S. Teixeira De Freitas
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Bio-based epoxy adhesives face significant challenges due to their relatively poor mechanical properties compared to their petroleum-based competitors, including low fracture toughness and abrupt failure. By mimicking the molecular structure of spider silk, which is one of the toughest materials in nature, 3D-printed polymer overlapping curls consisting of coiling fibers with sacrificial bonds and hidden lengths, were impregnated into a bio-based epoxy adhesive to improve its mode I fracture toughness. Such bio-inspired structures were designed specifically to toughen and improve the crack resistance of adhesive joints. These overlapping curls were embedded in the bio-based epoxy bondline with various adhesion patterning strategies, aiming to architect the fracture scenario and increase mode I energy dissipation. Double cantilever beam test results show that an extrinsic bridging is triggered by the embedded curls that promote progressive failure and delay crack growth, which improved the mean energy release rate by 133% and enhanced the mean peak energy release rate up to 313%. The proposed 3D-printed coiling fibers successfully improved the mechanical performance of the bio-based epoxy and retarded the crack growth within the bondline, opening new horizons for their use as carriers of bondlines in structural applications to control crack growth in adhesively bonded joints.
Tow-Based Discontinuous Composites (TBDCs) are a new class of composite materials that combine high strength and stiffness with in-plane isotropy making them of interest in high-end structural applications. Despite their potential, efficient connection methods are currently lacking and the adhesive bonding behaviour of TBDC structures remains unexplored. This work, therefore, seeks to address this gap by analysing the quasi-static performance of TBDC adhesive joints under mode I loading condition. Double Cantilever Beam (DCB) tests were performed using two adhesives with contrasting toughness levels: a moderate (∼600 J/m 2) and a high toughness adhesive (> 2400 J/m2). When a moderate-toughness adhesive was used, a combination of cohesive failure and composite damage was observed, with only a small scatter in the experimental results. In contrast, the use of the high-toughness adhesive led to a shift in damage mechanisms towards the composite micro-architecture, resulting in fracture toughness values in the region of 800 J/m2, with a larger experimental scatter. Acoustic Emission analysis identified matrix cracking and fibre/matrix debonding as the dominant damage mechanisms. These findings were validated by the post-mortem fractography analysis via Scanning Electron Microscopy. This work therefore provides the first detailed analysis of the damage mechanism in adhesively bonded TBDCs, which have potential in aerospace and automotive applications.
Designing for toughness
How substrate stiffness controls crack path and effective engagement of toughening layers in adhesively bonded CFRP joints
Tailoring the stacking sequence of composites bonded joints improves fracture toughness and damage tolerance of the joint by encouraging extrinsic toughening mechanisms, such as crack deflection and crack branching. Previous works show that in composite substrates with tailored laminates, each crack deflection into a new ply can increase the joint's toughness. Still, once a 0° layer is reached, toughness drops abruptly due to sudden delamination. To overcome this limitation, this work explores embedding a co-cured film-adhesive layer to prevent delamination in 0° plies. It examines how the substrate's bending stiffness influences the effectiveness of this toughening strategy. Quasi-static double cantilever beam tests on four different carbon fibre reinforced laminates, with and without the co-cured layer, revealed two regimes: (i) compliant substrates lead to high peel stresses, triggered crack deflection into ±45° plies, enabling bridging and rising R-curves—up to 200% toughness increase; (ii) stiffer substrates suppressed near-tip rotation, and promoted cleavage-like crack growth with minimal toughening.
Adhesive bonding has emerged as an attractive solution for the joining of lightweight structures, yet accurate stress analysis remains computationally demanding when relying on Finite Elements (FE). This paper introduces a novel plate Macro-Element (ME) formulation that extends previous beam-type approaches to enable three-dimensional stress analysis of bonded joints. High-order polynomial expansions are employed to describe the displacement field of the adherends, while the adhesive is modeled as an elastic foundation. Governing equations are derived using a variational principle and integrated within a standard FE framework. Through the derivation of a special stiffness matrix, a ME can simulate an entire overlap with just one element. The proposed methodology is validated against FE results for a single-lap bonded joint with a thin adhesive layer. The influence of different higher-order displacement assumptions and constitutive models is investigated. The results show that their inclusion in the formulation improves the solution accuracy.
