Evaluation of sources of uncertainties in microtensile bond strength of dental adhesive system for different specimen geometries

Objective: The aim of this research is to use finite element analysis (FEA) to quantify the effect of the sample shape and the imperfections induced during the manufacturing process of samples on the bond strength and modes of failure of dental adhesive systems through microtensile test. Using the FEA prediction for individual parameters effect, estimation of expected variation and spread of the microtensile bond strength results for different sample geometries is made. Methods: The estimated stress distributions for three different sample shapes, hourglass, stick and dumbbell predicted by FEA are used to predict the strength for different fracture modes. Parameters such as the adhesive thickness, uneven interface of the adhesive and composite and dentin, misalignment of axis of loading, the existence of flaws such as induced cracks during shaping the samples or bubbles created during application of the adhesive are considered. Microtensile experiments are performed simultaneously to measure bond strength and modes of failure. These are compared with the FEA results. Results: The relative bonding strength and its standard deviation for the specimens with different geometries measured through the microtensile tests confirm the findings of the FEA. The hourglass shape samples show lower tensile bond strength and standard deviation compared to the stick and dumbbell shape samples. ANOVA analysis confirms no significant difference between dumbbell and stick geometry results, and major differences of these two geometries compared to hourglass shape measured values. Induced flaws in the adhesive and misalignment of the angle of application of load have significant effect on the microtensile bond strength. Using adhesive with higher modulus the differences between the bond strength of the three sample geometries increase. Significance: The result of the research clarifies the importance of the sample geometry chosen in measuring the bond strength. It quantifies the effect of the imperfections on the bond strength for each of the sample geometries through a systematic and all embracing study. The results explain the reasons of the large spread of the microtensile test results reported by various researchers working in different labs and the need for standardization of the test method and sample shape used in evaluation of the dentin-adhesive bonding system. © 2007 Academy of Dental Materials.

Ultrastructure of head organs (anterior adhesive apparatus) and posterior secretory systems of Caballeria liewi Lim, 1995 (Monogenea, Ancyrocephalidae)

Caballeria liewi Lim, 1995, uses adhesive secretions from the head organs and posterior secretory systems to assist in locomotion and attachment. Ultrastructural investigations show that the head organs of C. liewi consist of three pairs of antero-lateral pit-like openings bearing microvilli and ducts leading from two types of uninucleated gland cells (located lateral to the pharynx), one type producing rod-like (S1) bodies with an electron-dense matrix containing less electron-dense vesicles and the second type producing oval (S2) bodies with a homogeneous electron-dense matrix. Interlinking band-like structures are observed between S1 bodies and between S2 bodies. S1 body is synthesised in the granular endoplasmic reticulum, transported to a Golgi complex to be packaged into vesicles and routed into ducts for exudation. The synthesis of the S2 body is unresolved. Haptoral secretions manifested externally as net-like structures are derived from dual electron-dense (DED) secretory body produced in the peduncular gland cells. The DED body consists of a less electron-dense oval core in a homogeneous electron-dense matrix. On exocytosis into the pyriform haptoral reservoir, DED bodies are transformed into a secretion with two types of inclusions (less electron-dense oval and electron-dense spherical inclusions) in an electron-dense matrix. The secretions are further transformed (as small, oval, electron-dense bodies) when transported to the superficial anchor grooves, and on exudation into the gill tissues, the secretions become an electron-dense matrix. Secretory bodies associated with uniciliated structures, anchor sleeves and marginal hooks are also observed.

Micromechanical analysis of cohesive granular materials using the discrete element method with an adhesive elasto-plastic contact model

An adhesive elasto-plastic contact model for the discrete element method with three dimensional non-spherical particles is proposed and investigated to achieve quantitative prediction of cohesive powder flowability. Simulations have been performed for uniaxial consolidation followed by unconfined compression to failure using this model. The model has been shown to be capable of predicting the experimental flow function (unconfined compressive strength vs. the prior consolidation stress) for a limestone powder which has been selected as a reference solid in the Europe wide PARDEM research network. Contact plasticity in the model is shown to affect the flowability significantly and is thus essential for producing satisfactory computations of the behaviour of a cohesive granular material. The model predicts a linear relationship between a normalized unconfined compressive strength and the product of coordination number and solid fraction. This linear relationship is in line with the Rumpf model for the tensile strength of particulate agglomerate. Even when the contact adhesion is forced to remain constant, the increasing unconfined strength arising from stress consolidation is still predicted, which has its origin in the contact plasticity leading to microstructural evolution of the coordination number. The filled porosity is predicted to increase as the contact adhesion increases. Under confined compression, the porosity reduces more gradually for the load-dependent adhesion compared to constant adhesion. It was found that the contribution of adhesive force to the limiting friction has a significant effect on the bulk unconfined strength. The results provide new insights and propose a micromechanical based measure for characterising the strength and flowability of cohesive granular materials. 

