Composites Science and Technology 70 (2010) 1660–1666 Contents lists available at ScienceDirect Composites Science and Technology journal homepage: www.elsevier.com/locate/compscitech Electrospun nanofibre toughened carbon/epoxy composites: Effects of polyetherketone cardo (PEK-C) nanofibre diameter and interlayer thickness Jin Zhang, Tong Lin *, Xungai Wang Centre for Material and Fibre Innovation, Deakin University, Geelong, VIC 3217, Australia a r t i c l e i n f o Article history: Received 28 March 2010 Received in revised form 22 May 2010 Accepted 29 June 2010 Available online 22 July 2010 Keywords: A. Polymer–matrix composites (PMCs) B. Fracture toughness C. Crack D. Polyetherketone cardo (PEK-C) nanofibres E. Electrospinning a b s t r a c t 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 (Tg) of the cured resin. Increasing nanofibre interlayer thickness improved the fracture toughness but compromised the flexure performance. The Tg of the cured resin deteriorated after the thickness increased to a certain extent. Ó 2010 Elsevier Ltd. All rights reserved. 1. Introduction Carbon fibre reinforced thermosetting matrix composites have been widely used as structural materials in aerospace, automotive and marine industries. The most common failure mode of this high performance laminated material is delamination as a consequence of low velocity impact, and/or cyclic loading during manufacturing or service life [1]. Insufficient fracture toughness and delamination resistance has been the main issue affecting the long-term reliability of thermosetting matrix composites. Two main strategies have been developed to toughen the thermosetting matrix composites, by either blending a toughener with the matrix resin [2–4] or incorporating a discrete tough interlayer between composite plies [5–7]. The addition of tougheners to the entire matrix resin could lead to decrease in in-plane mechanical properties such as compression and shear strengths. The increased viscosity arising from the addition of tougheners could also dramatically reduce the processing ability of matrix resin. However, interlayer toughening is less likely to cause those issues, and is used increasingly in the composite industry as a result. Indeed, several interlayer toughening methods have been developed, such as using thermoplastic or thermosetting films [8,9], porous membranes [10], and rubber and/or thermoplastic particles [11,12]. However, these methods suffered problems such as incompatibil* Corresponding author. Tel.: +61 3 52271245; fax: +61 3 52272539. E-mail address: tong.lin@deakin.edu.au (T. Lin). 0266-3538/$ - see front matter Ó 2010 Elsevier Ltd. All rights reserved. doi:10.1016/j.compscitech.2010.06.019 ity with liquid moulding processes associated with thermoplastic films, poor adhesion between the inserted interlayers and composite plies, and inhibition of resin flow during infusion. To avoid these issues, a highly porous material with an efficient resin infusion, a large surface area, and minimal extra weight, is highly desired to improve the fracture toughness. Polymer nanofibres produced by an electrospinning process have been shown excellent porous characteristics [13]. In most cases, electrospun nanofibres are collected in the form of randomly orientated nonwoven fibre membrane which is highly porous with excellent pore-interconnectivity and extremely large surfaceto-volume ratio [14,15]. Such a porous characteristic provides nanofibre membranes with remarkable permeability to facilitate resin flow, therefore ensuring complete impregnation of reinforcements. Recently, polysulfone (PSF) nanofibres have been used to enhance the Mode I delamination fracture toughness of composite prepregs [7]. The nanofibre membranes showed significantly better improvement in the fracture toughness compared to the dense film counterpart. However, depositing nanofibres on pre-impregnated composite prepreg surface could cause incomplete toughening of the entire resin layer. Toughening layer achieved by depositing nanofibres directly onto carbon fabrics followed by epoxy addition should ensure that the