Carbon nanofibers enhance the fracture toughness and fatigue performance of a structural epoxy system

This study investigates the monotonic and dynamic fracture characteristics of a discontinuous fiber reinforced polymer matrix. Specifically, small amounts (0-1 wt.%) of a helical-ribbon carbon nanofiber (CNF) were added to an amine cured epoxy system. The resulting nanocomposites were tested to failure in two modes of testing; Mode I fracture toughness and constant amplitude of stress tension-tension fatigue. Fracture toughness testing revealed that adding 0.5 and 1.0 wt.% CNFs to the epoxy matrix enhanced the resistance to fracture by 66% and 78%, respectively. Fatigue testing at 20 MPa peak stress showed a median increase in fatigue life of 180% and 365% over the control by the addition of 0.5 and 1.0 wt.% CNF, respectively. These results clearly demonstrate the addition of small weight fractions of CNFs to significantly enhance the monotonic fracture behavior and long-term fatigue performance of this polymer. A discussion is presented linking the two behaviors indicating their interdependence and reliance upon the stress intensity factor, K.     

A multiscale model to describe nanocomposite fracture toughness enhancement by the plastic yielding of nanovoids

The high fracture toughness improvements exhibited by nanofilled polymers is commonly thought of as due to the large amount of energy dissipated at the nanoscale.     

Simultaneously enhanced cryogenic tensile strength and fracture toughness of epoxy resins by carboxylic nitrile-butadiene nano-rubber

Epoxy resins are important matrices for composites. Carboxylic nitrile-butadiene nano-rubber (NR) particles are employed to improve the tensile strength and fracture toughness at 77 K of diglycidyl ether of bisphenol-F epoxy using diethyl toluene diamine as curing agent. It is shown that the cryogenic tensile strength and fracture toughness are simultaneously enhanced by the addition of NR. Also, the fracture toughness at room temperature (RT) is enhanced by the addition of NR. On the other hand, the tensile strength at RT first increases and then decreases with further increasing the NR content up to 5 phr. 5 phr NR is the proper content, which corresponds to the simultaneous enhancements in the tensile strength and fracture toughness at RT. Moreover, the comparison of mechanical properties between 77 K and room temperature indicates that the tensile strength, Young’s modulus and fracture toughness at 77 K are higher than those at RT but the failure strain shows the opposite results. The results are properly explained by the SEM observation.     

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.     

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.     

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.     

Modification of surface functionality of multi-walled carbon nanotubes on fracture toughness of basalt fiber-reinforced composites

In this work, we studied the influence of surface functionality of multi-walled carbon nanotubes (MWCNTs) on the mechanical properties of basalt fiber-reinforced composites. Acid and base values of the MWCNTs were determined by Boehm's titration technique. The surface properties of the MWCNTs were determined FT-IR, and XPS. The mechanical properties of the composites were assessed by measuring the interlaminar shear stress, fracture toughness, fracture energy, and impact strength. The chemical treatments led to a change of the surface characteristics of the MWCNTs and of the mechanical interfacial properties of MWCNTs/basalt fibers/epoxy composites. Especially the acid-treated MWCNTs/basalt fibers/epoxy composites had improved mechanical properties compared to the base-treated and non-treated MWCNTs/basalt fibers/epoxy composites. These results can probably be attributed to the improved interfacial bonding strength resulting from the improved dispersion and interfacial adhesion between the epoxy resin and the MWCNTs.     

Cyclic fatigue crack propagation of nanoparticle modified epoxy

An experimental study on the fatigue performance of nanoparticle modified epoxy was conducted. Seven material systems were examined which were: neat epoxy (E), 6 and 12 weight percent (wt.%) silica nanoparticle modified epoxy (S6, S12), 6 and 12 wt.% rubber nanoparticle modified epoxy (R6, R12), 3 wt.% each of silica and rubber nanoparticle modified epoxy (S3R3) and 6 wt.% each of silica and rubber nanoparticle modified epoxy (S6R6). Effects of those nanoparticles on the fatigue threshold (ΔG_th and ΔK_th) and fatigue crack propagation rates (da/dN) were studied. It was found that, compared to neat epoxy (E), nanosilica (S6, S12) increased ΔG_th (and ΔK_th) but nanorubber (R6 and R12) did not. However, a synergistic effect was observed on the fatigue threshold when both silica and rubber nanoparticles were added into epoxy. All these nanoparticles, individually or conjointly, decreased da/dN with silica the most effective. Morphology of the fracture surface was examined to understand the role of nanoparticles on toughening mechanisms under cyclic loading, which depended on the applied ΔG levels.     

