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.     

Mode I and Mode II interlaminar fracture toughness of composite laminates interleaved with electrospun nanofibre veils

In this study, the effects of interleaved nanofibre veils on the Mode I and Mode II interlaminar fracture toughness (ILFT) of autoclave cured unidirectional carbon/epoxy composite laminates were investigated. Various electrospun nanofibre veils consisting of a range of different polymer types, fibre diameters and veil architectures were placed in the laminate mid-planes, which were subsequently subjected to double cantilever beam and end-notch flexure tests. It was found that the polymer type and veil areal weight were the most important factors contributing to laminate performance. A 4.5 g/m² PA66 veil provided the best all-round performance with fracture toughness improvements of 156% and 69% for Mode I and Mode II, respectively.     

Improving the interlaminar properties of polymer composites using a situ accumulation method to construct the multi-scale reinforcement of carbon nanofibers/carbon fibers

A novel method was developed to realize the situ accumulation of carbon nanofibers (CNFs) in the carbon fiber reinforced polymer composites (CFRPs) to construct the multi-scale reinforcement for improving the interlaminar properties. In this method, the prepreg was sealed by the nanomicroporous nylon membrane, and the excess resin was extracted from the prepreg by the vacuum-assisted method. It was found that the use of nylon membrane resulted in effective CNFs accumulation, especially in the interlayer by scanning electron microscopy. Short-beam strength tests and the end-notched flexure tests were conducted respectively to evaluate the interlaminar properties of CFRPs under shear loading. The results indicated that the interlaminar shear strength (ILSS) and the Mode II interlaminar fracture toughness (G_IIC) of CFRPs made by the filtering membrane-assisted method remarkably increased compared with those prepared without using filtering membrane.     

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.     

PEK-C膜层间增韧碳纤维/环氧树脂复合材料的力学性能

为探究热塑性酚酞基聚醚酮（Polyaryletherketone with Cardo,PEK-C）树脂薄膜及膜厚对层间增韧碳纤维/环氧树脂复合材料力学性能的影响,利用浸渍提拉法制备了三种不同厚度（分别约为1 μm、10 μm、30 μm）的PEK-C膜,通过热压成型制备了层间增韧碳纤维/环氧树脂复合材料层合板,对其进行了Ⅰ型层间断裂韧性、冲击后压缩强度、层间剪切及弯曲性能测试,并利用SEM观察微观形貌及AFM扫描微观相图。结果表明:不同PEK-C膜厚增韧碳纤维/环氧树脂复合材料的Ⅰ型层间断裂韧性、冲击后压缩强度及层间剪切强度有不同程度提高,Ⅰ型层间断裂韧性及层间剪切强度以膜厚为10 μm最佳,分别增大了157.17%和17.57%,冲击后压缩强度以膜厚为30 μm最佳,达到了186.67 MPa,这是由于PEK-C与环氧树脂在热压固化过程中形成了双相结构,改善了材料韧性;但弯曲性能持续下降,强度及模量由未增韧的1 551 MPa、106 GPa分别降至30 μm时的965 MPa、79 GPa,这是由于PEK-C树脂扩散进入环氧树脂中,降低了纤维体积分数及材料刚度。      

Synergistic effects of PEK-C/VGCNF composite nanofibres on a trifunctional epoxy resin

Polyetherketone cardo (PEK-C) nanofibres containing vapour-grown carbon nanofibres (VGCNFs) were electrospun, and used for toughening and reinforcing a triglycidyl amino phenol (TGAP) epoxy resin. The addition of PEK-C/VGCNF nanofibres to the epoxy resin led to the distribution of VGCNFs primarily within the phase separated PEK-C-rich domains. Synergistic effects of thermoplastic PEK-C and VGCNFs on the mechanical properties, phase morphologies and thermal stability of the resultant epoxy matrix composites were observed when the PEK-C/CNF nanofibres were blended at a low content into the epoxy resin. Strong and tough multifunctional nanocomposites were prepared with the addition of 5 wt.% PEK-C/CNF nanofibres to the epoxy matrix.     

