Effect of graphene oxide on the interlaminar fracture toughness of carbon fiber/epoxy composites

Graphene oxide (GO) nanoparticles were introduced in the interlaminar region of carbon fiber–epoxy composites by dispersing it in a thermoplastic polymer carrier such as polyvinylpyrrolidone (PVP). Mode‐I fracture toughness (G_IC) was investigated using double cantilever beam testing to evaluate the effect of the GO on the delamination behavior of the composite. The GO content was varied from 0% to 7% by weight as a function of the PVP content. Improvement of ～100% in the Mode I fracture toughness (G_IC) was observed compared to composites with no GO. The optimum amount of nanoparticles for improving the interlaminar fracture toughness was found to be ～0.007% by weight of the composite. The increase in the value of flexural strength value was also observed. Scanning electron microscopy of fracture surfaces, X‐ray diffraction, and transmission electron microscopy, and reflectance Fourier transform infrared spectra, as well as Raman spectroscopy results, are presented to support the conclusions. POLYM. ENG. SCI., 59:1199–1208 2019. © 2019 Society of Plastics Engineers     

Determination of initiation value of mode I interlaminar fracture toughness of unidirectional polymer composites

The use of interlaminar fracture tests to measure the delamination resistance of unidirectional composite laminates is now widespread. However, because of the frequent occurrence of fiber bridging and multiple cracking during the tests, it leads to artificially high values of delamination resistance, which will not represent the behavior of the laminates. Initiation fracture from the crack starter, on the other hand, does not involve bridging, and should be more representative of the delamination resistance of the composite laminates. Since there is some uncertainty involved in determining the initiation value of delamination resistance in mode I tests in the literature, a power law of the form G_IC= A · Δ a^b (where G_IC is mode I interlaminar fracture toughness and Δ a is delamination growth) is presented in this paper to determine initiation value of mode I interlaminar fracture toughness. It is found that initiation values of the mode I interlaminar fracture toughness. G_ICini, can be defined as the G_IC value at which 1 mm of delamination from the crack starter has occurred. Examples of initiation values determined by this method are given for both carbon fiber reinforced thermoplastic and thermosetting polymers.     

Mode II interlaminar fracture behavior of carbon bead‐filled epoxy/glass fiber hybrid composite

To investigate the effect of including carbon beads on the mechanical properties of epoxy resin, the fracture toughness of carbon bead‐filled epoxy was earlier evaluated using a CT (compact tension) specimens and Mode I fracture toughness was observed. Based on those results, in this study, the Mode II interlaminar fracture toughness of carbon bead filled epoxy/glass fiber hybrid composites was evaluated using end notch flexure (ENF) specimens. The hybrid composites showed increased Mode II interlaminar fracture toughness. The optimal bead volume fraction was around 15%.     

The influence of various kinds of PA12 interlayer on the interlaminar toughness of carbon fiber‐reinforced epoxy composites

Modifying the impact toughness of carbon fiber‐reinforced epoxy composites by introducing thermoplastic inserts in the interlaminar layer is state‐of‐the‐art. This article compares the introduction of thermoplastics in continuous and discontinuous form. Test plate samples were produced using unidirectional noncrimp carbon fabrics with two different aircraft resin systems: HEXFLOW RTM6 (Hexcel) and Cycom 890 RTM (Cytec). In addition, Polyamide 12 (PA12) was laid in the interlaminar layer in the forms of two different laid scrims, as powder or as nonwoven fabric (NWF). The performance of the resulting combinations was assessed by testing the samples in Mode I and II interlaminar fracture toughness (GIc and GIIc), interlaminar shear strength (ILSS), and compression strength after impact (CAI). The results show that in nearly all the tests a fine‐mesh laid scrim performs similarly to a NWF with twice the weight per surface area. They show furthermore that the curing dynamics of the resin systems together with the melting characteristics of the thermoplastic during processing have an important effect on the performance of the test samples. Hardening of the resin before the PA12 reaches its melting point hinders the compacting of the thermoplastic. This limits the reduction in the original thickness of the insert, leading to an increase in the sample thickness and, thus, reducing the fiber volume content. Otherwise, the discrete arrangement of the laid scrim has positive effects on the material properties of the composite at elevated temperatures, considerably reducing the falloff in ILSS resulting from the temperature‐dependent Young's modulus of PA12. POLYM. COMPOS., 36:1249–1257, 2015. © 2014 Society of Plastics Engineers     

