Self-healing of delamination fatigue cracks in carbon fibre–epoxy laminate using mendable thermoplastic

This article examines the self-healing repair of delamination damage in mendable carbon fibre–epoxy laminates under static or fatigue interlaminar loading. The healing of delamination cracks in laminates containing particles or fibres of the mendable thermoplastic poly[ethylene-co-(methacrylic acid)] (EMAA) was investigated. The results showed that the formation of large-scale bridging zone of EMAA ligaments along the crack upon healing yielded a large increase (~300%) in the static mode I interlaminar fracture toughness, exceeding the requirement of full restoration. The mendable laminates retained high healing efficiency with multiple repair cycles because of the capability of EMAA to reform the bridging zone under static delamination crack growth conditions. Under fatigue loading, healing by the EMAA was found to restore the mode I fatigue crack growth resistance, with the rates of growth being slightly less than that pertinent to the unmodified laminate. The EMAA bridging zone, which generated high toughness under static loading conditions, does not develop under fatigue loading because of rapid fatigue failure of the crack bridging ligaments. Similar to the multiple healing capability of EMAA under static loading, multiple healing of delamination fatigue cracks is confirmed, with the fatigue crack growth rates remaining approximately unchanged. This study shows that EMAA was capable of full recovery of fatigue crack growth resistance and superior healing efficiency for static loading.     

Toughening and self-healing of epoxy matrix laminates using mendable polymer stitching

This paper presents an experimental study into a new type of stitched fibre–polymer laminate that combines high interlaminar toughness with self-healing repair of delamination damage. Poly(ethylene-co-methacrylic acid) (EMAA) filaments were stitched into carbon fibre/epoxy laminate to create a three-dimensional self-healing fibre system that also provides high fracture toughness. Double cantilever beam testing revealed that the stitched EMAA fibres increased the mode I interlaminar fracture toughness (by ∼120%) of the laminate, and this reduced the amount of delamination damage that must subsequently be repaired by the self-healing stitches. The 3D stitched network was effective in delivering self-healing EMAA material extracted from the stitches into the damaged region, and this resulted in high recovery in the delamination fracture toughness (∼150% compared to the original material). The new self-healing stitching method provides high toughness which resists delamination growth while also having the functionality to repeatedly repair multiple layers of damage in epoxy matrix laminates.     

Self-healing property of epoxy/nanoclay nanocomposite using poly(ethylene-co-methacrylic acid) agent

This paper investigates the self-healing repair of cracks in an epoxy/nanoclay nanocomposite using mendable poly[ethylene-co-methacrylic acid] (EMAA) particles. The effects of two different concentrations of EMAA agent on the self-healing efficiency were measured using single edge notch bar (SENB) testing. Inclusion of EMAA particles into the nanocomposite results an increase in the fracture strength and strain of the SENB specimens. Damaged SENBs were healed at 150 °C for 30 min to achieve up to 63% recovery in critical stress intensity and over 85% recovery in sustainable peak load. Also, X-ray diffraction (XRD) analysis and tensile test used in order to examine the nanocomposite structure and investigate the effects of EMAA inclusion on the nanocomposite mechanical properties. The pressure delivery mechanism of the healing agent is shown by scanning electron microscopy (SEM) images. It seems EMAA can be used as an effective self-healing agent for epoxy/nanoclay nanocomposites.     

Interlayer self-healing and toughening of carbon fibre/epoxy composites using copolymer films

This paper presents an investigation of the combined self-healing and toughening performance of two copolymers: thermoplastic poly(ethylene-co-methyl acrylate) (EMA) and poly(ethylene-co-methacrylic acid) (EMAA). Carbon fibre composites were manufactured from unidirectional prepregs with rectangular-shaped patches being placed between composite plies. Results from double-cantilever-beam and short-beam-shear testing show that the incorporation of mendable polymers improves interlaminar fracture toughness but causes a reduction in interlaminar shear strength. The healing efficiency in terms of restoration of the interlaminate fracture energy scales linearly with the areal percentage of self-healing material. Microstructure study revealed distinct difference in the fracture surfaces of composites with EMA and EMAA, with EMA displaying extensive nano-scale porous structures in contrast to the more homogenous single phase structure from EMAA.     

