Morphology and mechanical properties of nanostructured thermoset/block copolymer blends with carbon nanoparticles

Here we report the effect of multi-walled carbon nanotubes (MWCNTs) and thermally reduced graphene (TRG) on the miscibility, morphology and final properties of nanostructured epoxy resin with an amphiphilic poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) triblock copolymer. The addition of nanoparticles did not have any influence on the miscibility of PEO-PPO-PEO copolymer in the resin. However, MWCNTs and TRG reduced the degree of crystallinity of the PEO-rich microphases in the blends above 10 wt.% of copolymer while they did not change the phase morphology at the nanoscale, where PPO spherical domains of 20–30 nm were found in all the samples studied. A synergic effect between the self-assembled nanostructure and the nanoparticles on the toughness of the cured resin was observed. In addition, the nanoparticles minimized the negative effect of the copolymer on the elastic modulus and glass transition temperature in the resin.     

Phenoxy nanocomposite carriers for delivery of nanofillers in epoxy matrix for resin transfer molding (RTM)-manufactured composites

The use of phenoxy nanocomposite films as carriers of nanofillers involving multiwalled carbon nanotubes and nanoclays is successfully demonstrated for application in epoxy carbon fibers reinforced composites (CFRC) processed by RTM. Model studies on individual nanocomposite filaments embedded in epoxy precursors show that the nanofillers are passively transported by the interdiffusion gradient during heating over distance around 800 μm. A morphology gradient is generated after reaction induced phase separation and the nanofillers end up in the epoxy, despite their initial dispersion in the phenoxy. The proof of concept is extended to CFRC panels where nanocomposite phenoxy films are prepositioned between every odd carbon layer of the preform. Carbon nanotubes are filtered by the carbon fabrics, which limits their full diffusion and that of phenoxy through the preform. This has negative consequences on fracture toughness (G_Ic)_. For nanoclay, G_Ic is rather slightly improved although the origin is not fully clear.     

Hybrid effect of nanoparticles with carbon fibers on the mechanical and wear properties of polymer composites

Polyetheretherketone (PEEK) composites reinforced with carbon fibers (CFs) and nano-ZrO₂ particles were prepared by incorporating nanoparticles into PEEK/CF composites via twin-screw extrusion. The effects of nanoparticles on the mechanical and wear properties of the PEEK/CF composites were studied. The results showed that the incorporation of nano-ZrO₂ particles with carbon fiber could effectively enhance the tensile properties of the composites. The tensile strength and Young’s modulus of the composites increased with the increasing nano-ZrO₂ content. The enhancement effect of the particle was more significant in the hybrid reinforced composites. The compounding of the two fillers also remarkably improved the wear resistance of the composites under water condition especially under high pressures. It was revealed that the excellent wear resistance of the PEEK/CF/ZrO₂ composites was due to a synergy effect between the nano-ZrO₂ particles and CF. CF carried the majority of load during sliding process and prevented severe wear to the matrix. The incorporation of nano-ZrO₂ effectively inhibited the CF failures through reducing the stress concentration on the carbon fibers interface and the shear stress between two sliding surfaces. It was also indicated that the wear rates of the hybrid composites decreased with the increasing applied load and sliding distance under water lubrication. And low friction coefficient and low wear rate could be achieved at high sliding velocity.     

Effect of ZnO nanoparticles doped graphene on static and dynamic mechanical properties of natural rubber composites

In this work, effect of ZnO nanoparticles doped graphene (Nano-ZnO–GE) on static and dynamic mechanical properties of natural rubber composites were studied. Nano-ZnO–GE was synthesized by sol–gel method and thermal treatment. With the incorporation of nano-ZnO–GE into the matrix, the mechanical properties of NR nanocomposite significantly improved over that of NR composite containing with 5 phr of conventional-ZnO. The results demonstrated that the presence of nano-ZnO on the surface of graphene sheets not only conduces to suppressing aggregation of graphene sheets but also acts as a more efficient cure-activator in vulcanization process, with the formation of excellent crosslinked network at low nano-ZnO–GE content. This work also showed that NR/Nano-ZnO–GE nanocomposites exhibited higher wet grip property and lower rolling resistance compared with NR/Conventional-ZnO composite, which makes nano-ZnO–GE very competitive for the green tire application as a substitute of conventional-ZnO, enlarging versatile practical application to prepare high-performance rubber nanocomposites.     

