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.

@en

Here we investigate the adhesive properties of Selective Laser Melted (SLM) titanium surfaces in metal-composite cobonded joints without any prior surface treatment, to explore the inherent surface roughness of SLM parts to potentially create strong adhesive bonds. Double Cantilever Beam (DCB) tests were carried out to assess the joints mode I fracture toughness involving untreated SLM titanium and woven Carbon Fibre Reinforced Polymer (CFRP) adherends, co-bonded with an epoxy film adhesive. The same type of DCB joints, but now with sandblasted SLM titanium adherends, were tested to compare the adhesion strength of the untreated SLM surface versus the sandblasted surface. The findings reveal that joints with untreated SLM titanium adherends exhibit similar toughness to those with sandblasted SLM titanium adherends, indicating that the surface morphology of as-printed SLM titanium is suitable for manufacturing robust adhesive joints. The elimination of the surface treatment in the manufacturing of adhesive joints with SLM adherends could increase the interest of many industrial fields towards the use of adhesive bonding over other joining techniques.@en

This work aims to improve the damage tolerance of secondary adhesively bonded joints under quasistatic mode I loading conditions by architecting the carbon fibre-reinforced polymer substrates’ stacking sequences [1]. Double Cantilever Beam tests show that architecting the stacking sequence of the laminates composite substrates in combination with the adhesive layer’s fracture toughness affects the crack onset and triggers different crack paths throughout the joints’ thickness. In specimens bonded with a low-toughness bi-component adhesive, the tailored design, including a co-cured toughening layer, could increase the effective fracture toughness of the composite bonded joints up to 200%. From this study, it was possible to recognise the complexity and benefits of moving from the traditional cohesive failure to outbreaking multiple crack path propagation. @en

Bio-based epoxy materials face major challenges in 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, we manufactured polymer overlapping curls consisting of coiling fibers with sacrificial bonds and hidden lengths through 3D printing. These curls were embedded in a bio-based epoxy aiming to improve its toughness. The bio-based epoxy adhesive layer integrated by such 3D-printed coiling fibers was tested under mode I opening load using Double Cantilever Beam tests. The results show an extrinsic bridging triggered by the embedded curls that promote progressive failure and improve the mode I fracture toughness by 285%. The proposed 3D-printed coiling fibers can improve the performance of biobased epoxies and retard crack growth, opening new horizons for their use in structural applications and the use of these bio-inspired overlapping curls to control crack growth in adhesively bonded joints. @en

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.

@en

Aiming to aid the sustainable transition to fossil fuel-free epoxy materials and enhance the toughness of bio-based epoxies, here we integrate an overlapping curl microstructure consisting of coiling fiber with sacrificial bonds and hidden lengths into a bio-based epoxy matrix. Inspired by natural material, where exceptional properties are achieved at low environmental cost, the microstructure mimics the molecular structures of spider silk, known for its exceptional fracture resistance. The 3D-printed overlapping curl shows a saw-tooth mechanical response with continuous load-carrying ability thanks to the break of sacrificial bonds and unfolding of the hidden lengths. By embedding the overlapping curl into the compact-tension configuration of the bio-based epoxy, an extrinsic toughening mechanism is triggered as the hidden length unfolds. Experimental results show that a single-sided overlapping curl structure is able to improve the toughness of bio-based epoxy by 19%.@en

In marine structures adhesive joint structures are often exposed to cyclic conditioning where the ambient humidity changes cyclically during their service. Though some comprehensive studies on the aging of adhesives exist, these researches mainly focus on monotonic aging conditions where the adhesive joints are exposed to a wet condition continuously for a long time. However, the few investigations performed on the cyclic moisture absorption of adhesive materials show that the parameters obtained in monotonic aging conditions are not suitable for estimation of the aging behaviour of adhesive exposed to alternating humidity. An important question that can arise is whether or not this frequency affects the mechanical behaviour of adhesive joints under cyclic aging condition. In this investigation bulk dogbone and square samples were manufactured, subjected to cyclic aging conditions with four different aging frequencies and tested. The results show that the moisture diffusion constant of adhesives exposed to higher aging frequencies increase more than those exposed to lower aging frequency conditions. In addition, the moisture content only affects the degradation of strength and stiffness of the tested adhesives in different aging frequencies.@en

