Phase morphology of nanofibre interlayers: Critical factor for toughening carbon/epoxy composites

Electrospun thermoplastic nanofibres were employed to toughen carbon/epoxy composites by direct deposition on carbon fibre fabrics, prior to resin impregnation and curing. The toughening mechanism was investigated with respect to the critical role of phase morphology on the toughening effect in carbon/epoxy composites. The influences of solubility in epoxy and melting characteristics of thermoplastics were studied towards their effects on phase structure and delamination resistance. For the three different thermoplastic nanofibre interlayers used in this work, i.e. poly(ε-caprolactone) (PCL), poly(vinylidene fluoride) (PVDF) and polyacrylonitrile (PAN) nanofibre interlayers, only PCL nanofibres produced toughening. Although cylinder-shaped fibrous macrophases existed in all three interlayer regions, only PCL nanofibres had polymerisation-induced phase separation with epoxy, forming ductile thermoplastic-rich particulate microphases on the delamination plane. These findings clearly show that the polymerisation-induced phase separation is critical to the interlayer toughening by thermoplastic nanofibres. An optimal concentration (15 wt.%) of PCL solution for electrospinning was found to produce composites with enhanced mode I interlaminar fracture toughness (G_IC), stable crack growth and maintained flexural strength and modulus.     

Characterization of transverse tensile, interlaminar shear and interlaminate fracture in CF/EP laminates with 10 wt% and 20 wt% silica nanoparticles in matrix resins

The transverse tensile properties, interlaminar shear strength (ILSS) and mode I and mode II interlaminar fracture toughness of carbon fibre/epoxy (CF/EP) laminates with 10 wt% and 20 wt% silica nanoparticles in matrix were investigated, and the influences of silica nanoparticle on those properties of CF/EP laminates were characterized. The transverse tensile properties and mode I interlaminar fracture toughness (G_IC) increased with an increase in nanosilica concentration in the matrix resins. However, ILSS and the mode II interlaminar fracture toughness (G_IIC) decreased with increasing nanosilica concentration, especially for the higher nanosilica concentration (20 wt%). The reduced G_IIC value is attributed to two main competing mechanisms; one is the formation of zipper-like pattern associated with matrix microcracks aligned 45° ahead of the crack tip, while the other is the shear failure of matrix. The ratio of G_IIC/G_IC decreased with the concentration of silica nanoparticles, comparable with similar CF/EP laminates with dispersed CNTs in matrix. Fractographic studies showed that interfacial failure between carbon fibre and epoxy resin occurred in the neat epoxy laminate, whereas a combination of interfacial failure and matrix failure occurred in the nanosilica-modified epoxy laminates, especially those with a higher nanosilica concentration (20 wt%).     

On fracture toughness of nano-particle modified epoxy

A systematic study on the effects of silica and rubber nano-particles on the fracture toughness behavior of epoxy was conducted. Mode I fracture toughness (G_IC) of binary silica/epoxy, binary rubber/epoxy and ternary silica/rubber/epoxy nanocomposites with different particle weight fractions was obtained by compact tension tests. It is found that G_IC of epoxy can be significantly increased by incorporating either rubber or silica nano-particles. However, hybrid nanocomposites do not display any “synergistic” effect on toughness. Microstructures before and after fracture testing were examined to understand the role of nano-particles on the toughening mechanisms.     

Nanostructured systems based on SBS epoxidized triblock copolymers and well-dispersed alumina/epoxy matrix composites

In the present research, the effect of addition of (1 wt.% and 3 wt.%) alumina nanoparticles (Al₂O₃) to epoxy modified by poly(styrene-b-butadiene-b-styrene) (SBS) epoxidized triblock copolymer was studied. The microstructure of final hybrid composites was studied with atomic force microscopy (AFM). Composites showed homogeneously dispersed Al₂O₃ nanoparticles in the epoxy matrix containing polystyrene (PS) microphase separated nanodomains. Dynamic mechanical analyses (DMA), flexural and fracture toughness investigations were carried out. The glass transition temperature of epoxy matrix has been retained unchanged by the addition of Al₂O₃ nanoparticles. The nanostructured epoxy systems based on SBS epoxidized triblock copolymer and well-dispersed Al₂O₃ nanoparticles allowed an increase in fracture toughness maintaining the transparency and stiffness of neat epoxy.     

