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Two commercial carboxymethylcellulose acetate butyrate (CMCAB) polymers, high and low molecular weight (MW) forms, were analyzed in this study. High-solids water-borne dispersions of these polymers were studied as renewable wood adhesives. Neat polymer analyses revealed that the apart from MW, the CMCAB systems had different acid values, and that the high MW system was compromised with gel particle contaminants. Formulation of the polymer into water-dispersions was optimized for this study, and proved the "direct method", in which all formulation components were mixed at once in a sealed vessel, was the most efficient preparation technique. Applying this method, 4 high-solids water dispersions were prepared and evaluated with viscometry, differential scanning calorimetry, dynamic mechanical analysis, light and fluorescence microscopy, and mode I fracture testing. Thermal analyses showed that the polymer glass transition temperature significantly increased when bonded to wood. CMCAB dispersions produced fairly brittle adhesive-joints; however, it is believed toughness can likely be improved with further formulation optimization. Lastly, dispersion viscosity, film formation, adhesive penetration and joint-performance were all dependent on the formulation solvents, and moreover, these properties appeared to correlate with each other. / Master of Science

Hydroxymethyl resorcinol (HMR) is an effective adhesion promoter (primer) for wood bonding; it dramatically improves adhesion and enhances bond durability against moisture exposure. In an effort to improve understanding of the HMR mechanism of action, this work compared HMR with two other chemical treatments investigated as wood primers: alkyl-HMR (a-HMR), an HMR variant having reduced crosslink density, and a 5% solution of polymeric methylenebis(phenylisocyanate) in N-methylpyrrolidone (solution referred to as "pMDI"). The experimental system was red oak (Quercus rubra) bonded with a moisture-cure polyurethane adhesive (PUR). The objective was to document wood rheological changes induced by the three primers, and determine if these changes correlated to primer efficacy in PUR-bonded red oak. Adhesion was tested in mode-I (opening) fracture using dual cantilever beam specimens. HMR and a-HMR proved to be highly effective primers for PUR-bonded red oak; both primers dramatically improved bondline toughness and durability. Relative to HMR, the reduced crosslink density in a-HMR did not impair primer efficacy. In contrast, the pMDI primer was ineffective; it reduced bondline toughness and durability. Solvent-submersion, torsional dynamic mechanical analysis (DMA) was conducted on primer-treated red oak (with specimens immersed in dimethylformamide). Using all three grain orientations, the lignin glass/rubber transition was carefully studied with attention directed towards primer-induced changes in stiffness (storage modulus), the glass transition temperature (Tg), the associated damping (tan ° maximum intensity), and the breadth of tan ° transition. It was found that primer effectiveness correlated with a reduction in damping intensity, and also with a Tg increase greater than 5°C. Determination of these correlations was complicated by grain dependency, and also by rheological changes caused by solvent treatments that were used as primer control treatments. / Master of Science