Electric field effects on CNTs/vinyl ester suspensions and the resulting electrical and thermal composite properties

In this study, electrical conductivity of a vinyl ester based composite containing low content (0.05, 0.1 and 0.3 wt.%) of double and multi-walled carbon nanotubes with and without amine functional groups (DWCNTs, MWCNTs, DWCNT-NH₂ and MWCNT-NH₂) was investigated. The composite with pristine MWCNTs was found to exhibit the highest electrical conductivity. Experiments aimed to induce an aligned conductive network with application of an alternating current (AC) electric field during cure were carried out on the resin suspensions with MWCNTs. Formation of electric anisotropy within the composite was verified. Light microscopy (LM), scanning electron (SEM) and transmission electron microscopy (TEM) were conducted to visualize dispersion state and the extent of alignment of MWCNTs within the polymer cured with and without application of the electric field. To gain a better understanding of electric field induced effects, glass transition temperature (T_g) of the composites was measured via Differential Scanning Calorimetry (DSC). It was determined that at 0.05 wt.% loading rate of MWCNTs, the composites, cured with application of the AC electric field, possessed a higher T_g than the composites cured without application of the AC electric field.     

Thermoplastic polymer impregnation of cellulose nanofibre networks: Morphology,mechanical and optical properties

Biobased nanocomposite sheets of cellulose nanofibres (CNF) and cellulose acetate butyrate (CAB) were prepared using resin impregnation. Porous nanofibre networks together with a low viscosity thermoplastic resin were the key elements in the processing. SEM images of the network before the impregnation showed high porosity and after the impregnation indicated impregnated fibre network. A significant improvement in the visible light transmittance was observed for the nanocomposite compared to the nanofibre network, which is explained on the filling of the pores with a transparent matrix. The tensile tests showed an increase of 364% and 145% for stiffness and strength respectively for nanocomposites with 60 wt.% CNF when compared to CAB. Dynamic mechanical properties showed a good interaction between the CAB and cellulose nanofibres. These results show that CAB impregnated cellulose nanofibre networks are promising biocomposite that could be used in applications where transparency and good mechanical properties are of interest.     

Mode I interlaminar fracture behavior and mechanical properties of CFRPs with nanoclay-filled epoxy matrix

The mechanical properties and fracture behavior of nanocomposites and carbon fiber composites (CFRPs) containing organoclay in the epoxy matrix have been investigated. Morphological studies using TEM and XRD revealed that the clay particles within the epoxy resin were intercalated or orderly exfoliated. The organoclay brought about a significant improvement in flexural modulus, especially in the first few wt% of loading, and the improvement of flexural modulus was at the expense of a reduction in flexural strength. The quasi-static fracture toughness increased, whereas the impact fracture toughness dropped sharply with increasing the clay content.Flexural properties of CFRPs containing organoclay modified epoxy matrix generally followed the trend similar to the epoxy nanocomposite although the variation was much smaller for the CFRPs. Both the initiation and propagation values of mode I interlaminar fracture toughness of CFRP composites increased with increasing clay concentration. In particular, the propagation fracture toughness almost doubled with 7 wt% clay loading. A strong correlation was established between the fracture toughness of organoclay-modified epoxy matrix and the CFRP composite interlaminar fracture toughness.     

Experimental investigation on test methods for mode II interlaminar fracture testing of carbon fiber reinforced composites

In this paper, experimental investigation on the test methods for mode II interlaminar fracture testing of carbon fiber reinforced composites are carried out. Mode II interlaminar fracture testing of unidirectional composite of carbon fiber reinforced epoxy (T800/#3631) are conducted using four kinds of test methods, namely end notched flexure (ENF) test, end loaded split (ELS) test, four-point bend end notched flexure (4ENF) test, and over notched flexure (ONF) test. An analytical model based on a point-friction assumption and classical beam theory is proposed to evaluate the effect of friction between crack faces on the mode II interlaminar fracture toughness in the 4ENF and ONF tests. The analytical model is validated by the comparison of analytical results with previous ones obtained from finite element analysis. Experimental results show that the ENF test gives reliable initiation value of fracture toughness with a small scatter and that the average value of fracture toughness obtained from 4ENF test is about 2% higher than that obtained from the ENF test. The effect of friction in the 4ENF test is much lower than that in the ONF test in which the effect of friction increases with the crack growing. It is concluded that the 4ENF test method is an effective test method for the experimental evaluation of mode II propagation interlaminar fracture toughness of carbon fiber reinforced composites.     

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.     

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.     