Enhancement of interlaminar fracture toughness of carbon fiber–epoxy composites using polyamide‐6,6 electrospun nanofibers

In this study, carbon fiber–epoxy composites are interleaved with electrospun polyamide‐6,6 (PA 66) nanofibers to improve their Mode‐I fracture toughness. These nanofibers are directly deposited onto carbon fabrics before composite manufacturing via vacuum infusion. Three‐point bending, tensile, compression, interlaminar shear strength, Charpy impact, and double cantilever beam tests are performed on the reference and PA 66 interleaved specimens to evaluate the effects of PA 66 nanofibers on the mechanical properties of composites. To investigate the effect of nanofiber areal weight density (AWD), nanointerlayers with various AWD are prepared by changing the electrospinning duration. It is found that the electrospun PA 66 nanofibers are very effective in improving Mode‐I toughness and impact resistance, compressive strength, flexural modulus, and strength of the composites. However, these nanofibers cause a decrease in the tensile strength of the composites. The glass‐transition temperature of the composites is not affected by the addition of PA 66 nanofibers. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45244.     

Mode I interlaminar fracture toughness of Nylon 66 nanofibrilmat interleaved carbon/epoxy laminates

Carbon/epoxy laminates interleaved with laboratory scale electrospun Nylon 66 nanofibrilmat and spunbonded nonwoven mats were investigated. The effect of the nanoscale fibers on the fracture toughness of the composite under pure Mode I loading was evaluated. It was shown that the nanofibrilmat is responsible for a major interlaminar fracture toughness improvement, as high as 255–322%, compared to a noninterleaved carbon/epoxy reference laminate. We further studied the improvement mechanism of the electrospun nanofibrilmat compared to a commercial spunbonded nonwoven Nylon 66 mat. A combination of two interlayer fracture mechanisms responsible for the toughness improvement is suggested: the first is related to the high energy dissipated by bridged thermoplastic nanofibers and the second is attributed to the generation of a plastic zone near the crack tip. The interlaminar fracture mechanisms of both electrospun nanofibrilmat and the nonwoven mat interleaving was analyzed and discussed. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

Resin modification on interlaminar shear property of carbon fiber/epoxy/nano‐CaCO3 hybrid composites

Epoxy resin was modified by adding a silane coupling agent/nano‐calcium carbonate master batch. Then, samples of binary carbon fiber/epoxy composites and ternary fiber/nano‐CaCO₃/epoxy were prepared by hot press process. The interlaminar shear strength (ILSS) of the carbon fiber/epoxy composites was investigated and the results indicate that introduction of the treated nano‐CaCO₃ enhances ILSS obviously. In particular, the addition of 4 wt% nano‐CaCO₃ leads to 36.6% increase in the ILSS for the composite. The fracture surfaces of the carbon fiber/epoxy composites and the mechanical properties of epoxy resin cast are examined and both of them are employed to explain the change of ILSS. The results show that the change of ILSS is primarily due to an increase of the epoxy matrix strength and an increase of the fiber/epoxy interface. The bifurcation of propagating cracks, stress transfer, and cavitation are deduced for the reasons of strengthening and toughening effect of nano‐CaCO₃ particles. POLYM. COMPOS., 38:2035–2042, 2017. © 2015 Society of Plastics Engineers     

Rheological properties and fracture toughness of epoxy resin/multi‐walled carbon nanotube composites

