The Durability of Adhesively-bonded Ti-6Al-4V

The durability of chromic acid-anodized Ti-6Al-4V alloy, adhesively-bonded with FM-5 supported polyimide adhesive has been studied. The performance tests compared titanium samples that had been thermally treated and bonded, and samples that were bonded and thermally treated. Following the thermal treatment, the durability was examined (1) by immersing wedge-type specimens in boiling water and measuring the crack growth and (2) by measuring the lap shear strength for single lap specimens. In the wedge tests, failure occurs within the adhesive for specimens treated at temperatures below 371°C for less than one hour. For treatments at higher temperatures and for longer periods of time, failure occurs within the anodic oxide. From the lap shear tests, the principal finding is that the lap strength decreases with increasing treatment time at constant temperature and with increasing temperature at a fixed time. For the lap specimens, failure occurs to a greater extent within the oxide as the treatment time and temperature increase. Surface analysis results indicate the formation of an aluminum fluoride species. It is reasoned that the formation of fluorine-containing materials weakens the oxide and promotes failure within the anodic oxide.     

The effect of curing temperature on thermal,physical and mechanical characteristics of two types of adhesives for aerospace structures

The effects of cure temperatures on the thermal, physical and mechanical characteristics of two types of thermosetting structural epoxy film adhesives were determined in detail. The aim of this paper is to assess the effect of cure temperatures (82–121 °C) on the degree of cure of the two adhesives and the relevant void formations that need to be addressed in bonded part production and repair. Two thermal parameters were used to characterize the advancement of the reaction, such as degree of cure and glass transition temperature. The joint properties with respect to the cure temperatures were characterized by void content and bond-line thickness measurements and lap shear strength tests. Experimental results presented that all lap shear strengths were well within minimum shear strength (29 MPa) required by the specification of the film-type adhesive. However, the lap shear strength testing after aging at 82 °C and 95%R.H for 1000 h showed that the improved durability when the adhesive is cured at 121 °C did not occur for the 82 °C cure. Low curing conversion (75–77% degree of cure) combined with high voids (over 2 areal%) has a catastrophic effect on the bonding qualities at the metal-adhesive interface and due to lack of cohesion in the adhesive. The changes in the interface caused by the low temperature curing may contribute to an increased susceptibility of the bonded joint to moisture and consequent bond-line degradation.     

Adhesive bonding of aluminium with structural acrylic adhesives: durability in wet environments

The durability of EN AW 6082-T651 aluminium alloy joints bonded with a toughened acrylic adhesive was investigated upon exposure to wet environments (humidity, water immersion and salt water immersion). Environmentally-friendly surface treatments were used to avoid hexavalent chromium. Single lap shear tests were used to determine the durability of the adhesively bonded joints. Specimens were exposed to 31% and 95% relative humidity and submerged in deionized water and 3 wt% sodium chloride solution at 25°C and 50°C, for 10, 30 and 90 days. The data collected in the experiments showed that the durability was higher for surfaces treated with γ-methacryloxypropyltrimethoxysilane (γ-MPS) and sulfo-ferric etchant (P2 etch) than other surface treatments. Both these treatments improved considerably the durability in all environments tested. The results indicate that specimens even without surface treatment maintained a significant residual strength after exposure to low humidity environment (room temperature at 31% RH). The joints exposed to a high humidity environment showed a higher reduction in adhesive strength than those immersed in deionized water and saline solution.     

Comparison of fracture behavior between acrylic and epoxy adhesives

An experimental study was conducted on the strength of adhesively bonded steel joints, prepared epoxy and acrylic adhesives. At first, to obtain strength characteristics of these adhesives under uniform stress distributions in the adhesive layer, tensile tests for butt, scarf and torsional test for butt joints with thin-wall tube were conducted. Based on the above strength data, the fracture envelope in the normal stress-shear stress plane for the acrylic adhesive was compared with that for the epoxy adhesive. Furthermore, for the epoxy and acrylic adhesives, the effect of stress triaxiality parameter on the failure stress was also investigated. From those comparison, it was found that the effect of stress tri-axiality in the adhesive layer on the joint strength with the epoxy adhesive differed from that with the acrylic adhesive. Fracture toughness tests were then conducted under mode l loading using double cantilever beam (DCB) specimens with the epoxy and acrylic adhesives. The results of the fracture toughness tests revealed continuous crack propagation for the acrylic adhesive, whereas stick-slip type propagation for the epoxy one. Finally, lap shear tests were conducted using lap joints bonded by the epoxy and acrylic adhesives with several lap lengths. The results of the lap shear tests indicated that the shear strength with the epoxy adhesive rapidly decreases with increasing lap length, whereas the shear strength with the acrylic adhesive decreases gently with increasing the lap length.     