nanofibres take up the entire resin layer, hence complete toughening. In this study, polyetherketone cardo (PEK-C) nanofibres were used as interlayers to toughen carbon fibre/epoxy composite. PEK-C nanofibres were directly electrospun to one side of the dry J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 carbon fabric. The influences of nanofibre diameter and loading thickness on the Mode I delamination fracture toughness, flexure properties and thermal mechanical properties were examined. O C O C n O O C O Chemical structure of polyetherketone cardo (PEK-C) 1661 was performed under an applied voltage of 15–20 kV with a solution flow rate of 0.7 ml/h. During electrospinning, the nanofibres were collected onto the carbon fabric mounted on the collector, while the roller collector was rotating at a constant speed of 100 rpm. The carbon fabrics with one side deposited with PEK-C nanofibres were laid up with epoxy resin (epoxy/carbon 1:1, wt/wt) applied on the other side. The composite laminates [0/90]4 were finally cured in a hot press at 175 °C for 3 h. As a control, a composite laminate without electrospun nanofibre interlayers was prepared using the same process. 2.3. Characterisations 2. Experimental 2.1. Materials Formax multiaxial carbon fibre reinforcements [C12K, 450, 45/+45] were used for preparing carbon/epoxy composite laminates. The stitching thread is polyester and the stitch weight is 7 g/m2 (GSM). The epoxy resin was composed of triglycidyl amino phenol (TGAP, Araldite MY0510, Hunstman) with epoxy equivalent 95–106 and a 4,40 -diamino diphenyl sulfone (DDS, Aldrich, purity > 97%) cure agent. PEK-C from Xuzhou Engineering Plastics Co. and N,N-dimethylformamide (DMF) from Aldrich were used as received. 2.2. Electrospinning and preparation of interlayer toughened composites PEK-C powder was vacuum dried at 110 °C overnight and then dissolved in N,N-dimethylformamide with constant stirring for approximately 12 h at room temperature. The PEK-C solution was placed into a 5 ml syringe with a metal syringe needle (23 Gauge) which was connected to a syringe pump (KD scientific). Single layer carbon fabric mounted on a metal roller at a distance of 15 cm from the needle tip was used as a substrate to collect PEK-C nanofibres. A detailed introduction of laboratory-made electrospinning facilities can be found in Ref. [16]. The electrospinning Mode I delamination fracture toughness was measured by double cantilever beam (DCB) tests on a LLOYD 30K universal tester according to the protocol of the European Structural Integrity Society [17]. A 15 lm thick aluminium foil was treated with a Zyvax release agent and then inserted between the mid-layers prior to processing. A crosshead speed of 2 mm/min was used for DCB tests. The cured thickness of composite laminates was within the range of 1.55–1.75 mm. Correction factors for large displacements and stiffening by the end blocks were applied for calculating the Mode I critical strain energy release rate, GIC. Three point bending flexure tests were conducted according to ASTM D790. The specimen width was 25 mm, the specimen length was 50 mm and the span length was 32 mm. Five specimens were tested for calculating the fracture toughness and flexure properties of each composite laminate. Dynamic mechanical thermal analysis was performed using a TA Q800 analyzer at a fixed frequency of 1 Hz with a heating rate of 3 °C/min. A single cantilever mode was adopted. The microstructure analysis was conducted by using both optical microscope (Olympus DP70) and scanning electron microscope (SEM) (Zeiss Supra 55VP). The samples for SEM were coated with carbon prior to observation. The average diameters of the electrospun fibres were calculated based on the SEM micrographs using an image analysis software (Image J). For each PEK-C concentration, 100 fibres were counted and the average diameters were determined from the histogram graphs of size distribution. The weight Fig. 1. SEM images of PEK-C nanofibres electrospun from (a) 20 wt.%, (b) 23 wt.%, (c) 25 wt.% and (d) 30 wt.% PEK-C solutions. 