Effect of mendable polymer stitch density on the toughening and healing of delamination cracks in carbon–epoxy laminates

This paper presents an investigation into the effect of stitch density on the delamination toughening and self-healing properties of carbon–epoxy laminates. The stitches provide the laminate with the synergistic combination of high mode I interlaminar fracture toughness to resist delamination cracking and healing properties to repair delamination damage. The results show that the fracture toughness of the laminate increased with stitch density, due to higher traction (crack closure) loads exerted by the stitches bridging the delamination. During the healing process these bridging stitches first melt and then flow into the delamination, leading to self-healing with full restoration of the mode I fracture toughness. Furthermore, the stitches were capable of repairing delamination cracks many times larger than the original size of the stitches. The effect of stitch density on the healing process of delamination cracks and restoration of fracture toughness was found to remain approximately the same under multiple repair operations.     

Interlaminar fracture of CF/EP composite containing a dual-component microencapsulated self-healant

We present an experimental study of the self-healing ability of carbon fibre/epoxy (CF/EP) composite laminates with microencapsulated epoxy and its hardener (mercaptan) as a healing agent. Epoxy- and hardener-loaded microcapsules (average size large: 123 μm; small: 65 μm) were prepared by in situ polymerisation in an oil-in-water emulsion and were dry-dispersed at the ratio 1:1 on the surface of unidirectional carbon fabric layer. The CF/EP laminates were fabricated using a vacuum-assisted resin infusion (VARI) process. Width-tapered double cantilever beam (WTDCB) specimens were used to measure mode-I interlaminar fracture toughness of the CF/EP composites with a pre-crack in the centre plane where the microcapsules were placed. Incorporation of the dual-component healant stored in the fragile microcapsules provided the laminates with healing capability on delamination damage by recovering as much as 80% of its fracture toughness. It was also observed that the recovery of fracture toughness was directly correlated with the amount of healant covering the fracture plane, with the highest healing efficiency obtained for the laminate with large capsules.     

An efficient healing agent for high temperature epoxy composites based upon tetra-glycidyl diamino diphenyl methane

Poly(ethylene-co-methacrylic acid) (EMAA) as a thermally activated healing agent in a high performance, high temperature tetra-glycidyl methylene dianiline (TGDDM)/diethyl toluene diamine (DETDA) mendable epoxy composite is reported for the first time. Despite curing above EMAAs melting point (T_m = 85 °C), healing occurred by incorporating a preliminary low temperature curing step of 5 h at 80 °C, prior to cure at 177 °C. Healing occurred via the pressure delivery mechanism derived from tertiary amine catalysed surface condensation reactions between EMAA and hydroxyl groups from the epoxy resin. Healing efficiencies of 36%, 55% and 105% were achieved after heating at 150 °C, 200 °C and 230 °C respectively, but decreased rapidly with continued healing. Healing at 150 °C and 200 °C revealed significant healing despite remaining in the glassy state. In addition, EMAA enhanced mode I interlaminar fracture toughness by more than 270% for both the DETDA and 4,4-DDS networks.     

Fracture toughness of transverse cracks in graphite/epoxy laminates at cryogenic conditions

Stress singularity of a transverse crack normal to ply-interface in a composite laminate is investigated using analytical and finite element methods. Four-point bending tests were performed on single-notch bend specimens of graphite/epoxy laminates containing a transverse crack perpendicular to the ply-interface. The experimentally determined fracture loads were applied to the finite element model to estimate the fracture toughness. The procedures were repeated for specimens under cryogenic conditions. Although the fracture loads varied with specimen thickness, the critical stress intensity factor was constant for all the specimens indicating that the measured fracture toughness can be used to predict delamination initiation from transverse cracks. For a given crack length and laminate configuration, the fracture load at cryogenic temperature was significantly lower. The results indicate that fracture toughness does not change significantly at cryogenic temperatures, but the thermal stresses play a major role in fracture and initiation of delaminations from transverse cracks.     

