Mode-I adhesive fracture energy measurement with modified single-lap joint test geometry

The adhesive fracture energy or fracture toughness of adhesively-bonded joints comprising carbon-fiber-reinforced polymer composite substrates and three different types of adhesives was detemined using a modified single-lap joint (MSLJ). This joint was made by implanting end pre-cracks in the adhesive layer at the center of the bondline of a conventional single-lap joint (SLJ). This modification ensured that the crack propagated from a sharp starter crack from both ends of the overlap during testing, reducing the effect of spew fillets on the measured adhesive fracture toughness scatter band. The MSLJ specimens were tested to failure and the adhesive fracture energy was calculated using the Kinloch–Osiyemi model. The values of the adhesive fracture energy obtained from the MSLJ tests were compared with those from SLJ and the double-cantilever beam (DCB) test geometries. The fracture energy values obtained from the MSLJ specimens were significantly lower than those from SLJ specimens and agreed well with those from DCB specimens. The three differenent types of aerospace grade film adhesives tested were Redux 322, Redux 335K and Redux 319A.     

Comparison of laboratory techniques for evaluating the fracture toughness of glassy polymers

Several test methods were employed to determine polymer fracture toughness (??_Ic, the opening-mode strain energy release rate) at room temperature. The materials used included DGEBA epoxies and those modified by the addition of CTBN elastomers. Double-cantilever beam specimens were used to determine the fracture toughness both of bulk resins and of an adhesive layer bonded between two aluminum half-beams. The adhesive fracture toughness of a 0.025-cm bond was slightly less than the bulk ??_Ic value, attributed to the bond thickness effect. Fracture toughness of bulk resins was also evaluated by using both rectangular and round compact tension specimens. The results, when compared with those obtained with the bulk double-cantilever beams, are quite acceptable. The thickness of compact tension specimens, ranging from 0.64 to 1.0 cm, might not give pure plane-strain conditions, and thus some plane-stress contribution to ??_Ic should be expected for the tougher materials. Izod impact tests were also carried out to determine sample fracture toughness at high loading rate.     

Effect of bond thickness on creep lifetime of adhesive joints under mode I

An experimental investigation has been carried out on double cantilever beam specimens with different bond thicknesses to study the effect of bond thickness on lifetime of adhesive joints under mode I. This paper describes an approach to predict the rate of crack propagation. The approach is based on principles of linear elastic fracture mechanics and uses elevated temperature to accelerate the crack propagation under constant loads. The fracture energy of the joint is studied as a function of bond thickness. The results from short-term tests are analyzed and a simple model has been proposed to predict the variation of two kinetic parameters of the Paris law with bond thickness.     

Fracture behavior of carbon/epoxy laminated composite reinforced by iron powder

The fracture behaviors of a newly developed iron-powder reinforced carbon/epoxy laminated composite are investigated in this paper. Three kinds of DCB (double cantilever beam) specimens (without iron powder, with iron powder and with iron powder in a magnetic field) were prepared by the ASTM D 5528-94a. For the third DCB specimen, the unidirectional laminas were stacked with iron powder spread evenly on each lamina’s surface. This process was performed in a magnetic field to keep the iron powder standing along the out-plane direction. From the test data of Instron 5567, the fracture toughness, G _I , was calculated by using the compliance calibration method for each of the three kinds of specimens. The calculated fracture toughness shows that the iron powder effectively disturbs the progress of fiber branching between the laminates and provides a good stitching to the in-plane laminates during the fracture.     

Properties of compression densified wood. Part I: bond performance

Bond performance of hygro-thermally compression densified wood was studied using hygro-thermally treated and control yellow-poplar wood (Liriodendron tulipifera). Opening mode double cantilever beam fracture testing and cyclic boiling were used to evaluate bond performance. Phenol–formaldehyde (PF) film and polymeric diphenylmethane diisocyanate (pMDI) adhesives were used to bond specimens for fracture testing. Fracture toughness of hygro-thermal samples bonded with PF film was significantly higher than control samples, while no difference was found for densified samples. Fracture toughness of densified samples bonded with pMDI was significantly higher than control samples, however no change was seen for hygro-thermal samples. Cyclic boiling reduced the fracture toughness of hygro-thermal fracture samples only, irrespective of adhesive type.     

