Extraction of mangrove bark with 4.0% aqueous sodium sulfite and 0.4% aqueous sodium carbonate at 100° and 2 hours gives 24-26% yields compared with extraction by water at 70° for 2 hours which gives 21%. The hot water extracts are more acidic (pH 3.6) than is the sulfite extract (pH 5.6); both are reasonably reactive toward formaldehyde (Stiasny number 70.6 using water and 85.4 using aqueous sulfite-carbonate). The ¹³C NMR spectra of <I>R. mucronata </I>shows this tannin to have phloroglucinolic A-rings with hydroxy groups at C-5 and C-7 and pyrogallolic B-rings with hydroxy groups at C-3', C-4', and C-5'. The interflavanoid linkages are C-4→C-8 and C-4→C-6. The ¹³C NMR spectra also indicate the presence of a considerable amount of carbohydrate which is shown to be mainly rhamnose, glucose, arabinose, and uronic acids. Sulfitation of <I>R. mucronata </I>bark reduces the total carbohydrate and the rhamnose extracted but increases the amount of arabinose and uronic acids. The bark storage period has significant effects on the pH and the reactivity of the aqueous tannin solution. Barks stored for <4 weeks produce higher extraction yields than those stored for > 6 weeks and contain significantly larger amount of reactive tannin and have shorter gel times. The reactivity of bark extracts towards formaldehyde can be controlled either by limiting the duration of bark storage to 4 weeks or by maintaining the aqueous tannin solution at pH <10.0. The aqueous tannin solution from <I>R. mucronata </I>exhibited properties such as viscosity, solubility and tackiness which were superior to those from the <I>R. apiculata </I>extract while the mixed <I>R. mucronata-R. apiculata </I>aqueous tannin solution had properties in between these. These barks could be used singly or together as a source of tannin without the bond strength of the resulting glued joints being significantly affected. The "honeymoon" bonding technique improved the bond strengths of joints made using sulfited tannin but is suitable only for tannin solutions containing > 4% aqueous sodium hydroxide. The viscosity of sulfited tannin adhesives is influenced by (a) the amount of aqueous sodium hydroxide added to the aqueous tannin solution, and (b) the lapse time, i.e. the period between the addition of sodium hydroxide to the aqueous tannin solution and the addition of phenol-resorcinol-formaldehyde (PRF) resin, hardener, and paraformaldehyde. The present study shows that with the addition of 5% w/w sodium hydroxide and at a curing temperature of 40° the sulfited tannin extracts from the bark of mangrove trees can replace about 50% w/w of the PRF resin in cold-setting wood adhesives with the production of bond strengths comparable to those produced by 100% PRF resin.

Advanced composite materials are widely used for many structural applications in the aerospace/aircraft industries today. Joining of composite structures using adhesive bonding offers several advantages over traditional fastening methods. However, this technique is not yet employed for fastening the primary structures of aircrafts or space vehicles. There are several reasons for this: There are not any reliable non-destructive evaluation (NDE) methods that can quantify the strength of the bonds, and there are no certifications of quality assurance for inspecting the bond quality. Therefore, there is a significant need for an effective, reliable, easy to use NDE method for the analysis of composite adhesive joints. This research aimed to investigate an adhesively bonded composite-aluminum joints of variable bond strength using digital image correlation (DIC). There are many future possibilities in continuing this research work. As the application of composite materials and adhesive bond are increasing rapidly, the reliability of the composite structures using adhesive bond should quantified. Hence a lot of similar research using various adhesive bonds and materials can be conducted for characterizing the behavior of adhesive bond. The results obtained from this research will set the foundation for the development of ultrasonic DIC as a nondestructive approach for the evaluation of adhesive bond line.

This research provides the evaluation of the technical measurements of pavement marking materials from a two-year data collection on 2002 National Transportation Product Evaluation Program (NTPEP)?s Mississippi Test Deck from June, 2002 to June 2004. The materials studied in this research were divided into permanent and temporary material groups on two different pavement surfaces ---- asphalt and concrete. The retro reflectivity and durability of permanent marking materials among different surfaces, colors and groups were studied. Also the characteristics for temporary tapes, which include internal tape strength, adhesion, tackiness and dicernablity were compared and regressed. This correlation analysis is to see whether these ratings are correlated to each other. The results of this study can be used for estimating service lives of pavement marking materials. They also can be used by states to select appropriate pavement marking materials for different needs.

