using these membranes as a substrate or template for processing nanowires, nanodots and nanofibers for applications noble. Previous studies showed that the membranes that have undergone heat treatment temperature to 1300° C underwent changes in morphology, crystal structure and optical properties. This aim, this thesis, a study of the heat treatment of porous anodic alumina membranes, in order to obtain and to characterize the behavior changes structures during the crystallization process of the membranes, at temperatures ranging between 300 and 1700° C. It was therefore necessary to mount a system formed by a tubular furnace resistive alumina tube and controlled environment, applying flux with special blend of Ag-87% and 13% N2, in which argon had the role of carrying out the oxygen nitrogen system and induce the closing of the pores during the densification of the membrane. The duration of heat treatment ranged from 60 to 15 minutes, at temperatures from 300 to 1700° C respectively. With the heat treatment occurred: a drastic reduction of porosity, grain growth and increased translucency of the membrane. For the characterization of the membranes were analyzed properties: Physical - thermogravimetric, X-ray diffraction, BET surface area; morphological - SEM, EDS through compositional and, optical absorbance, and transmittance in the UV-VIS, and FTIR. The results using the SEM showed that crystallization has occurred, densification and significant changes in membrane structure, as well as obtaining microtube, the BET analysis showed a decrease in specific surface area of the membranes has to 44.381 m2.g-1 to less than 1.8 m2.g-1 and in the analysis of transmittance and absorbance was found a value of 16.5% in the range of 800 nm, characteristic of the near infrared and FTIR have confirmed the molecular groups of the material. Thus, one can say that the membranes were mixed characteristics and properties which qualify for use in gas filtration system, as well as applications in the range of optical wavelength of the infra-red, and as a substrate of nanomaterials. This requires the continuation and deepening of additional study

Sistema de instrumentação mecanizada Hyflex EDM

A Endodontia é uma área em constante evolução. Consideráveis desenvolvimentos nos materiais e técnicas têm sido essenciais para o melhoramento dos resultados nos tratamentos realizados. É exemplo disso mesmo a constituição dos instrumentos Endodônticos primordiais, construídos em cordas de piano, com evolução para aço de carbono, material este que sofria corrosão provocado pelo cloro presente no hipoclorito de sódio. O aço de carbono evoluiu para aço inoxidável e deste as limas endodônticas passaram a ser feitas em níquel-titânio, conferindo-lhes melhor flexibilidade e efeito de memória de forma. Mesmo com todas estas melhorias significativas, fraturas de instrumentos e erros durante a instrumentação continuam a acontecer e com eles veio a necessidade da pesquisa de possíveis melhorias da constituição das limas em NiTi. Como resultado surgiram ligas como o M-wire, fase-R e CM-wire, criadas a partir de tratamentos térmicos, que trouxeram às limas Endodônticas maior flexibilidade e resistência à fratura que os instrumentos feitos em NiTi convencional. A mais recente evolução das limas Ni-Ti, desenvolvida pela Coltene Whaldent (Allstätten, Suiça), são as limas Hyflex EDM, limas para canais radiculares de 5ª geração. O seu processo de fabrico por eletroerosão cria uma superfície única fazendo com que estas limas sejam mais duras e resistam mais à quebra, aliado à sua alta flexibilidade. É possível assim reduzir o número de limas para a limpeza e modelagem dos canais durante os tratamentos endodônticos sem comprometer a preservação da anatomia dos canais. As limas Hyflex EDM possuem, tal como as limas Hyflex CM, o efeito de controle de memória (CM), o que confere propriedades muito similares entre os dois sistemas.

Perfil metabólico e ponderal de leitões submetidos a dietas com diferentes teores de fósforo em ambientes térmicos distintos

O objetivo deste trabalho foi avaliar o efeito de dietas com diferentes concentrações de fósforo disponível sobre o perfil metabólico e o peso corporal de leitões em fase inicial de crescimento, mantidos em ambientes térmicos distintos. Foram utilizados 120 leitões machos castrados, de linhagem comercial e com peso corporal médio de 15 kg. Os tratamentos consistiram de dietas com 0,107, 0,214, 0,321, 0,428 e 0,535% de fósforo disponível, e de dois ambientes: termoneutro e quente. O peso corporal foi determinado no início e no final da fase experimental, e amostras de sangue foram coletadas para a medição de eletrólitos, albumina, proteína total, substâncias nitrogenadas, fosfatase alcalina total e óssea, hormônios tireoidianos, glicose e lactato. Tanto as dietas quanto os ambientes produziram efeito sobre o ganho de peso corporal e sobre os valores de sódio, potássio, cálcio total, magnésio, fósforo, fosfatase alcalina total e óssea, T4 livre e lactato. O aumento nos teores de fósforo na dieta tem efeito positivo sobre o peso corporal, nos ambientes estudados, mas desequilibra as relações sanguíneas cálcio:fósforo. O estresse por calor diminui as concentrações de glicose, fosfatase alcalina total e T4 livre no sangue, e aumenta as de lactato. Parâmetros bioquímicos sanguíneos retratam o estado metabólico dos animais e podem ser usados para avaliação do balanço nutricional e para detecção precoce de alterações metabólicas.

Avaliação de tratamentos de superfície em diferentes sistemas cerâmicos e seu efeito na resistência de união a um cimento resinoso

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influência de tratamentos superficiais e termociclagem na resistência da união resina/metal

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)