Crack Path Selection in Adhesively-Bonded Joints: The Role of Material Properties

This paper investigates the role of material properties on crack path selection in adhesively bonded joints. First, a parametric study of directionally unstable crack propagation in adhesively-bonded double cantilever beam specimens (DCB) is presented. The results indicate that the characteristic length of directionally unstable cracks varies with the Dundurs' parameters characterizing the material mismatch. Second, the effect of interface properties on crack path selection is investigated. DCB specimens with substrates treated using various surface preparation methods are tested under mixed mode fracture loading to determine the effect of interface properties on the locus of failure. As indicated by the post-failure analyses, debonding tends to be more interfacial as the mode II fracture component in the loading increases. On the other hand, failures in specimens prepared with more advanced surface preparation techniques appear more cohesive for given loading conditions. Using a high-speed camera to monitor the fracture sequence, DCB specimens are tested quasi-statically and the XPS analyses conducted on the failure surfaces indicate that the effect of crack propagation rate on the locus of failure is less significant when more advanced surface preparation techniques are used. The effect of asymmetric interface property on the behavior of directionally unstable crack propagation in adhesive bonds is also investigated. Geometrically-symmetric DCB specimens with asymmetric surface pretreatments are prepared and tested under low-speed impact. As indicated by Auger depth profile results, the centerline of the crack trajectory shifts slightly toward the interface with poor adhesion due to the asymmetric interface properties. Third, through varying the rubber content in the adhesive, DCB specimens with various fracture toughnesses are prepared and tested. An examination of the failure surfaces reveals that directionally unstable crack propagation is more unlikely to occur as the toughness of the adhesive increases, which is consistent with the analytical predictions that were discussed using an energy balance model.     

Crack Path Selection in Adhesively-Bonded Joints: The Role of Material Properties

This paper investigates the role of material properties on crack path selection in adhesively bonded joints. First, a parametric study of directionally unstable crack propagation in adhesively-bonded double cantilever beam specimens (DCB) is presented. The results indicate that the characteristic length of directionally unstable cracks varies with the Dundurs' parameters characterizing the material mismatch. Second, the effect of interface properties on crack path selection is investigated. DCB specimens with substrates treated using various surface preparation methods are tested under mixed mode fracture loading to determine the effect of interface properties on the locus of failure. As indicated by the post-failure analyses, debonding tends to be more interfacial as the mode II fracture component in the loading increases. On the other hand, failures in specimens prepared with more advanced surface preparation techniques appear more cohesive for given loading conditions. Using a high-speed camera to monitor the fracture sequence, DCB specimens are tested quasi-statically and the XPS analyses conducted on the failure surfaces indicate that the effect of crack propagation rate on the locus of failure is less significant when more advanced surface preparation techniques are used. The effect of asymmetric interface property on the behavior of directionally unstable crack propagation in adhesive bonds is also investigated. Geometrically-symmetric DCB specimens with asymmetric surface pretreatments are prepared and tested under low-speed impact. As indicated by Auger depth profile results, the centerline of the crack trajectory shifts slightly toward the interface with poor adhesion due to the asymmetric interface properties. Third, through varying the rubber content in the adhesive, DCB specimens with various fracture toughnesses are prepared and tested. An examination of the failure surfaces reveals that directionally unstable crack propagation is more unlikely to occur as the toughness of the adhesive increases, which is consistent with the analytical predictions that were discussed using an energy balance model.     