Self-healing property of epoxy/nanoclay nanocomposite using poly(ethylene-co-methacrylic acid) agent

This paper investigates the self-healing repair of cracks in an epoxy/nanoclay nanocomposite using mendable poly[ethylene-co-methacrylic acid] (EMAA) particles. The effects of two different concentrations of EMAA agent on the self-healing efficiency were measured using single edge notch bar (SENB) testing. Inclusion of EMAA particles into the nanocomposite results an increase in the fracture strength and strain of the SENB specimens. Damaged SENBs were healed at 150 °C for 30 min to achieve up to 63% recovery in critical stress intensity and over 85% recovery in sustainable peak load. Also, X-ray diffraction (XRD) analysis and tensile test used in order to examine the nanocomposite structure and investigate the effects of EMAA inclusion on the nanocomposite mechanical properties. The pressure delivery mechanism of the healing agent is shown by scanning electron microscopy (SEM) images. It seems EMAA can be used as an effective self-healing agent for epoxy/nanoclay nanocomposites.     

Experimental investigation of composite lockbolt fastened joints under in-plane low velocity impact

Two different composite fastened configurations, i.e. the filled hole and the single-lap double-fastener joint, are experimentally investigated in tensile mode through different loading rates. The composite material system is the UD carbon/epoxy AS4/8552 and the coupons are fastened with titanium countersunk lockbolts. The experiments are performed in a range from quasi-static to 2.8 m/s impact velocity, using an innovative testing device developed and adapted in a drop tower machine. The main experimental observations are the limited loading rate sensitivity in terms of strength for both tested configurations, the elevated absorbed energy values in the dynamic tests of the lap joint samples, as well as the differences in their failure evolution and modes between quasi-static and impact loading.     

Microwave curing of carbon–epoxy composites: Penetration depth and material characterisation

Microwave heating has several major advantages over conventional conductive heating when used to cure carbon–epoxy composites, especially in speed of processing. Despite this and many other well-known advantages, microwave heating of carbon–epoxy composites has not taken off in industry, or even academia, due to the problems associated with microwave energy distribution, arcing, tool design and (ultimately) part quality and consistency, thus leading to a large scepticism regarding the technique/technology for heating such type of materials. This paper presents some evidence which suggests that with the correct hardware and operating procedure/methodology, consistent and high quality carbon–epoxy laminates can be produced, with the possibility of scaling up the process, as demonstrated by the micro- and macro-scale mechanical test results. Additionally, the author proposes a methodology to practically measure the maximum microwave penetration depth of a carbon–epoxy composite material.     

Toughening performance of glass fibre composites with core–shell rubber and silica nanoparticle modified matrices

The fracture energies of glass fibre composites with an anhydride-cured epoxy matrix modified using core–shell rubber (CSR) particles and silica nanoparticles were investigated. The quasi-isotropic laminates with a central 0°/0° ply interface were produced using resin infusion. Mode I fracture tests were performed, and scanning electron microscopy of the fracture surfaces was used to identify the toughening mechanisms.The composite toughness at initiation increased approximately linearly with increasing particle concentration, from 328 J/m² for the control to 842 J/m² with 15 wt% of CSR particles. All of the CSR particles cavitated, giving increased toughness by plastic void growth and shear yielding. However, the toughness of the silica-modified epoxies is lower as the literature shows that only 14% of the silica nanoparticles undergo debonding and void growth. The size of CSR particles had no influence on the composite toughness. The propagation toughness was dominated by the fibre toughening mechanisms, but the composites achieved full toughness transfer from the bulk.     

Mode III interlaminar fracture of carbon/epoxy laminates using the Six-Point Edge Crack Torsion (6ECT)

The recently proposed Six-Point Edge Crack Torsion (6ECT) test was used to evaluate the mode III interlaminar fracture of carbon/epoxy laminates. Plate specimens with starter delaminations in 0/0, 0/90 and 0/45 interfaces were tested. Data reduction was performed with an effective crack scheme validated in a previous numerical study. The tests allowed the evaluation of fairly unambiguous initiation G_IIIC values and of subsequent R-curves. Examinations of specimen cross-section showed considerable lengths of pure interlaminar propagation in specimens with starter delaminations in 0/90 and 0/45 interfaces. The latter specimens had the lowest initiation G_IIIC values.     