Adhesive bonding of fiber-reinforced polymer (FRP) patches is increasingly used to strengthen steel structures. While carbon FRP (CFRP) and epoxy adhesives are the primary materials in industrial applications, this study explores hybrid Carbon/Flax FRP as an alternative for reinforcing steel plates under flexural loading. Four composite layups were tested: F5 (flax), C5 (carbon), CFC, and FC (carbon/flax hybrids). These patches were bonded to steel plates using three adhesives: a flexible and ductile silane-modified polymer (SMP-FD), a medium flexibility-ductility acrylate (ACR-MFD), and a rigid and brittle epoxy (EP-RB), representing a wide range of adhesive properties. Three-point bending tests were conducted to evaluate mechanical performance compared to unreinforced steel plates. Results demonstrated that composite patch bonding significantly enhances load-bearing capacity. The EP-RB adhesive provided the highest reinforcement, followed by ACR-MFD and SMP-FD. Hybrid FC and CFC configurations achieved reinforcement comparable to or greater than pure carbon (C5), highlighting the potential of hybrid designs for structural applications.
Mode I fracture toughness of co-bonded metal–composite joints with additively manufactured titanium
Influence of printing parameters
The strength of adhesive joints is influenced by the surface of the adherends, which is often treated before bonding to prevent interfacial (adhesive) failure. Laser Powder Bed Fusion (LPBF) offers promising potential for bonding without time-consuming surface treatments, since LPBF parts have an inherently rough surface, which is usually associated with good adhesion strength. Here we study the effect of the printing parameters on the mode I fracture toughness of co-bonded joints between untreated LPBF Ti6Al4V and Carbon Fiber Reinforced Polymer (CFRP) substrates. A factorial Design of Experiment (DoE) was set varying the laser scan speed and the build angle of the Ti6Al4V substrates, which were co-bonded with a CFRP woven laminate to form Double Cantilever Beam (DCB) joints. The results showed that increasing the scan speed from 500 mm/s to 2000 mm/s led to higher titanium surface roughness (+125% on average). On the other hand, the mode I fracture toughness was mainly affected by the build angle: the joints with vertically printed (90° with respect to the build platform) titanium adherends exhibited, on average, a 200% increase in toughness compared to the samples with titanium printed at an angle. This behavior was due to the higher number of partially melted particles on the surface of the vertical joints. A particle counting method was introduced to quantify the partially fused particles and their correlation with the mode I fracture toughness was demonstrated. Moreover, to the authors’ knowledge, for the first time an original approach was proposed to assess their interlocking contribution to joint toughness.
Further development of thermoplastic composites for advanced structural applications, such as in aerospace, requires tough interfaces at bimaterials junctions such as composite-metal interfaces. Mode I failure being the most critical failure mode of interfaces, surface roughening or patterning techniques are commonly used to improve the mode I interface toughness. Patterning typically involves creating grooves on the surface via laser ablation or 3D printing. However, crack propagation may follow two distinct paths: along the groove pattern (interfacial failure) or through the polymer within the grooves (cohesive failure). Cohesive failure is often the toughest mechanism. However, design criteria linking groove geometry to joint materials are currently lacking. This study investigates the influence of groove dimensions, joint dimensions, and material and interface properties on the resulting failure mechanism using a cohesive zone model. First, a small-scale yielding (SSY) model is developed. The results indicate that the characteristic fracture length of the material filling the grooves plays a critical role in determining the failure mechanism. Specifically, cohesive failure is promoted when the groove depth is at least ten times greater than the characteristic length, and when the groove aspect ratio (depth-to-width) exceeds 10. Additionally, filling the grooves with a more compliant material, such as a polymer, helps to prevent interfacial failure. Finally, a double-cantilever model is developed, indicating that the loading configuration significantly influences the failure mechanisms taking place. For the DCB configuration, crack propagation along the interface is promoted, compared to the SSY case, owing to the bending of the adherends.