The effect of thermal cycling on the state of stress in polymeric materials bonded to stiff elastic substrates was investigated using numerical techniques, including finite element methods. The work explored the relationship between a cyclic temperature environment, temperature-dependent viscoelastic behavior of polymers, and thermal stresses induced in a constrained system. Due to the complexity of developing a closed-form solution for a system with time, temperature, material properties, and boundary conditions all coupled, numerical techniques were used to acquire approximate solutions. Descriptions of attempted experimental verification are also included. The results of the numerical work indicate that residual stresses in an elastic-viscoelastic bimaterial system incrementally shift over time when subjected to thermal cycling. Tensile axial and peel stresses develop over a long period of time as a result of viscoelastic response to thermal stresses induced in the polymeric layer. The applied strain energy release rate at the crack tip of layered specimens is shown to similarly increase. The rate of change of the stress state is dependent upon the thermal cycling profile and the adhesive’s thermo-mechanical response. Discussion of the results focuses on the probability that the incrementing tensile residual stresses induced in an adhesive bond subjected by thermal cycling may lead to damage and debonding, thus reducing durability. / Master of Science

The objective of this study is to evaluate the bond durability of an epoxy-based polymer concrete wearing surface bonded to aluminum bridge decks. In the bridge design, an aluminum alloy bridge deck is used with a polymer concrete wearing surface. A modified mixed mode flexure fracture test was developed to assess the bond durability of specimens aged in the following environmental conditionings: 30°C [86°F], 98% RH; 45°C [113°F], 98% RH; 60°C [140°F], 98% RH; freezing and thawing; salt (NaCl) water soak; and 60°C [140°F], dry. The exposure times varied from none to twelve months. The critical strain energy release rate (Gc) of the bond was determined using a compliance technique. In spite of considerable scatter in the data, the results suggested that the interfacial bond toughness had been degraded by exposure conditions. The aging appeared to affect the polymer concrete overlay (silica aggregates/epoxy bond) as well. Fracture analysis and finite element modeling were completed for linear elastic behavior. Analytical and numerical solutions were in reasonably good agreement. Characterization of the bridge components and failure specimens were accomplished using analytical measurements including thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), and dynamic mechanical analysis (DMA). Techniques employed in the surface analysis included x-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). / Master of Science

