Prestandardization study on mode II interlaminar fracture toughness test for cfrp in japan

A three year long cooperative research programme has been carried out to establish a Japanese standard for an interlaminar fracture toughness test method for CFRPs. For mode II fracture toughness tests, the end-notched flexure test was employed. Two series of round robin tests (RRTs) were carried out using conventional brittle epoxy CFRPs, a toughened epoxy CFRP and APC-2. The following points became clear in the investigation: 1) crack shear displacement measurement gives precise information on crack initiation; 2) the fracture toughness values at the start of non-linear behaviour showed a considerably large scatter; 3) the toughness at the 5% offset points has a lower scatter and is still conservative; and 4) it is necessary to take account of the increase in crack length for the toughness calculation after the 5% offset point. Considering this information, together with other important observations obtained in the RRTs, a proposal for the mode II fracture toughness test was made and it was established as Japanese Industrial Standard K 7086 in March 1993.     

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%).     

Influence of clamping method on tensile properties of unidirectional CFRP in 0° and 90° directions — round robin activity for international standardization in Japan

This paper summarizes round robin tests performed in four laboratories with two specific aims: first, to establish the reproducibility of values from 0° and 90° tests of unidirectional carbon fibre-reinforced plastic laminates carried out on two materials in different laboratories; second, to investigate the effects of tab design and gripping condition on tensile properties. The strength of the carbon fibres used was about 6 GPa, these fibres being chosen to determine the applicability of the test method to high strength composites. The matrices used were a relatively brittle epoxy and a toughened epoxy. Statistical analysis was carried out to verify the results. For the case of 0° tests, two tab shapes were compared. No significant difference was observed between square cut tabs and tapered tabs. For the case of 90° tests, tab materials and gripping condition were compared. Specimens with glass fibre-reinforced plastic tabs broke at the end of tabs, and gave lower strength. Specimens with rubber tabs and tabless specimens with abrasive paper inserts broke within the gauge section, and gave higher strength.     

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 of Carbon Fibre‐Reinforced Polymer Laminates With Nano‐ and Micro‐Fillers

Abstract: Vapour growth carbon nanofibres (CNF) and lead zirconate titanate (PZT) piezoelectric particles were added in the matrix of carbon fibre‐reinforced polymer laminates. The fracture toughness of the modified composites was measured under mode I and mode II loading and compared with plain epoxy carbon fibre‐reinforced composites. The mode I fracture toughness of the composites improved with the incorporation of the carbon nanofibres and deteriorated with the incorporation of PZT piezoelectric particles. When both fillers were added in the composite matrix, the mode I fracture toughness improved but to a lesser extend. The mode II fracture toughness of the modified composites was improved in all three cases. The aforementioned behaviour was attributed to competing fracture mechanisms instigated by the different fillers, and backed by fractographic evidence from the failed composite coupons; during the tests, the acoustic emission activity of the coupons was monitored and classified in three major energy absorbing mechanisms which were attributed to the failure of distinct composite phases.     

Improving interlaminar fracture toughness of carbon fibre/epoxy laminates by incorporation of nano-particles

Double-cantilever-beam tests were applied to investigate the mode I interlaminar fracture toughness of carbon fibre/epoxy laminates, in which the epoxy matrices were incorporated with rubber and silica nano-particles, either singly or jointly. It is shown that the toughness is improved owing to the presence of these nano-particles although nano-rubber is more effective than nano-silica. Further, by keeping the total particle weight percentage constant in epoxies (e.g., at 8 and 12 wt.%) filled with equal amount of nano-silica and nano-rubber, the interlaminar toughness values of the hybrid laminates are always higher than those with nano-silica filled epoxies but lower than those with nano-rubber filled matrices. Scanning electron microscopy examination of the delaminated surfaces of composite laminates filled with nano-particles revealed that cavitation of nano-rubber particles/void growth and debonding of nano-silica from epoxy matrix are responsible for the improved interlaminar toughness observed. It is also shown that the bulk toughness of nano-particle filled epoxies cannot be fully transferred to the interlaminar toughness of composite laminates, being limited by the constraint effect imposed by the carbon fibres. Finally, the role of fibre-bridging on the delaminated crack and hence delamination toughness is discussed.     