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

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

Effect of graphene oxide on the physical,mechanical and thermo-mechanical properties of neoprene and chlorosulfonated polyethylene vulcanizates

The present research work demonstrated the effect of graphene oxide (GO) on the physical, mechanical, thermo-mechanical etc., properties of neoprene (CR) and chlorosulfonated polyethylene (CSPE) vulcanizates. CR and CSPE based nanocomposites were prepared by both solution intercalation and melt intercalation methods. The changes obtained in the morphology, cure characteristics, mechanical, thermal, thermo-mechanical properties of the rubber nanocomposites have been widely investigated. X-ray diffraction analysis (XRD) and transmission electron microscopic (TEM) analysis of the samples revealed partial exfoliated structure of GO containing rubber composites. Mechanical, thermal, cure and thermo-mechanical properties of the elastomeric nanocomposites were improved compared to the neat rubbers.     

Influence of plastic deformation on single-fiber push-out tests of carbon fiber reinforced epoxy resin

In our study we present a procedure to measure and analyze single-fiber push-out force–displacement curves on carbon fiber reinforced polymers using a cyclic loading–unloading scheme. The measured cyclic force–displacement curves allow an energy-based evaluation of the interfacial failure, taking into account elastic, plastic and other dissipative energy contributions. Experimental and modeling results demonstrate that a deviation of the push-out curve from linear behavior does not correspond to crack opening but to a plastic deformation of the matrix. Evaluating the plastic energy yields a linear increase of the total plastic energy after a certain indenter displacement. This linear increase is attributed to stable crack propagation. Back-extrapolation of the linear part to zero total plastic energy using a linear regression yields the initiation of crack growth. It is concluded that for ductile matrix materials like polymers, a reliable interpretation of push-out data has to take into account plastic material deformation.     

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

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

Interfacial properties and impact toughness of methylphenylsilicone resin composites by chemically grafting POSS and tetraethylenepentamine onto carbon fibers

Octaglycidyl polyhedral oligomeric silsesquioxane (gly-POSS) was successfully grafted on carbon fibers (CFs) surface to enhance interfacial properties and impact toughness of CFs reinforced methylphenylsilicone resin (MPSR) composites. After gly-POSS modification, POSS grafted CF (CF-POSS) with many epoxy functional groups was modified with tetraethylenepentamine (TEPA) to further enhance the interfacial strength. Atomic force microscopy (AFM) images showed that POSS and TEPA were grafted onto CFs surface uniformly and the surface roughness enhanced obviously. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) confirmed the chemical bonding nature between CFs and POSS, as well as between POSS and TEPA. POSS and TEPA modification could increase the fiber polarity, wettability and surface energy significantly. The interlaminar shear strength (ILSS) and impact toughness of composites showed a dramatic improvement, especially for grafting with POSS and further with TEPA (CF-POSS-TEPA). Additionally, the reinforcing and toughening mechanisms were also analyzed. Meanwhile, single fiber tensile strength (TS) had no decrease after modification.     

Evaluation of impact damage mechanism of multi-axial stitched CFRP laminate

This study focuses on multi-axial stitched fabric, which is a thick, high performance reinforcement for large-scale composite structures. The effects of impact damage on multi-axial stitched CFRP laminates molded by vacuum-assisted resin transfer molding (VARTM) method were evaluated. Impact damage within material was evaluated by ultrasonic scanning device and optical cross-sectional observations. Probed images obtained by both non-destructive and destructive methods were compared, and internal damage distributions of multi-axial stitched CFRP laminates were clarified. In addition, residual compressive strength and fatigue property of impact-damaged CFRP laminates were evaluated by in situ damage growth monitoring using the thermo-elastic stress analyzer (TESA). Three-dimensional damage distribution of impacted CFRP laminate was obtained from ultrasonic C-scan images and cross-sectional photographs. Damage progress behavior was observed on a destructive and non-destructive basis by post-impact fatigue (PIF) test.     

An efficient healing agent for high temperature epoxy composites based upon tetra-glycidyl diamino diphenyl methane

Poly(ethylene-co-methacrylic acid) (EMAA) as a thermally activated healing agent in a high performance, high temperature tetra-glycidyl methylene dianiline (TGDDM)/diethyl toluene diamine (DETDA) mendable epoxy composite is reported for the first time. Despite curing above EMAAs melting point (T_m = 85 °C), healing occurred by incorporating a preliminary low temperature curing step of 5 h at 80 °C, prior to cure at 177 °C. Healing occurred via the pressure delivery mechanism derived from tertiary amine catalysed surface condensation reactions between EMAA and hydroxyl groups from the epoxy resin. Healing efficiencies of 36%, 55% and 105% were achieved after heating at 150 °C, 200 °C and 230 °C respectively, but decreased rapidly with continued healing. Healing at 150 °C and 200 °C revealed significant healing despite remaining in the glassy state. In addition, EMAA enhanced mode I interlaminar fracture toughness by more than 270% for both the DETDA and 4,4-DDS networks.     