La transition entre le comportement effusif et explosif des volcans de magma riche en silice est en partie contrôlée par la capacité des surpressions gazeuses à se dissiper hors du magma. La libération efficace des gaz est associée aux éruptions effusives tandis que la rétention de ces gaz contribue aux processus explosifs. L’une des approches pour évaluer la facilité d’échappement des gaz est de considérer l’évolution et le développement de la perméabilité dans la colonne magmatique et dans l'édifice. J'évalue dans ce travail de thèse le rôle des changements post-mise en place sur la microstructure dans des andésites basaltiques du Merapi (Indonésie). La perméabilité de ces roches est principalement contrôlée par des fissures liées à leur mise en place. Malgré l’influence importante de ces fissures post-mise en place pour dégazer à travers l'édifice, elles ne contribuent pas au dégazage intrinsique du magma en cours d’ascension. Pour s’affranchir de l'influence des microstructures post-mise en place du magma, j'étudie le développement et l'évolution in situ des réseaux perméables en déformant des magmas à deux phases (bulles de gaz et liquide silicaté) en cisaillement simple dans une presse Paterson selon des viscosités et des vitesses de déformation réalistes pour la partie haute des conduits des strato-volcans. Le développement de la perméabilité est confirmé in situ et se développe à des vitesses de déformation supérieures à 4,5 x 10⁻⁴ s⁻¹. À des vitesses de déformation élevées (> 5 x 10⁻⁴ s⁻¹) le magma est fragile et l’échappement du gaz est lente, facilitée par l'interconnexion de courtes fractures de Mode I. À des vitesses de déformation < 5 × 10⁻⁴ s⁻¹, le magma se comporte à la fois de manière fragile et visqueuse et la perméabilité se développe lorsque la déformation est importante; le gaz s’échappe rapidement par de longues fractures de Mode I bien développées. Les fractures de Mode I sont idéalement orientées pour le dégazage du conduit central et sont, surtout, soumises à peu de déformation jusqu'à ce qu'elles soient réorientées dans la direction de cisaillement. Ces caractéristiques de dégazage peuvent, à long terme, favoriser un dynamisme éruptif effussif. / The transition from effusive to explosive behaviour at silicic volcanoes is, in part, governed by how efficiently gas overpressures are dissipated from the volcanic plumbing. Efficient gas release is associated with effusive eruptions while inadequate outgassing contributes to explosive processes. One approach to assessing the facility of gas escape is by considering how permeability develops and evolves in the magma column and surrounding edifice. Here, I appraise the role of post-emplacement changes to microstructure in edifice-forming basaltic andesites from Merapi (Indonesia). The permeability of these rocks is dominantly crack-controlled and while these features exert important controls on gas escape through the edifice, they do not represent the escape pathways available to gas within ascending magma. To avoid the influence of postemplacement microstructure, I investigate the development and evolution of permeable networks in magmas by deforming initially impermeable two-phase magmas in simple shear. This is done in a Paterson apparatus at viscosities and shear strain rates appropriate to upper conduits in stratovolcanoes. Permeability development is confirmed in situ and develops at moderate to high shear strain rates (> 4.5 × 10⁻⁴ s⁻¹). At very high strain rates (> 5 × 10⁻⁴ s⁻¹) the magma behaves in a brittle manner and gas egress is slow, facilitated by the interconnection of short, Mode I fractures. At moderate shear strain rates (< 5 × 10⁻⁴ s⁻¹), the magma displays both brittle and viscous behaviour and permeability develops at high strain; gas escape is rapid owing to long, well-developed, sample-length Mode I fractures. Mode I fractures are ideally oriented for outgassing of the central conduit and, critically, accommodate little deformation until they are rotated into the direction of shear, making them long-lived outgassing features that may favour volcanic effusion.

An experimental evaluation of the mixed-mode fracture behavior of bonded composite joints is presented. Commonly used experimental techniques for characterizing the mode I, mixed-mode I/II, mode II, and mode III fracture behavior have been employed for the purpose of developing a fracture envelope to be utilized in the automotive design process. These techniques make use of such test geometries as the double cantilever beam (DCB), asymmetric double cantilever beam (ADCB), single-leg bend (SLB), end-loaded split (ELS), and split cantilever beam (SCB) specimens. Symmetric versions of the DCB, SLB, and ELS specimens produced mode mixities of 0°, 41°, and 90° respectively, while the testing of ADCB specimens allowed for mode mixities of 18°, 31°. Pronounced stick-slip behavior was observed for all specimen test geometries under both quasi-static and dynamic loading conditions. Due to the nature of the adhesive studied, a limited number of data points were obtained under mode I loading conditions. A significant increase in the number of measurable crack initiation events was observed for mixed-mode I/II loading conditions, where stick slip behavior was less pronounced. Additionally, a comparison of the measured fracture energies obtained under mixed-mode I/II loading conditions reveals that the addition of a small mode II component results in a decrease in the mode I fracture energy by roughly 50%, as the crack was driven to the interface between the adhesive layer and composite adherends. Furthermore, the propensity of debonds to propagate into the woven composite laminate adherends under mode II loading conditions limited the number of crack initiation points that could be obtained to one or two usable data points per specimen. A limited number of experimental tests using the SCB specimen for mode III fracture characterization, combined with a numerical analysis via finite element analysis, revealed a significant mode II contribution toward the specimen edges. Similarly, FE analyses on full bond width and half bond width SCB specimens was conducted, and results indicate that by inducing a bond width reduction of 50%, the mode II contribution is greatly decreased across the entire width of the specified crack front. To provide a means for comparison to results obtained using the standard DCB specimen, an alternative driven wedge test specimen geometry was analyzed, as this geometry provided a significant increase in the number of measurable data points under mode I loading conditions. A three-dimensional finite element analysis was conducted to establish ratios of simple beam theory results to those obtained via FEA, GSBT/GFEA, were of particular interest, as these ratios were used to establish correction factors corresponding to specific crack lengths to be used in correcting results obtained from an experimental study utilizing a driven wedge technique. Corrected results show good agreement with results obtained from traditional mode I double cantilever beam tests. Finally, bulk adhesive experiments were conducted on compact tension specimens to establish a correlation between adhesively bonded composite joint and bulk adhesive fracture behavior under mode I loading conditions. Measured fracture energy values were shown to gradually drop across a range of applied loading rates, similar to the rate-dependent behavior observed with both the DCB and driven wedge specimens. Application of the time-temperature superposition principle was explored to determine whether or not such techniques were suitable for predicting the fracture behavior of the adhesive studied herein. Good correlation was established between the fracture energy values measured and the value of tan d obtained from dynamic mechanical analysis tests conducted at corresponding reduced test rates. / Master of Science