For strengthening or rehabilitation of existing structures, patches of fiber-reinforced polymers (FRP) materials are being adhesively bonded to the existing metallic structures. So far, Carbon FRP (CFRP) are the main composite materials industrially implemented for metal structural reinforcement, due to their reliability and high mechanical performances. However, multiple researchers have highlighted the negative environmental impact of synthetic composite materials, and interest is shifting towards the use and development of bio-based composite materials. This paper presents an FE numerical investigation of the use of Hybrid Carbon/Flax FRP as an alternative solution for structural reinforcement of steel plates under flexural loading. Four different configurations of patches are studied to be bonded to steel rectangular plates, and three point bending tests are numerically modelled to simulate the flexural behaviour of the assemblies. Compared to the unreinforced steel plate baseline, reinforcements C5, F5, CFFFC, and FFFCC exhibited improvements of 149%, 120%, 137%, and 145% in bending stiffness, respectively.@en

The bondline thickness is a crucial parameter affecting the strength and toughness of adhesive joints. This parameter is responsible for the stress distribution, and thus, the efficiency of the stress transfer between the adherends, the failure modes, and the correspondent failure loads. However, the available literature reports different trends and relationships during testing between the thickness and strength, or thickness and toughness. In this chapter, the effect of adhesive thickness on the mechanical properties of adhesive joints is explored using the fracture mechanics framework. Two testing cases are discussed in detail: (i) soft bondlines joining rigid adherends, that is, butt joint and single end notch testing specimens, and (ii) rigid bondlines joining flexible adherends, that is, double cantilever beam geometry. These cases represent two extremes in terms of where the energy is stored while testing: in the first one, the energy is stored in the adhesive while in the second, the energy is stored in the adherends. From this discussion, the bondline thickness emerges as a critical geometrical parameter dictating transition between the two extreme cases. A single theoretical framework is provided that merges the two cases and is used to disclose the recently obtained experimental results.

@en

Aiming to increase damage tolerance of adhesively bonded joints, this work explores the influence of CFRP layup of the adherends on the crack onset and crack propagation of composite bonded joints under mode I loading. Quasi-static Double Cantilever Beam tests were performed using four different CFRP layups bonded with two adhesives. Parallel to the experimental program, finite element analyses were performed to aid in understanding and identifying the various damage mechanisms in each specimen type. The results show that the CFRP layup and adhesive fracture toughness significantly influence the joint fracture phenomena at crack onset and further crack propagation. An enhancement of the joint's mode I fracture toughness values at crack onset was observed in the specimens where a crack competition between the propagation within the bondline and the composite's layers was triggered. During crack propagation, the fracture toughness of the joint increases at crack deflections between the different plies of the CFRP layup until reaching the 0° ply, where sudden delamination occurs. It has been shown that CFRP layup tailoring is a promising toughening method that, when carefully designed, has the potential to increase the maximum effective fracture toughness up to 100% when compared to pure cohesive failure.

@en

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.

@en

Spacecraft experience minimal mechanical loads in space, but with the development of reusable spacecraft for interplanetary exploration and repeated landings, structures will be subjected to increased mechanical stress. The impact of the space environment on the aging of adhesive materials used in space structures over long-term applications is not well understood. This study investigates two commonly used adhesives in spacecraft assembly, namely Scotch-Weld™ EC-2216 and Scotch-Weld™ EC-9323-2, under two aging conditions: (1) high-energy electron irradiation using a Van de Graaf accelerator, and (2) thermal vacuum cycling. The research evaluates the evolution of intrinsic adhesive properties and adhesion to CFRP (carbon fiber-reinforced polymer) and aluminum adherents before and after exposure to these environmental conditions through tensile tests, peel tests, double-cantilever beam (DCB) tests, and dynamic mechanical analysis (DMA).@en

The present study proposes a comprehensive integrity assessment approach for a full-scale adhesively-bonded bi-material joint for maritime applications. The joint represents a cross-section of the bond-line connection of a ship with a steel hull and a sandwich composite superstructure. The full-scale joint consists of a sandwich composite core adhesively bonded to two U-shaped steel brackets. The joint was subjected to a quasi-static loading profile including 6 load cycles up to the final failure. Each load cycle was followed by a dwell segment holding the joint at the maximum displacement for 30 s and then unloading to 50% of the maximum displacement. Three Structural Health Monitoring (SHM) techniques including Acoustic Emission (AE), Fiber Optic Sensor (FOS), and Digital Image Correlation (DIC) were employed during the test to assess the damage state of the joint. Moreover, a Finite Element Model (FEM) was developed to simulate the evolution behavior of different damage mechanisms in the joint and the FE results were compared against the experimental findings. The obtained results showed that the integration of all the employed techniques could successfully detect the damage initiation, assess the severity of the damage, localize the critical regions of the joint, and distinguish the different damage mechanisms.