1662 J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 of PEK-C solution, a similar trend on the fibre morphology was also observed. For example, electrospinning of 10 wt.% PEK-C solution (10 g PEK-C in 100 ml N,N-dimethylformamide) led to beads-onstring fibres. When the PEK-C concentration was larger than 20 wt.%, bead-free uniform nanofibres were produced. Fig. 1 shows the morphologies of PEK-C nanofibres electrospun from four different concentrations. The relationship between the fibre diameter and the PEK-C concentration is given in Fig. 2. With an increase in the PEK-C concentration from 20 wt.% to 23 wt.%, 25 wt.% and 30 wt.%, the average fibre diameter increased from 275 nm to 450 nm, 750 nm and 950 nm, respectively. 1000 800 600 400 200 22 24 26 28 30 3.2. Mechanical properties and SEM morphology PEK-C concentration (wt%) Fig. 2. Dependency of PEK-C nanofibre diameter on the PEK-C concentration. fractions of PEK-C in the composites were calculated based on the flow rate of the polymer solution being electrospun, the electrospinning time, polymer concentration and the weight of carbon fabrics and epoxy resin. 3. Results and discussion 3.1. Nanofibre morphologies Electrospun PEK-C nanofibres were obtained from PEK-C solutions with various PEK-C concentrations. It has been established that electrospinning a polymer solution could result in individual beads, beads-on-structure and bead-free fibres [18]. In the case (a) (a) 250 500 800 400 elastic modulus0 600 IC GIC-PROP0 150 200 control fibre diameter 450 nm fibre diameter 750 nm fibre diameter 950 nm 50 0 400 300 200 100 0.05 0.06 0.07 0.08 0.09 0.10 200 GIC-INI0 200 300 400 500 600 700 800 0 900 1000 Fibre diameter (nm) 0.11 (b) 700 Crack length a (m) flexure strength0 800 600 600 500 500 elastic modulus0 600 2 GIC (J/m ) (b) 1000 flexure strength0 2 GIC(J/m ) 300 2 600 400 350 G (J/m ) Electrospun nanofibres were directly electrospun on dry carbon fabrics to form a randomly orientated nanofibre nonwoven membrane, and they served as an interlayer toughening agent for preparing carbon/epoxy composite laminates. To investigate the influence of fibre diameter on the mechanical performance of interlayer toughened composites, PEK-C nanofibres with average diameters of 450 nm, 750 nm and 950 nm, electrospun respectively from 23 wt.%, 25 wt.% and 30 wt.% PEK-C solutions, were used. With an equal weight loading of PEK-C nanofibres on the carbon fabric, the effects of fibre diameter on the Mode I delamination fracture toughness and flexure properties were examined. To achieve approximate 0.44% weight fraction of PEK-C nanofibres in the composite laminates, the electrospinning time for different polymer concentrations varied. PEK-C solution (23 wt.%) needs 60 min of electrospinning time, while for IC 2 G (J/m ) 400 400 400 300 300 200 200 G IC-INI0 GIC-PROP0 control interlayer thickness 40 μm interlayer thickness 70 μm interlayer thickness 105 μm 100 0 0.05 0.06 0.07 0.08 0.09 0.10 Flexure property 20 0.11 Crack length a (m) Fig. 3. Delamination fracture toughness of the composite specimens. 100 10 20 200 30 40 50 60 70 80 90 100 110 Flexure property Fibre diameter (nm) 1200 0 Interlayer thickness (μm) Fig. 4. Mode I delamination fracture toughness and flexure properties of nanofibremodified composites as a function of (a) nanofibre diameter and (b) interlayer thickness. –h– GIC-INI; –j– GIC-PROP; –s– elastic modulus (E-1GPa); –d– flexure strength (MPa). The dotted lines underneath different properties indicate the corresponding average data for the control composite specimen. J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 25 wt.% and 30 wt.