Desde o início dos anos 70, novos conceitos de mecânica da fratura foram desenvolvidos para explicar o comportamento das rochas. A tenacidade à fratura foi medida e considerada como uma propriedade intrínseca importante da rocha, a qual indica a magnitude da resistência à fratura ou sua habilidade para resistir à propagação da trinca. A mecânica da fratura foi amplamente aplicada em operações de desmonte por explosivos, fraturamento hidráulico, fragmentação mecânica, análise da estabilidade de taludes, geofísica, mecânica de terremotos, na energia de extração geotermal e em outros problemas práticos. Salienta-se que ela é também relevante em tectônica, na tecnologia de recuperação e armazenamento de energia e na engenharia de rochas. Nas últimas três décadas, diversos métodos para estudar a propagação da fratura no modo I foram desenvolvidos e uma série de artigos foi escrita para aumentar o conhecimento da tenacidade à fratura das rochas no modo I. Um grande número de metodologias de ensaio da tenacidade à fratura tem aparecido na literatura. Alguns procedimentos de ensaio para a determinação da tenacidade à fratura em rochas no modo I foram padronizados pela ISRM em 1988 e em 1995. Entretanto, estes métodos de ensaio apresentam algumas dificuldades relacionadas à preparação do corpo de prova, à complexidade da instalação e à interpretação e validade dos resultados. O objetivo deste estudo é o de comparar os métodos sugeridos pela ISRM com outros métodos sugeridos por outros pesquisadores. Alguns ensaios não padronizados podem ser úteis se conduzirem a resultados confiáveis e se seus procedimentos forem mais simples do que aqueles sugeridos pela ISRM / Since early 1970's new fracture mechanics concepts have been developed to explain rock fracture behavior. Fracture toughness has been measured and considered as an important intrinsic property of rock indicating the magnitude of fracture strength or its ability to resist crack propagation. Rock fracture mechanics has been widely applied to tectonics, energy recovery and storage technology and rock engineering. It is relevant in blasting, hydraulic fracturing, mechanical fragmentation, rock slope analysis, geophysics, earthquake mechanics, geothermal energy extraction and many other practical problems. Over the last three decades, several methods for studying the mode I fracture propagation have been developed and a series of papers have been written to increase the knowledge of the mode I fracture toughness in rocks. A great number of fracture toughness testing methodologies have appeared in the literature. Some related mode I rock fracture toughness test procedures have been standardized by ISRM in 1988 and in 1995. However, these testing methods present some relative difficulties in sample preparation, set-up complexity, interpretation and results trustworthiness. The aim of this study is to compare the fracture toughness ISRM suggested testing methods with other suggested methodologies for other researchers. Some of the non-standardized tests may be useful, if they lead to reliable results, and if their procedures are simpler than those suggested by ISRM