Wear rate and fracture toughness of porous particle-filled phenol composites

We experimentally investigated the effects of filler volume fraction of the phenol composites filled with porous particles on the fracture toughness and the wear rate against a smooth metal surface under multi-pass condition. Porous particles, made from rice husks, of various volume fractions from 0 to 0.5 were added to phenol resin as carbon filler. For the reported results of adhesive wear under multi-pass condition, we correlated the bulk parameters associated with the fracture toughness to the wear rate. We found an empirical power–law relation between the reciprocal of the product of stress and strain at rupture in bending test and the wear rate with various filler volume fractions. We also proposed the modified mixture law of the wear rate by taking account of the area fraction of transfer layer, which can provide a good prediction of the filler volume fraction dependence.     

Fracture toughness of the nano-particle reinforced epoxy composite

Although thermoset polymers have been widely used for engineering components, adhesives and matrix for fiber-reinforced composites due to their good mechanical properties compared to those of thermoplastic polymers, they are usually brittle and vulnerable to crack. Therefore, ductile materials such as micro-sized rubber or nylon particles are added to thermoset polymers are used to increase their fracture toughness, which might decrease their strength if micro-sized particles act like defects.In this work, in order to improve the fracture toughness of epoxy adhesive, nano-particle additives such as carbon black and nanoclay were mixed with epoxy resin. The fracture toughness was measured using the single edge notched bend specimen at the room (25 °C) and cryogenic temperature (−150 °C). From the experimental results, it was found that reinforcement with nano-particles improved the fracture toughness at the room temperature, but decreased the fracture toughness at the cryogenic temperature in spite of their toughening effect.     

Nanostructured systems based on SBS epoxidized triblock copolymers and well-dispersed alumina/epoxy matrix composites

In the present research, the effect of addition of (1 wt.% and 3 wt.%) alumina nanoparticles (Al₂O₃) to epoxy modified by poly(styrene-b-butadiene-b-styrene) (SBS) epoxidized triblock copolymer was studied. The microstructure of final hybrid composites was studied with atomic force microscopy (AFM). Composites showed homogeneously dispersed Al₂O₃ nanoparticles in the epoxy matrix containing polystyrene (PS) microphase separated nanodomains. Dynamic mechanical analyses (DMA), flexural and fracture toughness investigations were carried out. The glass transition temperature of epoxy matrix has been retained unchanged by the addition of Al₂O₃ nanoparticles. The nanostructured epoxy systems based on SBS epoxidized triblock copolymer and well-dispersed Al₂O₃ nanoparticles allowed an increase in fracture toughness maintaining the transparency and stiffness of neat epoxy.     

Influence of electroless nickel-plating on fracture toughness of pitch-based carbon fibre reinforced composites

Nickel-Pitch-based carbon fibres (Ni-PFs) were prepared by electroless nickel-plating to enhance fracture toughness of Ni-PFs reinforced epoxy matrix composites (Ni-PFs/epoxy). The surface properties of Ni-PFs were determined by scanning electron microscopy (SEM), X-ray photoelectron spectrometry (XPS), and X-ray diffraction (XRD). The fracture toughness of the Ni-PFs/epoxy was assessed by critical stress intensity factor (K_IC) and critical strain energy release rate (G_IC). The fracture toughness of Ni-PFs/epoxy was enhanced compared to those of PFs/epoxy. These results were attributed to the increase of the degree of adhesion at interfaces between Ni-PFs and matrix resins in the composites.     

Nesting effect on the mode I fracture toughness of woven laminates

The fracture toughness of two woven laminates is evaluated for different nesting/shifting values between advanced layers. The analysed woven composites are manufactured using the same resin-reinforcement and same architecture, but have a different tow size (3K/12K). Three different nesting/shifting configurations are applied to the plies at the fracture surface: zero shifting, middle shifting and maximum shifting. Before being tested, the internal geometry of the material is evaluated and any shifting error is measured. For all these configurations mode I fracture tests are carried out. The differences obtained between 3K and 12K cases can be explained by fibre bridging, but not the differences between the nesting configurations. Depending on the nesting/shifting value the delaminated surface waviness is different, and consequently the fracture toughness is also influenced.     

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.     