@en

Using fiber-reinforced composite patches for repairing damaged structures made of metal or/and concrete is an interesting and widely available solution on the market using synthetic materials. These repairing patches are bonded on the structures’ surfaces to increase their strength against internal stresses, as well as protect them from external physico-chemical attacks, thereby limiting crack propagation. Natural fibers offer a potential alternative to replacing glass or carbon fibers commonly used for bonded repair patches. Similarly, bio-based polymers represent an important sustainable alternative for partially or entirely replacing the petroleum-based polymers. In this study, an epoxy matrix reinforced with flax fiber is proposed as the material for the patches, and bonded to a steel plate using four different types of adhesive materials, including a castor-oil derived polyurethane resin. Floating roller peel tests were performed to assess the adhesion and viability of these new patches. The resulting peeling loads and fracture surface analysis are presented. Polyurethane demonstrates promising performance for epoxy-to-steel joints, but major improvements of the bio-based polyurethane application process and curing conditions may be necessary for its successful industrial implementation.@en

When a composite laminate is subjected to humidity, moisture diffusion occurs depending on the number and thickness of the lamina. Water diffusion changes the mechanical response of laminates and usually causes a significant reduction of the mechanical properties of the composite specimens in ocean structures. One of the most important mechanical properties of laminates is flexural stiffness which should be considered in the design procedure. Despite the extensive research on single cycle aging of composites, cyclic aging of these materials is less explored. The aim of the current research is to investigate the variation of mechanical properties of carbon fiber reinforced polymer (CFRP) and glass fiber reinforced polymer (GFRP) composites as a substrate in adhesive joints with the same initial flexural stiffness values subjected to cyclic wet/dry aging conditions for long-term structural applications. The matrix used in the CFRP and GFRP composites are based on epoxy and vinyl ester, respectively. Both unaged and cyclically aged samples were characterized by tensile and three-point bending tests. In order to simulate the moisture absorption condition of composites in adhesive joints, one side of the composite laminates was sealed with aluminum foils and three sides were exposed to humidity. The interaction between the composite thickness and the number of aging cycles was also investigated. The experimental results show that in cyclic aging condition, the reduction of flexural stiffness in CFRP is more than GFRP laminates and GFRP laminates is more suitable for ocean applications.

@en

Adhesive joints are frequently exposed to cyclic ageing conditions during their service life, which can have a substantial impact on the mechanical properties of both the adhesive and the substrates. The safe life philosophy, commonly employed in the design of bonded joints, underscores the importance of obtaining an accurate estimate of the adhesive's durability. Therefore, it is essential to enhance the predictive capabilities of the adhesive's mechanical behavior under cyclic ageing conditions. This research aims to expand the use of quasi-static cohesive zone modelling (CZM) for damage and fracture analysis of dissimilar adhesive joints subjected to cyclic ageing environments. The first step involved measuring the mechanical properties of the adhesive through tensile tests on unaged and cyclically aged dogbone specimens, considering their moisture content and ageing cycles. Based on the results, a degradable CZM was developed. To validate the numerical model, dissimilar double cantilever beam specimens (DCBs) of glass fibre reinforced polymer (GFRP) and aluminium were manufactured and tested before and after ageing. The load-displacement curves of the bi-materials bonded joints were successfully predicted using the developed model where the properties of the material are defined as a function of the moisture uptake and ageing cycles at each material element. The obtained results showed that after 4 ageing cycles, the maximum load of DCB specimens decrease considerably.

@en

Understanding the relationship between the sensors’ outputs and the damage evolution within the joints is becoming increasingly crucial to improving structural health monitoring systems and collecting data to improve the joint’s design. Therefore, a study of the acoustic emission method associated with visual fracture evaluation was proposed to give insights into the toughening of composite bonded joints and better understand the relationship between the acoustic emission features and the damage mechanism involved. Thus, two different layups were proposed for the substrates: [0]8 and [0/902/0]S. In addition, a toughened epoxy adhesive with an embedded carrier (AF163-2k) was used to bond the substrates. Five specimens of each stacking sequence were tested under quasi-static mode I loading conditions. A travelling microscope and a regular digital camera were used on the lateral sides of the specimens to track the crack propagation paths. One piezoelectric sensor linked to the AMSY-6 Vallen system was used to assess the acoustic emission features produced within the joints during the tests. Unsupervised machine learning algorithms based on artificial neural networks and the Morlet continuous wavelet transformation were used to pattern recognition of the acoustic emission data. Self-organising maps, together with k-means algorithms, were used for data clustering. Following that, the acoustic emission features of each cluster were associated with the insights obtained from the crack propagation images. Finally, it was observed that the different layups triggered simultaneous toughening mechanisms. The combination of the acoustic emission and the visual evaluation was crucial for a deeper understanding of the underlying phenomena.@en