Monitoring of delamination onset and growth during Mode I and Mode II interlaminar fracture tests using guided waves

A delamination monitoring method was proposed to characterize Mode I and Mode II delamination onset in carbon fiber/epoxy (CF/EP) composite laminates through interrogation of guided waves activated and captured using piezoelectric actuators and sensors in a pitch–catch configuration. Mode I and Mode II interlaminar fracture tests were conducted using double cantilever beam (DCB) and end notch flexure (ENF) specimens to evaluate the proposed method. The changes in wave propagation velocity and wave magnitude (or attenuation), and the degree of waveform similarity between excitation and response signals, were calculated as delamination-sensitive wave parameters and plotted versus displacement recorded using a materials testing system. The kink points determined from wave parameter–displacement curves agreed well with the deviation from linearity (NL), visual observation (VIS) and maximum load (Max) points, which are often used in conventional methods for determining interlaminar fracture toughness. The propagation characteristics of the A₀ wave mode in a low frequency range were demonstrated to have high sensitivity to Mode I and in particular Mode II delamination onset in CF/EP composite laminates. It was concluded that the guided waves propagating in the DCB and ENF specimens were capable of determining Mode I and Mode II interlaminar fracture toughness, complementing current practices based on visual inspection or trivial interrogation using load–displacement curve alone.     

Role of Interface Modification on the Mode I and Mode II Fracture Behavior of Glass Fabric / Vinyl Ester Composites

The objective of this study was to determine the influence of five different combinations of silane coupling agents on the Mode I and Mode II fracture toughness and strength of woven glass fabric / vinyl ester composite laminates. Double Cantilever Beam (DCB) and End Notch Flexure (ENF) tests were conducted to estimate the influence of surface treatment of glass fabric wilh methacryl silane and methanol washing, on the Mode I and Mode II fracture toughness, respectively. The results were compared with those of a conventional epoxy silane coated composite. It was found that an increasing content of methacryl silane (0.01 wt.% to 1.0 wt.%) reduced the Model fracture toughness and enhanced the Mode II fracture toughness values. Methanol washing after treatment with melhacryl sitane resulted in an increase of both Mode I and Mode II fracture toughness values.     

Mixed Bending-Tension (MBT) test for mode I interlaminar and intralaminar fracture

A new Mixed Bending-Tension (MBT) test is proposed for mode I fracture of laminated composites. The MBT specimen consists of a relatively small pre-cracked laminate adhesively bonded to pin-loaded steel beams. This design reduces significantly the bending stresses that prevent successful application of DCB tests to certain laminates. The MBT was here applied to carbon/epoxy unidirectional [0°]₂₆ and [90°]₂₆ laminates with starter delaminations. Interlaminar initiation G_IC values of [0°]₂₆ laminates agreed well with previous DCB test results, while [90°]₂₆ laminates exhibited 50% higher values. Significant lengths of fairly planar intralaminar crack propagation were seen in the latter laminates. The results showed a fibre bridging related R-curve, which was more pronounced in [0°]₂₆ laminates. The consistency of the present results indicates that the MBT opens new possibilities for the interlaminar and intralaminar mode I fracture.     

Bisphenol A based polyester binder as an effective interlaminar toughener

Bisphenol A based thermoplastic polyesters are commonly used in the industry as binders, or tackifiers, to produce cost-saving preforms in Liquid Composite Moulding processes such as Vacuum Assisted Resin Transfer Moulding (VARTM). However, it is often reported that the presence of these polyesters has a detrimental effect on the mechanical properties of the resulting composite laminates. In contrast, this study shows that interlaminar toughness can be increased without negatively affecting other properties by coating the reinforcing plies with a bisphenol A based thermoplastic polyester if some precautions are taken in mind.The polyester was added to an epoxy resin in order to study its effect on the thermophysical properties and fracture toughness of the bulk epoxy. The polyester molecules acted as a plasticizer for the epoxy resin when the polyester was added in low amounts. This increased the bulk fracture toughness of the epoxy resin by 30%. Polyester modified glass/epoxy laminates were produced and tested for Mode I interlaminar fracture toughness and flexural properties. The increased toughness of the epoxy matrix led to a 60% increased Mode I interlaminar fracture toughness of the laminates, without negatively affecting flexural stiffness and strength of the laminates.     