Modified Ring specimens are of the shape of discs having a hole inside and flattened ends. These specimens are used for determination of Mode I fracture toughness. Finite element program, named ABAQUS, is used for numerical modeling for finding stress intensity factors. Varying disc geometries were used for the experiments and numerical modeling in which size of the flat ends, radius of the hole inside, and external radius of the specimen were varied. Experiments were done by using pink Ankara andesite. Effects of internal hole radius, external disc radius and size of the flat ends on both stress intensity factor and fracture toughness were studied. In order to compare the results, fracture tests with semi-circular specimens under three point bending (SCB) were also performed. From a similar previous study, fracture toughness values of gray andesite were recalculated and compared to the fracture toughness values of pink andesite for varying geometrical factors. Size effect studies were performed as well for varying diameter of core specimens.Fracture toughness values of andesite were found to increase with increasing specimen size. Fracture toughness of 100 mm specimens was determined as 1.11&plusmn / 0.07 MPa&amp / #8730 / m, whereas fracture toughness of 75 mm specimens was 0.96&plusmn / 0.08 MPa&amp / #8730 / m. 100 mm or larger diameter specimens were suggested for the fracture toughness determination with the modified ring tests.

Desde o início dos anos 70, novos conceitos de mecânica da fratura foram desenvolvidos para explicar o comportamento das rochas. A tenacidade à fratura foi medida e considerada como uma propriedade intrínseca importante da rocha, a qual indica a magnitude da resistência à fratura ou sua habilidade para resistir à propagação da trinca. A mecânica da fratura foi amplamente aplicada em operações de desmonte por explosivos, fraturamento hidráulico, fragmentação mecânica, análise da estabilidade de taludes, geofísica, mecânica de terremotos, na energia de extração geotermal e em outros problemas práticos. Salienta-se que ela é também relevante em tectônica, na tecnologia de recuperação e armazenamento de energia e na engenharia de rochas. Nas últimas três décadas, diversos métodos para estudar a propagação da fratura no modo I foram desenvolvidos e uma série de artigos foi escrita para aumentar o conhecimento da tenacidade à fratura das rochas no modo I. Um grande número de metodologias de ensaio da tenacidade à fratura tem aparecido na literatura. Alguns procedimentos de ensaio para a determinação da tenacidade à fratura em rochas no modo I foram padronizados pela ISRM em 1988 e em 1995. Entretanto, estes métodos de ensaio apresentam algumas dificuldades relacionadas à preparação do corpo de prova, à complexidade da instalação e à interpretação e validade dos resultados. O objetivo deste estudo é o de comparar os métodos sugeridos pela ISRM com outros métodos sugeridos por outros pesquisadores. Alguns ensaios não padronizados podem ser úteis se conduzirem a resultados confiáveis e se seus procedimentos forem mais simples do que aqueles sugeridos pela ISRM / Since early 1970's new fracture mechanics concepts have been developed to explain rock fracture behavior. Fracture toughness has been measured and considered as an important intrinsic property of rock indicating the magnitude of fracture strength or its ability to resist crack propagation. Rock fracture mechanics has been widely applied to tectonics, energy recovery and storage technology and rock engineering. It is relevant in blasting, hydraulic fracturing, mechanical fragmentation, rock slope analysis, geophysics, earthquake mechanics, geothermal energy extraction and many other practical problems. Over the last three decades, several methods for studying the mode I fracture propagation have been developed and a series of papers have been written to increase the knowledge of the mode I fracture toughness in rocks. A great number of fracture toughness testing methodologies have appeared in the literature. Some related mode I rock fracture toughness test procedures have been standardized by ISRM in 1988 and in 1995. However, these testing methods present some relative difficulties in sample preparation, set-up complexity, interpretation and results trustworthiness. The aim of this study is to compare the fracture toughness ISRM suggested testing methods with other suggested methodologies for other researchers. Some of the non-standardized tests may be useful, if they lead to reliable results, and if their procedures are simpler than those suggested by ISRM

<p>QC 20110523</p>