Thicker bondlines along with manufacturing-tolerant and fracture-resistant adhesives are trends visible across different industries, especially maritime. In this work, two contrasting adhesives: an elastic-brittle epoxy-based, and a nonlinear-ductile methyl methacrylate (MMA) are characterized and compared via tensile, compact tension (CT) and double cantilever beam (DCB) testing, for steel-to-steel adherends. Significant differences are captured between the two bonding materials in terms of the energy required for crack growth: in the MMA “ductile” adhesive is ∼4 and 10 times more than for the epoxy “relatively brittle” adhesive for CT and DCB testing, respectively. While epoxy bondlines fail due to a symmetric in-plane crack, the MMA bondlines experience multiple cracking originating from high deformations and Poisson's effects. Moreover, in the case of MMA adhesive, the DCB testing led to plastic deformation of steel adherends. The existing evaluation protocols are adopted for data reduction and the effect of plastic dissipation is theoretically addressed. Despite adherend plasticity, it is concluded that the crack growth is driven by the elastic energy release, and thus, after small correction taking into account initial adherend plasticity, the existing simple models can still be used. This study highlights the potential use of ductile adhesive instead of the commonly used brittle ones to significantly improve the adhesively bonded joints in maritime applications in which thick bondlines, manufacturing-tolerant and fracture-resistance characteristics are required.

@en

The adhesive layer in the adhesive joints can experience different modes of loading. Although the fracture energy of adhesive is generally considered to be a material parameter, it is found to be a function of the joint configuration too. Thus, to accurately simulate the behaviour of bonded joints, it is recommended to obtain the fracture energy of the joints using the same substrate(s) as in real applications. In some applications, it is necessary to join dissimilar substrates using adhesives. However, for pure mode fracture tests it is essential to reach the desired loading mode even in a dissimilar joint. Not only the joint configuration but also the environmental conditions need to be considered in fracture tests. In this condition, due to the aging, the stiffness of substrates and adhesive layer might change, and as a result, the adhesive may experience a mixed-mode loading condition. The current study aims to investigate the variation of the mode mixity for dissimilar double cantilever beam adhesive joints with composite/metal substrates subjected to cyclic aging. At different stages of the aging cycles, the mode mixity was calculated during the test using displacement fields obtained by digital image correlation and based on the Williams series expansion. In addition, the variation of flexural stiffness of polymer matrix composite substrates after cyclic aging was investigated using a three-point bending test Finally, based on the variation of composite substrate flexural stiffness and using the finite element method, the variation of the mode-mixity ratio was calculated numerically and compared to the experimental results. The obtained results show that during the cyclic aging the moisture diffusion decreases flexural stiffness of polymer matrix composite substrates significantly, but the variation of substrate flexural stiffness deviates the mode mixity in the aged double cantilever beam specimens.

@en

Spacecrafts are subjected to very few mechanical loads but in the future with reusable spacecraft designed for interplanetary explorations and with the repetition of landing and take off, structures will be subjected to significant mechanical loads. The degradation due to space aging conditions, of the adhesive materials used as joints in space structure is not known yet for such a reusable spacecraft on long term exploration. Two adhesives used in spacecraft structures were investigated: Scotch-Weld EC-2216 and Scotch- WeldTM EC-9323-2. Those adhesives were exposed to two aging conditions from a space environment point of view: (1) electron irradiation using a Van de Graaf particle accelerator and (2) thermal vacuum cycling. Change in the adhesives properties was assessed before and after space environment exposure to understand related effect on their mechanical performance using CFRP and aluminium adherents, including, tensile tests, peel tests, double cantilever beam (DCB) tests, as well as evolution of their intrinsic properties by mean of dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC) and fourier transformed infrared spectroscopy (FTIR). It has been found that electron irradiation accelerates the completion of the curing reaction in EC-2216 and reduces fracture toughness, peel load, Young’s modulus, tensile strenght for both adhesives, which degrade adhesion integrity. The effects of thermal vacuum cycling on adhesives and adhesion differ, with certain attributes being reduced as Young Modulus, tensile strength or glass transition temperature and others being increased as fracture toughness. Effects of space environment are visible and very significant on these adhesives. The results of this study form a preliminary basis for long term prediction of adhesive bond behaviour in space. @en