The Use of a Modified Mixed Mode Bending Test for Characterization of Mixed-mode Fracture Behavior of Adhesively Bonded Metal Joints

This paper summarizes recent mixed-mode I and II fracture experiments on adhesively bonded metal joints using a modified mixed-mode bending (MMB) test fixture and double cantilever beam (DCB)-type specimens. The MMB test had been previously developed and used for mixed-mode I and II delamination testing of composite laminates, but in the present research it is adapted and modified for fracture testing of adhesively bonded joints with metallic adherends. Strain energy release rates were evaluated by the use of improved analytical models. Mixed-mode fracture behavior of AA5754-0 aluminum alloy specimens bonded with a tough one-part epoxy adhesive (Dow Automotive Betamate 4601 ® ) was characterized.     

Porous LSCF/dense 3YSZ interface fracture toughness measured by single cantilever beam wedge test

Sandwich specimens were prepared by firing a thin inter-layer of porous La_0.6Sr_0.4Co_0.2Fe_0.8O₃ (LSCF) to bond a thin tetragonal yttria-stabilised zirconia (3YSZ) beam to a thick 3YSZ substrate. Fracture of the joint was evaluated by introducing a wedge between the two YSZ adherands so that the stored energy in the thin YSZ cantilever beam drives a stable crack in the adhesive bond. It was found that the extent of adhesive fracture increased with firing temperature and decreased with LSCF layer thickness. The adhesive failures were mainly at the interface between the LSCF and the thin YSZ beam and FEM modelling revealed that this is due to asymmetric stresses in the LSCF. The intrinsic adhesive fracture toughness of the LSCF/YSZ interface was estimated to be 11 J m⁻² and was not firing temperature dependent within the temperature range investigated.     

Influence of graphene nanoplatelets (GNPs) on mode I fracture toughness of an epoxy adhesive under thermal fatigue

Abstract

The contribution of graphene nanoplatelets (GNPs) for enhancing the fracture toughness of a commonly used room-cured epoxy, used to bond E-glass/epoxy composite adherends, is evaluated. A comprehensive experimental investigation is conducted to examine the performance and degradation of adhesively bonded joints subject to cyclic thermal loading using the standard double cantilever beam (DCB) specimens. Several groups of DCB specimens were fabricated using the adhesive reinforced with four different GNPs weight-percentages (i.e. 0.0, 0.25, 0.5 and 1%). The specimens are subsequently subjected to various numbers of thermal cycles (to a maximum of 1000 heating/cooling cycles), and then tested, and the resulting mode I fracture toughness values are evaluated and compared. The extent and modes of damage captured through microscopy and scanning electron microscopy images are presented and discussed. In addition, a computational framework, using the cohesive zone modeling technique, is developed for predicting the response of the adhesives and their damage evolution.     

Interlaminar fracture toughness of woven fabric composite laminates with carbon nanotube/epoxy interleaf films

The Mode I interlaminar fracture behavior of woven carbon fiber/epoxy composite laminates incorporating partially cured carbon nanotube/epoxy composite films has been investigated. Laminates with films containing carbon nanotubes (CNTs) in the as‐received state and functionalized with polyamidoamine were evaluated, as well as laminates with neat epoxy films. Double‐cantilever beam (DCB) specimens were used to measure G_Ic, the critical strain energy release rate (fracture toughness) versus crack length. Post‐fracture microscopic inspection of the fracture surfaces was performed. Results show that initial fracture toughness was improved with the amino‐functionalized CNT/epoxy interleaf films, but the important factor appears to be the polyamidoamine functionalization, not the CNTs. The initial fracture toughness remained relatively unaffected with the incorporation of neat epoxy and as‐received CNT/epoxy interleaf films. Plateau fracture toughness was unchanged with the use of functionalized CNT/epoxy interleaf films, and was reduced with the use of neat epoxy and as‐received CNT/epoxy interleaf films. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Mode-I adhesive fracture energy of carbon fibre composite joints with nanoreinforced epoxy adhesives

The effect of the addition of carbon nanoreinforcements to an epoxy adhesive on the strength and toughness of carbon fibre/epoxy composite joints was studied. The laminate surfaces, treated with peel ply, were characterised by profilometry, image analysis and wettability. The mechanical properties of the joints were determined by lap shear testing and double cantilever beam testing. The fracture mechanisms were studied by scanning electron microscopy.The addition of carbon nanofibres and carbon nanotubes caused an increase in the mode-I adhesive fracture energy, G_IC, of the joints while their lap shear strengths remained approximately constant. This improvement in the fracture behaviour was attributed to the occurrence of toughening mechanisms when carbon nanoreinforcements were added to the epoxy adhesive. Additionally, the use of carbon nanotubes improved the interfacial strength between the adhesive and the substrate, changing the crack growth behaviour and the macroscopic failure mode.     

