Wastewater activated sludge is produced during the biological treatment of wastewater. After treating the sewage, the sludge is allowed to settle. Part of the settled material is returned to the treatment process as return activated sludge (RAS) and the excess is removed as waste activated sludge (WAS). The handling and disposal of the sludge are energy and capital-intensive treatments, with a significant environmental impact. This work studies the possibility to utilize RAS (an example of wastewater sludge) as a source of surface active agents. The results indicate that higly surface active materials can be extracted from RAS, and that the RAS extract has potential applications as a detergent and wood adhesive. The results also suggest that recovering a suite of products from RAS, a biological heterogenous source, can be technically feasible. An effective alkaline treatment was developed (at pH>12) that can extract up to 75% of the sludge’s organic matter, a yield higher than previously reported. Increasing the extraction pH increased the extract surface activity, which is linked to increasing the amount of higher molecular weight molecules and the presence of phospholipids. Increasing the extraction pH beyond 11 was also related to extensive cell lysis, increasing significantly the amount of recovered material and the surface activity of the extract. The alkaline extract has properties comparable to commercial detergents. Without further purification, the extract has a low surface tension (37 mN/m on average) and performs similarly to synthetic detergents. Further assessment of the RAS extract (insensitivity to pH, surface tension, interfacial tension) suggests that it may be suitable for commercial applications. The RAS extract can also be formulated into wood adhesives using glutaraldehyde as a crosslinker. The extract fraction with 10-50 kDa constituents at pH 9 achieves high adhesive shear strengths (4.5 MPa on average, at 30% relative humidity and 25°C) with 40% of wood failure. The adhesive strength of RAS-based adhesives is strongly correlated to its protein content.

The main aim of this research was to investigate the behaviour of adhesive joints exposed to repeated low-velocity impact i.e. impact fatigue (IF), and to compare this loading regime with standard fatigue (SF), i.e. non-impacting, constant amplitude, sinusoidal loading conditions. Two types of lap joint configuration using rubber toughened modified epoxy adhesives were used and exposed to various loading conditions in order to determine the fatigue behaviour of the joints for each load conditions. The fatigue life was investigated using bonded aluminium alloy (7075-T6) single lap joint (SLJ) specimens, where it was seen that IF is an extremely damaging load regime compared to SF. Different trends were visible in force-life plots for these two types of loading. In SF a gradual decrease in the fatigue life with increasing load was observed, whereas, in IF a significant decrease in life was seen at relatively modest levels of maximum force after relatively few cycles. Comparisons of the fatigue life show a considerably earlier failure in IF than in SF for comparable levels of force and energy. Additionally, it was demonstrated that the maximum force per cycle, loading time, stiffness and strength decreased as a result of damage generated in the sample during IF.

In vitro bond strength studies are of great importance and interest since they allow the prediction of clinical success of orthodontic adhesives. There are many studies that have investigated bond strength values of bonding systems. However, due to the variation in the materials and methods employed, it is very difficult and often impossible to make comparisons among data. The use of a substrate as an alternate to enamel for mechanical tests would minimize these variables and reduce the challenges faced with in vitro bond strength tests. The purpose of this study was to investigate the suitability of Macor as a substrate for bond strength testing of orthodontic adhesives. Macor samples were custom prepared in a shape similar to that of a human maxillary premolar. The groups tested were: Group 1: acid-etched with 9.6% hydrofluoric acid (HFA) for 60 seconds; Group 2: acid-etched with 9.6% HFA for 90 seconds; Group 3: acid-etched with 9.6% HFA for 120 seconds; Group 4: surface roughened with silicon carbide (Sic); and control group: human premolars etched with 37% phosphoric acid. Following surface preparation, samples were primed and brackets were bonded using Transbond XT (3MlUnitek). Mounted samples were stored in water for 24 hours at 37OC until mechanical testing. Brackets were debonded in the shear mode using an Instron Universal Testing Machine and the force at debond was recorded. The nature of adhesive bond failure among the groups was also compared using an adhesive remnant index (ARI). One-way ANOVA and Weibull analysis statistical tests were used to evaluate and compare the groups. Sample surfaces were analyzed under the light microscope to determine the mode of bond failure for ARI. The Kruskall-Wallis test was used to determine differences in the ARI scores. There were statistically significant differences in shear bond strengths among the enamel and Macor groups (p 0.05). The shear bond strength values of the Macor groups were significantly lower than those of the enamel control group, (p < 0.05). ARI scores were significantly different between the groups (p 10.0001); Macor samples treated with hydrofluoric acid had more adhesive remaining on their surfaces than those in the control and Sic groups. Based on the results of this study, Macor may not be a suitable substrate for bond strength testing in orthodontics.