Hygrothermal Properties of Adhesively Bonded Joints and Their Correlation with Bulk Adhesive Properties

The combined effects of heat (50[ddot]C) and humidity (95% R.H.) on the lap shear and T-peel strengths of 120[ddot]C, 150[ddot]C and 215[ddot]C service epoxy film adhesives have been characterized. Experimental results have indicated that effects of hygrothermal conditioning on lap shear and peel properties vary with exposure time and final testing temperatures and type of adhesive tested. In the cases where cohesive failure was observed in the shear and peel specimens, a correlation could be established between the bulk properties of the adhesives (tensile strength and elongation) and their adhesively bonded joint properties (shear and peel). When testing was carried out at room temperature, a general correlation between the tensile elongation and T-peel or shear could be obtained. At below freezing temperatures, lap shear strength seemed to be correlated with bulk tensile strength while peel correlated with bulk tensile elongation. At elevated temperatures, the relative contributions of bulk strength and elongation were the decisive factors as far as shear and peel strengths are concerned.     

Microscale groove effect on shear strength of epoxy-bonded dissimilar metal plate

In this study, the shear strengths of Al 7075–HSS adhesive bonded, grooved and smooth plates were investigated. The proven toughness and durability of adhesives have drawn the attention of researchers who want to take advantage of the technology to benefit the development of ballistic resistance sandwich panels. However, the strength of the panel depends on the design of surface topography. Therefore, it is essential to understand the fracture upon loading parallel to the plane of the adhesive bonded metal plates. In this experiment, toughened epoxy was used to bond dissimilar metal plates at 1 mm thickness. The shear tests were performed with a universal-testing machine to identify the maximum fracture loads. The results showed that a shear lap joint specimen with a grooved surface yields a higher strength than a smooth specimen. From the fracture behaviour of all specimens, interfacial failure with some degree of cohesive failure was observed. This indicates that the strength of the adhesive-bonded metal plate driven by a mechanical interlocking effect and mode of failure for thick bondline was the result of interfacial strength rather than adhesive bulk strength. Shear value results and fractography for 1 mm bond thickness provide insights towards steel fibre application in epoxy.     

Characterization of Surface Pretreatments on Al/Li Alloy and Related Mechanical Properties of Polysulfone Adhesive Bonds

An investigation of polysulfone-Al/Li alloy interaction involved single lap shear joints and wedge samples following an FPL etch, sulfuric acid anodization (SAA) and phosphoric acid anodization (PAA). The study of the Al/Li surfaces involved the determination of the elemental composition and morphological features of the pretreated adherend before bonding and following fracture. When polysulfone was either thermally pressed or primed onto the microporous surface, the polysulfone indeed penetrated into the porous oxide and thereby provided a mechanical means of adhesion. The wedge test results for the adherend pretreated by PAA and SAA were superior to those for the FPL etched adherend. The failure path for the FPL etched samples was at the adhesive/oxide interface whereas the failure path for the PAA samples was within the adhesive but with occasional divergence of the crack into the oxide. The porous oxides on Al/Li alloy formed after PAA and SAA treatment were shown to undergo dramatic changes in morphology on short term (< 95 hrs) exposure to 71°C and 100% R.H. environment. The mechanism of failure was due to moisture which caused hydration and subsequent weakening of the surface oxide layer and the bonded joint. Lithium was not surface concentrated in the PAA treated Al/Li alloy as shown by AES depth profiling and therefore the effect of Li on the durability of the bonded alloy is considered minimal.     