Multi‐walled carbon nanotubes (MWCNTs), surface‐treated via chemical functionalization, i.e., oxidation and amidation, were used to reinforce diglycidylether of bisphenol F (DGEBF) epoxy resin. The effects of the functionalization on the dispersion stability, rheological properties, and fracture toughness of DGEBF/MWCNT composites were investigated. The dispersion homogeneity of the MWCNTs in the epoxy matrix improved after functionalization. In addition, isothermal rheology measurements revealed that the DGEBF/dodecyl amine‐functionalized MWCNT (D‐MWCNT) composite had a longer gel time and higher activation energy of cross‐linking than the DGEBF/acid‐treated MWCNT (A‐MWCNT) composite. The fracture toughness of the former was also significantly higher than that of the latter; this resulted from the relatively high dispersion stability of the D‐MWCNTs in the epoxy matrix, owing to the presence of alkyl groups on the D‐MWCNT surface. POLYM. ENG. SCI., 55:2676–2682, 2015. © 2015 Society of Plastics Engineers     

The effect of silicon carbide whiskers on the Mode I interlaminar fracture of carbon fiber composites

This paper reports on the Mode I interlaminar fracture toughness improvement of carbon fiber-epoxy composites as a result of incorporating SiC whiskers in the epoxy matrix. Five laminates of unidirectional carbon fiber-epoxy composites at different weight fractions of SiC whiskers were manufactured using hand layup vacuum bagging process. Optical and scanning electron microscopic analysis were conducted to give an insight into the fracture morphogoloy, failure mechanisms, and the energy dissipation mechanisms created by the presence of the whiskers in the composite. Experimental results showed that composites containing 5 wt% whiskers exhibited 67% increase in the crack initiation interlaminar fracture toughness G_IC, whereas it exhibited 55% increase in the maximum G_IC compared to pristine composite. The optical and SEM fractographs revealed a strong relation between the microstructure of the fractured surfaces and the energy release rate trend of the composites.     

Toughness improvement of an epoxy/anhydride matrix. Influence on processing and fatigue properties of unidirectional glass–fiber composites

Wet filament winding processing for unidirectional composites uses specific reactive systems with low viscosity and long-pot life. This work describes improvement of toughness of an epoxy/anhydride matrix using, first, the increasing of the average molecular weight of the diepoxy prepolymer and, second, the introduction of a functionalized elastomer. Thermomechanical behaviors (glass transition temperature, elasticity, plastic, and fracture properties) are discussed in terms of (1) the increase of the average molecular weight between crosslinks in the first case and(2) the amount of elastomer dissolved in the matrix in the second case. Dynamic mechanical spectroscopy confirms that phase separation occurred, during curing, between the epoxy system and the elastomer. A good correlation is obtained between matrix toughness and fatigue behavior of unidirectional composites. © 1993 John Wiley & Sons, Inc.     

Silane coupling agent modification on interlaminar shear strength of carbon fiber/epoxy/nano‐CaCo3 composites

Four different types of composites were prepared based on unmodified and modified epoxy matrices: (A) unmodified epoxy/carbon fiber composites, (B) modified epoxy/carbon fiber composites by silane coupling agent/nano‐CaCO₃ master batch, (C) modified epoxy/carbon fiber composites by nano‐CaCO₃ particles directly, and (D) modified epoxy/carbon fiber composites by nano‐CaCO₃ particles and silane coupling agent together. The interlaminar shear strength (ILSS) of the carbon fiber‐reinforced composites was investigated. The results show that the silane coupling agent/nano‐CaCO₃ master batch can increase the ILSS to the highest degree. Nevertheless, Sample D, i.e., modified by nano‐CaCO₃ particles and silane coupling agent together, even presents a decrease of the ILSS. The integration effect of silane coupling agent/nano‐CaCO₃ master batch was concluded. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

Mode I interlaminar fracture behavior of 2D woven ceramic matrix composites

Interlaminar fracture properties of melt-infiltrated woven SiC/SiC ceramic matrix composites were investigated using traditional and wedge-loaded double cantilever beam methods. The two methods produced comparable G_IC results for some specimens. The difference in boundary conditions between the two methods appeared to influence the crack propagation path. The DCB method, having free-end boundary condition, allowed more interaction between the crack and the composite microstructure than the wedge method did. The effect of fiber tow layout sequence had an effect on the interlaminar properties. Higher toughness was observed for the orientation where crack propagation occurs between planes with more transverse tows. Jump-arrest phenomenon was found to have higher significance on the rising R-curve behavior than fiber bridging.     