Objetivo: verificar, através de análise por elementos finitos e de uma etapa experimental, se o ensaio de torção, como ensaio de resistência de interfaces adesivas, seria capaz de levar os espécimes à ruptura sob tensões de cisalhamento e se ele seria vantajoso em relação ao ensaio de cisalhamento. Material e Método: para a análise de tensões pelo método dos elementos finitos, os modelos tridimensionais dos dois ensaios foram constituídos por cilindro de compósito, uma camada de adesivo e um cilindro de dentina com maior diâmetro. Os espécimes foram simulados nos tamanhos convencional e micro, numa proporção de 5:1, exceto pela camada de adesivo, de espessura constante. Foram simulados dois módulos de elasticidade do cilindro de compósito (híbrido e baixa viscosidade) e, para os modelos de cisalhamento, variaram as distâncias entre o local de carregamento e a interface adesiva. Foram analisados os valores das tensões máxima principal e cisalhamento máximo e a proporção entre elas ao longo da interface dentina/adesivo; a direção dos vetores de tensão máxima principal; e o local dos picos de tensão. Na etapa experimental, foram construídos cilindros de compósito (híbrido e de baixa viscosidade) nos tamanhos convencional e micro, aderidos a uma superfície de dentina bovina por meio de três sistemas adesivos. O esforço de cisalhamento foi aplicado com fio ortodôntico a uma distância da interface adesiva baseada na literatura e, para os ensaios de torção e microtorção, foram desenvolvidos dispositivos específicos para a aplicação do torque. Os resultados de tensão de ruptura foram submetidos à análise de variância e teste de Tukey. Todas as superfícies de fratura foram analisadas por meio de microscopia eletrônica de varredura. As frequências das fraturas adesivas e coesivas foram submetidas ao teste exato de Fisher e relacionadas aos valores de tensão de ruptura experimentais, bem como suas características foram relacionadas às tensões observadas pelo método dos elementos finitos. Os parâmetros experimentais de comparação entre os ensaios foram: poder de detecção de diferenças significantes entre os sistemas adesivos; constância da classificação relativa dos mesmos ao alterar as configurações dos ensaios e frequências dos tipos de fratura. Resultados: ambos os ensaios apresentaram um estado complexo de tensões com distribuição nãouniforme. Não foi notada menor sensibilidade dos resultados do ensaio de torção às mudanças das configurações do teste, nem uma maior capacidade para detectar diferenças significantes entre os adesivos do que o ensaio de cisalhamento. O ensaio de torção apresentou maior dificuldade de execução prática e maiores frequências de fraturas coesivas, porém, estas ocorreram mais no cilindro de compósito, enquanto no cisalhamento, ocorreram mais na dentina. Não houve certeza sobre o tipo de tensão que tenha levado à fratura nos dois tipos de ensaio. Conclusões: embora não se tenha certeza se o ensaio de torção leva à ruptura sob tensões de cisalhamento e tenham sido notadas desvantagens práticas de execução do ensaio, este apresenta uma característica que sugere novos estudos: ocorrência de fraturas coesivas principalmente no cilindro de compósito, o que poderia, talvez, ser resolvido com o reforço do material do cilindro. / Objective: verify, by finite element analysis (FEA) and laboratorial tests, if the torsion bond strength test is able to lead adhesive interface to fracture under shear stress and if it would be more advantageous than wire-loop shear test. Material and method: for stress analysis by finite element method, the 3D models of both tests consisted of a resin composite cylinder, an adhesive layer and a dentin cylinder with a larger diameter. The specimens were simulated with both conventional and micro sizes, in a 5:1 ratio, except for the adhesive layer, kept in a constant thickness. Two values of elastic modulus were simulated for the composite cylinder (hybrid and flowable). For the shear models, different distances were simulated between the load point and the adhesive interface. The values of maximum principal and maximum shear stresses and the ratio between both types were analyzed along the adhesive interface, as well as the maximum principal vectors direction and the local of stress peaks. For the laboratorial tests, cylinders of hybrid and flowable resin composite, in both micro and conventional sizes, were adhered onto dentin surfaces by means of 3 adhesive systems. The shear load was applied with a metallic wire-loop at distances from the interface based on literature and, for the torsion test, the torque was applied by specific apparatus developed for that. The values of bond strength were submitted to analysis of variance and Tukeys test. Fracture surfaces were analyzed by scan electron microscopy. The frequencies of fracture types were compared by Fishers test and its relationship with bond strength values were verified, as well as the relationship between fracture features and stresses results obtained by FEA. The experimental parameters for comparison between both tests were: ability for detecting significant differences among the 3 adhesives, change of adhesives ranking while varying the test configuration and frequency of fracture types. Results: both tests showed non-uniform stress distribution. It was not noticed a lower sensibility of torsion test results to changes of the test configurations, nor a major ability for detecting significant differences among the adhesive systems than showed the shear test. The torsion test showed to be more difficult to execute and exhibited a higher frequency of cohesive fracture, however, that occurred most of the time in the composite cylinder, while it occurred mainly in dentin in shear test. There was no certainty about the kind of stress that lead to specimen fracture in both tests. Conclusions: although there was no certainty about the kind of stress that lead to specimen fracture and the major difficulty of execution of torsion test, this test exhibited a feature that suggests future studies: the occurrence of cohesive fracture mainly in the composite cylinder, which could be solved, maybe, by reinforcing the cylinder material.

Introduction: Adhesive technology represents a significant advancement among different treatment options of dental caries. Its advantages involve not only highly aesthetic reconstructions, but also ability to preserve hard dental tissues compared to more traditional filling materials such as amalgam, where the material retention was achieved through undercuts. A potential of adhesive technology to arrest progression of an incipient caries has triggered its wider use in dental caries management, potentiated by an ongoing development of new adhesive systems and composite materials that assure an acceptable long-term stability of adhesive reconstructions. Adhesive bonds of dental reconstructions are in the oral cavity constantly challenged by various mechanical, chemical and biological factors. One of the chemical agents with detrimental potential is peroxide bleaching gel used for teeth brightening. Currently bleaching belongs to the most frequent cosmetic dental procedures. The active ingredient of bleaching gels is hydrogen peroxide or its precursors. It is assumed that free oxygen radicals released from peroxides attack double bonds of chromophore molecules captured within the tooth tissues. Because of the high reactivity and nonspecific nature of these oxygen radicals, they may affect also dental...