Process optimization of solvent based polybenzimidazole adhesive for aerospace applications

The use of adhesive bonding for high temperature applications is becoming more challenging because of low thermal and mechanical properties of commercially available adhesives. However, the development of high performance polymers can overcome the problem of using adhesive bonding at high temperature. Polybenzimidazole (PBI) is one such recently emerged high performance polymer with excellent thermal and mechanical properties. It has a tensile strength of 160 MPa and a glass transition of 425 °C. Currently, PBI is available in solution form with only 26% concentration in Dimethyl-acetamide solvent. Due to high solvent contents, the process optimization required lot of efforts to form PBI adhesive bonded joints with considerable lap shear strength. Therefore, in present work, efforts are devoted to optimize the adhesive bonding process of PBI in order to make its application possible as an adhesive for high temperature applications. Bonding process was optimized using different curing time and temperatures. Epoxy based carbon fiber composite bonded joints were successfully formed with single lap shear strength of 21 Mpa. PBI adhesive bonded joints were also formed after performing the atmospheric pressure plasma treatment of composite substrate. Plasma treatment has further improved the lap shear strength of bonded joints from 21 MPa to 30 MPa. Atmospheric pressure plasma treatment has also changed the mode of failure of composite bonded joints.     

Strength and Durability of Epoxy-Aluminum Joints

The adhesive strength and durability of adhesively-bonded aluminum joints in wet environments was analyzed. A2024-T4 alloy was subjected to two different surface treatments based on etching with chromic-sulfuric acid (FPL) and with sulfuric acid-ferric sulfate (P2). Small differences were observed in the lap shear strength as a function of the applied surface treatment. However, durability in humid environments was higher for the joints whose adherends were treated with P2.

Although the amount of water absorbed by the epoxy adhesive is lower in saline environments, the effects on the glass transition temperature of the epoxy adhesive and on the lap shear strength of the joints are more marked than the effects caused by aging with distilled water.

Finally, a new epoxy adhesive with a siloxanic hardener was tested, obtaining good mechanical properties, high glass transition temperature, moderate values of lap shear strength, and high durability in wet environments.     

An Investigation of the Effect of Plasma Treatment on the Surface Properties and Adhesion in Sheet Molded Composite (SMC) Material

Sheet molded composite was treated with different plasmas (oxygen, dry air, nitrogen, and argon). Plasma treatment of SMC alters the surface properties in a manner dependent on the type of plasma used and the time of treatment. The surface properties were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Fourier transform infrared spectros-copy (FTIR). A two-part urethane adhesive was used to prepare lap shear specimens. Untreated SMC, plasma-treated SMC, and primer-treated SMC were prepared, bonded and tested. The surface properties of the failed specimens were measured. The adhesion characteristics of SMC and the surface properties of the failed specimens were correlated with the type of treatment and the surface properties of treated SMC. Comparison of the surface and adhesive properties of plasma-treated samples with those for untreated samples indicates a) an increase in roughness, b) an increase in the level of SMC surface oxidation, and c) an increase in the failure force for lap shear tests.     

Water-Resistant Oxide Layers at the Interface of Zinc/Epoxy Bonded Joints

The durability properties of bonded lap shear joints made from an epoxy/dicyandiamide adhesive and zinc metal coupons have been investigated. The metal coupons were anodized in sodium hydroxide solutions before bonding. The influence of the anodizing conditions on the morphology and composition of the oxide layers has been studied using SEM and TEM imaging analyses as well as X-ray photoelectron spectroscopy. The hydrolytic stability of the bonded joints has been assessed by storing the joints in water at 70 °C or 90 °C for periods of time up to 5 weeks. Polypropylene has been used as a model adhesive to study the influence of mechanical interlocking effects on the performance of the bonded joints. Depending on the anodizing conditions, the improved durability properties have been attributed either to „mechanical interlocking effects“ or to the higher hydrolytic stability of the oxide layers generated during the anodizing treatment.

Some of the results gained from the anodization of zinc have been extrapolated to hot-dipped galvanized steel. Bonded joints made from hot-dipped galvanized coupons anodized under smooth conditions (2% NaOH) displayed residual shear strengths of up to 70% higher than specimens simply degreased after immersion test. The generation of stable oxide layers as well as the suppression of intergranular corrosion phenomena at the metal/adhesive interface can explain the improved durability properties.     

An Investigation of the Effect of Plasma Treatment on the Surface Properties and Adhesion in Sheet Molded Composite (SMC) Material

Sheet molded composite was treated with different plasmas (oxygen, dry air, nitrogen, and argon). Plasma treatment of SMC alters the surface properties in a manner dependent on the type of plasma used and the time of treatment. The surface properties were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Fourier transform infrared spectros-copy (FTIR). A two-part urethane adhesive was used to prepare lap shear specimens. Untreated SMC, plasma-treated SMC, and primer-treated SMC were prepared, bonded and tested. The surface properties of the failed specimens were measured. The adhesion characteristics of SMC and the surface properties of the failed specimens were correlated with the type of treatment and the surface properties of treated SMC. Comparison of the surface and adhesive properties of plasma-treated samples with those for untreated samples indicates a) an increase in roughness, b) an increase in the level of SMC surface oxidation, and c) an increase in the failure force for lap shear tests.     