Grafting of Epoxy Resin on Surface-modified Poly(tetrafluoroethylene) Films

An epoxy/PTFE composite was prepared by curing the epoxy resin on the surface-modified PTFE film. Surface modification of PTFE films was carried out via argon plasma pretreatment, followed by UV-induced graft copolymerization with glycidyl methacrylate (GMA). The film composite achieved a 90°-peel adhesion strength above 15 N/cm. The strong adhesion of the epoxy resin to PTFE arose from the fact that the epoxide groups of the grafted GMA chains were cured into the epoxy resin matrix to give rise to a highly crosslinked interphase, as well as the fact that the GMA chains were covalently tethered on the PTFE film surface. Delamination of the composite resulted in cohesive failure inside the PTFE film and gave rise to an epoxy resin surface with a covalently-adhered fluoropolymer layer. The surface composition and microstructures of the GMA graft-copolymerized PTFE (GMA-g-PTFE) films and those of the delaminated epoxy resin and PTFE film surfaces were characterized by X-ray photoelectron spectroscopy (XPS), water contact angle and scanning electron microscope (SEM) measurements. The delaminated epoxy resin surfaces were highly hydrophobic, having water contact angles of about 140°C. The value is higher than that of the pristine PTFE film surface of about 110°. The epoxy resin samples obtained from delamination of the epoxy/GMA-g-PTFE composites showed a lower rate of moisture sorption. All the fluorinated epoxy resin surfaces exhibited rather good stability when subjected to the Level 1 hydrothermal reliability tests.     

Grafting of Epoxy Resin on Surface-modified Poly(tetrafluoroethylene) Films

An epoxy/PTFE composite was prepared by curing the epoxy resin on the surface-modified PTFE film. Surface modification of PTFE films was carried out via argon plasma pretreatment, followed by UV-induced graft copolymerization with glycidyl methacrylate (GMA). The film composite achieved a 90°-peel adhesion strength above 15 N/cm. The strong adhesion of the epoxy resin to PTFE arose from the fact that the epoxide groups of the grafted GMA chains were cured into the epoxy resin matrix to give rise to a highly crosslinked interphase, as well as the fact that the GMA chains were covalently tethered on the PTFE film surface. Delamination of the composite resulted in cohesive failure inside the PTFE film and gave rise to an epoxy resin surface with a covalently-adhered fluoropolymer layer. The surface composition and microstructures of the GMA graft-copolymerized PTFE (GMA-g-PTFE) films and those of the delaminated epoxy resin and PTFE film surfaces were characterized by X-ray photoelectron spectroscopy (XPS), water contact angle and scanning electron microscope (SEM) measurements. The delaminated epoxy resin surfaces were highly hydrophobic, having water contact angles of about 140°C. The value is higher than that of the pristine PTFE film surface of about 110°. The epoxy resin samples obtained from delamination of the epoxy/GMA-g-PTFE composites showed a lower rate of moisture sorption. All the fluorinated epoxy resin surfaces exhibited rather good stability when subjected to the Level 1 hydrothermal reliability tests.     

Characterization of ramie fiber/soy protein concentrate (SPC) resin interface

Ramie fiber/soy protein concentrate (SPC) polymer (resin) interfacial shear strength (IFSS) was measured using the microbond technique. To characterize the effect of plasticization, SPC resin was mixed with glycerin. Fibers were also treated with ethylene plasma polymer to reduce fiber surface roughness and polar nature to control the IFSS. Fiber surfaces after ethylene plasma polymerization, and fracture surfaces of specimens before and after the microbond tests were characterized using a scanning electron microscope (SEM). Some specimens were also characterized using electron microprobe analyzer (EMPA) to map the residual resin on the fiber surface after the microbond test. Effects of glycerin concentration in SPC and ethylene plasma fiber surface treatment time on the IFSS were investigated. Preparation of SPC resin requires a large amount of water. As expected, during drying of SPC resin, the microdrops shrank significantly. The high IFSS values indicate strong interfacial interaction in the ramie fiber/SPC resin system. This strong interfacial interaction is a result of a highly polar nature of both the ramie fiber and the SPC resin and rough fiber surface. Ethylene plasma polymerization was used to control the IFSS. The plasma polymer imparted a polyethylene-like, non-polar polymer coating on the fiber surface. As a result, the fiber surface became smoother compared to the untreated fiber. Both fiber smoothness and non-polar nature of the coating reduced the ramie fiber/SPC resin IFSS. Plasticization of the SPC resin by glycerin also decreased the adhesion strength of the ramie fibers with the SPC resin. The load-displacement plots for IFSS tests obtained for different resin and fiber combinations indicate different interfacial failure modes.     