Tribo-mechanical characterization of reinforced epoxy resin under dry and lubricated contact conditions

The aim of the present work is to investigate the influence of the reinforcing material and architecture on the voids content, mechanical properties and tribological behavior of fiber reinforced epoxy composite laminates manufactured by VARTM under different processing conditions. Two different textile architectures, namely unidirectional non-crimp fabrics (UD) and 0/90 plain wave (PW), were considered, reinforcing an EPIKOTE RIMR 135 epoxy matrix with glass (GF) as well as carbon (CF) continuous fibers. Optical observations revealed an unexpected trend relatively to the intra- and inter-bundle voids concentration with respect to the impregnation velocity, especially using UD-CF and UD-GF reinforcements and low impregnation rate. Tensile and three points bending tests highlighted the dominant role of fiber material and architecture on mechanical properties, whereas the presence of voids played a minor role with respect to the analyzed features. Tribological outcomes evidenced a reduction of the friction coefficient (μ) when the resin is reinforced by carbon or glass fibers. The lowest values were detected when the sliding direction of the counterbody is oriented parallel to the fiber direction for UD samples. Further reduction of μ, for both UD and PW specimens, was obtained by interposing a lubricant at the interface.     

Enhancement of dielectric and electrical properties in BT/SiC/PVDF three-phase composite through microstructure tailoring

A polymer composite with high dielectric permittivity was prepared by embedding silicon carbide (SiC) whisker with an average diameter of 500 nm–1 μm in poly(vinylidene fluoride) (PVDF). However, the high dielectric loss and electrical conductivity of the two-phase composite prohibits its potential applications. Barium titanate (BT) particles with average diameter of 100 nm and 1 μm were incorporated as a third phase to fabricate a three-phase composite. The morphology structure, dielectric and electrical properties before and after the addition of BT particles were investigated. The three-phase composite exhibits largely suppressed dielectric loss and electrical conductivity without sacrificing the high dielectric permittivity, which was extremely hard to be realized for two-phase composite. It is also found that the nano-size BT is more favorable in achieving high dielectric permittivity than the micro-size BT, where their dielectric loss and electrical conductivity are similar. Furthermore, electric modulus analysis confirms the largely suppressed electron conduction process which results in the enhanced dielectric and electrical properties in three-phase composite.     

Elastic behaviour and failure mechanism in epoxy syntactic foams: The effect of glass microballoon volume fractions

A representative elementary volume (REV) in epoxy syntactic foams was generated to incorporate randomly distributed glass microballoons that followed a log-normal size distribution. Finite element modelling of the REV foam was developed and experimentally validated to investigate the elastic behaviour and failure mechanism in the foams with different microballoon volume fractions (V). The localised stresses concentrate in various zones within the foam, and can cause the vertical splitting fracture of microballoons and the micro-crack formation in the matrix. Dependent on the microballoon volume fraction, micro-cracks can propagate to join adjacent micro-cracks and voids left by fractured microballoons, and finally develop into a macro-crack either in the preferred longitudinal (for low V) or diagonal (for high V) directions. This is consistent with the macroscopic observations of the fracture process in the foam specimens. It was also found that elastic characteristics of the foam vary with microballoon volume fractions.     

Toughening modification of polycarbonate/poly(butylene terephthalate) blends achieved by simultaneous addition of elastomer particles and carbon nanotubes

Small quantities of maleic anhydride grafted styrene-ethylene-butylene-styrene (SEBS-g-MAH) copolymer and carbon nanotubes (CNTs) were introduced into polycarbonate (PC)/poly(butylene terephthalate) (PBT) blends. The results demonstrated that simultaneously adding SEBS-g-MAH and CNTs greatly enhanced the fracture toughness of the samples and the impact strength increased with increasing CNT content. The morphologies, the dispersion of CNTs, the relaxation behaviors and the crystallization behaviors of samples were systematically investigated. SEBS-g-MAH formed the dispersed particles in the system. The particle diameter was decreased in the blend composites. CNTs exhibited homogeneous dispersion in the blend composites and they also formed a percolated network structure at relatively high content. The transesterification between PC and PBT components was suppressed by SEBS-g-MAH, and the crystallization ability of the PBT component was greatly enhanced. The toughening mechanisms were mainly related to the suppressed transesterification, the decreased elastomer particle size, and the formation of a CNT network structure.