Effect of Adherend Thickness and Mixed Mode Loading on Debond Growth in Adhesively Bonded Composite Joints

Symmetric and unsymmetric double cantilever beam (DCB) specimens were tested and analyzed to assess the effect of (1) adherend thickness and (2) a predominantly mode I mixed mode loading on cyclic debond growth and static fracture toughness. The specimens were made of unidirectional composite (T300/5208) adherends bonded together with EC3445 structural adhesive. The thickness was 8, 16 or 24 plies. The experimental results indicated that the static fracture toughness increases and the cyclic debond growth rate decreases with increasing adherend thickness. This behavior was related to the length of the plastic zone ahead of the debond tip. For the symmetric DCB specimens, it was further found that displacement control tests resulted in higher debond growth rates than did load control tests. While the symmetric DCB tests always resulted in cohesive failures in the bondline, the unsymmetric DCB tests resulted in the debond growing into the thinner adherend and the damage progressing as delamination in that adherend. This behavior resulted in much lower fracture toughness and damage growth rates than found in the symmetric DCB tests.     

Novel surface and interfacial analysis techniques as aids to the development of new, high fracture toughness film adhesives

An experimental film adhesive of high fracture toughness had given a promising range of adhesive properties on pickled 2024-T3 clad aluminum alloy, but a wide variation in peel performance resulted when this adhesive was used to bond anodized aluminum adherends. High resolution scanning electron microscopy/ energy dispersive X-ray analysis of the fracture interfaces coupled with transmission electron microscopy of ultramicrotomed sections through the same specimens has shown that the problem was non-wetting of the substrate on a microscopic scale. The rheological properties of the adhesive system have been altered to overcome the problem, yielding a high fracture toughness film adhesive of consistent performance.     

A detailed experimental study of the effects of pre-bond contamination with a hydraulic fluid,thermal degradation,and poor curing on fracture toughness of composite-bonded joints

Adhesive bonding is applied by the aircraft industry both for assembling composite structural parts and implementing composite patch repairs in damaged structural parts. In both applications, there exist several scenarios, related to surface contamination and processing, that could affect bonding quality and thus, degrade bond strength. In this paper, the detailed effects of pre-bond contamination with a hydraulic fluid, thermal degradation of the composite substrate, as well as poor curing (lower curing temperature) on strength of composite-bonded joints were studied experimentally by conducting mode I fracture toughness tests on double-cantilever beam specimens. These three application scenarios are possible to appear in the implementation of a composite patch repair in a damaged composite structural part. The experimental results showed a contradictory effect as the presence of the hydraulic fluid and poor curing degrades the fracture toughness whereas thermal degradation enhances fracture toughness of the composite-bonded joints. These findings are explained by means of extended non-destructive inspection, surface analysis, and evaluation of fracture surfaces.     

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.     

Effect of Pressure Cycling on Fracture Energy of Polyurethane/Aluminum Adhesive Bonds

An experimental study was conducted to investigate the effect of pressure-cycling on adhesive bond fracture energy of polyurethane/aluminum adhesive bond joints. Initially, two types of peel tests were conducted to characterize adhesive bond strength and challenges associated with pre-mature polyurethane cracking and failure during these tests are discussed. A modified double cantilever beam (MDCB) specimen configuration was specially designed and opening-mode loading conditions were employed to determine the interfacial adhesive bond energy (G_C). The test specimens were pressure-cycled in water-filled tanks for 1 to 4 weeks with an increment of 1 week. The G_C of pressure-cycled specimens was compared with both control and water-soaked samples (without pressure-cycling). The results indicated that pressure-cycling decreased G_C values to those of the control and water-soaked samples: hence, prolonged pressure-cycling could be problematic to polymer/metal adhesive bonds of hardware installed outboard of submarine pressure hulls.     

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.     