Thermally activated healing in a mendable resin using a non woven EMAA fabric

This paper explores the efficacy of polyethylene-co-ethacrylic acid (EMAA), as a thermally activated thermoplastic healing agent embedded within a carbon fibre reinforced epoxy composite. EMAA fibres have been shown to effectively restore mode I properties in a fibre reinforced composite after thermal activation yet other forms of the healing agent or modes of deformation have so far not been studied at all. This work, uses EMAA in the form of a non-woven mesh, rather than a woven fabric to study the healing mechanism and effectiveness of property restoration for mode I (crack opening) and mode II (shear) failure as well as for high speed impact. Property restoration after mode I damage was found to be over 200% and increased with increasing EMAA concentration. For mode II shear failure, the property restoration was reduced to a little over 100% regardless of EMAA concentration. Mode II analysis also showed that the modulus could be restored to about 80% of its original value when modified with EMAA. Repeated impacting using a falling weight test produced no property restoration after healing, yet the modified laminates appeared protected from further damage compared with an unmodified laminate. This was attributed to the formation of a ductile thermoplastic layer mitigating further damage. Scanning electron microscopy revealed that regardless of the extent of healing, the form of the healing agent or the mode of damage, the unique pressure delivery mechanism previously identified, was always observed to occur.     

Delamination cracking in advanced aluminum-lithium alloys - Experimental and computational studies

Delamination cracking in advanced aluminum-lithium (Al-Li) alloys plays a dominant role in the fracture process. With the introduction of these materials into components of aerospace structures, a quantitative understanding of the interplay between delamination cracking and macroscopic fracture must be established as a precursor to reliable design and defect assessment. Delamination cracking represents a complex fracture mechanism with the formation of transverse cracks initially on the order of the grain size. In this work, interrupted fracture toughness tests of C(T) specimens, followed by incremental polishing, reveal the locations, sizes and shapes of delamination cracks and extensions of the primary macrocrack. These observations suggest that delamination crack sizes scale with loading of the primary crack front expressed in terms of J/σ₀. Using a 3-D, small-scale yielding framework for Mode I loading, a companion finite element study quantifies the effects of prescribed delamination cracks on local loading along the macroscopic (primary) crack and ahead of the delamination cracks. An isotropic hardening model with an anisotropic yield surface describes the constitutive behavior for the 2099-T87 Al-Li alloy plate examined in this study. The computational results characterize the plastic zone size, the variation of local J ahead of the macrocrack front and the stress state that serves to drive growth of the macrocrack and delamination crack. The computational studies provide new, quantitative insights on the observed increase in toughness that has been observed during fracture experiments caused by delamination cracks that divide the primary crack front.     

Influence of adsorption behaviour of a silane coupling agent on interlaminar fracture in glass fibre fabric-reinforced unsaturated polyester laminates

The relationship between the interphase consisting of physisorbed and chemisorbed silane on glass fibres and the resultant composite Mode I delamination fracture toughness in glass fibre fabric laminate, was studied. The Mode I interlaminar fracture toughness of the laminate specimen was obtained by using a double cantilever beam (DCB) specimen. The delamination resistance of the laminate specimen finished with two silane concentrations and washed in methanol solvent, is discussed on the basis of the interlaminar fracture toughness. In order to determine the amount of physisorbed and chemisorbed silane on the glass fibre, the amount of total carbon was determined using an analysis instrument. The physisorbed silane migrated into the resin matrix and influenced the mechanical properties and interlaminar fracture of the laminate specimen. The amount of unsaturated polyester resin blended with a silane coupling agent was measured using dynamic mechanical spectroscopy, and a DCB specimen for mechanical properties and fracture toughness.     

Interactions between propagating cracks and bioinspired self-healing vascules embedded in glass fibre reinforced composites

This study considers the embedment of a bioinspired vasculature within a composite structure that is capable of delivering functional agents from an external reservoir to regions of internal damage. Breach of the vascules, by propagating cracks, is a crucial pre-requisite for such a self-healing system to be activated. Two segregated vascule fabrication techniques are demonstrated, and their interactions with propagating Mode I and II cracks determined. The vascule fabrication route adopted played a significant role on the resulting laminate morphology which in-turn dictated the crack-vascule interactions. Embedment of the vascules did not lower the Mode I or II fracture toughness of the host laminate, with vascules orientated transverse to the crack propagation direction leading to significant increases in G_I and G_II through crack arrest. Large resin pockets were found to redirect the crack around the vascules under Mode II conditions, therefore, it is recommended to avoid this configuration for self-healing applications.     