% PEK-C solutions, the electrospinning time was 55 and 46 min, respectively. The average interlayer thickness of the cured composite laminates was 58 lm, 65 lm and 70 lm for the membranes with fibre diameters of 450 nm, 750 nm and 950 nm, respectively. Fig. 3a reveals the delamination resistance curves for both the control and the composite laminates modified by nanofibres with different diameters. For the control specimen, there existed a considerable scatter in the calculated GIC, which was attributed to the [0/90]4 carbon fibre orientation and the bonding stitches pre-existed in the carbon fabrics [19,20]. Compared with the control, the PEK-C nanofibre-modified composite specimens showed increased GIC. The delamination resistance curves showed unstable crack growth and the stick/slip fracture behaviour. The fluctuation of the delamination resistance curves became more significant as the fibre diameter increased. Visual detection was applied as the criteria to define the initiation of crack propagation. The strain energy release rate for crack initiation (GIC-INI) and for crack propagation (GIC-PROP) influenced by nanofibre diameter were compared and included in Fig. 4a. The average GIC-INI for the control specimen was 151 J/m2, whereas the GIC-INI value for the nanofibre-modified specimens with average fibre diameters of 450 nm, 750 nm and 950 nm was 249 J/m2, 228 J/m2 and 241 J/m2, respectively, indicating increased GIC-INI value for the nanofibre-modified composite specimens. The presence of nanofibre interlayer also led to increased average GIC-PROP. It 1663 should be noted that the weight loading of the nanofibres in the nanofibre-modified specimens was less than 1 wt.% (around 0.4 wt.%). The improvement in GIC-INI and GIC-PROP due to such a low weight loading is quite significant. The effect of fibre diameter on the flexure strength and elastic modulus is also shown in Fig. 4a. By comparison with the control specimen, the flexure strength of the nanofibre-modified specimens decreased slightly when the average nanofibre diameter increased from 450 nm to 750 nm, however, a noticeable decrease in the flexure strength was observed in the specimen with a larger average fibre diameter (950 nm). Similarly, a considerable reduction in the elastic modulus was observed when coarse nanofibres (e.g. 950 nm) were employed as interlayers. This suggested that composites modified with finer nanofibres had better improvement in the interlaminar property without compromising the inplane performance of the toughened composites. Fig. 5a shows the morphology of the delaminated control specimen, and the phase morphologies of delaminated composite specimens toughened by PEK-C nanofibres with average diameters of 450 nm, 750 nm and 950 nm are shown in Fig. 5b, c and e, respectively. In contrast to the control specimen, PEK-C-rich particulate phases with various sizes were shown on the delamination fracture surface of modified composites. Despite the equal weight loading of the PEK-C nanofibres, the size of PEK-C-rich phases and their distance increased with the increase in the fibre diameter. Fig. 5. SEM images of delamination fracture surface. (a) Control composite specimen, (b–f) nanofibre-modified composites; (b) fibre diameter: 450 nm, interlayer thickness: 70 lm; (c) fibre diameter: 750 nm, interlayer thickness: 70 lm; (d) diameter: 950 nm, interlayer thickness: 40 lm; (e) fibre diameter: 950 nm, interlayer thickness: 70 lm; (f) fibre diameter: 950 nm, interlayer thickness: 105 lm. The PEK-C-rich particulate phases have been removed by solvent DMF and are shown as dark holes in the images. J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 3.3. Dynamic thermal mechanical analysis Fig. 6 shows the tan d curves for the control and PEK-C nanofibre-modified composite specimens. The control sample displayed a well-defined relaxation peak at 281 °C, which corresponds to the glass transition temperature of the epoxy resin. All the PEK-C nanofibre-modified composites showed two separate glass transitions. The glass transition temperature for PEK-C powder was measured by differential scanning calorimetry (DSC), where Tg was determined from the midpoint of the slope change of the heat capacity plot of the second scan. A glass transition at 219 °C was obtained from the DSC curve. Since the Tg values measured by DSC are generally 20–30 °C lower than those measured by DMA at the same compositions, the relaxation peak at lower temperature shown in the tan d curves of modified composites was attributed to the PEK-C-rich phase, which is TgPEK-C. The relaxation peak at higher temperature displayed in