Characterisation of GFRP surfaces amenable for bonding and their effect on the strength of co-cured vacuum resin infused single lap joints

The choice of a fabrication method is of primary importance in order to optimise and control the performance of composite materials. This becomes increasingly crucial when the fabrication method itself becomes in parallel an adhesive bonding co-cure technique. In this paper, the manufacturing process of the vacuum resin infusion jointing is introduced and specimens of co-cured single lap joints are fabricated and tested under a tensile load. The aim is to show the correlation between the surface characteristics of mechanically treated composite laminates and the adhesion performances of the corresponding surface assemblies using the vacuum resin infusion as a jointing procedure. The mechanisms that govern adhesion are investigated by measuring several physical and chemical parameters of the bonded surfaces with techniques such as surface profilometry, contact angle and surface energy measurements, X-ray photoelectron spectroscopy and scanning electron microscopy. These methods qualitatively and quantitatively measure the influence of surface characteristics towards adequate interfacial bond strength and reveal the importance of the mechanical interlocking, kinetics of wetting, chemical reactivity and intermolecular adhesion of the vacuum resin infusion joint interfaces. The results clearly demonstrate the major influence of the surface contamination and surface topography but also the role of the joining process itself, having no distinct adhesive layer, on the adhesion properties. It is shown that the interfacial adhesion qualities alter significantly the fragmentation process and the strength of the vacuum resin infused joints.     

Control over wettability of textured surfaces by electrospray deposition

Microtextured surfaces were prepared by electrospray deposition (ESD) from hydrophilic and hydrophobic acrylic resin solutions. The surface morphologies and topologies were characterized using scanning electron microscopy and laser profile microscopy, respectively. Wetting behaviors on the surfaces were characterized by contact angle and sliding angle measurements. The contact angle of the water droplet on the hydrophilic resin‐coated surfaces decreased with an increase in the surface roughness. On the other hand, the contact angle on the hydrophobic resin‐coated surfaces increased with an increase in the surface roughness. In addition, a patterned surface composed of aligned fibers by ESD showed anisotropy of both wetting and sliding behaviors. These results indicate that ESD is a useful method for designing a textured surfaces and controlling the surface wettability. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3811–3817, 2007     

Modeling of the fracture mechanism of HDPE subjected to environmental stress crack resistance test

Environmental stress crack resistance (ESCR) is a commonly used test to characterize cracking failure of high‐density polyethylene in applications such as wires, cables, blow molded containers, and other rigid packaging applications. From a resin design standpoint, it is important to understand the mechanism of environmental stress cracking especially in the case of materials with significantly different ESCR values. Currently, two standard ESCR tests, ASTM D1693 and ASTM F2136, are commonly accepted to measure environmental stress crack resistance of HDPE. An accurate observation of ESC is important to understand the fracture mechanism of samples. In this study, the ESCR performance of six HDPE samples was determined per ASTM D1693. The failed specimens were further characterized by scanning electron microscopy and fractographic methodology to investigate the failure mechanism. HDPE resins with low ESCR values had crack surfaces characterized by shorter and fewer fibrils. A new empirical model to predict polymer ESCR using tie chain concentration with different integration range, and water vapor transmission rate, to characterize detergent diffusion in the crack, was developed. The proposed empirical parameter improves the prediction of ESCR. The ability to predict ESCR performance from resin properties is a beneficial tool for new product development. POLYM. ENG. SCI., 2009. © 2009 Society of Plastics Engineers     

Adhesive properties of epoxy resin modified by end‐functionalized liquid polybutadiene

Adhesive properties of epoxy resin networks modified with different functionalized liquid polybutadiene were evaluated by using aluminum adherent. The end‐functionalized polybutadiene rubbers were hydroxyl‐ (HTPB), carboxyl‐ (CTPB), and isocyanate‐terminated polybutadiene (NCOTPB). The adhesive properties depend upon the morphology and the degree of interaction between the rubber–epoxy system. The most effective adhesive for Al–Al joint in both butt and single‐lap shear testing was epoxy resin–NCOTPB system. This system presents stronger rubber–epoxy interactions and a higher degree of rubber particle dispersion with particle size diameter in the nanoscale range. These characteristics were not important for improving the toughness of the bulk network but are fundamental for the improvement of adhesive strength. The effect of the pretreatment of the aluminum surface on the roughness was also evaluated by using profilometry analysis. The type of failure was also investigated by analyzing the adhered surfaces after fracture by scanning electron microscopy and profilometry. A proportion of cohesion failure higher than 90% was observed in all systems. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 2370–2378, 2004     