Shear Strength and Durability Testing of Adhesive Bonds in Cross-Laminated Timber

The paper addresses the quality of the interface and edge bonded joints in layers of cross-laminated timber (CLT) panels. The shear performance was studied to assess the suitability of two different adhesives, Polyurethane (PUR) and Phenol-Resorcinol-Formaldehyde (PRF), and to determine the optimum clamping pressure. Since there is no established testing procedure to determine the shear strength of the surface bonds between layers in a CLT panel, block shear tests of specimens in two different configurations were carried out, and further shear tests of edge bonded specimen in two configurations were performed. Delamination tests were performed on samples which were subjected to accelerated aging to assess the durability of bonds in severe environmental conditions. Both tested adhesives produced boards with shear strength values within the edge bonding requirements of prEN 16351 for all manufacturing pressures. While the PUR specimens had higher shear strength values, the PRF specimens demonstrated superior durability characteristics in the delamination tests. It seems that the test protocol introduced in this study for crosslam bonded specimens, cut from a CLT panel, and placed in the shearing tool horizontally, accurately reflects the shearing strength of glue lines in CLT.

Experimental and numerical study of debonding in composite adhesive joints

The mode I and mode II fracture properties of the FM300-2 adhesive bond between 5HS/RTM6 laminates are determined experimentally by DCB and ELS test. The crack propagation is studied numerically by means of interface elements based on the decohesive zone model. The latter is characterized by material degradation, which is usually assumed to be linear. In the present study it is shown that if a non-linear material degradation is used with an increased magnitude of the interface relative displacement at failure it is possible to model more correctly the experimentally observed significant non-linear behaviour before the start of crack propagation. An adhesive stepped flush joint is studied experimentally and numerically. A mixed mode interaction criterion is used together with the nonlinear material degradation of the interface. Sensitivity studies are performed to study the influence of the parameters defining it.

Fracture toughness determination of adhesive and co-cured joints in natural fibre composites

Adhesive bonding has become more efficient in the last few decades due to the adhesives developments, granting higher strength and ductility. On the other hand, natural fibre composites have recently gained interest due to the low cost and density. It is therefore essential to predict the fracture behavior of joints between these materials, to assess the feasibility of joining or repairing with adhesives. In this work, the tensile fracture toughness (Gc n) of adhesive joints between natural fibre composites is studied, by bonding with a ductile adhesive and co-curing. Conventional methods to obtain Gc n are used for the co-cured specimens, while for the adhesive within the bonded joint, the J-integral is considered. For the J-integral calculation, an optical measurement method is developed for the evaluation of the crack tip opening and adherends rotation at the crack tip during the test, supported by a Matlab sub-routine for the automated extraction of these quantities. As output of this work, an optical method that allows an easier and quicker extraction of the parameters to obtain Gc n than the available methods is proposed (by the J-integral technique), and the fracture behaviour in tension of bonded and co-cured joints in jute-reinforced natural fibre composites is also provided for the subsequent strength prediction. Additionally, for the adhesively- bonded joints, the tensile cohesive law of the adhesive is derived by the direct method.

Tensile behaviour of a structural adhesive at high temperatures by the extended finite element method

Component joining is typically performed by welding, fastening, or adhesive-bonding. For bonded aerospace applications, adhesives must withstand high-temperatures (200°C or above, depending on the application), which implies their mechanical characterization under identical conditions. The extended finite element method (XFEM) is an enhancement of the finite element method (FEM) that can be used for the strength prediction of bonded structures. This work proposes and validates damage laws for a thin layer of an epoxy adhesive at room temperature (RT), 100, 150, and 200°C using the XFEM. The fracture toughness (G Ic ) and maximum load ( ); in pure tensile loading were defined by testing double-cantilever beam (DCB) and bulk tensile specimens, respectively, which permitted building the damage laws for each temperature. The bulk test results revealed that decreased gradually with the temperature. On the other hand, the value of G Ic of the adhesive, extracted from the DCB data, was shown to be relatively insensitive to temperature up to the glass transition temperature (T g ), while above T g (at 200°C) a great reduction took place. The output of the DCB numerical simulations for the various temperatures showed a good agreement with the experimental results, which validated the obtained data for strength prediction of bonded joints in tension. By the obtained results, the XFEM proved to be an alternative for the accurate strength prediction of bonded structures.