Doctor of Philosophy / Department of Grain Science and Industry / Xiuzhi Susan Sun / Soy protein is one of the most promising bio-degradable adhesives, with great potential as alternatives synthetic petroleum based adhesives for wood composite industries. However, its intrinsic drawbacks such as low water resistance, high viscosity, and short shelf life still limit its broad application. In this research, soy protein was further modified and characterized to improve adhesion properties, flow-ability, water resistance, and long shelf life, which could facilitate the industrialization of soy protein based adhesives. In this study, we exploited the in situ sodium bisulfite (NaHSO3) modification on soy protein in soy flour-water extracts, and then the modified soy protein was obtained through acid precipitation. First, different concentrations of NaHSO3 were used to modify soy flour slurry, then glycinin-rich and β-conglycinin-rich fractions were precipitated at pH 5.4 (SP 5.4) and pH 4.5 (SP 4.5), respectively. Unmodified sample SP 5.4 and SP 4.5 showed clay-like properties and viscoelastic properties, respectively; whereas with addition of NaHSO3 in range of 2-8 g/L, both SP 5.4 and SP 4.5 had the viscous cohesive phase with good handability and flow-ability. The overall adhesion performance of SP 4.5 was better than SP 5.4; the wet strength of these two fractions was in the range of 2.5-3.2 MPa compared to 1.6 MPa of control soy protein isolate. Then soy protein with various β-conglycinin/glycinin (7S/11S) ratios were extracted from soy flour slurry and characterized for adhesion properties based on the different solubility of 7S and 11S globulins. Seven glycinin-rich soy protein fractions and six β- conglycinin-rich soy protein fractions were obtained. According to the morphology, viscosity, and particle size results, we proposed that proper protein-protein interaction, hydration capacity (glycinin-rich fractions), and certain 7S/11S ratios (β-conglycinin-rich fractions) in modified soy protein are crucial to continuous protein phase formation. The viscous cohesive samples were stable for up to several months without phase separation at room temperature, with the wet adhesion strength of 2.0-2.8 MPa. The soy protein modified with NaHSO3 showed good compatibility with commercial glues applied on plywood and paper labeling fields. The modified soy protein made some functional groups, carboxylic (-COOH), hydroxyl (-OH) and amino groups (-NH2) available, which cross-linked with hydroxymethyl groups (-CH2-OH) from urea formaldehyde (UF) wood glue. The modified soy protein (MSP) with pH 4.8 also acted as an acidic catalyst for the self-polymerization of UF based resin. The wet adhesion strength of MSP/UF blends (40/60) was 6.4 MPa with 100% wood cohesive failure, as compared to 4.66 MPa of UF. As to the paper labeling application, peel strength of MSP on glass substrate increased rapidly, with curing time much shorter than commercial polyvinyl acetate based adhesives (PVAc). And the MSP/ PVAc blends showed shorter curing time, higher water resistance and lower viscosity than pure PVAc. Chemical modification could also enhance the adhesion strength of MSP. 2-octen-1- ylsuccinic anhydride (OSA) was proved to be grafted on soy protein through reaction between amine, hydroxyl groups of protein and anhydride groups. The oily nature and hydrophobic long alkyl chains of OSA mainly contributed to the significant water resistance improvement of MSP.