Effective stiffness concept in bending modeling of laminates with damage in surface 90-layers

Simple approach based on Classical Laminate Theory (CLT) and effective stiffness of damaged layer is suggested for bending stiffness determination of laminate with intralaminar cracks in surface 90-layers and delaminations initiated from intralaminar cracks. The effective stiffness of a layer with damage is back-calculated comparing the in-plane stiffness of a symmetric reference cross-ply laminate with and without damage. The in-plane stiffness of the damaged reference cross-ply laminate was calculated in two ways: (1) using FEM model of representative volume element (RVE) and (2) using the analytical GLOB-LOC model. The obtained effective stiffness of a layer at varying crack density and delamination length was used to calculate the A, B and D matrices in the unsymmetrically damaged laminate. The applicability of the effective stiffness in CLT to solve bending problems was validated analyzing bending of the damaged laminate in 4-point bending test which was also simulated with 3-D FEM.     

Dynamic delamination fracture toughness of a graphite/epoxy laminate under impact

Dynamic delamination fracture toughness in a [90/0]_5s T300/934 graphite/epoxy laminate was investigated using impact loading. Delamination cracks of three different sizes were embedded at the mid-plane of the composite specimen. The threshold impact velocity that causes propagation of the delamination crack was used in the dynamic analysis with the finite element method. From the finite element solution, the time-history of the strain energy release rate was calculated. The critical strain energy release rate was taken to equal the maximum value of the response history.     

Effect of delamination failure in crashworthiness analysis of hybrid composite box structures

In the present paper the effects of delamination failure of hybrid composite box structures on their crashworthy behaviour will be studied and also their performance will be compared with non-hybrid ones. The combination of twill-weave and unidirectional CFRP composite materials are used to laminate the composite boxes. Delamination study in Mode-I and Mode-II with the same lay-ups was carried out to investigate the effect of delamination crack growth on energy absorption of hybrid composite box structures. The end-loaded split (ELS) and double-cantilever beam (DCB) standard test methods were chosen for delamination studies. In all hybrid composite boxes the lamina bending crushing mode was observed. Regarding the delamination study of hybrid DCB and ELS the variation of the specific energy absorption (SEA) versus summation of G_IC and G_IIC were plotted to combine the effect of Mode-I and Mode-II interlaminar fracture toughness on the SEA. From this relationship it was found the hybrid laminate designs which showed higher fracture toughness in Mode-I and Mode-II delamination tests, will absorb more energy as a hybrid composite box in crushing process. The crushing process of hybrid composite boxes was also simulated by finite element software LS-DYNA and the results were verified with the relevant experimental result.     

Interlaminar properties of polymer laminates containing internal sensor cavities

This research paper presents an experimental investigation into the sensitivity of the interlaminar properties of polymer laminates to long, narrow interlaminar galleries used in comparative vacuum monitoring (CVM). CVM is a structural health monitoring technique for the non-destructive detection of cracks in engineering materials. The paper examines the effect of CVM galleries on the mode I delamination toughness, interlaminar shear strength, and impact damage resistance of a carbon/epoxy laminate. It was found that the galleries improve the mode I delamination toughness by blunting and/or deflecting the crack tip; with the maximum improvement being double the toughness of the laminate free of galleries. The toughness increased with the diameter of the gallery up to a critical size, above which no further improvement was achieved. However, the composite is more prone to unstable delamination cracking in the presence of the galleries. The apparent interlaminar shear strength (ILSS) decreased at a linear rate with an increase in the diameter and volume fraction of galleries. The loss in ILSS is due to the reduction in the effective interlaminar load-bearing area caused by the galleries. Low-energy impact testing revealed that the galleries do not affect the impact damage resistance when below a critical diameter; however, above a threshold gallery size the impact resistance is degraded. This study shows that the incorporation of CVM galleries into laminates can have the added benefit of increased mode I delamination toughness, although the ILSS is degraded and the impact resistance is reduced by large galleries.     

