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.     

Assessment of three oxide/oxide ceramic matrix composites: Mechanical performance and effects of heat treatments

Mechanical performance of three oxide/oxide ceramic matrix composites (CMCs) based on Nextel 610 fibers and SiOC, alumina, and mullite/SiOC matrices respectively, is evaluated herein. Tensile strength and stiffness of all materials decreased at 1000 °C and 1200 °C, probably because of degradation of fiber properties beyond 1000 °C. Microstructural changes in the composites during exposure at 1000 °C and 1200 °C for 50 h reduce their flexural strength, fracture toughness and work of fracture. A literature review regarding mechanical properties of several oxide/oxide CMCs revealed lower influence of fiber properties on composite strength compared with elastic modulus. The tested composites exhibit comparable stiffness and strength but higher fracture toughness compared with average values determined from a literature review. Considering CMCs with different compositions, we observed an interesting linear trend between strength and fracture toughness. The validity of the linear relationship between fracture strength and flexural toughness for CMCs is discussed.     

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

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

Silane modification on mesoporous silica coated carbon nanotubes for improving compatibility and dispersity in epoxy matrices

A simple synthetic method for placing a mesoporous silica coating on multi-wall carbon nanotubes (CNTs@MS) was developed to improve the surface compatibility with regard to a polar epoxy matrix. In addition, the mesoporous silica shell with silanol groups on the CNTs provides a platform to attach silane molecules (e.g. 3-glycidoxypropyltrimethoxysilane, GPTMS) that enable the CNTs@MS to be incorporated into the epoxy matrix at a content of up to 20 wt.%. The viscosities of the CNTs@MS- and GPTMS-modified-CNTs@MS–epoxy composites are much lower than that of the CNTs–epoxy, and then the voids in the GPTMS-modified-CNTs@MS–epoxy composites are most significantly reduced. The effects of the CNTs@MS and GPTMS-modified CNTs@MS on the mechanical and thermal properties of the epoxy composite are investigated. The results show that the GPTMS-modified CNTs@MS improved the filler–epoxy matrix interaction, and has better compatibility in epoxy than the CNTs@MS. As the surface compatibility and interaction strength increase in the epoxy matrix, the enhancement in storage modulus, thermal conductivity and reduction in the coefficient of thermal expansion are in the following order: GPTMS-modified CNTs@MS > CNTs@MS ≫ CNTs.     

Size-scale effects of silica on bis-GMA/TEGDMA based nanohybrid dental restorative composites

The present study focuses on the effect of size-scale combination of silica on the mechanical and dynamic mechanical properties of acrylate based (50% Bis-GMA and 50% TEGDMA by weight) composites with an aim to overcome the conventional problem of high-volume fraction filling of acrylate based composites, typically used in restorative dentistry. Two classes of light-cured composites based on the size-scale combination of silica (7 nm + 2 μm; 14 nm + 2 μm) as the filler were prepared. FTIR spectroscopy revealed functionality and interactions whereas morphological investigations concerning the state of distribution and dispersion of nano- and micro-silica has been carried out by SEM–EDX Si-dot mapping. The dynamic mechanical properties, compressive, flexural and diametral tensile strengths were characterized. Micromechanical analysis of viscoelastic storage moduli following Kerner composite model has revealed an enhancement in the reinforcement efficiency of the nanohybrid composites based on the filler size-scale combination of 14 nm + 2 μm with 10 wt.% nanofiller loading. The compressive strength of the micro-filled composite (with 2 μm silica only) was found to remain comparable to that of the nanohybrid with 5 wt.% of 7 nm silica and 10 wt.% of 14 nm silica filled composites. Diametral tensile strength has been observed to be influenced by the size-scale combination and extent of nanofiller loading. The effective volume fractions in the composites validating the experimentally determined DTS were calculated following Nicolais–Narkis model. Our study demonstrates the conceptual feasibility of exploring the optimization of size-scale combinations of filler for enhancement in reinforcement efficiency by manipulating the volume fraction of filler induced immobilized polymer chains by resorting to the principle of micromechanics.     

Thermal conductivity of Cu/diamond composites prepared by a new pretreatment of diamond powder

Cu/diamond composites were fabricated by spark plasma sintering (SPS) after the surface pretreatment of the diamond powders, in which the diamond particles were mixed with copper powder and tungsten powder (carbide forming element W). The effects of the pretreatment temperature and the diamond particle size on the thermal conductivity of diamond/copper composites were investigated. It was found that when 300 μm diamond particles and Cu–5 wt.% W were mixed and preheated at 1313 K, the composites has a relatively higher density and its thermal conductivity approaches 672 W (m K)⁻¹.     