O desenvolvimento de adesivos bioativos mostra-se como uma alternativa interessante para agregar benefícios aos novos materiais. O objetivo do estudo foi sintetizar nanopartículas de prata (NAg) e de hidroxiapatita (NHA), avaliar sua influencia no efeito antibacteriano, citotoxicidade de um adesivo com NAg e sua resistência de união à dentina associado ao uso de NHA. As nanopartículas foram caracterizadas por fluorescência de raio x por reflexão total (TRXF), difratometria de raio x (DRX), microscopia eletrônica de transmissão (TEM) e espalhamento de luz visível (DLS). O sistema Scotchbond Multi-Purpose (SBMP) foi modificado com adição de 0,05% e 0,1% de NAg no primer e no bond. Molares humanos foram restaurados com o sistema adesivo modificado após o pre-tratamento da dentina com suspensão aquosa de NHA a 0,5% e 1% para realização do ensaio de resistência de união imediata (24h) e após 1 ano de envelhecimento. A interface adesiva foi caracterizada por Microscopia Confocal Raman (MCR). Para mensurar o efeito antibacteriano (S.mutans) do adesivo com NAg foi realizado o ensaio de difusão em ágar com template e contagem de Unidades Formadoras de Colônias (UFC). A citotoxicidade foi avaliada com uso de células tronco da polpa dentária (DPSCs) em contato com adesivos não polimerizados e polimerizados em diferentes concentrações de meio condicionado (0% 25%, 75% e 100%). Foram produzidas NAg esféricas, com estrutura cúbica de face centrada, e com 16 nm de diâmetro médio. As NHA exibiram estrutura prismática com tamanho médio de 79,4 nm. O adesivo com NAg e o tratamento da dentina com NHA não afetaram a resistência de união imediata ou após 1 ano de envelhecimento, e as interfaces adesivas mostraram-se íntegras. Os adesivos modificados por NAg exibiram citotoxicidade similar ao adesivo controle e maior efeito antibacteriano. Os adesivos com adição de NAg são promissores quanto à obtenção de um material bioativo antimicrobiano que não altera a resistência de união ou a biocompatibilidade. / The development of bioactive adhesives is shown an interesting alternative to add benefits to the new materials. The aim of the study was to synthesize silver nanoparticles (NAg) and hydroxyapatite (NHA) and to evaluate their influence on the bond strength, antimicrobial effect, and biomaterials cytotoxicity. The nanoparticles were characterized by x-ray fluorescence by total reflection (TRXF), x-ray diffractometry (XRD), transmission electron microscopy (TEM) and visible light scattering (DLS). The Scotchbond Multi-Purpose system (SBMP) was modified with 0.05% and 0.1% silver in the primer and bond. Human molars were restored with the modified adhesive after pre-treatment of dentin with 0.5% and 1% NHA for the immediate bond strength test (24h), and after 1 year of aging. The adhesive interface was characterized by Confocal Raman Microscopy (MCR). To measure the antibacterial effect (S.mutans) of the adhesive with NAg, the agar diffusion assay with template was performed and counting of Colony Forming Units (UFC). In order to evaluate the cytotoxicity, dental pulp stem cells (DPSCs) were used in contact with unpolymerized and polymerized adhesives in different concentrations of conditioned medium (0% 25%, 75% and 100%). Spherical NAg, with a cubic face centered structure, and 16 nm in diameter were produced. The NHA exhibited a prismatic structure with approximately 79.4 nm. The adhesive with NAg and the treatment of dentin with NHA did not affect the bond strength immediately or after 1 year of aging, and the adhesive interfaces were shown to be intact. NAg-modified adhesives exhibited cytotoxicity similar to the control adhesive and higher antibacterial effect. The adhesives with NAg addition are promising in obtaining a bioactive antimicrobial material that does not alter the bond strength or the biocompatibility.

Atualmente, os adesivos de contato de policloropreno base aquosa, possuem capacidade de adesão, variando entre 1,15 até 2,75 kgf/cm2. Em contrapartida, os adesivos de policloropreno base solvente, suportam tensões médias de cisalhamento de 3,8 kgf/cm2. Esta pesquisa apresenta uma proposta inovadora de condicionamento magnético do adesivo de contato de policloropreno base aquosa com o objetivo de aumentar a capacidade de aderência entre o adesivo e o substrato. Para promover um incremento na capacidade de adesão do adesivo de policloropreno base aquosa, formulou-se um adesivo utilizando um nanoaditivo, o gás carbônico como catalisador e um processo de condicionamento magnético precedente à etapa de aplicação sobre os substratos. Os resultados obtidos demonstraram aumento médio de 292 % na tensão de cisalhamento do adesivo condicionado magneticamente quando comparado com o adesivo de mesma formulação sem o condicionamento magnético, e quando comparado com um adesivo comercial de policloropreno base aquosa, o aumento foi de 122 %. / Currently, the aqueous based polychloroprene contact adhesive presents an adhesion capacity variation between 1,15 and up to 2,75 kgf/cm2. However, the solvent based polychloroprene adhesives support average tensions of shearing of 3,8 kgf/cm2. This research is an innovative proposal for magnetic conditioning of the aqueous based polychloroprene contact adhesive with the purpose of increasing the adherence capacity between the adhesive and the substrate. To promote an increase of adhesion to the aqueous based polychloroprene contact adhesive, we formulated one adhesive using a nano-additive, carbon dioxide as catalyst, and a magnetic conditioning process before the phase of application on the substrates. The results obtained show an average increase of 292 % in the shearing tension of the adhesive magnetically conditioned when compared with an adhesive of the same formulation without the magnetic conditioning and 122 % increase when compared to the commercial aqueous based polichloroprene adhesive.