Enhancement of fracture toughness of hierarchical carbon fiber composites via improved adhesion between carbon nanotubes and carbon fibers

Hierarchical +1 composites consisting of carbon fibers with carbon nanotubes (CNTs) grown onto them and an epoxy matrix were processed, and the mode I fracture toughness of these composites was evaluated. The mode I fracture toughness of the initial batches of the hierarchical composites was lower than that of the baseline samples without CNTs. Hence, efforts to enhance the adhesion between carbon fibers and CNTs were made, resulting in enhanced adhesion. The enhanced adhesion was confirmed by Scotch tape tests and mode I fracture toughness tests followed by fractographic studies. The mode I fracture toughness of the hierarchical composites with enhanced adhesion was 51% and 89% higher than those of the baseline samples and hierarchical composites with poor adhesion, respectively. Moreover, fractographic studies of the fracture surfaces of the hierarchical composites with enhanced adhesion showed that CNTs were still attached to carbon fibers even after the mechanical tests.     

Characterization of the interlaminar fracture toughness of a laminated carbon/epoxy composite

Delamination between layers is an important problem in applications of fiber reinforced composite laminates. Tests were carried out to determine the interlaminar fracture toughness of AS4/3501-6 (carbon/epoxy) composite laminates using mixed-mode bending tests. Analysis of the test specimens in terms of mode I and mode II energy release rates showed good agreement between methods based on beam equations, compliance measurements, and detailed finite element analyses. The results showed that the critical mode I energy release rate for delamination decreased monotonically with increasing mode II loading. This is in contrast to some results in the literature. Various analytic representations of the mode interaction from the literature were compared, and shown to fit the data with reasonable accuracy.     

Interfacial adhesion improvement of plain woven carbon fiber reinforced epoxy filled with micro-fibrillated cellulose by addition liquid rubber

In certain application of fiber reinforced polymer composites fracture resistance is required. The aim of this study was to improve the interfacial adhesion between plain woven carbon fiber (CF) and epoxy matrix filled with microfibrillated cellulose (MFC) modified with carboxyl-terminated butadiene acrylonitrile (CTBN) as liquid rubber. CF/Epoxy/MFC/CTBN composite was characterized by different techniques, namely, tensile, bending, fracture toughness (mode I) test, and scanning electron microscope (SEM). The results reveal that at a fiber content 1% of MFC and 10% CTBN, initiation and propagation interlaminar fracture toughness in mode I improved significantly by 96 and 127%, respectively, which could be attribute to strong adhesion between filled epoxy, CF, and rubber. This can be explained by SEM at given weight as well; SEM images showed that in front of the tip, fiber breakage during initiation delimination as well as the extensive matrix deformation between fibers accounting for increase fracture toughness.     

苎麻短纤维层间增韧碳纤维/环氧树脂复合材料

采用热压机层压成型工艺制备了苎麻短纤维(SRF)层间增韧碳纤维/环氧树脂(CF/EP)复合材料层压板,研究了SRF的长度、面密度及其表面偶联处理对CF/EP复合材料层间断裂韧性的影响,并进一步研究了SRF的铺入对复合材料弯曲、拉伸性能的影响。研究结果表明,层间SRF的铺入明显改善了CF/EP复合材料的I型和II型层间断裂韧性(G_(IC)和G_(IIC)),当表面偶联处理的纤维长度为6mm、面密度为12g·m~(-2)时,增韧效果最佳,GIC由497.48J·m~(-2)增加到667.54J·m~(-2),提高了34.24%;GIIC由508.52J·m~(-2)增加到862.11J·m~(-2),提高了69.54%。此外,铺入SRF对复合材料的弯曲、拉伸性能也有一定程度的提高。通过SEM观察发现,SRF的增韧机制与其层间桥联以及裂纹扩展过程中从基体中拔出与劈裂等现象有关。     

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。      

Mode I and mode II fracture toughness of E-glass non-crimp fabric/carbon nanotube (CNT) modified polymer based composites

In this study, mode I and mode II interlaminar fracture toughness, and interlaminar shear strength of E-glass non-crimp fabric/carbon nanotube modified polymer matrix composites were investigated. The matrix resin containing 0.1 wt.% of amino functionalized multi walled carbon nanotubes were prepared, utilizing the 3-roll milling technique. Composite laminates were manufactured via vacuum assisted resin transfer molding process. Carbon nanotube modified laminates were found to exhibit 8% and 11% higher mode II interlaminar fracture toughness and interlaminar shear strength values, respectively, as compared to the base laminates. However, no significant improvement was observed for mode I interlaminar fracture toughness values. Furthermore, Optical microscopy and scanning electron microscopy were utilized to monitor the distribution of carbon nanotubes within the composite microstructure and to examine the fracture surfaces of the failed specimens, respectively.     