Strap repairs using embedded patches: numerical analysis and experimental results

Adhesively bonded repairs offer an attractive option for repair of aluminium structures, compared to more traditional methods such as fastening or welding. The single-strap (SS) and double-strap (DS) repairs are very straightforward to execute but stresses in the adhesive layer peak at the overlap ends. The DS repair requires both sides of the damaged structures to be reachable for repair, which is often not possible. In strap repairs, with the patches bonded at the outer surfaces, some limitations emerge such as the weight, aerodynamics and aesthetics. To minimize these effects, SS and DS repairs with embedded patches were evaluated in this work, such that the patches are flush with the adherends. For this purpose, in this work standard SS and DS repairs, and also with the patches embedded in the adherends, were tested under tension to allow the optimization of some repair variables such as the overlap length (L_O) and type of adhesive, thus allowing the maximization of the repair strength. The effect of embedding the patch/patches on the fracture modes and failure loads was compared with finite elements (FE) analysis. The FE analysis was performed in ABAQUS® and cohesive zone modelling was used for the simulation of damage onset and growth in the adhesive layer. The comparison with the test data revealed an accurate prediction for all kinds of joints and provided some principles regarding this technique.     

Laboratory investigation of cracking resistance performance of the cold-mixed epoxy resin

Cold-mix epoxy resin (CER) is an excellent binder material but with weak crack resistance and brittle failure risk. Therefore, it is of significance to find a feasible parameter to constrain the failure potential. To this end, the dynamic mechanical test, tensile test, volume shrinkage test, fracture test, and scanning electron microscopy (SEM) were used to analyze and evaluate mechanical properties, curing shrinkage, and fracture toughness of the CER. Subsequently, the bivariate correlation analysis was used to feature the relationship among different indicators. The results indicated that the amount of curing agent has a significant influence on the tensile strength, elongation at break, volume shrinkage, fracture toughness, and plastic radius of CER. Meanwhile, there is a close correlation between tensile strength, elongation at break, and fracture toughness. Fracture toughness can be used as an evaluation index to represent the crack resistance of CER, and tensile test can be used as a confirmatory parameter. However, the volume shrinkage of CER cannot be ignored. Small voids distributed on the fracture surface of the CER can increase the toughness and then improve the crack resistance of the CER through SEM analysis.     

Design guidelines for composite patches bonded to cracked aluminum substrates

Design guidelines are proposed for boron fiber-reinforced epoxy composite patches bonded to cracked aluminum substrates. Stress analysis was performed on the composite patch bonded to an uncracked aluminum substrate. The load transfer via the adhesive and the stress levels in the aluminum substrate and the patch were determined. The local stress and stress distribution in the repaired V-shape side cracked substrates were obtained. The effects of crack length and patch geometries including the length and number of plies on the failure behavior of the repair were identified. The results were validated by static tensile tests. It was found that the theoretical calculations were in agreement with the experimental results. This indicates that the proposed analysis can be used as design guidelines for composite repairs of cracked structures. These guidelines coupled with a simple surface preparation technique developed in this work might aid composite patch installation in service.     

Fracture behavior of polyetherimide (PEI) and interlaminar fracture of CF/PEI laminates at elevated temperatures

To investigate the effects of environmental temperature on fracture behavior of a polyetherimide (PEI) thermoplastic polymer and its carbon fiber (CF/PEI) composite, experimental and numerical studies were performed on compact tension (CT) and double cantilever beam (DCB) specimens under mode‐I loading. The numerical analyses were based on 2‐D large deformation finite element analyses (FEA). Elevated temperatures greatly released the crack tip triaxiality (constraint) and promoted matrix deformation due to low yield strength and enhanced ductility of the PEI matrix, which resulted in the greater plane‐strain fracture toughness of the bulk PEI polymer and the interlaminar fracture toughness of its composite during delamination propagation with increasing temperature. Furthermore, the high triaxiality was developed around the delamination front tip in the DCB specimen, which accounted for the poor translation of matrix toughness to the interlaminar fracture toughness by suppressing the matrix deformation and reducing the plastic energy dissipated in the plastic zone. Especially, at delamination initiation, the weakened fiber/matrix adhesion at elevated temperatures led to premature failure of fiber/matrix interface, suppressing matrix deformation and preventing the full utilization of matrix toughness. Consequently, low interlaminar fracture toughness was obtained at elevated temperatures. POLYM. COMPOS., 26:20–28, 2005. © 2004 Society of Plastics Engineers.     