O objetivo deste trabalho foi analisar em Microscopia Ótica (MO), Espectroscopia micro-Raman (µR) e Microscopia Eletrônica de Varredura (MEV), a interface adesiva em dentina proporcionada por três sistemas adesivos aplicados in vivo e in vitro. Na condição in vivo, pacientes com primeiros prémolares superiores hígidos indicados para extração, por razões ortodônticas, foram utilizados. Cavidades classe I com 0,5mm além da junção esmalte-dentina foram realizadas, nos dentes, com broca carbide 245 em alta rotação. Foram, então aplicados três sistemas adesivos diferentes foram aplicados, de acordo com as instruções dos respectivos fabricantes: Single Bond (SB-3M), Clearfil SE Bond (CSEB-Kuraray) e One Up Bond-F (OUB-Tokuyama). Aplicados esses, as cavidades foram restauradas incrementalmente com resina composta TPH Spectrum (Dentsply). Em seguida os dentes foram extraídos e armazenados em solução de timol a 0,1%. In Vitro, os mesmos procedimentos foram realizados em pré-molares extraídos. Após os dentes foram levados à uma máquina de cortes e seccionados, com auxílio de um disco de corte em espécimes contendo a interface, com dimensões 2mmx2mmx6mm de comprimento, sendo 2 espécimes para cada dente. Um dos espécimes foi levado a um micrótomo de tecido duro onde fatias com espessura de 5µm foram obtidas e coradas com Tricromo de Goldner. As fatias foram, então, analisadas em um microscópio óptico com aumento de 100 vezes. Nesta técnica a dentina mineralizada se cora de verde, o colágeno não infiltrado de vermelho e o sistema adesivo de beje translúcido. Após o mesmo espécime foi utilizado para análise em espectroscopia micro-Raman. O espécime adjacente foi desidratado em seqüência ascendente de etanol e analisado em microscopia eletrônica de varredura. Os resultados da MO para o sistema SB mostraram a presença de uma grande área corada de vermelho, indicando colágeno exposto ou não devidamente infiltrado pelo sistema adesivo para ambas as situações porém, in vivo, esta camada se mostrou maior. Para o sistema CSEB esta camada se corou de roxa, consistente ao longo de toda interface, indicando também a presença de colágeno disponível para reação com o corante, para ambas as situações. Para o sistema OUB esta camada também se corou de roxa, porém in vivo esta se mostrou mais fina e irregular que in vitro. Em MEV o sistema SB apresentou uma camada híbrida granular e porosa para ambas as situações. In vitro esta se mostrou mais espessa e regular ao longo da interface ao contrário da condição in vivo. Grandes diferenças foram observadas em relação aos tags de resina, onde in vivo, se apresentaram mais finos e curtos. Para o sistema CSEB a camada híbrida se mostrou mais fina quando comparada ao sistema SB porém, mais homogênea e compacta ao longo da interface para ambas as situações. Grandes diferenças foram observadas em relação aos tags de resina onde in vivo foram significativamente em menor número, curtos e finos. Para o sistema OUB in vitro a camada híbrida se apresentou fina porém, homogênea em sua extensão com a presença de longos tags. In vivo a camada híbrida se apresentou bastante fina e até difícil de se detectar. O tags se apresentaram quase inexistes ou muito dobrados devido à pobre polimerização desse sistema. As análises em µR para o sistema SB mostraram uma maior contribuição do sistema adesivo nos dois primeiros micrometros da interface, ao passo que, no restante da mesma, houve pouca contribuição dos monômeros adesivos na proteção do colágeno. Para o sistema CSEB a interface se mostrou bastante fina (1µm), para ambas as condições, porém com contribuição, no complexo hibridizado, dos componentes adesivos, colágeno e mineral. Para o sistema OUB in vitro, os espectros também indicaram a presença de uma interface fina, em torno de 1µm, mas também com contribuição dos componentes adesivos, colágeno e mineral. In vivo, esta não pôde ser detectada pelo Raman por ser inexistente ou ser mais fina que a resolução do Raman (1 µm). Realizada as análises da interface em ambas condições experimentais, com os diferentes sistemas adesivos utilizados, conclui-se que: a condição in vivo proporcionou uma interface de menor qualidade para todos os sistemas. O sistema CSEB aparentemente proporcionou uma melhor qualidade