CF/EP composite laminates with carbon black and copper chloride for improved electrical conductivity and interlaminar fracture toughness

An experimental study was conducted to improve the electrical conductivity of continuous carbon fibre/epoxy (CF/EP) composite laminate, with simultaneous improvement in mechanical performance, by incorporating nano-scale carbon black (CB) particles and copper chloride (CC) electrolyte into the epoxy matrix. CF/EP laminates of 65 vol.% of carbon fibres were manufactured using a vacuum-assisted resin infusion (VARI) technique. The effects of CB and the synergy of CB/CC on electrical resistivity, tensile strength and elastic modulus and fracture toughness (K_IC) of the epoxy matrix were experimentally characterised, as well as the transverse tensile modulus and strength, Mode I and Mode II interlaminar fracture toughness of the CF/EP laminates. The results showed that the addition of up to 3.0 wt.% CB in the epoxy matrix, with the assistance of CC, noticeably improved the electrical conductivity of the epoxy and the CF/EP laminates, with mechanical performance also enhanced to a certain extent.     

Interlaminar fracture toughness and associated fracture behaviour of bead-filled epoxy/glass fibre hybrid composites

To investigate enhancement of matrix-dominated properties (such as interlaminar fracture toughness) of a composite laminate, two different bead-filled epoxies were used as matrices for the bead-filled epoxy/glass fibre hybrid composites. The plane strain fracture toughness of two different bead-filled epoxies have been measured using compact tension specimens. Significant increases in toughness were observed. Based on these results the interlaminar fracture toughness and fracture behaviour of hybrid composites, fabricated using bead-filled epoxy matrices, have been investigated using double cantilever beam and end notch flexure specimens for Mode I and Mode II tests, respectively. The hybrid composites based on carbon bead-filled matrix shows an increase in both G _IC initiation and G _IIC values as compared to a glass fibre reinforced plastic laminate with unmodified epoxy matrix. The optimum bead volume fraction for the hybrid composite is between 15% and 20%. However, the unmodified epoxy glass-fibre composite shows a higher G _IC propagation value than that of hybrid composites, due to fibre bridging, which is less pronounced in the hybrids as the presence of the beads results in a matrix-rich interply region.     

Electrospun nanofibre toughened carbon/epoxy composites: Effects of polyetherketone cardo (PEK-C) nanofibre diameter and interlayer thickness

Polyetherketone cardo (PEK-C) nanofibres were produced by an electrospinning technique and directly deposited on carbon fabric to improve the interlaminar fracture toughness of carbon/epoxy composites. The influences of nanofibre diameter and interlayer thickness on the Mode I delamination fracture toughness, flexure property and thermal mechanical properties of the resultant composites were examined. Considerably enhanced interlaminar fracture toughness has been achieved by interleaving PEK-C nanofibres with the weight loading as low as 0.4% (based on weight of the composite). Finer nanofibres result in more stable crack propagation and better mechanical performance under flexure loading. Composites modified by finer nanofibres maintained the glass transition temperature (T_g) of the cured resin. Increasing nanofibre interlayer thickness improved the fracture toughness but compromised the flexure performance. The T_g of the cured resin deteriorated after the thickness increased to a certain extent.     

A two-parameter approach to assessing notch fracture behaviour in clay/epoxy nanocomposites

Fracture toughness and other mechanical properties of epoxy are known to be affected by the addition of nanoclays. Fracture toughness has been shown by many researchers to depend on the nanocomposite structure with well-dispersed and distributed nanoparticles resulting in improvements in this property by up to 50%. Notch fracture toughness depends on the acuity of the notch as well as on the structure of the nanocomposite. In the present work, a two-parameter fracture criterion based on a critical notch stress intensity factor, K_ρ,c, and effective T-stress, T_ef, was used to study the effect of notch severity and nanoclay addition on the fracture toughness of the epoxy matrix. The results show that the average value of K_ρ,c for neat epoxy increased with increasing notch radius while the absolute value of T_ef decreased with notch radius. The addition of nanoclay to pristine epoxy reduced the average value of K_ρ,c and increased the absolute value of T_ef. The critical notch radius was found to be around 1.0 mm and the notch sensitivity was higher for neat epoxy. SEM analysis of the fractured surfaces revealed that the lower K_ρ,c for nanocomposites in both mode I and mixed mode fractures was due to early crack initiation at clay clusters or voids at the notch root.     