Polyimide–silica hybrids containing novel phenylethynyl imide silanes as coupling agents for surface-treated titanium alloy

Polyimide–silica hybrids composed of an organic precursor containing a novel phenylethynyl imide silane and an inorganic precursor were evaluated as an adhesion-promoting interphase between surface-treated titanium alloy and a phenylethynyl-containing imide adhesive. The phenylethynyl groups present in the organic precursor, either as a pendent or end group, can bond chemically with a phenylethynyl-containing imide adhesive during processing, while the silane groups of the organic precursor would react chemically with the inorganic precursor. In addition, the inorganic precursor is able to react with the titanium alloy to form a stable bond with the metal oxide. Bond strength and durability were evaluated by single lap shear tests at various conditions. Lap shear specimens exhibited predominantly cohesive failure after a 3-d water boil with 92% retention of the initial room temperature strength. Morphology and chemical composition of the hybrid interphase were investigated with scanning electron microscopy, X-ray photoelectron spectroscopy, and Auger electron spectroscopy, which revealed development of a silicon-gradient, hybrid structure between the metal substrate and the adhesive.     

Static and fatigue behavior of adhesive joints in SMC-SMC composites

This paper discusses the static and fatigue behavior of adhesively bonded single lap joints in SMC-SMC composites. Effects of lap length and adhesive thickness on the static and fatigue strength of SMC-SMC adhesive joints are studied. Effects of SMC surface preparation and test speed on the joint performance are evaluated. Finally, the effect of water exposure on the joint durability is also investigated. Results show that the static behavior of adhesive joints in SMC-SMC composites is significantly influenced by the lap length and adhesive thickness. With an increase in lap length from 12.7 mm to 38.1 mm, the joint failure load increases by 37%. The joint failure load also increases with the adhesive thickness, but it reaches a maximum at an adhesive thickness of 0.33 mm and then decreases. However, lap length and adhesive thickness have negligible effect on the ratio of fatigue strength to static strength. The fatigue strength at 10⁶ cycles is approximately 50% to 54% of the static strength for various adhesive thicknesses and lap lengths investigated in this study. Adhesive failure, fiber tear or combination of these two failure modes are observed during both static and fatigue tests.     

Experimental Analysis of the Bondline Stress Concentrations to Characterize the Influence of Adhesive Ductility on the Composite Single Lap Joint Strength

Adhesively bonded composite single lap joints were experimentally investigated to analyze the bondline stress concentrations and characterize the influence of adhesive ductility on the joint strength. Two epoxy paste adhesives—one with high tensile strength and low ductility, and the other with relatively low tensile strength and high ductility—were used to manufacture composite single lap joints. Quasi-static tensile tests were conducted on the single lap joints to failure at room temperature. High magnification two-dimensional digital image correlation was used to analyze strain distributions near the adhesive fillet regions. The failure mechanisms were examined using scanning electron microscopy to understand the effect of adhesive ductility on the joint strength. For a given surface treatment and laminate type, the results show that adhesive ductility significantly increases the joint strength by positively influencing stress distribution and failure mechanism near the overlap edges. Moreover, it is shown that high magnification two-dimensional digital image correlation can successfully be used to study the damage initiation phase in composite bonded joints.     

Atmospheric plasma modification of polyimide sheet for joining to titanium with high temperature adhesive

This investigation highlights the rationale of adhesive bonding of atmospheric pressure plasma treated high temperature resistant polymeric sheet such as polyimide sheet (Meldin 7001), with titanium sheets. The surface of polyimide (PI) sheet was treated with atmospheric pressure plasma for different exposure times. The surface energy was found to increase with increase in exposure time. However, longer exposure time of plasma, results in deterioration of the surface layer of PI resulting in degradation and embrittlement.Contact angle measurements with sessile drop technique were carried out for estimation of surface energy. SEM (EDS) and AFM analyses of treated and untreated specimens were carried out to examine the surface characteristics and understanding morphological changes following surface treatment. Untreated samples and atmospheric pressure plasma treated samples of polyimide Meldin 7001 sheet were bonded together as well as with titanium substrates to form overlap joints. Single lap shear tensile testing of these adhesively bonded joints was performed to measure bond strength and to investigate the effect of surface treatment on adhesive bond strength. An optimized plasma treatment time results in maximum adhesive bond strength and consequently, this technology is highly acceptable for aviation and space applications.     