Effect of hybridization on the mode II fracture toughness properties of flax/vinyl ester composites

In this study, flax fiber reinforced and flax/basalt hybridized vinyl ester composites were produced and their interlaminar fracture toughness (mode II) behavior was investigated using the three‐point bend end‐notched flexural (3ENF) testing. From the results, the average of the maximum values for each group of specimen obtained for critical strain energy release rate G _IIC and stress intensity factor K _II for flax/vinyl ester specimens were 1,940 J/m² and 134 kPam^0.5. Similarly, G _IIC and K _II values recorded for hybridized specimens were 2,173 J/m² and 178 kPam^0.5, respectively. The results for the flax/basalt hybridized composites exhibited an improved fracture toughness behavior compared to flax/vinyl ester composites without hybridization. The cohesive zone modeling (CZM) was also used to predict the delamination crack propagation in mode‐II in laminated composite structures. After the experimental study, the 3ENF specimens were modeled and simulated using ANSYS. The CZM/FEA results were in reasonable agreement with the experimental results. POLYM. COMPOS., 38:1732–1740, 2017. © 2015 Society of Plastics Engineers     

Drape behavior of 3D woven glass‐epoxy composites

This article deals with the drapability of 3D woven glass fabrics for composite applications. The study focuses on forming a 3D fabric over the mold, the result is a preform, which generally is then injected with a polymer matrix by so called Liquid Composite Molding (LCM) technique. When draping pre–impregnated composites, the fabric is embedded in the epoxy resin as matrix material. Various drape models for dry and pre‐impregnated fabrics have been proposed in the work. Solidworks and ANSYS are the software used for modeling and simulation of 3D woven fabric composites. Given the linear density (tex) and density of E‐glass fiber, the radius of the yarn was calculated. So far the cross section of yarn is assumed to be perfectly circular in shape, keeping the perimeter of yarn constant the circular cross section was deformed into a race track shape which is a much more practical and realistic shape of a yarn cross section. After calculating all the required dimensions, all the three 3D woven structures namely angle interlock, warp interlock and orthogonal were developed in solidworks. All the parameters like total number of warp and weft yarn per unit distance and thickness of the fabric were kept constant in all three structures. The analysis is based on first principles and the parameters of yarn and fabric construction. Results obtained through simulation are reported. These are validated with experimental composite samples. The model used to predict drapability of 3D woven glass‐epoxy composite gives good results. Orthogonal structure proves to be the best as far as resistance to deformation is concerned. However, if a relatively more flexible and formable prepreg is desired, it is advisable to use angle interlock or warp interlock structures. Warp interlock 3D structure proves most beneficial for draping on a mold. POLYM. COMPOS., 37:472–480, 2016. © 2014 Society of Plastics Engineers     

The effect of chemical modification on the fracture toughness of montmorillonite clay/epoxy nanocomposites

The change in fracture toughness and its dependence on the content of clay nanoplatelets and adhesion at the interface between clay nanoplatelets and anhydride-cured epoxy matrix are discussed. Three clay nanoplatelets with different chemical modifications were used in this investigation. To fabricate nanocomposites, the clay nanoplatelets were sonicated in acetone for 2 h. The role of the clay nanoplatelets in the mechanical/fracture properties was investigated by transmission electron microscopy (TEM). Bright-field TEM micrographs showed excellent dispersion of clay nanoplatelets in epoxy matrix. Both intercalation and exfoliation of clay nanoplatelets were observed depending on clay modification. Compact tension specimens were used for fracture testing. The fracture toughness increased with increasing clay content. The fracture toughness of clay/epoxy nanocomposites varied with the clay morphology in the epoxy matrix. Different morphologies of the fracture surfaces, highly dependent on the morphology of dispersed clay nanoplatelets, were observed using environmental scanning electron microscopy (ESEM). The fracture toughness was found to be correlated with the fracture surface roughness measured by confocal laser scanning microscopy (CLSM).     