Microstructure and mechanical properties of titanium carbonitride whisker reinforced β-sialon matrix composites

The microstructure, hardness, fracture toughness and thermal shock resistance were investigated for 15 vol.% TiC_0.3N_0.7 whisker reinforced β-sialon (Si_6−zAl_zO₂N_8−z with z=0.6) composites with additions of three different volume fractions 2, 5 and 20 vol.%, of an yttrium-containing glass oxynitride phase. The composites were prepared by hot pressing at 1750°C for 90 min under a uniaxial pressure of 30 MPa in nitrogen atmosphere. The TiC_0.3N_0.7 whiskers were found to survive without deteriorating in morphology or reacting with the β-sialon matrix and/or the glass phase. The TiC_0.3N_0.7 whiskers had no obvious influence on the matrix microstructure, but their presence improved both the hardness and the fracture toughness of the composites. The highest hardness was obtained for the whisker composite with 2 vol.% glass phase (H_v=18.6 GPa). The fracture toughness and thermal shock resistance improved with increasing glass content. The whisker reinforced composite containing 20 vol.% glass showed the highest fracture toughness (K_1C=6.8 MPa m^1/2). No unstable crack extension occurred during the thermal shock test of the obtained composites in the temperature interval 90-700°C, but above 700°C severe oxidation of the whiskers precludes further evaluation of thermal shock properties by the indentation-quench method applied.     

Influence of thermoplastic diffusion on morphology gradient and on delamination toughness of RTM-manufactured composites

We explore the influence of the interdiffusion of two thermoplastic tougheners and RTM6 epoxy resin precursors on the resulting morphologies after curing and the consequences on delamination toughness of the corresponding carbon fiber reinforced composites. Two thermoplastics with contrasting T_g and compatibility, i.e. poly(ether sulfone) (PES) and phenoxy are compared. The dramatic improvement of the interlaminar fracture toughness (G_IC) found for the phenoxy-RTM6 system as compared to the pure thermoset reference can be ascribed to the broad morphology gradient only observed for that system. By contrast, the PES-RTM6 system is characterized by a steep morphology gradient and a corresponding decrease of as compared to the reference.     

Temperature dependence of fracture toughness of silica/epoxy composites: Related to microstructure of nano- and micro-particles packing

Temperature dependence of the fracture toughness of epoxy composites reinforced with nano- and micro-silica particles was evaluated. Epoxy composites containing varied composition ratios Φ_SP of spherical nano- and micro-silica particles, 240 nm and 1.56 μm, were prepared at a fixed volume fraction (V_P = 0.30). The thermo-viscoelasticity and fracture toughness of the composites and neat epoxy were measured at 143 K, 185 K, 228 K, 296 K, 363 K, and 399 K. Experimental results revealed that fracture toughness strongly depended on the microstructure of nano- and micro-particles bidispersion as well as its interactions with the matrix at all temperature, but depended on toughened matrix due to increase in mobility of matrix at the relaxation temperatures.     

Structure property relation of hybrid biocomposites based on jute,viscose and polypropylene: The effect of the fibre content and the length on the fracture toughness and the fatigue properties

In the present study, the extent of jute and viscose fibre breakage during the extrusion process on the fracture toughness and the fatigue properties was investigated. The composite materials were manufactured using direct long fibre thermoplastic (D-LFT) extrusion, followed by compression moulding. The fracture toughness (K_IC) and the fracture energy (G_IC) of the PP–J30 composites were significantly improved (133% and 514%, respectively) with the addition of 10 wt% viscose fibres, indicating hindered crack propagation. The addition of viscose fibres resulted in three times higher fatigue life compared with that of the unmodified jute composites. Further, with the addition of (2 wt%) MAPP, the PP–J30–V10 resulted in a higher average viscose fibre length of 8.1 mm, and the fracture toughness and fracture energy increased from 9.1 to 10.0 MPa m^1/2 and 28.9 to 31.2 kJ/m², respectively. Similarly, the fatigue life increased 51% compared with the PP–J30–V10, thus demonstrating the increased work energy due to hindrance of the propagation of cracks.     