Double Cantilever Beam (DCB) tests were carried out to determine the mode I fracture toughness of joints comprising as-printed titanium (Ti6Al4V) adherends, namely titanium-titanium secondary bonded and titanium-Carbon Fibre Reinforced Polymer (CFRP) co-bonded joints. The effect of high-temperature oxidation on the fracture toughness was also evaluated by testing a batch of joints in which the titanium underwent a post-printing thermal treatment. The as-printed specimens were compared to the same type of joints but with sandblasted titanium adherends to evaluate the effect of this surface pre-treatment on the value of fracture toughness.
The results indicate that non-oxidised titanium joints with untreated adherends had an average of 11% higher fracture toughness than their sandblasted counterparts. On the other hand, sandblasting proved beneficial for oxidised joints, increasing the fracture toughness by 64% on average over the untreated samples. ...
Double Cantilever Beam (DCB) tests were carried out to determine the mode I fracture toughness of joints comprising as-printed titanium (Ti6Al4V) adherends, namely titanium-titanium secondary bonded and titanium-Carbon Fibre Reinforced Polymer (CFRP) co-bonded joints. The effect of high-temperature oxidation on the fracture toughness was also evaluated by testing a batch of joints in which the titanium underwent a post-printing thermal treatment. The as-printed specimens were compared to the same type of joints but with sandblasted titanium adherends to evaluate the effect of this surface pre-treatment on the value of fracture toughness.
The results indicate that non-oxidised titanium joints with untreated adherends had an average of 11% higher fracture toughness than their sandblasted counterparts. On the other hand, sandblasting proved beneficial for oxidised joints, increasing the fracture toughness by 64% on average over the untreated samples.
Bio-inspired overlapping curl structures for toughening bio-based epoxy
A study on the fracture phenomena
In this study, a 3D-printed biomimetic overlapping curl structure inspired by spider silk molecular structure, containing sacrificial bonds and hidden lengths, is studied as a toughening mechanism for a bio-based epoxy. Experimental results of the fracture phenomena of the overlapping curl-reinforced bio-based epoxy identify three toughening mechanisms triggered by the overlapping curl: (1) crack re-initiation, (2) overlapping curl bridging, and (3) epoxy ligament. First, the integrated overlapping curl creates a void within the epoxy matrix. As the crack tip reaches the end of this void, the crack re-initiates. Then, as the hidden length of overlapping curl unfolds, it leads to a bridging effect in resisting crack growth. In addition, for the smallest hidden length, an epoxy ligament is formed due to crack branching, significantly improving the energy release rate. The epoxy fracture energy release rate increased by 13 %. The overall modest improvement is attributed to the large plastic dissipation energy of the epoxy and the relatively low overlapping curl load-capacity. However, when expanding the design space numerically, it was shown that as the failure load of the overlapping curl increases, the bridging effect increases progressively. The introduction of the bio-inspired overlapping curl structure into bio-based epoxy proves the concept of a toughening strategy for developing high-performance sustainable composite materials.
Driven by sustainability goals outlined in the European Green Deal, most of the industrial sectors (i.e. automotive, aerospace and civil infrastructures) require reliable, lightweight, and durable materials. Accurate crack detection significantly extends the operational life of bonded structural components, reducing maintenance, waste, and environmental impact. This study presents acoustic emission (AE) techniques for accurately monitoring crack length in adhesively bonded joints, primarily targeting Titanium-Carbon Fiber Reinforced Polymer (Ti-CFRP) bi-material specimens, with Titanium-Titanium (Ti-Ti) joints included as a benchmark. Titanium Ti6Al4V substrates fabricated via Laser Powder Bed Fusion (LPBF) were prepared with various surface conditions: as-printed and sandblasted. The mode I fracture toughness was evaluated via Double Cantilever Beam tests, which were supported by continuous AE monitoring with high-resolution equipment capturing around 200,000 waveforms. Principal Component Analysis and machine learning techniques, including Self-Organising Maps and K-means clustering, classified AE signals into clusters associated with damage or background noise. A linear localisation algorithm tracked crack initiation and growth phases. Results validated the accuracy of AE signals to localise crack propagation under the bi-material quasi-static mode I load condition. The study highlights AE's potential for precise and sustainable structural health monitoring, informing future numerical modelling to predict joint durability.