the spectrum is ascribed to the glass transition of the cured epoxy resin, which is TgER. Fig. 6a displays the tan d curves influenced by the nanofibre diameter. It is noted that there was almost no reduction or slight increase in TgER with the addition of PEK-C nanofibres. The peaks centred at 283 °C, a 0.14 0.12 control fibre diameter 450 nm fibre diameter 750 nm fibre diameter 950 nm 0.10 tan δ It should be noted that the penetration of epoxy at room temperature did not lead to dissolution or ‘‘deterioration” of nanofibres and PEK-C nanofibres started dissolving into the epoxy resin as the curing temperature increased to 70 °C. However, the high viscosity of PEK-C retained the diffusion of dissolved PEK-C into the epoxy resin, which led to unique phase structure after curing. Coarser nanofibres caused higher local concentration of PEK-C in epoxy resin, resulting in larger PEK-C-rich particulate phases as revealed on the delamination fracture surface. The PEK-C-rich phases create stress concentrations at their equators and also act as sites for initiating shear bands. When the shear bands created by one toughener-enriched phase interact with another, they may stop propagating and keep the matrix yielding localised [21,22]. Therefore the cracks were hindered intermittently by the PEK-C-rich phases and forced to propagate between two unstable jumps. The membrane composed of finer fibre diameters gave rise to reduced distance between the ductile PEK-C-rich phases, which assisted with maintaining a more stable crack growth during delamination. Analogous findings were reported where poly(acrylonitrile–butadiene–styrene) particles (ABS) particles were used for interlayer toughening of glass fibre/vinyl-ester resin composites [1]. By using particles with a similar size, the stability of crack propagation was improved by increasing the particle concentration in the interlayer. The interlayer thickness was adjusted through the electrospinning time. Here nanofibres with the average diameter of 950 nm were chosen. With an increase in the electrospinning time from 23 min to 46 min and 68 min, the average interlayer thickness of the cured composite laminates changed from 40 lm to 70 lm and 105 lm, which led to changes of the GIC-INI from 198 J/m2 to 241 J/m2 and 236 J/m2 and the GIC-PROP from 272 J/m2 to 296 J/m2 and 376 J/m2. In comparison with the control specimens, whose GIC-INI and GIC-PROP values are 151 J/m2 and 207 J/m2, respectively, the presence of nanofibre interlayer resulted in higher delamination fracture toughness (Figs. 3b and 4b). It is also noted that the weight fraction of PEK-C in the cured composites was approximately 0.22%, 0.44% and 0.65% for the laminates with average interlayer thickness of 40 lm, 70 lm and 105 lm, respectively. The influence of interlayer thickness on the flexure properties is also shown in Fig. 4b. Both the flexure strength and the elastic modulus showed a decreasing trend as the nanofibre interlayer thickness increased. Fig. 5d–f shows the morphology of delamination fracture surface influenced by nanofibre interlayer thickness. Larger PEK-C-rich phases were observed to scatter on the fracture surface of thicker nanofibre interlayer. 0.08 0.06 0.04 0.02 50 100 150 200 250 300 250 300 o Temperature ( C) b 0.12 0.10 control interlayer thickness 40 μm interlayer thckness 70 μm interlayer thickness 105 μm 0.08 tan δ 1664 0.06 0.04 0.02 50 100 150 200 o Temperature( C) Fig. 6. Tan d traces of both control and nanofibre-modified composites. 280 °C and 285 °C correspond to the TgER for the composites modified by PEK-C nanofibres with average fibre diameter of 450 nm, 750 nm and 950 nm respectively. Similar shifts of relaxation peaks to higher temperature have been reported in the literature on the thermal mechanical properties of nanocomposites [23]. Nano-reinforcements have been shown to affect the segmental motions of polymer matrices when they are well dispersed [24]. The large surface areas of nanofibre membranes provide complete interaction with the epoxy matrix, which may prohibit the epoxy chains from moving freely as in the neat resin [25]. No noticeable shifts occurred in the relaxation peaks for the TgPEK-C as the average fibre diameter changed. It is also noticed from Fig. 6b that both the TgER and TgPEK-C reduced to lower temperatures as the thickness of PEKC interlayers increased to 105 lm. This result indicates the level of interaction and compatibility between the PEK-C nanofibres and the epoxy resin deteriorated after the inclusion of nanofibre membranes increased to a certain extent. 