Enhancement of fracture toughness,mechanical and thermal properties of rubber/epoxy composites by incorporation of graphene nanoplatelets

Carboxyl terminated butadiene acrylonitrile (CTBN) was added to epoxy resins to improve the fracture toughness, and then two different lateral dimensions of graphene nanoplatelets (GnPs), nominally <1 μm (GnP-C750) and 5 μm (GnP-5) in diameter, were individually incorporated into the CTBN/epoxy to fabricate multi-phase composites. The study showed that GnP-5 is more favorable for enhancing the properties of CTBN/epoxy. GnPs/CTBN/epoxy ternary composites with significant toughness and thermal conductivity enhancements combined with comparable stiffness to that of the neat resin were successfully achieved by incorporating 3 wt.% GnP-5 into 10 wt.% CTBN modified epoxy resins. According to the SEM investigations, GnP-5 debonding from the matrix is suppressed due to the presence of CTBN. Nevertheless, apart from rubber cavitation and matrix shear banding, additional active toughening mechanisms induced by GnP-5, such as crack deflection, layer breakage and separation/delamination of GnP-5 layers contributed to the enhanced fracture toughness of the hybrid composites.     

Cryogenic mechanical behaviors of carbon nanotube reinforced composites based on modified epoxy by poly(ethersulfone)

Cryogenic mechanical properties are important parameters for epoxy resins used in cryogenic engineering areas. In this study, multi-walled carbon nanotubes (MWCNTs) were employed to reinforce diglycidyl ether of bisphenol F (DGBEF)/diethyl toluene diamine (DETD) epoxy system modified by poly(ethersulfone) (PES) for enhancing the cryogenic mechanical properties. The epoxy system was properly modified by PES in our previous work and the optimized formulation of the epoxy system was reinforced by MWCNTs in the present work. The results show that the tensile strength and Young’s modulus at 77 K were enhanced by 57.9% and 10.1%, respectively. The reported decrease in the previous work of the Young’s modulus of the modified epoxy system due to the introduction of flexible PES is offset by the increase of the modulus due to the introduction of MWCNTs. Meanwhile, the fracture toughness (K_IC) at 77 K was improved by about 13.5% compared to that of the PES modified epoxy matrix when the 0.5 wt.% MWCNT content was introduced. These interesting results imply that the simultaneous usage of PES and MWCNTs in a brittle epoxy resin is a promising approach for efficiently modifying and reinforcing epoxy resins for cryogenic engineering applications.     

Short-fiber/particle hybrid reinforcement: Effects on fracture toughness and fatigue crack growth of metal matrix composites

We have studied the effects of short-fiber/particle hybrid reinforcement on fracture toughness and fatigue crack growth in metal matrix composites. Reinforcement hybridization was achieved by a hybrid preform process, and composites were fabricated by the squeeze casting method. Al6061 matrix alloy and four composites having different short-fiber/particle ratio were tested. The fracture toughness (K_IC) and the fatigue threshold (ΔK_th) increased with increasing particle contents, whereas the Paris’ exponent (m) was insensitive to the short-fiber:particle ratio. These results emerged as a shift of the crack growth curve which implies on enhanced crack resistance over the entire stress intensity factor range. The positive aspect of particulate reinforcement is advocated by comparison of microstructural variables, and by observation of the crack path and surfaces. The characteristics of hybrid composites in damage tolerance are emphasized.     