“Ex situ” concept for toughening the RTMable BMI matrix composites,Part I: Improving the interlaminar fracture toughness

Aerospace‐grade bismaleimide matrix composites was toughened based on a novel ex situ resin transfer molding (RTM) technique using a special manufactured ES? carbon fabrics. The toughening mechanism and toughening effect by the technique are studied using thermoplastic PAEK as toughener. Mode I fracture toughness (G_IC) of the composites toughened by ex situ RTM technique increased up to three times higher than that of the control system, and Mode II fracture toughness (G_IIC) increased two times higher as well. The composite without toughening was denoted as control system. The microstructure revealed that a reaction‐induced phase decomposition and inversion happened in the interlaminar region, which resulted in a particles morphology that showed the thermosetting particles were surrounded with the PAEK phase. The plastic deformation and rupture of the continuous PAEK phase are responsible to the fracture toughness improvement. And the influence of PAEK concentration on toughness improvement was also investigated. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Interlaminar fracture toughness testing of composite mode I and mode II DCB specimens

A computer controlled test procedure for evaluating mode I and mode II interlaminar fracture behavior was used in experiments with eight different resin matrix/graphite fiber composites. Four analytical methods for calculating fracture toughness were compared. These included an energy rate determination of the J-integral, a compliance calibration procedure, equations based on linear beam bending, and an Area method calculation. Methods that account for nonlinear material behavior, such as the J-integral, were needed for characterizing the systems with high fracture toughness. The ratio of mode II to mode I fracture toughness ranged from 1.5 to 8.0, depending on the material system. Finally, preliminary work with a technique for constant strain rate testing of mode I DCB specimens is presented.     

Use of polyester/glass‐fiber residues as fillers for composites

In this work, the performance of polyester (P)/glass fiber mats (G) and P/G/calcium carbonate (CaCO₃) composites was compared with that of P/G/fiberglass waste composites. The residues used were conventional P/G postconsumer light resin‐transfer‐molding parts, obtained via knife or ball milling. Composites with up to 50 wt % reinforcement were prepared by hot compression molding and characterized via physical (density and water sorption), thermal (thermogravimetry and burnout), and mechanical (impact, Barcol hardness, and tensile) testing. The results show that the simple grinding and reincorporation of the composite residues yielded new composites with generally worse characteristics than the ones with calcium carbonate. Then, the waste was sorted by removing most of the pure resin particles from it. This yielded a resin‐rich fraction, which could be better used for energy recovery and resin‐covered fibers. The use of the latter as a filler yielded composites with better overall properties than those with calcium carbonate for a controlled amount of W; thus showing potential use as a replacement for the commonly used inorganic filler, maintaining the mechanical properties, decreasing the raw material cost, and reducing the amount of composite waste discarded in the environment. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Fatigue delamination,initiation, and growth,under mode I and II of fracture in a carbon‐fiber epoxy composite

In this article, interlaminar crack initiation and propagation under mode I and II dynamic loading of an epoxy matrix reinforced with unidirectional carbon fibers were evaluated. Delamination in mode I was carried out employing the DCB test (Double Cantilever Beam). In mode II, the ENF test (End Notched Flexure) was used. The fracture toughness in mode I was obtained using the methods of the ASTM D5528 Standard, whereas in mode II, the methods were applied in accordance with the ESIS (European Structural Integrity Society) Protocol. Employing this experimental program, the fatigue curves (ΔG,N) and growth rate curves (ΔG, da/dN) in both fracture modes were determined for an asymmetry ratio R = 0.2. The influence of the manufacturing process of the material on its behavior with respect to crack growth onset may be deduced from the experimental results, mainly the presence of resin bags. Moreover, as the crack growth rate decreases for large crack lengths, crack growth may even cease if the critical fracture energy does not increase above the values obtained in the static characterization of the material. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Time–temperature dependency of mode II fracture toughness for bisphenol A type epoxy resin

We investigated the mode II fracture toughness (K_IIc) with time and temperature dependence of the bisphenol A type of epoxy resin. We performed an asymmetric four‐point bending test under various conditions of temperature and displacement rate. We found that K_IIc strongly depended on the displacement rate and the temperature, even at room temperature. Moreover, it was governed by the time–temperature equivalence principle in regard to the fracture time. The time–temperature dependency of K_IIc was similar to that of the loss modulus (E″), and the transition of brittle to ductile fractures occurred nearly simultaneously when E″ peaked. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 51–55, 2005