Fracture mechanisms of epoxy filled with ozone functionalized multi-wall carbon nanotubes

This work focused on the fracture mechanisms and reinforcing effects of ozone-treated multi-walled carbon nanotubes (MWCNTs) in epoxy matrix. Ozone functionalization of MWCNTs was found to be of help for a better dispersion and stronger interfacial bonding with epoxy matrix, which in turn improve the strength and fracture toughness of the resin. The MWCNT/epoxy composites showed complicated failure modes than the conventional fibrous composites, which have been quantitatively investigated and correlated with the fracture toughness of the nanocomposites studied.     

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.     

A cut-ply specimen for the mixed-mode fracture toughness and fatigue characterisation of FRPs

The characterisation of mixed-mode fracture toughness and fatigue delamination growth in fibre-reinforced composites is crucial for assessing the integrity of structural elements in service. An asymmetric cut-ply coupon (ACP) loaded in four-point bending is here proposed to carry out the aforementioned characterisations. Analytical expressions of the energy release rate and mode-mixity for the ACP are derived and validated by means of finite element analysis. A fracture toughness and fatigue characterisation of the carbon/epoxy material IM7/8552 is carried out via ACP specimens. It is proved that the material data obtained from ACP specimens match those generated using ASTM standard mixed-mode bending (MMB) coupons. The main reason for the introduction of the ACP test resides in its applicability to characterisation scenarios where measuring the delamination length with optical means, as required for MMB coupons, is difficult. Such scenarios include the investigation of static and fatigue delamination growth at low and high temperatures, which requires the usage of environmental chambers. This poses significant constraints in terms of volume available for the test rigs, and, most importantly, limitations on visual access to observe delamination propagation. However, the manufacturing of ACP coupons is more complex than for MMB specimens and the testing requires several additional precautions that are here discussed in detail.     

The effect of PVDF nanofibers on mode-I fracture toughness of composite materials

In this study, the fracture behavior of carbon/epoxy laminates interleaved by polyvinylidene fluoride (PVDF) nanofibers is investigated. For this aim, a mode-I fracture test is conducted on virgin and modified laminates. Unlike the results of other studies, it is shown that PVDF nanofibers can increase mode-I fracture toughness (G_I) noticeably in a specific situation. The results show that G_I is enhanced about 43% and 36% in initiation and propagation stages of the fracture, respectively, using PVDF nanofibers. The morphology of the fractured surface is also presented for investigating the mechanism of toughening.     

A comparative study of the electrical and mechanical properties of epoxy nanocomposites reinforced by CVD- and arc-grown multi-wall carbon nanotubes

In this study, three different types of multi-wall carbon nanotubes (MWCNTs) were compared as nanostructured reinforcements in epoxy polymers: commercially available CVD-MWCNTs, synthesised in an industrial process, aligned-CVD-MWCNTs and arc-grown MWCNTs, both obtained from a lab-scale processes. The nanocomposite properties were characterised by means of electron microscopy, rheological, electrical and mechanical methods. Industrial CVD-MWCNTs are favourable for the implication of an electrical conductivity in the epoxy due to their high tendency to form conducting networks. The less entangled structure of aligned-CVD-MWCNTs turns out to be favourable for an easy dispersion and low viscosity in epoxy at similar conductivities compared to the CVD-MWCNTs. Additionally, they provide the highest increase in fracture toughness (∼17%). Arc-grown MWCNTs do not offer any electrical conductivity in epoxy without sufficient purification methods. Their high level of impurities and short length further complicate the transfer of their good electrical and mechanical properties into the nanocomposite.     

Interlaminar properties of carbon fiber composites with halloysite nanotube-toughened epoxy matrix

Halloysite nanotubes (HNTs), which are geometrically similar to multi-walled carbon nanotubes, can improve the impact strength of epoxy substantially, according to our previous work [1]. Using a HNT-toughened epoxy as the matrix, a set of hybrid composites was prepared with carbon fiber-woven fabrics. The interlaminar properties of the composites were investigated by a short-beam shear test, a double-cantilever-beam test and an end-notched flexure test. The results showed that the addition of HNTs to the composites improved the interlaminar shear strength and the fracture resistance under Mode I and Mode II loadings greatly. The morphological study of the hybrid composites revealed that HNTs were non-uniformly dispersed in the epoxy matrix, forming a unique microstructure with a large number of HNT-rich composite particles enveloped by a continuous epoxy-rich phase. A study of the fracture mechanism uncovered the important role of this special morphology during the fracturing of the hybrid composites.