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.     

Synthesis and properties of sandwiched films of epoxy resin and graphene/cellulose nanowhiskers paper

Graphene (GN)-based composite paper containing 10 wt.% cellulose nanowhiskers (CNWs) exhibiting a tensile strength of 31.3 MPa and electrical conductivity of 16 800 S/m was prepared by ultrasonicating commercial GN powders in aqueous CNWs suspension. GN/CNWs freestanding paper was applied to prepare the sandwiched films by dip coating method. The sandwiched films showed enhanced tensile strength by over two times higher than the neat resins. The moduli of the sandwiched films were around 300 times of the pure resins due to the high content of GN/CNWs paper. The glass transition temperature of the sandwiched films increased from 51.2 °C to 57.1 °C for pure epoxy (E888) and SF (E888), and 49.8 °C to 64.8 °C for pure epoxy (650) and SF (650), respectively. The bare conductive GN/CNWs paper was well protected by the epoxy resin coating, which is promising in the application as anti-static materials, electromagnetic interference (EMI) shielding materials.     

Dynamic fracture of carbon nanotube/epoxy composites under high strain-rate loading

We investigate dynamic fracture of three types of multiwalled carbon nanotube (MWCNT)/epoxy composites and neat epoxy under high strain-rate loading (${10}^5''–''{10}^6$ s⁻¹). The composites include randomly dispersed, 1 wt%, functionalized and pristine CNT/epoxy composites, as well as laminated, ∼50 wt% CNT buckypaper/epoxy composites. The pristine and functionalized CNT composites demonstrate spall strength and fracture toughness slightly higher and lower than that of neat epoxy, respectively, and the spall strength of laminated CNT buckypaper/epoxy composites is considerably lower; both types of CNTs reduce the extent of damage. Pullout, sliding and immediate fracture modes are observed; the fracture mechanisms depend on the CNT–epoxy interface strength and fiber strength, and other microstructures such as the interface between CNT laminates. Compared to the functionalized CNT composites, weaker CNT–epoxy interface strength and higher fiber strength lead to a higher probability of sliding fracture and higher tensile strength in the pristine CNT composites at high strain rates. On the contrary, sliding fracture is more pronounced in the functionalized CNT composites under quasistatic loading, a manifestation of a loading-rate effect on fracture modes. Despite their helpful sliding fracture mode and large CNT content, the weak laminate–laminate interfaces play a detrimental role in fracture of the laminated CNT buckypaper/epoxy composites. Regardless of materials, increasing strain rates leads to pronounced rise in tensile strength and fracture toughness.     

Preparation of YAG gel coated ZrB2–SiC composite prepared by gelcasting and pressureless sintering

In this paper, gelcasting and pressureless sintering of YAG gel coated ZrB₂–SiC (YZS) composite were conducted. YAG gel coated ZrB₂–SiC (YZS) suspension was firstly prepared through sol–gel route. Poly (acrylic acid) was used as dispersant. YZS suspension had the lowest viscosity when using 0.6 wt.% PAA as dispersant. Gelcasting was conducted based on AM–MBAM system. The gelcast YZS sample was then pressureless sintered to about 97% density. During sintering, YAG promoted the densification process from solid state sintering to liquid phase sintering. The average grain sizes of ZrB₂ and SiC in the YZS composite were 3.8 and 1.3 μm, respectively. The flexural strength, fracture toughness and microhardness were 375 ± 37 MPa, 4.13 ± 0.45 MPa m^1/2 and 14.1 ± 0.5 GPa, respectively.     

Strain and damage monitoring in carbon-nanotube-based composite under cyclic strain

The resistive behavior of multi-walled carbon nanotube (MWCNT)/epoxy resins, tested under mechanical cycles and different levels of applied strain, was investigated for specimens loaded in axial tension. The surface normalized resistivity is linear with the strain for volume fraction of MWCNTs between 2.96 × 10⁻⁴ and 2.97 × 10⁻³ (0.05 and 0.5% wt/wt). For values lower than 0.05% wt/wt, close to the electrical percolation threshold (EPT) a non-linear behavior was observed. The strain sensitivity, in the range between 0.67 and 4.45, may be specifically modified by controlling the nanotube loading, in fact the sensor sensitivity decreases with increasing the carbon nanotubes amount. Microscale damages resulted directly related to the resistance changes and hence easily detectable in a non-destructive way by means of electrical measurements. In the fatigue tests, the damage is expressed through the presence of a residual resistivity, which increases with the amount of plastic strain accumulated in the matrix.     