Effect of fibre content on the interlaminar fracture toughness of unidirectional glass-fibre/polyamide composite

In this paper, the effects of fibre content on the interlaminar fracture in continuous glass-fibre/polyamide 12 composite have been investigated under model I (DCB) loading condition. The specimens were fabricated with different fibre volume contents (21%, 26%, 34% and 39%) by using a powder impregnation method. It was observed that the values of G_IC(NL) and G_IC(PROP) of this material have a dropping tendency with increasing fibre volume content in the range of 21%–39%, while no general trends in G_IC(5%) and G_IC(VIS). Results show that the glass-fibre/polyamide 12 composites possess high mode I fracture toughness, which is mainly attributed to the high ductility of the polyamide 12 matrix, and the increased fibre bridging caused by the increasing of the fibre volume content can not change the decrease tendency of G_IC(PROP). The fracture surfaces of the specimens were observed by scanning electron microscopy, and the fracture mechanism was analysed.     

Controlling fracture toughness of matrix for ductile fiber reinforced cementitious composites

An experimental study was carried out to find material parameters for making fiber reinforced cementitious composites (FRCC) more ductile. One of the dominant factors to control the ductility might be hidden in fracture property of matrix as well as the interface property between fiber and matrix. Therefore this study varied air content and water-binder ratio as the parameters to change the fracture property of matrix and experimentally examined their influence on the ductility of FRCC by three-point bend test with notched beams. As a result, it is concluded that fracture toughness of the matrix could be one of key parameters to control the ductility of FRCC. In case of a polyethylene fiber used in this study, the optimum value of the fracture toughness (critical strain energy release rate): G_IC of the matrix was obtained to be 7.5-8.0 N/m.     

Improvement of tensile properties and toughness of an epoxy resin by nanozirconium-dioxide reinforcement

Zirconium dioxide (ZrO₂) nanoparticles were systematically added as reinforcement to a diglycidyl ether of bisphenol A (DGEBA)-based epoxy resin. A series of composites with varying amounts of nanoparticles was prepared and their morphology and mechanical properties were studied. The obtained nanocomposites were characterized by tensile tests, dynamic mechanical thermal analysis, and fracture toughness (K_IC) investigations; by standardized methods, to define the influence of the nanoparticle content on their mechanical and thermal properties. The morphological analysis of the composites shows that nanoparticles form small clusters, which are uniformly distributed into the matrix bulk. The tensile modulus (E) and the K_IC of the epoxy matrix increase at rising zirconia content. Improvements of more than 37% on modulus and 100% on K_IC were reached by the nanocomposite containing 10 vol.-% ZrO₂ with respect to the neat epoxy (E_o = 3.1 GPa, K_ICo = 0.74 MPam^0.5). The presence of nanoparticles produces also an increment on glass transition temperature (T _g). The epoxy resin added with 8 vol.-% ZrO₂ records a T _g approximately 8% higher than the unmodified matrix (T _go = 100.3 °C).     

Multiscale carbon fibre–reinforced polymer (CFRP) composites containing carbon nanotubes with tailored interfaces

Pristine and functionalized multiwalled carbon nanotubes (MWCNTs) with tailored interfaces were efficiently dispersed in an epoxy matrix using a three‐roll mill and further reinforced with carbon fibres. 1.3‐Dipolar cycloaddition of azomethine ylides was used for the chemical modification of MWCNTs by a solvent‐free approach. The influence of different loadings and types of MWCNTs on the final properties of the epoxy matrix was studied. Moreover, the most promising formulations were selected for manufacturing of prepreg sheets. The transversal tensile properties and the interlaminar fracture toughness under mode I loading (G_IC) of multiscale carbon fibre–reinforced polymer (CFRP) composites were characterized. The results point out that it is not straightforward to transfer the remarkable intrinsic properties of MWCNTs to the composite level, although an overall positive trend was found. Double cantilever beam experiments showed that G_IC of CFRP composites was improved 44% at ultralow content of functionalized MWCNTs (0.043 wt%).     

Fracture mechanisms of epoxy filled with ozone functionalized multi-wall carbon nanotubes

This work focused on the fracture mechanisms and reinforcing effects of ozone-treated multi-walled carbon nanotubes (MWCNTs) in epoxy matrix. Ozone functionalization of MWCNTs was found to be of help for a better dispersion and stronger interfacial bonding with epoxy matrix, which in turn improve the strength and fracture toughness of the resin. The MWCNT/epoxy composites showed complicated failure modes than the conventional fibrous composites, which have been quantitatively investigated and correlated with the fracture toughness of the nanocomposites studied.