Cyclic fatigue delamination of carbon fiber-reinforced polymer-matrix composites: Data analysis and design considerations

Activities toward standardization of fracture mechanics tests on carbon fiber-reinforced polymer-matrix (CFRP) composites have recently focused on cyclic fatigue under mode I (tensile opening), mode II (in-plane shear) and mixed-mode I/II loading. Data from recent round robins performed by Technical Committee 4 (TC4) of the European Structural Integrity Society (ESIS) and from preliminary testing of additional CFRP epoxy laminates at the authors’ laboratories are analyzed with different approaches in attempts to reduce scatter and to identify parameters for CFRP structural design. Selected test data comparing load and displacement control for the cyclic fatigue tests are also discussed. Specifically, threshold values from Paris-law data fitting are compared with values from fitting with a modified Hartman–Schijve approach. Independent of the approach used for the analysis, mode I threshold values of selected CFRP seem to be in the range between about 30 and 100 J/m², i.e., roughly around the range of critical mode I energy release rate values (denoted by G_IC) obtained from fracture testing of neat commercial epoxy resins, but clearly below quasi-static initiation G_IC-values for unidirectional CFRP composites. Implications for CFRP structural design based on mode I fatigue fracture mechanics test data are briefly discussed.     

Enhancement of mechanical performance of epoxy/carbon fiber laminate composites using single-walled carbon nanotubes

Carbon nanotubes (CNT) in their various forms have great potential for use in the development of multifunctional multiscale laminated composites due to their unique geometry and properties. Recent advancements in the development of CNT hierarchical composites have mostly focused on multi-walled carbon nanotubes (MWCNT). In this work, single-walled carbon nanotubes (SWCNT) were used to develop nano-modified carbon fiber/epoxy laminates. A functionalization technique based on reduced SWCNT was employed to improve dispersion and epoxy resin-nanotube interaction. A commercial prepregging unit was then used to impregnate unidirectional carbon fiber tape with a modified epoxy system containing 0.1 wt% functionalized SWCNT. Impact and compression-after-impact (CAI) tests, Mode I interlaminar fracture toughness and Mode II interlaminar fracture toughness tests were performed on laminates with and without SWCNT. It was found that incorporation of 0.1 wt% of SWCNT resulted in a 5% reduction of the area of impact damage, a 3.5% increase in CAI strength, a 13% increase in Mode I fracture toughness, and 28% increase in Mode II interlaminar fracture toughness. A comparison between the results of this work and literature results on MWCNT-modified laminated composites suggests that SWCNT, at similar loadings, are more effective in enhancing the mechanical performance of traditional laminated composites.     

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

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

多壁碳纳米管对Ti-碳纤维/反应型聚酰亚胺超混杂层板力学性能的影响

为了改善Ti/反应型聚酰亚胺（PMR）树脂界面的黏结强度,从而提高Ti-碳纤维（CF）/PMR超混杂层板的力学性能,本文探究了添加多壁碳纳米管（MWCNTs）对Ti-CF/PMR超混杂层板力学性能的影响。将不同质量分数（0wt%、2.5wt%、5.0wt%和7.5wt%）的MWCNTs利用超声分散法均匀分散于PMR树脂中,随后进行Ⅰ型断裂韧性试验,探究添加MWCNTs对Ti-CF/PMR超混杂层板界面性能的影响,最后选取最优含量的MWCNTs同时添加到PMR胶层和CF/PMR树脂中,并进行弯曲试验,探究添加MWCNTs对Ti-CF/PMR超混杂层板力学性能的影响。通过SEM观察和分析了相应的失效模式和增强机制。结果表明:当MWCNTs含量为5.0wt%时,Ⅰ型层间断裂韧性提高了74%;同时添加5.0wt% MWCNTs于PMR胶层和CF/PMR复合材料树脂中,Ti-CF/PMR超混杂层板的弯曲性能较未添加MWCNTs提高了42%。这是由于MWCNTs在PMR胶层和CF/PMR树脂中的分布均匀性较高,且能分散并承受界面层转移到纤维层的载荷,并利用自身拔出、断裂、桥接、脱黏来吸收并消耗断裂能量,进一步提升Ti-CF/PMR超混杂层板的弯曲性能。