Fracture analysis of epoxy/SWCNT nanocomposite based on global–local finite element model

A global–local multiscale finite element method (FEM) is proposed to study the interaction of nanotubes and matrix at the nanoscale near a crack tip. A 3D FE model of a representative volume element (RVE) in crack tip is built. The effects of the length and chirality of single walled carbon nanotube (SWCNT) in a polymer matrix on the fracture behavior were studied in the presence of van der Waals (vdW) interaction as inter-phase region. Detailed results show that with increasing the weight percentage of SWCNT, fracture toughness improves. Three situations of nanotube directions with respect to crack are considered. Results show that bridging condition has minimum stress intensity factor. In addition, it can be seen that the crack resistance improves by increasing the length and chirality for all kinds of nanotubes. Finally, epoxy/SWCNT 10 wt.% has lower stress intensity factor compared to epoxy/halloysite 10 wt.% in similar loading state.     

An investigation of the effect of SiC particle size on Cu–SiC composites

In this study mechanical properties of copper were enhanced by adding 1 wt.%, 2 wt.%, 3 wt.% and 5 wt.% SiC particles into the matrix. SiC particles of having 1 μm, 5 μm and 30 μm sizes were used as reinforcement. Composite samples were produced by powder metallurgy method and sintering was performed in an open atmospheric furnace at 700 °C for 2 h. Optical and SEM studies showed that the distribution of the reinforced particle was uniform. XRD analysis indicated that the dominant components in the sintered composites were Cu and SiC. Relative density and electrical conductivity of the composites decreased with increasing the amount of SiC and increased with increasing SiC particle size. Hardness of the composites increased with both amount and the particle size of SiC particles. A maximum relative density of 98% and electrical conductivity of 96% IACS were obtained for Cu–1 wt.% SiC with 30 μm particle size.     

Survival of actively cooled microvascular polymer matrix composites under sustained thermomechanical loading

Exposure to high heat can cause polymer matrix composites (PMC) to fail under mechanical loads easily sustained at room temperature. However, heat is removed and temperature reduced in PMCs by active cooling through an internal vascular network. Here we compare structural survival of PMCs under thermomechanical loading with and without active cooling. Microchannels are incorporated into autoclave-cured carbon fiber/epoxy composites using sacrificial fibers. Time-to-failure, material temperature, and heat removal rates are measured during simultaneous heating on one face (5–75 kW/m²) and compressive loading (100–250 MPa). The effects of applied compressive load, heat flux, channel spacing, coolant flow rate, and channel distance from the heated surface are examined. Actively cooled composites containing 0.33% channel volume fraction survive without structural failure for longer than 30 min under 200 MPa compressive loading and 60 kW/m² heat flux. In dramatic comparison, non-cooled composites fail in less than a minute under the same loading conditions.     

Nano-epoxy resins containing electrospun carbon nanofibers and the resulting hybrid multi-scale composites

For the first time, electrospun carbon nanofibers (ECNFs, with diameters and lengths of ∼200 nm and ∼15 μm, respectively) were explored for the preparation of nano-epoxy resins; and the prepared resins were further investigated for the fabrication of hybrid multi-scale composites with woven fabrics of conventional carbon fibers via the technique of vacuum assisted resin transfer molding (VARTM). For comparison, vapor growth carbon nanofibers (VGCNFs) and graphite carbon nanofibers (GCNFs) were also studied for making nano-epoxy resins and hybrid multi-scale composites. Unlike VGCNFs and GCNFs that are prepared by bottom-up methods, ECNFs are produced through a top-down approach; hence, ECNFs are more cost-effective than VGCNFs and GCNFs. The results indicated that the incorporation of a small mass fraction (e.g., 0.1% and 0.3%) of ECNFs into epoxy resin would result in substantial improvements on impact absorption energy, inter-laminar shear strength, and flexural properties for both nano-epoxy resins and hybrid multi-scale composites. In general, the reinforcement effect of ECNFs was similar to that of VGCNFs, while it was higher than that of GCNFs.     