Mode II interlaminar fracture properties of Moso bamboo

Bamboo is a kind of biological composites reinforced by unidirectional long fiber. Once there exists crack, the propagation of delamination is controlled by the interlaminar fracture toughness instead of by strength. In this paper, the end notched flexure (ENF) beam specimen was used to test the Mode II interlaminar fracture toughness G_IIC along grain of Moso bamboo internode and the fracture surface was analyzed. The results were obtained that the Mode II interlaminar fracture toughness G_IIC calculated by the experiment parameter substitution method was more accurate and the value was 1303.18 J/m² (coefficient of variation = 8.96%) which was about three times higher than the value of Mode I interlaminar fracture toughness; the crack propagation of Mode II interlaminar fracture was mainly self-similar cracking, but the fracture surface was rougher. Ground tissue in the zone of Mode II crack propagation was characterized by hackle shearing deformation. The SEM photos showed that ground tissue separated from fiber along middle lamella under shear stress and as the increasing of the dislocation of upper and lower layer, the thin-walled ground tissue would fracture transversely by tension, while to thick-walled fiber cell, only middle lamella and primary wall were torn then debonded, fragments remained.     

Improvement of interlaminar mechanical properties of CFRP laminates using VGCF

In order to improve the interlaminar mechanical properties of CFRP laminates, hybrid CFRP/VGCF laminates have been fabricated by using a newly-developed method, i.e., powder method, where the powder of vapor grown carbon fiber (VGCF) is added at the mid-plane of [0°/0°]₁₄ CFRP laminates. Experimental results of double cantilever beam (DCB) tests indicate the improvement on the interlaminar mechanical properties of Mode-I fracture behavior with much higher critical load P_C and fracture toughness G_IC with VGCF interlayer. Crack propagation and fracture surface have also been observed to interpret this improvement mechanism. Moreover, based on experimental G_IC, numerical simulations using finite element method (FEM) with cohesive elements have been carried out to analyze the delamination propagation. The interlaminar tensile strength of hybrid CFRP/VGCF laminates, which is obtained by matching the numerical load–COD (crack opening displacement) curves to experimental ones, is higher than that of base CFRP laminates.     

Influence of cobalt phase on thermal shock resistance of Al2O3-TiC composites evaluated by indentation technique

Cobalt-coated Al₂O₃ and TiC powders were prepared using an electroless method to improve resistance to thermal shock. The mixture of cobalt-coated Al₂O₃ and TiC powders (about 70 wt.% Al₂O₃-Co + 30 wt.% TiC-Co) was hot-pressed into an Al₂O₃-TiC-Co composite. The thermal shock properties of the composite were evaluated by indentation technique and compared with the traditional Al₂O₃-TiC composite. The composites containing 3.96 vol.% cobalt exhibited better resistance to crack propagation, cyclic thermal shock and higher critical temperature difference (ΔT_c). The calculation of thermal shock resistance parameters (R parameters) shows that the incorporation of cobalt improves the resistance to thermal shock fracture and thermal shock damage. The thermal physic parameters are changed very little but the flexure strength and fracture toughness of the composites are improved greatly by introducing cobalt into Al₂O₃-TiC (AT) composites. The better thermal shock resistance of the composites should be attributed to the higher flexure strength and fracture toughness.     

热塑性树脂含量对CCF800H碳纤维环氧复合材料Ⅰ型层间断裂韧度的影响

采用国产CCF800H高强中模碳纤维增强环氧制备了复合材料,研究不同热塑性树脂含量对复合材料张开(Ⅰ)型层间断裂韧度的影响,研究表明:随着热塑组分含量的提高,复合材料的裂纹起始应变能量释放率(GⅠC-init)与裂纹稳态扩展应变能量释放率(GⅠC-prop)都获得了大幅度提升,在增韧组分质量分数大于20%时,增韧聚芳醚酰亚胺粉体可在复合材料层间富集形成层间高韧区,并在复合材料层间形成了由"连续相"和"分散相"组成的层间增韧结构。     

Effect of variation in fibre volume fraction on modes I and II delamination behaviour of 5HS woven composites manufactured by RTM