Moisture and temperature degradation of double cantilever beam adhesive joints

In this work, the double cantilever beam (DCB) test is analysed in order to evaluate the combined effect of temperature and moisture on the mode I fracture toughness of adhesives used in the automotive industry. Very few studies focus on the combined effect of temperature and moisture on the mechanical behaviour of adhesive joints. To the authors’ knowledge, the simultaneous effect of these conditions on the fracture toughness of adhesive joints has never been determined. Specimens using two different adhesives for the automotive industry were subjected to two different ageing environments (immersion in distilled water and under 75% of relative humidity). Once they were fully degraded, they were tested at three different temperatures (?40, 23 and 80 °C), which covers the range of temperature an adhesive for the automotive industry is required to withstand. The aim is to improve the long term mechanical behaviour prediction of adhesive joints. The DCB substrates were made of a high strength aluminium alloy to avoid plastic deformation during test. The substrates received a phosphoric acid anodisation to improve their long term adhesion to the adhesive. Results show that even though a phosphoric acid anodization was applied to the adherends, when the aged specimens were tested at room temperature and at 80 °C, they suffered interfacial rupture. At ?40 °C, however, cohesive rupture was observed and the fracture toughness of the aged specimens was higher.     

Evolution of crack path and fracture surface with degradation in rubber-toughened epoxy adhesive joints: Application to open-faced specimens

The crack path and fracture surface in the mixed-mode fracture of two different rubber-toughened epoxy adhesives were evaluated using double-layered open-faced double cantilever beam (ODCB) specimens in which the primary adhesive layer had been environmentally aged. The crack path in the mixed-mode fracture of unaged ODCB specimens was unexpectedly in the secondary adhesive layer, and several hypotheses were examined to explain this. It was concluded that a reduced residual stress in the secondary adhesive layer produced stable crack growth in the secondary layer instead of the expected path in the primary layer. The average crack path depth, fracture surface roughness and maximum elevation in the fracture surface profiles were then measured using optical profilometry as a function of the degree of aging. The results showed a strong relationship between all these parameters and the critical strain energy release rate, G_cs, irrespective of the type of adhesive. In the case of adhesive A where significant irreversible degradation was observed, all these parameters varied approximately linearly with G_cs. In the case of adhesive B, aging did not result in permanent degradation (G_cs was unchanged) and so all these fracture surface parameters also remained unchanged after aging. The results indicate that quantifying fracture surface parameters as a post-failure analysis can be of use in the estimation of the fracture toughness at which a practical joint fails.     

A method for testing the interface toughness of ceramic environmental barrier coatings (EBCs) on ceramic matrix composites (CMCs)

A simple interface fracture test for ceramic environmental barrier coatings (EBCs) on ceramic matrix composites (CMCs) was developed. A variation on the asymmetric double cantilever beam (ADCB) test was proposed so that the interface toughness could be measured in a small specimen of simple shape without applying interlaminar loading to the CMC substrate. The proposed test was applied to an EBC consisting of a mullite layer and Si bond coat on a monolithic SiC substrate. A pre-crack was introduced by pop-in cracking, and then a notch overlapping the pre-crack was machined. The pre-crack was opened by inserting a wedge into the notch. From the critical notch opening displacement the crack starts to propagate, interface toughness is calculated. The measured interface toughness was 4.1?J/m2. Finally, the application range of the test was discussed and suggestions were made for introduction of the notch and pre-crack.     

High-Temperature Transverse Fracture Toughness of Nicalon-Fiber-Reinforced CAS-II Glass-Ceramic Matrix Composite

Cracking parallel to the fibers in off-axis plies is usually the initial form of damage in composite laminates. This cracking process has been associated with the (transverse) fracture toughness, defined by the critical strain energy release rate, G _Ic. The measurement of G _Ic provides basic information about the transverse crack resistance. In this study, the utility of the double torsion (DT) test technique to determine _G Ic in a glass-ceramic matrix composite (Nicalon/CAS-II) at temperatures up to 1000°C has been demonstrated. _G Ic did decrease moderately with increasing temperature (as does the bulk matrix); however, no evidence of an interphase oxidizing effect on crack growth (parallel to the fibers) could be found. The inevitable misalignment of fibers in the material was not very efficient at bridging the crack in the DT specimens, in contrast to the significant matrix crack interactions with the fibers reported for other geometries such as double cantilever beam and flexure specimens.