Mechanical performance of epoxy matrix hybrid nanocomposites containing carbon nanotubes and nanodiamonds

A novel class of epoxy matrix hybrid nanocomposites has been developed containing multiwalled carbon nanotubes (MWCNTs) and nanodiamonds (NDs) to explore the combined effect of nanoreinforcements on the mechanical performance of nanocomposites. Both the nanofillers were functionalized before incorporating into epoxy matrix to promote interfacial interactions. The concentrations of both MWCNTs and NDs in the nanocomposites were increased systematically, i.e. 0.05 wt.%, 0.1 wt.% and 0.2 wt.% while composites containing individual nanoreinforcements were also manufactured for comparison. The developed nanocomposites were characterized microstructurally by scanning electron microscopy (SEM) and mechanically by tensile, flexural, impact and hardness tests. Homogeneous dispersion of MWCNTs and NDs was observed under SEM, which resulted in the enhancement of mechanical properties of nanocomposites. The composites containing 0.2 wt.% MWCNTs and 0.2 wt.% NDs showed 50% increase in hardness while tensile strength and modulus enhanced to 70% and 84%, respectively. Flexural strength and modulus also showed a rise of 104% and 56%, respectively. Interestingly, fracture strain also increased in both the tensile and flexural testing. The impact resistance increased to 161% showing a significant improvement in the toughness of hybrid nanocomposites.     

Advanced multifunctional properties of aligned carbon nanotube-epoxy thin film composites

Carbon nanotube (CNT)/epoxy composite films were successfully developed by a combination of layer-by-layer and vacuum-assisted resin transfer molding methods using directly chemical vapor deposition (CVD)-spun CNT plies. CNT fractions in the composite films were found to be dramatically enhanced as the number of CNT plies increased. The as-prepared CNT/epoxy composite films with 24.4 wt.% CNTs exhibited ~ 10 and ~ 5 times enhancements in their strength and Young's modulus, respectively, and high toughness of up to 6.39 × 10³ kJ/m³. Electrical conductivity reached 252.8 S/cm for the 20-ply CNT/epoxy films, which was 20 times higher over those of the CNT/epoxy composites obtained by conventional dispersion methods. This work proposed a route to fabricate high-CNT-fraction CNT/epoxy composites on a large scale. The high toughness of these CNT/epoxy composite films also makes them promising candidates as protective materials.     

Effect of alkali treatment on interfacial bonding in abaca fiber-reinforced composites

Abaca fibers demonstrate enormous potential as reinforcing agents in composite materials. In this study, abaca fibers were immersed in 5, 10 or 15 wt.% NaOH solutions for 2 h, and the effects of the alkali treatments on the mechanical characteristics and interfacial adhesion of the fibers in a model abaca fiber/epoxy composite system systematically evaluated. After 5 wt.% NaOH treatment, abaca fibers showed increased crystallinity, tensile strength and Young’s modulus compared to untreated fibers, and also improved interfacial shear strength with an epoxy. Stronger alkali treatments negatively impacted fiber stiffness and suitability for composite applications. Results suggest that mild alkali treatments (e.g. 5 wt.% NaOH for 2 h) are highly beneficial for the manufacture of abaca fiber-reinforced polymer composites.     

Improved cryogenic interlaminar shear strength of glass fabric/epoxy composites by graphene oxide

The cryogenic interlaminar shear strength (ILSS) at cryogenic temperature (77 K) of glass fabric (GF)/epoxy composites is investigated as a function of the graphene oxide (GO) weight fraction from 0.05 to 0.50 wt% relative to epoxy. For the purpose of comparison, the ILSS of the GF/epoxy composites is also examined at room temperature (RT, 298 K). The results show that the cryogenic ILSS is greatly improved by about 32.1% and the RT ILSS is enhanced by about 32.7% by the GO addition at an appropriate content of 0.3 wt% relative to epoxy. In addition, the ILSS of the composite at 77 K is much higher than that at RT due to the relatively strong interfacial GF/epoxy adhesion at 77 K compared to the RT case.     

Fabrication and characterization of 3-D Cf/ZrC composites by low-temperature liquid metal infiltration

Three-dimensional braided carbon fiber-reinforced ZrC matrix composite, 3-D C_f/ZrC, were prepared by liquid metal infiltration process at 1200 °C using a Zr₂Cu intermetallic compound as infiltrator. The microstructure and properties of the composites were investigated. The results indicated that ZrC with a yield of 35.2 ± 1.8 vol.% was certified as the major phase of the composites. The formation of ZrC was controlled by a solution-precipitation mechanism. The obtained composites exhibited good mechanical properties, with a flexural strength of 293.0 ± 12.1 MPa, a flexural modulus of 82.7 ± 6.4 GPa and a fracture toughness of 9.8 ± 0.9 MPa m^1/2. The mass and linear ablation rates of the composites exposed to oxyacetylene torch were 0.0013 ± 0.0005 g s⁻¹ and −0.0009 ± 0.0003 mm s⁻¹, respectively. The formation of a dense ZrO₂ protective layer and the evaporation of residual Cu contributed mainly to the excellent ablation resistance.