Modelling adhesive joints with cohesive zone models: effect of the cohesive law shape of the adhesive layer

Adhesively-bonded joints are extensively used in several fields of engineering. Cohesive Zone Models (CZM) have been used for the strength prediction of adhesive joints, as an add-in to Finite Element (FE) analyses that allows simulation of damage growth, by consideration of energetic principles. A useful feature of CZM is that different shapes can be developed for the cohesive laws, depending on the nature of the material or interface to be simulated, allowing an accurate strength prediction. This work studies the influence of the CZM shape (triangular, exponential or trapezoidal) used to model a thin adhesive layer in single-lap adhesive joints, for an estimation of its influence on the strength prediction under different material conditions. By performing this study, guidelines are provided on the possibility to use a CZM shape that may not be the most suited for a particular adhesive, but that may be more straightforward to use/implement and have less convergence problems (e.g. triangular shaped CZM), thus attaining the solution faster. The overall results showed that joints bonded with ductile adhesives are highly influenced by the CZM shape, and that the trapezoidal shape fits best the experimental data. Moreover, the smaller is the overlap length (LO), the greater is the influence of the CZM shape. On the other hand, the influence of the CZM shape can be neglected when using brittle adhesives, without compromising too much the accuracy of the strength predictions.

Single-lap joints of similar and dissimilar adherends bonded with an acrylic adhesive

In this study, the tensile strength of single-lap joints (SLJs) between similar and dissimilar adherends bonded with an acrylic adhesive was evaluated experimentally and numerically. The adherend materials included polyethylene (PE), polypropylene (PP), carbon-epoxy (CFRP), and glass-polyester (GFRP) composites. The following adherend combinations were tested: PE/PE, PE/PP, PE/CFRP, PE/GFRP, PP/PP, CFRP/CFRP, and GFRP/GFRP. One of the objectives of this work was to assess the influence of the adherends stiffness on the strength of the joints since it significantly affects the peel stresses magnitude in the adhesive layer. The experimental results were also used to validate a new mixed-mode cohesive damage model developed to simulate the adhesive layer. Thus, the experimental results were compared with numerical simulations performed in ABAQUS®, including a developed mixed-mode (I+II) cohesive damage model, based on the indirect use of fracture mechanics and implemented within interface finite elements. The cohesive laws present a trapezoidal shape with an increasing stress plateau, to reproduce the behaviour of the ductile adhesive used. A good agreement was found between the experimental and numerical results.

Adherend thickness effect on the tensile fracture toughness of a structural adhesive using an optical data acquisition method

Adhesive bonding is nowadays a serious candidate to replace methods such as fastening or riveting, because of attractive mechanical properties. As a result, adhesives are being increasingly used in industries such as the automotive, aerospace and construction. Thus, it is highly important to predict the strength of bonded joints to assess the feasibility of joining during the fabrication process of components (e.g. due to complex geometries) or for repairing purposes. This work studies the tensile behaviour of adhesive joints between aluminium adherends considering different values of adherend thickness (h) and the double-cantilever beam (DCB) test. The experimental work consists of the definition of the tensile fracture toughness (GIC) for the different joint configurations. A conventional fracture characterization method was used, together with a J-integral approach, that take into account the plasticity effects occurring in the adhesive layer. An optical measurement method is used for the evaluation of crack tip opening and adherends rotation at the crack tip during the test, supported by a Matlab® sub-routine for the automated extraction of these quantities. As output of this work, a comparative evaluation between bonded systems with different values of adherend thickness is carried out and complete fracture data is provided in tension for the subsequent strength prediction of joints with identical conditions.