de interface e o sistema OUB a pior. O uso dessas três técnicas integradas permitiu uma análise completa, qualitativa e quantitativa da interface adesiva produzida por esses três sistemas, em ambas as condições testadas. / The aim of this research was to analyze in Light Microscopy (LM), micro-Raman Spectroscopy (µR) and Scanning Electron Microscopy (SEM), the dentin-adhesive interface produced by three different bonding systems applied in vivo and in vitro. In in vivo condition patients with the first upper premolars, to be extract for orthodontic reasons, were used. Class I cavities with 0.5mm below the dentin-enamel junction were performed, with carbide bur in high speed. Following, three different bonding systems were applied in accordance with their manufacturer instruction: Single Bond (SB-3M), Clearfil SE Bond (CSEB-KURARAY) and One Up Bond-F (OUBTokuyama), and the cavities restored, incrementally, with composite resin TPH Spectrum (Dentsply). After restoration the teeth were extracted and stored in 0,1% tymol solution. In vitro, the same procedures were performed in extracted upper premolars. Following, the teeth were taken to a cutting machine and cross-sectioned with as diamond saw in specimens with 2mmX2mmx6mm dimensions, being 2 specimens for each tooth. One of the specimen was taken to a hard tissue microtome were 5µm slabs were obtained and stained with Goldner´s Tricrome. The slabs were analyzed in a Light Microscope with 100 times magnification. In this technique, the mineralized dentin is stained green, the collagen is stained red and the bonding system a pale orange. After, the same specimen was used for micro-Raman analysis. The adjacent specimen was dehydrated in ascendant ethanol sequence and analyzed in scanning electron microscopy. The LM results for SB showed the presence of a large area stained red for both conditions, indicating the presence of exposed or non protected collagen by the bonding system. This area was larger in vivo than in vitro. For CSEB this layer war purple stained and consistent along the interface for both situations, indicating, also, collagen available to react with the staining. For OUB this layer was also purple however, in vivo, this layer was thinner and inconsistent than in vitro. In SEM analysis, SB bonding system presented a porous hybrid layer for both situations. In vitro this layer was thicker and regular along the interface and, in vivo, thinner and irregular. Big differences were observed related to the resin tags. In vivo they were thinner and shorter. For CSEB the hybrid layer was thinner when compared with SB however, more homogeneous and compact along the interface for both situations. Big differences were observed related to the resin tags. In vivo, they were significantly in fewer amounts, shorter and thinner. For OUB in vitro, the hybrid layer was thin, however, homogeneous and with long tags. In vivo, the hybrid layer was very thin, almost undetectable. The resin tags were almost non-existent or bended due to poor polymerization of this system. In micro-Raman analysis for SB showed a greater contribution of the bonding system in the first two micrometers of the interface was detected and, in the rest of the interface, there was few contribution of the resin monomers in the collagen protection. For CSEB the interface was thin (1µm), for both conditions, however, with contribution, in the hybridized complex, of the adhesives components, collagen and mineral. For OUB in vitro, the spectras also indicated the presence of a thin interface, among 1µm, but also, with contribution of the bonding components, collagen and mineral. In vivo, the interface could not be detected by the Raman, for being inexistent, or by the fact to be thinner than the Raman resolution (1µm). After all these analysis of the bonding interface, for both conditions, and with these different bonding systems, it can be concluded that: in vivo condition produced a less-quality interface for all the system. CSEB apparently produced a better-quality interface and OUB the worst. The use of these three techniques together allowed a complete analysis, qualitative and quantitative, of the dentin-bonding interface produced by these three bonding systems, for both situations.