Composites produced by resin infusion techniques will inevitably suffer from variation in resin distribution due to imprecise fibre placement and distortion of the preform during mould closure and infusion. This paper describes an investigation into the effect of variations in fibre volume fraction (FVF) on mode I and mode II delamination behaviour for 5 harness satin (5HS) woven carbon–fibre/epoxy resin composites manufactured by resin transfer moulding (RTM). Additionally, the effect of satin face tow orientation on interlaminar toughness was investigated. In mode I, it was found that toughness increased with increasing FVF and that a strong correlation between fracture surface damage and measured interlaminar fracture toughness was observed. In mode II, measured toughness values were higher than expected and tests were repeated using a mixed-mode rig with 5% mode I. It was found that fracture toughness measurements in pure mode II are significantly affected by friction or mechanical interlocking between the delamination surfaces.     

Multiscale molecular modeling of SWCNTs/epoxy resin composites mechanical behaviour

Atomistic and mesoscale simulations were conducted to estimate the effect of the diameter and weight fraction of single walled carbon nanotubes (SWCNTs) on mechanical behaviour and glass transition temperature (T_g) of SWCNTs reinforced epoxy resin composites. Atomistic periodic systems of epoxy resin and epoxy resin/SWCNTs were built with different weight ratios and were subject of an extensive multistage equilibration procedure. Molecular dynamics simulations were used to estimate glass transition temperature, Young modulus and solubility parameter of epoxy resin and epoxy resin/SWCNTs composites. Dissipative particle dynamics method and Flory–Huggins theory was employed to predict epoxy resin/SWCNTs morphologies. The results show that incorporation of SWCNTs with diameters ranging from 10 to 14 ? has beneficial effect on mechanical integrity and T_g. Overall, the agreement between predicted material properties and experimental data in the literature is very satisfactory.     

Multiscale molecular modeling of SWCNTs/epoxy resin composites mechanical behaviour

Atomistic and mesoscale simulations were conducted to estimate the effect of the diameter and weight fraction of single walled carbon nanotubes (SWCNTs) on mechanical behaviour and glass transition temperature (T_g) of SWCNTs reinforced epoxy resin composites. Atomistic periodic systems of epoxy resin and epoxy resin/SWCNTs were built with different weight ratios and were subject of an extensive multistage equilibration procedure. Molecular dynamics simulations were used to estimate glass transition temperature, Young modulus and solubility parameter of epoxy resin and epoxy resin/SWCNTs composites. Dissipative particle dynamics method and Flory–Huggins theory was employed to predict epoxy resin/SWCNTs morphologies. The results show that incorporation of SWCNTs with diameters ranging from 10 to 14 Ǻ has beneficial effect on mechanical integrity and T_g. Overall, the agreement between predicted material properties and experimental data in the literature is very satisfactory.     

Poly(ether ether ketone) with pendent methyl groups as a toughening agent for amine cured DGEBA epoxy resin

A diglycidyl ether of bisphenol-A (DGEBA) epoxy resin was modified with poly(ether ether ketone) with pendent methyl groups (PEEKM). PEEKM was synthesised from methyl hydroquinone and 4,4′-difluorobenzophenone and characterised. Blends of epoxy resin and PEEKM were prepared by melt blending. The blends were transparent in the uncured state and gave single composition dependent T _g. The T _g-composition behaviour of the uncured blends has been studied using Gordon–Taylor, Kelley–Bueche and Fox equations. The scanning electron micrographs of extracted fracture surfaces revealed that reaction induced phase separation occurred in the blends. Cocontinuous morphology was obtained in blends containing 15 phr PEEKM. Two glass transition peaks corresponding to epoxy rich and thermoplastic rich phases were observed in the dynamic mechanical spectrum of the blends. The crosslink density of the blends calculated from dynamic mechanical analysis was less than that of unmodified epoxy resin. The tensile strength, flexural strength and modulus were comparable to that of the unmodified epoxy resin. It was found from fracture toughness measurements that PEEKM is an effective toughener for DDS cured epoxy resin. Fifteen phr PEEKM having cocontinuous morphology exhibited maximum increase in fracture toughness. The increase in fracture toughness was due to crack path deflection, crack pinning, crack bridging by dispersed PEEKM and local plastic deformation of the matrix. The exceptional increase in fracture toughness of 15 phr blend was attributed to the cocontinuous morphology of the blend. Finally it was observed that the thermal stability of epoxy resin was not affected by the addition of PEEKM.