The Use of Carboxy Terminated Liquid Natural Rubber (CTNR) as an Adhesive in Bonding Rubber to Rigid and Non-rigid Substrates

Carboxy Terminated Liquid Natural Rubber (CTNR) was prepared by photochemical reaction using maleic anhydride and masticated natural rubber (NR). The use of CTNR as an adhesive in bonding rubber to rubber and rubber to metal was studied. The peel strengths and lap shear strengths of the adherends which were bonded using CTNR were determined. The effect of using a tri isocyanate with CTNR in rubber to metal bonding was also studied. It is found that CTNR can effectively be used in bonding rubber to rubber and rubber to mild steel.

Novel adhesive systems based on neoprene-phenolic blends

The aim of the investigation is to develop new high performance adhesive systems based on neoprene-phenolic blends. Initially the effect of addition of all possible ingredients like fillers, adhesion promoters, curing agents and their optimum compositions to neoprene solution is investigated. The phenolic resin used is a copolymer of phenol-cardanolformaldehyde prepared in the laboratory. The optimum ratio between phenol and cardanol that gives the maximum bond strength in metal-metal, rubber-rubber and rubber-metal specimens has been identified. Further the ratio between total phenols and formaldehyde is also optimised. The above adhesive system is further modified by the addition of epoxidized phenolic novolacs. For this purpose, phenolic novolac resins are prepared in different stoichiometric ratios and are subsequently epoxidized. The effectiveness of the adhesive for bonding different metal and rubber substrates is another part of the study. To study the ageing behaviour, different bonded specimens are exposed to high temperature, hot water and salt water and adhesive properties have been evaluated. The synthesized resins have been characterized by FTIR , HNMR spectroscopy. The molecular weights of the resins have been obtained by GPC. Thermogravimetric analysis and differential scanning calorimetry are used to study the thermal properties. The fractured surface analysis is studied by scanning electron microscopy. The study has brought to light the influence of phenol/ formaldehyde stoichiometric ratio, addition of cardanol (a renewable resource), adhesion promoters and suitability of the adhesive for different substrates and the age resistance of adhesive joints among other things.

Carbohydrate-based anti-adhesive inhibition of Vibrio cholerae toxin binding to GM1-OS immobilized into artificial planar lipid membranes

We have studied 'food grade' sialyloligosaccharides (SOS) as anti-adhesive drugs or receptor analogues, since the terminal sialic acid residue has already been shown to contribute significantly to the adhesion and pathogenesis of the Vibrio cholerae toxin (Ctx). GM1-oligosaccharide (GM1-OS) was immobilized into a supporting POPC lipid bilayer onto a surface plasmon resonance (SPR) chip, and the interaction between uninhibited Ctx and GM1-OS-POPC was measured. SOS inhibited 94.7% of the Ctx binding to GM1-OS-POPC at 10 mg/mL. The SOS EC50 value of 5.521 mg/mL is high compared with 0.2811 mu g/mL (182.5 pM or 1.825 x 10(-10) M) for GM1-OS. The commercially available sialyloligosaccharide (SOS) mixture Sunsial E (R) is impure, containing one monosialylated and two disialylated oligosaccharides in the ratio 9.6%. 6.5% and 17.5%, respectively, and 66.4% protein. However, these inexpensive food-grade molecules are derived from egg yolk and could be used to fortify conventional food additives, by way of emulsifiers, sweeteners and/or preservatives. The work further supports our hypothesis that SOS could be a promising natural anti-adhesive glycomimetic against Ctx and prevent subsequent onset of disease. (C) 2009 Elsevier Ltd. All rights reserved

An adhesive elastomeric supramolecular polyurethane healable at body temperature

In this paper, we report the synthesis and healing ability of a non-cytotoxic supramolecular polyurethane network whose mechanical properties can be recovered efficiently (> 99%) at the temperature of the human body (37 ºC). Rheological analysis revealed an acceleration in the drop of the storage modulus above 37 ºC, on account of the dissociation of the supramolecular polyurethane network, and this decrease in viscosity enables the efficient recovery of the mechanical properties. Microscopic and mechanical characterisation has shown that this material is able to recover mechanical properties across a damage site with minimal contact required between the interfaces and also demonstrated that the mechanical properties improved when compared to other low temperature healing elastomers or gel-like materials. The supramolecular polyurethane was found to be non-toxic in a cytotoxicity assay carried out in human skin fibroblasts (cell viability > 94% and non-significantly different compared to the untreated control). This supramolecular network material also exhibited excellent adhesion to pig skin and could be healed completely in situ post damage indicating that biomedical applications could be targeted, such as artificial skin or wound dressings with supramolecular materials of this type.