Effects of cyclic ageing frequencies on the ageing and mechanical behaviour of adhesive materials
Experimental analysis and numerical study
Acoustic emission approach for identifying fracture mechanisms in composite bonded Joints
A study on varying Substrate's stacking sequence
This study uses the acoustic emission structural health monitoring method to identify fracture mechanisms in composite bonded joints when varying the substrate stacking sequence. Quasi-static mode I loading tests were performed on secondary adhesively bonded multidirectional composite substrates (0, 90, 45, −45, 60 and −60° fibre orientations). An unsupervised artificial neural network combined with the visual fracture evaluation of the specimens and the Morlet continuous wavelet transform was used to cluster and give the acoustic emission signals a physical meaning. Different fracture mechanisms could be identified within the adhesive layer (i.e., cohesive failure) and in the composite substrates, including non-visible damage mechanisms (matrix micro-cracking, fibre/matrix debonding, fibre pull-out and fibre breakage). Using the Morlet continuous wavelet transform, it was possible to recognise that the highest peak frequency does not always represent the most relevant signature of the fracture mechanism. Moreover, multiple peak frequencies can be associated with multiple fracture mechanisms, such as the fibre pull-out that occurs in the combination of matrix cracking and fibre breakage. Furthermore, no differences were observed in mode I loading conditions between the acoustic emission signatures from the cohesive failure in the adhesive layer and the matrix cracking within the composite substrate. The findings of this study present a great opportunity to gain more insight into the fracture behaviour of polymer materials and fibre-reinforced polymer materials and to improve the quality of adhesively bonded joints.
Biomimetic toughening design of 3D-printed polymeric structures
Enhancing toughness through sacrificial bonds and hidden lengths
Spider silk is known for its excellent strength and fracture resistance properties due to its molecular design structure, characterized by sacrificial bonds and hidden lengths. These structures have inspired reinforcements of synthetic polymer materials to enhance toughness. In this study, we mimic these natural toughening mechanisms by designing and manufacturing 3D-printed polymeric structures incorporating overlapping curls consisting of coiling fiber with sacrificial bonds and hidden lengths. Utilizing the liquid rope coiling effect, we manufactured overlapping curls using three polymers: polylactic acid (PLA), liquid crystal polymer (LCP), and polyamide 6 (PA6). Uniaxial tensile tests were performed to characterize the mechanical properties of overlapping curl as a function of geometries, post-treatments, and material constitutive parameters. Our results show that single-sided overlapping curls can fully unfold while double-sided curls are prone to premature failure. Heat-pressure post-treatment was found to significantly increase the load-capacity of the sacrificial bonds by up to [Formula presented] due to increased contact area. However, the defects introduced in the fibre after the break of the sacrificial bonds, make the structure more susceptible to premature failure, limit the complete unfolding of the hidden length, and lead to a decrease up to [Formula presented] of the toughness. To guarantee the complete unfolding of the hidden lengths and improve the toughness, we demonstrate that selecting a polymer material with either high fracture strength (e.g., LCP, [Formula presented]) or high fracture strain (e.g., PA6, >2) is crucial, and increase toughness up to [Formula presented] and [Formula presented], respectively.
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This chapter discusses the mixed-mode loading of adhesive joints. The importance of mixed-mode loading is first introduced and then test methods commonly used to measure the mixed-mode fracture resistance of adhesive joints are presented and briefly discussed. The approaches to determine the fracture resistance are briefly reviewed and then the partitioning of mixed-mode fracture energies is discussed. The limitations of the local singular field and global approaches to mixed-mode partitioning are discussed and the use and application of a semianalytical cohesive zone analysis partitioning scheme is evaluated. The limitations of the global partitioning approach are further discussed in the context of developing a scheme to design and analyze adhesive joints with dissimilar adherends (a bi-material interface). A longitudinal strain criterion is proposed in addition to the matching of flexural rigidities and the approach is validated numerically. Finally, the practical issues of crack stability, failure path selection, and the use of mixed-mode failure envelopes is considered.