Influence of silane coupling agents on interlaminar fracture in glass fibre fabric reinforced unsaturated polyester laminates

The relationship between the adhesive properties of the interphase of glass fibre/resin and the resultant composite Mode I delamination fracture toughness in glass fibre fabric laminate (GFFL) was studied. The Mode I interlaminar fracture toughness of GFFL was obtained by using a double cantilever beam (DCB) specimen. The delamination resistance of GFFLs which have two silane coupling agents and three concentration finishes is discussed on the basis of interlaminar fracture toughness. The crack propagation behaviour of DCB testing was mainly divided into stable and unstable manners. The fracture toughness and the crack propagation behaviour were dependent on the types and concentration of silane coupling agents.     

Retardation and repair of fatigue cracks in a microcapsule toughened epoxy composite—Part II: In situ self-healing

Successful arrest and retardation of fatigue cracks is achieved with an in situ self-healing epoxy matrix composite that incorporates microencapsulated dicyclopentadiene (DCPD) healing agent and Grubbs’ first generation Ru catalyst. Healing agent is released into the crack plane by the propagating crack, where it polymerizes to form a polymer wedge, generating a crack tip shielding mechanism. Due to the complex kinetics of healing a growing crack, the resulting in situ retardation and arrest of fatigue cracks exhibit a strong dependence on the applied range of cyclic stress intensity ΔK_I. Significant crack arrest and life-extension result when the in situ healing rate is faster than the crack growth rate. In loading cases where the crack grows too rapidly (maximum applied stress intensity factor is a significant percentage of the mode-I fracture toughness value), a carefully timed rest period can be used to prolong fatigue life up to 118%. At moderate ΔK_I, in situ healing extends fatigue life by as much as 213%. Further improvements in fatigue life-extension are achieved by employing a rest period, which leads to permanent arrest at this moderate ΔK_I. At lower values of applied stress intensity factor, self-healing yields complete arrest of fatigue cracks providing infinite fatigue life-extension.     

Thermal characteristics of the self-healing response in poly(ethylene-co-methacrylic acid) copolymers.

A class of poly(ethylene-co-methacrylic acid) (EMAA) copolymers and ionomers has shown the unique ability to instantaneously self-heal following ballistic puncture. It is noteworthy that the thermomechanical healing process active in these materials appears to be significantly different in capability and mechanism than any of the other self-repairing systems studied. To better understand this phenomenon, the thermal response during EMAA self-healing was examined. Tests of various damage types, including sawing, cutting and puncture, revealed high-energy transfer damage modes to produce heat and store energy favourable to healing. DSC probed healed specimens revealing they had reached the viscoelastic melt believed requisite to healing response. Low-temperature ballistic experiments demonstrated films continue healing even when punctured at -30 degrees C; analysis showed healing efficacy comparable to room temperature, holding significant pressures of approximately 3 MPa. At the lowest temperature, brittle fracture occurred in one material indicating insufficient heat transfer to store recoverable energy. In total, the results supported the defined healing model and provided additional information on the healing process in both its thermal dependence and general mechanism. Finally, a new DSC method was developed for probing the thermal history of healed films which may lead to a more complete mechanistic model.     

Interaction between matrix cracking and edge delamination in composite laminates

Matrix cracking and edge delamination are two main damage modes in continuous-fibre composite laminates. They are often investigated separately, and so the interaction between two damage modes has not yet been revealed. In this paper, a simple parallel-spring model is introduced to model the longitudinal stiffness reduction due to matrix cracking and edge delamination together. The energy release rate of edge delamination eliminating the matrix crack effect and the energy release rate of matrix cracking in the presence of edge delamination are then obtained. Experimental materials include carbon- and glass-fibre-reinforced bismaleimide composite laminates under static tension. The growth of matrix cracks and edge delaminations was recorded by means of NDT techniques. Results show that matrix cracks may initiate before or after edge lamination. This depends on the laminate layup, and especially on the thickness of the 90° plies. Edge delamination may also induce matrix cracking. Matrix cracking has a significant effect on the stiffness reduction in GRP laminates. The present model can predict the stiffness reduction in a laminate containing both matrix cracks and edge delaminations. The mixed-mode delamination fracture toughness obtained from the present model shows up to 50% differences compared with O'Brien's model for GRP laminates. However, matrix cracking has a small effect on the mixed-mode interlaminar fracture toughness of the CFRP laminates.