Introduction: An adhesive bond between hard dental tissues and composite reconstructions is exposed to mechanical load, water, bacteria, enzymes and different chemical compounds. These factors could impair durability and resistance of composite reconstructions. In contrast with extensive research of negative influence of water on degradation of adhesive bonds, the influence of chemical substances on adhesive bond has not been investigated to a greater extent. Aim: The aim of the experimental part of the thesis was to evaluate the influence of hydrogen peroxide containing tooth-whitening products and mouth rinses containing chlorhexidine and fluoride on a long-term stability of class V composite restorations created using four contemporary adhesive systems by a microleakage method. Materials and methods: The following adhesive systems were investigated: total-etch Gluma Comfort Bond (GLU), and self-etch adhesives Clearfil SE Bond (CLF), Adper Prompt (ADP) and iBond (IBO). Standardized class V cavities were prepared in 192 extracted human teeth (one cervical margin in the cementum and one in the enamel). Subsequently, the cavities were restored using microhybride composite Charisma. The specimens were then exposed to the tooth whitening system Opalescence PF 20, mouth rinse Corsodyl containing...

Objetivo: verificar, através de análise por elementos finitos e de uma etapa experimental, se o ensaio de torção, como ensaio de resistência de interfaces adesivas, seria capaz de levar os espécimes à ruptura sob tensões de cisalhamento e se ele seria vantajoso em relação ao ensaio de cisalhamento. Material e Método: para a análise de tensões pelo método dos elementos finitos, os modelos tridimensionais dos dois ensaios foram constituídos por cilindro de compósito, uma camada de adesivo e um cilindro de dentina com maior diâmetro. Os espécimes foram simulados nos tamanhos convencional e micro, numa proporção de 5:1, exceto pela camada de adesivo, de espessura constante. Foram simulados dois módulos de elasticidade do cilindro de compósito (híbrido e baixa viscosidade) e, para os modelos de cisalhamento, variaram as distâncias entre o local de carregamento e a interface adesiva. Foram analisados os valores das tensões máxima principal e cisalhamento máximo e a proporção entre elas ao longo da interface dentina/adesivo; a direção dos vetores de tensão máxima principal; e o local dos picos de tensão. Na etapa experimental, foram construídos cilindros de compósito (híbrido e de baixa viscosidade) nos tamanhos convencional e micro, aderidos a uma superfície de dentina bovina por meio de três sistemas adesivos. O esforço de cisalhamento foi aplicado com fio ortodôntico a uma distância da interface adesiva baseada na literatura e, para os ensaios de torção e microtorção, foram desenvolvidos dispositivos específicos para a aplicação do torque. Os resultados de tensão de ruptura foram submetidos à análise de variância e teste de Tukey. Todas as superfícies de fratura foram analisadas por meio de microscopia eletrônica de varredura. As frequências das fraturas adesivas e coesivas foram submetidas ao teste exato de Fisher e relacionadas aos valores de tensão de ruptura experimentais, bem como suas características foram relacionadas às tensões observadas pelo método dos elementos finitos. Os parâmetros experimentais de comparação entre os ensaios foram: poder de detecção de diferenças significantes entre os sistemas adesivos; constância da classificação relativa dos mesmos ao alterar as configurações dos ensaios e frequências dos tipos de fratura. Resultados: ambos os ensaios apresentaram um estado complexo de tensões com distribuição nãouniforme. Não foi notada menor sensibilidade dos resultados do ensaio de torção às mudanças das configurações do teste, nem uma maior capacidade para detectar diferenças significantes entre os adesivos do que o ensaio de cisalhamento. O ensaio de torção apresentou maior dificuldade de execução prática e maiores frequências de fraturas coesivas, porém, estas ocorreram mais no cilindro de compósito, enquanto no cisalhamento, ocorreram mais na dentina. Não houve certeza sobre o tipo de tensão que tenha levado à fratura nos dois tipos de ensaio. Conclusões: embora não se tenha certeza se o ensaio de torção leva à ruptura sob tensões de cisalhamento e tenham sido notadas desvantagens práticas de execução do ensaio, este apresenta uma característica que sugere novos estudos: ocorrência de fraturas coesivas principalmente no cilindro de compósito, o que poderia, talvez, ser resolvido com o reforço do material do cilindro. / Objective: verify, by finite element analysis (FEA) and laboratorial tests, if the torsion bond strength test is able to lead adhesive interface to fracture under shear stress and if it would be more advantageous than wire-loop shear test. Material and method: for stress analysis by finite element method, the 3D models of both tests consisted of a resin composite cylinder, an adhesive layer and a dentin cylinder with a larger diameter. The specimens were simulated with both conventional and micro sizes, in a 5:1 ratio, except for the adhesive layer, kept in a constant thickness. Two values of elastic modulus were simulated for the composite cylinder (hybrid and flowable). For the shear models, different distances were simulated between the load point and the adhesive interface. The values of maximum principal and maximum shear stresses and the ratio between both types were analyzed along the adhesive interface, as well as the maximum principal vectors direction and the local of stress peaks. For the laboratorial tests, cylinders of hybrid and flowable resin composite, in both micro and conventional sizes, were adhered onto dentin surfaces by means of 3 adhesive systems. The shear load was applied with a metallic wire-loop at distances from the interface based on literature and, for the torsion test, the torque was applied by specific apparatus developed for that. The values of bond strength were submitted to analysis of variance and Tukeys test. Fracture surfaces were analyzed by scan electron microscopy. The frequencies of fracture types were compared by Fishers test and its relationship with bond strength values were verified, as well as the relationship between fracture features and stresses results obtained by FEA. The experimental parameters for comparison between both tests were: ability for detecting significant differences among the 3 adhesives, change of adhesives ranking while varying the test configuration and frequency of fracture types. Results: both tests showed non-uniform stress distribution. It was not noticed a lower sensibility of torsion test results to changes of the test configurations, nor a major ability for detecting significant differences among the adhesive systems than showed the shear test. The torsion test showed to be more difficult to execute and exhibited a higher frequency of cohesive fracture, however, that occurred most of the time in the composite cylinder, while it occurred mainly in dentin in shear test. There was no certainty about the kind of stress that lead to specimen fracture in both tests. Conclusions: although there was no certainty about the kind of stress that lead to specimen fracture and the major difficulty of execution of torsion test, this test exhibited a feature that suggests future studies: the occurrence of cohesive fracture mainly in the composite cylinder, which could be solved, maybe, by reinforcing the cylinder material.