3.4. Phase structure Fig. 7 presents the phase structure of the interlayer region from PEK-C nanofibre-modified carbon fibre reinforced TGAP/DDS epoxy matrix composites. Fig. 7a is an optical micrograph for the cross section of a modified composite laminate. The bright part is a pre-inserted aluminium film, which was located in the midplane of composite laminate. A dark interlayer region composed of both an epoxy-rich macrophase and PEK-C-rich macrophases was found to be sited between the top [0] and the bottom [90] carbon fibre layers. As shown in Fig. 7b–e, cylinder-shaped macrophase structures were observed to be embedded in the continuous epoxy J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 1665 Fig. 7. Phase structure of interlayer region of a nanofibre-modified composite specimen (average nanofibre diameter: 950 nm, average interlayer thickness: 105 lm). Optical micrographic (a) and SEM (b) images of interlayer region; (c–f) phase structures of the PEK-C-rich macrophases after etched with DMF; (d and f) are magnified images of the selected areas in (c and e); (g and h) phase structure of the epoxy-rich macrophase. resin. Fig. 7d–f are enlarged views of the PEK-C-rich macrophases showing a fibrous structure inside of the cylinder-shaped macrophase. Since the specimens have been etched with N,N-dimethylformamide, the PEK-C should be removed. These fibrous structures could come from undissolved PEK-C nanofibres which were covered by cured epoxy resin. Fig. 7g and h shows the morphology of a detached epoxy-rich macrophase from carbon fibre. It clearly indicated that the PEK-C-rich microphases (particulate phases) dispersed in the continuous epoxy-rich matrix. Although the mechanism of multiple phase changes in PEK-C nanofibres/ epoxy system warrants further research, the separated phases in the interlayer region supported our findings on toughening of carbon/epoxy composites. 4. Conclusions Interlayer toughening of carbon/epoxy composites was achieved by using polyetherketone cardo (PEK-C) nanofibre membranes electrospun directly onto carbon fabrics. With the same weight loading of nanofibres, finer nanofibre stabilised the crack propagation during delamination and assisted with maintaining the flexure property. With the same average fibre diameter (950 nm), increased nanofibre interlayer thickness led to enhanced Mode I delamination fracture toughness and reduced flexure strength. Glass transition temperatures of the cured epoxy did not drop until the interlayer thickness increased to 105 lm while the nanofibres with an average diameter of 950 nm were used. The phase structure generated from 1666 J. Zhang et al. / Composites Science and Technology 70 (2010) 1660–1666 phase separation was composed of fibrous PEK-C-rich macrophases and a continuous epoxy-rich macrophase, both of which consisted of microphases from secondary phase separation. Acknowledgements The authors would like to acknowledge the kind help from Mr. August Deveth for the fabrication of composite laminates. Funding support from Deakin University under the Central Research Grant scheme is acknowledged. References [1] Stevanovic D, Kalyanasundaram S, Lowe A, Jar PYB. Mode I and mode II delamination properties of glass/vinyl-ester composite toughened by particulate modified interlayers. Compos Sci Technol 2003;63:1949–64. [2] Tsotsis TK. Interlayer toughening of composite materials. Polym Compos 2009;30:70–86. [3] Quaresimin M, Varley RJ. Understanding the effect of nano-modifier addition upon the properties of fibre reinforced laminates. Compos Sci Technol 2008;68:718–26. [4] Lowe A. 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