Effect of thermoplastic veils on interlaminar fracture toughness of a glass fiber/vinyl ester composite

The effects of two thermoplastic micro‐veils, polyamide (PA) and polyethylene terephthalate (PET) veil, on the interlaminar fracture toughness of a glass fiber/vinyl ester (GF/VE) composite were investigated. The veils incorporated into the composite as interleaving materials were first characterized via scanning electron microscopy (SEM), differential scanning calorimetry (DSC), contact angle and tensile testing in order determine the best candidate as toughening agent for the GF/VE composite. Composite laminates were manufactured by vacuum‐assisted resin infusion process. Double cantilever beam (DCB) testing was performed to investigate the Mode I type interlaminar fracture toughness of the composites, which was characterized by critical strain energy release rate (G _IC). An increased G _IC was obtained by incorporating the PA veil, but it changed negligibly by the addition of the PET veil. The analysis of the composites fracture surface via SEM revealed increased fiber bridging between adjacent plies in the case of PA veil interleaved composites which played a key role in enhancing the Mode I interlaminar fracture toughness. However, the PET veil present in the interlaminar region did not take part in any energy absorbing mechanism during the delamination, thus keeping the G _IC of the composite unaltered. POLYM. COMPOS., 38:2501–2508, 2017. © 2015 Society of Plastics Engineers     

Influence of oxygen plasma treatment on interfacial properties of poly(p‐phenylene benzobisoxazole) fiber‐reinforced poly(phthalazinone ether sulfone ketone) composite

The influence of oxygen plasma treatment on both surface properties of poly(p‐phenylene benzobisoxazole) (PBO) fibers and interfacial properties of PBO fiber reinforced poly(phthalazinone ether sulfone ketone) (PPESK) composite were investigated. Surface chemical composition, surface roughness, and surface morphologies of PBO fibers were analyzed by X‐ray photoelectron spectroscopy (XPS), Atomic force microscopy (AFM), and scanning electron microscopy (SEM), respectively. Surface free energy of the fibers was characterized by dynamic contact angle analysis (DCAA). The interlaminar shear strength (ILSS) and water absorption of PBO fiber‐reinforced PPESK composite were measured. Fracture mechanisms of the composite were examined by SEM. The results indicated that oxygen plasma treatment significantly improved the interfacial adhesion of PBO fiber‐reinforced PPESK composite by introducing some polar or oxygen‐containing groups to PBO fiber surfaces and by fiber surface roughening. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Adhesion behavior of different annealed polyphenylquinoxaline foils treated using low pressure plasma

The aim of this study was to investigate the adhesion behavior of polyphenylquinoxaline (PPQ) foils. PPQ foils were initially produced and then annealed in vacuum furnace at different temperatures. The surface of PPQ was activated with GHz‐low pressure plasma (lp‐plasma) using oxidative (O₂) and noble (Ar, Ar/He) gases. An epoxy adhesive was used to glue the PPQ foil with a sheet of steel. The adhesions of foils were examined using 90°‐peel test. Observations from scanning electron microscopy (SEM) and atomic force microscopy (AFM) in addition to the gravimetry measurements were used to interpretate the effects of plasma treatment of adhesion of foils. The results showed that the peeling resistance values were significantly dependent on plasma treatment time and power as well as annealing conditions. In case of PPQ foils where the adhesion was significantly enhanced, it was observed that the fracture changed from adhesion mode at the interface between the adhesive layer and the PPQ foil to cohesive mode, which was seen either in the layer nearby the PPQ surfaces or in the foil itself. Furthermore, furrowed structures were observed at the fracture surface and they were oriented transversely to the peeling direction. SEM and AFM graphs showed that the surface roughness of PPQ foils increased significantly with increasing plasma treatment time and it was more pronounced when using oxidative than noble gas. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 39949.     