The Lamb wave based, non-contact damage detection techniques are developed using the Modified Time Reversal (MTR) method and the model based inverse problem approach. In the first part of this work, the Lamb wave-based MTR method along with the non-contacting sensors is used for structural damage detection. The use of non-contact measurements for MTR method is validated through experimental results and finite element simulations. A novel technique in frequency-time domain is developed to detect linear damages using the MTR method. The technique is highly suitable for the detection of damages in large metallic structures, even when the damage is superficial, and the severity is low. In this technique, no baseline data are used, and all the wave motion measurements are made remotely using a laser vibrometer. Additionally, this novel MTR based technique is not affected due to changes in the material properties of a structure, environmental conditions, or structural loading conditions. Further, the MTR method is improved for two-dimensional damage imaging. The damage imaging technique is successfully tested through experimental results and finite element simulations. In the second part of this work, an inverse problem approach is developed for the detection and estimation of major damage types experienced in adhesive joints. The inverse problem solution is obtained through an optimization algorithm wherein the objective function is formulated using the Lamb wave propagation data. The technique is successfully used for the detection/estimation of cohesive damages, micro-voids, debonds, and weak bonds. Further, the inverse problem solution is separately obtained through a fully connected artificial neural network. The neural network is trained using the Lamb wave propagation data generated from Wavelet Spectral Finite Element (WSFE) model which is computationally much faster than a conventional finite element model. This inverse problem approach technique requires a single point measurement for the inspection of the entire width of the adhesive joint. The proposed technique can be used as an automated quality assurance tool during the manufacturing process, and as an inspection tool during the operational life of adhesively bonded structures.