O clareamento e os procedimentos adesivos são soluções muito utilizadas na Odontologia atual. Assim, o objetivo deste trabalho foi avaliar, in vitro, a resistência adesiva ao esmalte clareado através do ensaio mecânico de microtração. Dois sistemas adesivos autocondicionantes (Clearfil SE Bond - Kuraray e Adper Prompt LPop - 3M Espe) e um adesivo convencional (Adper Single Bond 2 - 3M Espe) foram aplicados imediatamente, 7 e 14 dias após o clareamento com peróxido de hidrogênio a 35% (Whiteness HP - FGM) ao esmalte. Foram utilizados 60 dentes bovinos que tiveram a superfície de esmalte planificada e em seguida divididos em 12 grupos (9 experimentais e 3 controles) de acordo com o adesivo empregado e o intervalo entre o clareamento e os procedimentos adesivos. O ensaio de microtração foi realizado 24 h após a confecção das restaurações e a área de fratura foi avaliada através da microscopia eletrônica de varredura. Houve redução significativa da resistência adesiva nos dentes restaurados imediatamente após o clareamento com todos os adesivos utilizados. Após 7 e 14 dias do término do clareamento, os valores de resistência adesiva se igualaram e foram semelhantes aos valores dos grupos controles dos respectivos sistemas adesivos empregados. O adesivo Adper Single Bond 2 apresentou os maiores valores de resistência adesiva e o Adper Prompt L Pop os mais baixos. Houve predominância de fraturas adesivas e mistas em todos os grupos. / Bleaching and adhesive proceedings are solutions much used in current Dentistry. Thus, this work aimed at assessing, in vitro, the adhesive resistance to bleached enamel through the microtensile mechanical trial. Two self-etch adhesive systems (Clearfil SE Bond - Kuraray and Adper Prompt L-Pop - 3M Espe) and a conventional adhesive (Adper Single Bond 2 - 3M Espe) were immediately employed, 7 and 14 days after bleaching with hydrogen peroxide at 35% (Whiteness HP - FGM) in the enamel. 60 bovine teeth were used, which had the enamel surface planned and following randomly divided into 12 groups (9 experimental and 3 controls) according to the employed adhesive and to the interval between the bleaching ending and the adhesive proceedings. The microtensile trial was accomplished 24 hours after the confection of the tooth fillings and the fracture area was assessed through scanning electronic microscopy. There was significant reduction of the adhesive resistance in the filled teeth immediately after bleaching with all employed adhesives. After 7 and 14 days of the bleaching ending, the adhesive resistance values were equated and were similar to the values of the control groups and to the respective adhesive systems employed. The Adper Single Bond 2 adhesive presented the highest adhesive resistance values and the Adper Prompt L-Pop presented the lowest ones. There was predominance of adhesive and mixed factures in all groups.

Este estudo teve como objetivos avaliar se a delimitação da área adesiva a ser testada no ensaio mecânico de microcisalhamento é capaz de alterar os resultados de resistência de união obtidos; determinar se a delimitação da área adesiva do ensaio mecânico de microcisalhamento pode alterar o ranqueamento dos sistemas adesivos analisados e correlacionar os tipos de fratura encontrados com valores de resistência adesiva obtidos em cada um dos grupos experimentais. As unidades experimentais foram confeccionadas sobre 18 superfícies de dentina obtidas a partir de incisivos bovinos distribuídas aleatoriamente em 3 grupos, segundo o sistema adesivo a ser utilizado (Adper Single Bond 2, Clearfil Se Bond, Clearfil S3 Bond). Desta forma foram compostos 6 grupos experimentais segundo os dois fatores de variação a serem estudados: sistema adesivo e delimitação da área adesiva. Sobre cada superfície dentinária foram confeccionados 4 cilindros em resina composta, sendo 2 com delimitação da área adesiva e 2 sem a delimitação desta área, totalizando n=12. Após 24 horas de armazenamento os espécimes foram submetidos ao ensaio mecânico de microcisalhamento. O teste estatístico ANOVA (p<0,01) e o teste auxiliar de Tukey determinaram que todos os grupos experimentais em que a delimitação da área adesiva foi realizada apresentaram menores valores de resistência adesiva quando comparados aos seus respectivos grupos controle (sem delimitação da área adesiva). Para os grupos em que não foi realizada a delimitação da área não foram observadas diferenças estatisticamente significantes entre os adesivos empregados. Em contrapartida, quando não foi realizada a delimitação, o sistema adesivo Clearfil S3 Bond mostrou maiores valores de resistência adesiva quando comparado aos sistemas Adper Single Bond 2 e Clearfil SE Bond, que por sua vez não se mostraram estatisticamente diferentes