Roughness of oxide glass subcritical fracture surfaces

An original setup combining a very stable loading stage, an atomic force microscope and an environmental chamber, allows to obtain very stable subcritical fracture propagation in oxide glasses under controlled environment, and subsequently to finely characterize the nanometric roughness properties of the crack surfaces. The analysis of the surface roughness is conducted both in terms of the classical root mean square roughness to compare with the literature, and in terms of more physically adequate indicators related to the self‐affine nature of the fracture surfaces. Due to the comparable nanometric scale of the surface roughness, the AFM tip size and the instrumental noise, a special care is devoted to the statistical evaluation of the metrologic properties. The roughness amplitude of several oxide glasses was shown to decrease as a function of the stress intensity factor, to be quite insensitive to the relative humidity and to increase with the degree of heterogeneity of the glass. The results are discussed in terms of several modeling arguments concerning the coupling between crack propagation, material's heterogeneity, crack tip plastic deformation and water diffusion at the crack tip. A synthetic new model is presented combining the predictions of a model by Wiederhorn et al (J Non‐Cryst Solids, 353, 1582‐1591, 2007) on the effect of the material's heterogeneity on the crack tip stresses with the self‐affine nature of the fracture surfaces.     

Effect of fiber chemical treatment of nonwoven coconut fiber/epoxy composites adhesion obtained by RTM process

In this work untreated and alkali treated nonwoven coconut fiber mats/epoxy resin composites were manufactured using the resin transfer molding process. The alkaline solution removes some impurities present on fibers superficial layers and the effect regarding fiber/matrix adhesion were investigated by thermogravimetric analysis, dynamic mechanical analysis (DMA), scanning electron microscopy (SEM), ultrasonic C‐scan, and quasi‐static flexural test. Results show a removing of some amorphous fibers constituents, mainly waxes, extractives, and hemicellulose, revealing the fiber roughness surface but no initial degradation temperature changing. Regarding the composites, a similar interfacial adhesion was observed in both one through the results of SEM, DMA and quasi‐static flexural tests. The conclusion is that chemical treatment conditions applied on the fiber surface was been suitable to improve fiber roughness but did not the adhesion between coconut fibers mat and epoxy resin. POLYM. COMPOS., 38:2518–2527, 2017. © 2015 Society of Plastics Engineers     

Non‐food application of camelina meal: Development of sustainable and green biodegradable paper‐camelina composite sheets and fibers

Recycled newspaper‐reinforced sustainable and biodegradable composite sheets and fibers were fabricated with camelina meal, a by‐product of camelina oil extraction‐based resin. To prepare uniform composite sheets and fibers, the camelina meal was ground and sieved to remove large particles and some impurities and converted into resin by dissolving it in water and precuring at 75°C water bath. Sieving process improved protein contents by 4.7% and reduced fat contents by 4.2%. Recycled newspaper was used as a reinforcing agent to improve tensile properties and increase water resistance of the camelina meal‐based biodegradable composite sheets and fibers. Increasing newspaper content increased fracture stress, Young's modulus, and water resistance property. However, the uniform sheet could not be formed when recycled newspaper content was above 30% (wt/wt camelina). Scanning electron microscope photomicrographs of fracture surfaces showed that at higher newspaper content longer fibers protruded out from the camelina resin. POLYM. COMPOS., 33:1969–1976, 2012. © 2012 Society of Plastics Engineers     

Different surface treatments to improve the adhesion of polypropylene

Injection-molded samples of polypropylene were exposed to oxygen plasma and SACO (SAndblasting and COating) treatments. The pretreated surfaces were successively adhesively bonded or lacquered. The adhesion strength and failure mode of these specimens were examined. The surfaces obtained after treatments were characterized by electron spectroscopy for chemical analysis (ESCA), contact angle measurements, and scanning electron microscopy (SEM). Both microroughness and chemical modification of the surface led to an increase in adhesion by up to a factor of 10. The stability of the surface changes generated during the plasma and SACO pretreatments was observed by different kinds of aging experiments in air and water. The aging of SACO-treated surfaces led to no significant change on the surface. In the case of plasma-treated surfaces, hydrophobic recovery during aging in air reduced the polarity of the surface layer. During aging in water, no hydrophobic recovery on the surface was observed.