Evaluation of a thermoplastic polyimide (422) for bonding GR/PI composite

A hot-melt processable copolyimide designated 422 previously synthesized and characterized as an adhesive at NASA Langley Research Center for bonding Ti-6A1-4V has been used to bond Celion 6000/LARC-160 composite. Comparisons are made for the two adherend systems. A bonding cycle was determined for the composite bonding and lap shear specimens were prepared which were thermally exposed in a forced-air oven for up to 5000 h at 204°C. Lap shear strengths (LSSs) were determined at room temperature, 177°C, and 204°C. After thermal exposure to 5000 h at 204°C, room temperature and 177°C LSSs decreased significantly; however, a slight increase was noted for the 204°C test. Initially the LSS values were higher for the bonded Ti-6AI-4V than for the bonded composite; however, the LSS decreased dramatically between 5000 and 10 000 h of 204°C thermal exposure. Longer periods of thermal exposure up to 20 000 h resulted in further decreases in LSSs. Although the bonded composite retained useful strengths ( > 11.1 MPa) for exposures up to 5000 h, based on the poor results of the bonded Ti-6A1-4V beyond 5000 h, the 422 adhesive bonded composites would most likely also produce poor strengths beyond 5000 h exposure. Adhesive bonded composite lap shear specimens exposed to boiling water for 72 h exhibited greatly reduced strengths at all test temperatures. The percent retained after water boil for each test temperature was essentially the same for both systems.     

Effect of temperature on the shear strength of aluminium single lap bonded joints for high temperature applications

An experimental and numerical investigation into the shear strength behaviour of adhesive single lap joints (SLJs) was carried out in order to understand the effect of temperature on the joint strength. The adherend material used for the experimental tests was an aluminium alloy in the form of thin sheets, and the adhesive used was a high-strength high temperature epoxy. Tensile tests as a function of temperature were performed and numerical predictions based on the use of a bilinear cohesive damage model were obtained. It is shown that at temperatures below T_g, the lap shear strength of SLJs increased, while at temperatures above T_g, a drastic drop in the lap shear strength was observed. Comparison between the experimental and numerical maximum loads representing the strength of the joints shows a reasonably good agreement.     

Effect of the temperature on the strength of adhesively bonded single lap and T joints for the automotive industry

Adhesively bonded lap and T joints are used extensively in the manufacture of automotive structures. In order to determine the effect of using a structural adhesive instead of spot-welding, a detailed series of tests, supported by finite element analyses, was conducted using a range of loadings. The adhesive was a toughened epoxy and the adherend was a grade of mild steel typical of that used in the manufacture of car bodyshells. The lap joints were tested in tension (which creates shear across the bondline) and three point bending. Previous studies at room temperature have shown that joint failure is dictated by adherend yielding and adhesive strain to failure. In the present study, to asses the effect of temperature that an automotive joint might experience in service, tests were carried out at ?40 and +90 °C. It is shown that the failure criterion proposed at room temperature is still valid at low and high temperatures, the failure envelope moving up and down as the temperature increases or decreases, respectively.     

Tensile Strength of Joints Bonded With a Nano-particle-Reinforced Adhesive

In order to improve the tensile lap shear strength of adhesively bonded joints, nano-particles were dispersed in the adhesive using a 3-roll mill. The dispersion states of nano-particles in the epoxy adhesive were observed with TEM (Transmission Electron Microscopy) with respect to the mixing conditions, and the effect of nano-particles on the mechanical properties of the adhesive was measured with respect to dispersion state and weight content of nano-particles. Also the static tensile load capability of the adhesively bonded double lap joints composed of uni-directional glass/epoxy composite and nano-particle-reinforced epoxy adhesive was investigated to assess the effect of nano-particles on the lap shear strength of the joint. From the experimental and FE analysis results, it was found that the nano-particles in the adhesive improved the mechanical properties of the adhesive. Also the increased failure strain and the reduced CTE (coefficient of thermal expansion) of the nano-particle-reinforced adhesive improved the lap shear strength of adhesively bonded joints.