entre si. Concluiu-se que a delimitação da área adesiva no ensaio de microcisalhamento alterou os resultados de resistência adesiva obtidos, e que a modificação da metodologia do ensaio mecânico de microcisalhamento foi capaz de alterar o ranqueamento dos sistemas adesivos analisados. / This study had as objectives to evaluate if the delimitation of adhesive area on microshear test is capable to modify the values of shear bond strength; to determine if this delimitation can modify the ranking of the analyzed adhesive systems and to correlate the found types of failure with the values of bond strength in each experimental group. The specimens were confectioned on 18 incisors bovine dentine surfaces randomly distributed into 3 groups, according to adhesive system used (Adper Single Bond 2, Clearfil If Bond, Clearfil S3 Bond). In such a way, 6 experimental groups were designed according to two factors of variation to be studied: adhesive system and delimitation of the adhesive area. Over each dentin surface were confectioned 4 composite resin cylinders, being 2 with delimitation of the adhesive area and 2 without the delimitation of this area, totalizing n=12. After 24 hours of storage the specimens were submitted to microshear test Statistical test ANOVA (p<0,01) and Tukey?s test determined that all the experimental groups where the delimitation of the adhesive area was carried through presented lesser values of shear bond strength when compared with its respective control groups (without delimitation of adhesive area). Groups without area delimitation did not been demonstrate statistical significant differences between adhesives. On the other hand, when such delimitation was not carried through, the adhesive system Clearfil S3 Bond demonstrates greater values of shear bond strength compared to Adper Single 2 Bond and Clearfil SE Bond, which did not showed statistical difference between them. It was concluded that the delimitation of the adhesive area in the microshear test altered the obtained results of adhesive resistance, and that the modification of microshear test methodology was capable to modify the ranking of the analyzed adhesive systems.

No presente trabalho avaliou-se a resistência mecânica do bambu nos estágios pré e pós processamento mecânico para servir de referências básicas do estudo das propriedades mecânicas de vigas laminadas coladas simples, de seção composta e de seção composta na forma de I, industrializadas em laboratório. Iniciou-se com a caracterização do material bruto na forma de ripa que representa toda a parede do colmo, passando-se pelo material processado na forma de lâmina que representam a parte industrialmente útil da parede do colmo e culminando na manufatura e qualificação das vigas laminadas coladas. Na produção dos corpos de prova do material bruto manteve-se a espessura original da ripa, exceto para alguns produzidos para se avaliar a resistência ao cisalhamento radial das camadas interna e externa da parede do colmo. As ripas foram usinadas em diversas máquinas para serem transformadas em lâminas que são as unidades de composição das seções compostas pela técnica de aglutinação e adesão a frio. Foi estudada também a influência do nó na resistência ao cisalhamento radial e tangencial tanto do material sólido quanto do plano de cola e nas propriedades da flexão. A geometria e as dimensões dos corpos de prova de cisalhamento foram adaptadas da norma ASTM D 905 e os de flexão da norma NBR 7190. As resistências ao cisalhamento no plano de cola e as propriedade da flexão foram determinadas segundo três combinações de faces de contato no processo de colagem com o adesivo à base de resorcinolformaldeído (RF). Estudou-se também a pressão adequada para colagem dos corpos de prova e eleita a mais adequada à colagem de vigas laminadas coladas. Os corpos de prova intactos e rompidos nos ensaios foram observados em microscópio eletrônico de varredura, em microscópio óptico, em microscópio óptico de fluorescência e microscópio estereoscópico. Observou-se ampla variabilidade das propriedades mecânicas tanto do material sólido quanto do material composto, mas em qualquer dos casos de resistência houve ampla variabilidade dos dados e, no geral o material sem nó foi mais resistente do que o com nó. As rupturas ocorreram na maioria das vezes no tecido parenquimático desviando-se dos feixes de fibras e tendendo a seguir a grã do material observando que o plano de ruptura só coincide com o plano planejado para a ruptura quando o corpo de prova é feito com a consideração precisa da orientação da grã. Os corpos de prova montados com a cola à base de PVA e com lâminas nodais responderam de forma satisfatória à colagem a baixa pressão, enquanto que os fabricados com lâminas internodais apresentaram melhor desempenho a alta pressão. Para os corpos de prova manufaturados com o adesivo à base de RF, a melhor combinação de colagem se deu no contato entre faces externas de lâminas. Foi possível observar a penetração do adesivo nos elementos anatômicos das lâminas com o uso da microscopia óptica e de fluorescência. As vigas laminadas coladas de seção transversal composta foram ensaiadas à flexão, mas não romperam por tensão normal, pois apresentaram instabilidade lateral durante o carregamento à flexão. As vigas também apresentaram baixo módulo de elasticidade porque o esmagamento da mesa inferior, nos apoios, foi cofundida e somada pelo sistema de medida, ao valor da flecha. Numa análise geral, a qualidade mecânica da Viga \"I\" pode ser considerada muito boa dentro do correto cálculo do momento de inércia se seções transversais compostas. As camadas perpendiculares ao eixo da via, tanto na alma quanto na mesa, foram tão eficientes na absorção do esforço cortante que não houve nenhuma limitação de capacidade de carga pela ligação alma-mesa mesmo com a viga trabalhando numa faixa de alta influência de tensões cisalhantes. / In this study it was evaluated the bamboo strength in the stages before and after mechanical processing in order to obtain basic references to study the mechanical properties of simple glued laminated beams of composite section and composed section as I joist, manufactured in laboratory scale. It started with the characterization of raw material as strip representing the crude bamboo culm wall, moved to the processed material as in the shape of laminas which were representing the majority of bamboo culm wall industrially useful and culminating to the manufacture and qualification of glued laminated beams. In the production of specimens of raw material it was maintained the original thickness for the strip except for a few ones which were produced to evaluate the radial shear strength in the inner and outer layers of the culm wall. The strips were machined on some machines to be turned into laminas that were the units for assembling composite sections by agglutination and adhesion under pressure in environmental conditions. It was also studied the node influence in the radial and tangential shear strength in both solid material and in the adhesive plan and in properties got from the bending tests. The geometry and dimensions of the shear specimens were adapted from ASTM D 905 and the bending from NBR 7190. Shear strength in the adhesive plane and bending property were determined following three combinations of contact faces on the gluing process using resorcinol-formaldehyde based adhesive. It was studied also the proper pressure for gluing the specimens and elect the most suitable for glued laminated beams. The intact specimens and failed on mechanical tests were observed under a Scanning Electron Microscope, Optical Microscope, Optical fluorescence microscope and stereomicroscope. It was observed huge variation of mechanical properties in both solid and composite materials, but in all cases there was considerable variability of strength data and in general the material without node was more resistant than with node. The ruptures mechanisms occurred most often in the parenchyma tissue by passing the fiber bundles and tend to follow the grain of the material by observing the rupture plane that only coincides with the plan designed to rupture when the specimen is done with precise consideration of grain orientation. The specimens manufactured with PVA adhesive and components with nodes responded satisfactorily to the low pressure bonding, while the specimens produced with internodes components performed better at high pressure. For specimens manufactured with resorcinol-formaldehyde adhesive the best gluing combination was given by the contact of outer laminas surfaces to each other. It was possible to observe the anchorage of the adhesive into the anatomical tissues by using optical microscopy and fluorescence optical microscopy. Glued laminated beams with composite cross section were tested in bending, but not failed by normal stresses, once there occurred only lateral instability during loading time. The I beams also showed low modulus of elasticity because the crush in the inferior flange was added by the measurement system to the bending deflection. In general the mechanical quality of the \"I\" joist can be considered very high with correct calculation of the moment of inertia of composite cross sections. The layers perpendicular to the beam axis both in web and in the flanges, were so efficient in absorbing the shear that there was no limitation of carrying load web-frange connection even with the beam working in a critical influence of high shear stresses.