Effect of processing temperature on the micro- and macro-interfacial properties of carbon fiber/epoxy composites

Three different temperature schemes were applied on carbon fiber/epoxy composite to elucidate the effect on interfacial shear strength (IFSS) and inter-laminar shear strength (ILSS). It showed that carbon fiber/epoxy IFSS was significantly influenced by the processing temperature, while ILSS was only slightly changed. Moreover, the mechanical properties revealed no necessary relationship between the micro- and macro-interfacial strengths with the properties of epoxy matrix. Among all the temperature schemes, Pro2 (the one-platform curing scheme with relatively rapid heating rate) produced highest IFSS and ILSS. Fourier transform infrared spectroscopy analysis demonstrated that the sizing agent can chemically react itself and also react with epoxy resin at temperature 180?°C. The resin rheological data showed that different temperature schemes can considerably impact diffusion behavior of the resin molecules. Hence, the highest interfacial strengths for Pro2 scheme were ascribed to large extent of chemical reactions and good inter-diffusion between components, at the interface region.     

Preparation and Characterization of Linear Low Density Polyethylene/Carbon Nanotube Nanocomposites

Linear low‐density polyethylene (LLDPE)/multiwalled carbon nanotube (MWNT) nanocomposites were prepared via melt blending. The morphology and degree of dispersion of nanotubes in the polyethylene matrix were investigated using scanning electron microscopy (SEM). Both individual and agglomerates of MWNTs were evident. The rheological behavior and mechanical and electrical properties of the nanocomposites were studied using a capillary rheometer, tensile tester, and Tera ohm‐meter, respectively. Both polyethylene and its nanocomposites showed non‐Newtonian behavior in almost the whole range of shear rate. Addition of carbon nanotubes increased shear stress and shear viscosity. It was also found that the materials experience a fluid‐solid transition below 1 wt% MWNT. Flow activation energy for the nanocomposites was calculated using an Arrhenius type equation. With increasing nanotube content, the activation energy of flow increases. A decrease of about 7 orders of magnitude was obtained in surface and volume resistivity upon addition of 5 wt% MWNT. In addition, a difference between electrical and rheological percolation thresholds was observed. The results confirm the expected nucleant effect of nanotubes on the crystallization process of polyethylene. A slight increase in Young's modulus was also observed with increasing MWNT content.     

Improving the performance of conventional glass fiber epoxy matrix composites by incorporating nanodiamonds

Multiscale glass fiber epoxy matrix composites containing nanodiamonds were fabricated using vacuum bagging technique. Three different loadings of nanodiamonds were incorporated in epoxy resin after their functionalization through ozone-treatment, i.e., 0.1, 0.3 and 0.5 wt%. The functionalization of nanodiamonds was confirmed by infrared spectroscopy, which improved the dispersion of nanodiamond in epoxy resin thus improving the mechanical properties. Tensile, compression, flexural and interlaminar shear properties of the composites were improved. The tensile, compression and flexural strengths improved up to 36, 56 and 30% by the addition of 0.5 wt% nanodiamonds while the corresponding moduli increased to 30, 125 and 46%, respectively. An improvement of 38% in interlaminar shear strength was observed. The microscopy of the composites was performed using optical and electron microscopy and proper impregnation of glass fibers and the absence of the agglomerates of nanodiamonds were ensured. The homogeneous dispersion of nanodiamonds and their adhering role at fiber/matrix interface improved the mechanical properties of the composites. The developed composites are ideal candidate materials for engineering applications demanding high specific mechanical properties.     

The Effect of Triethylene-Tetramine Treatment of Carbon Fibers on Performance of Composites

Amino groups can be introduced to the surface of carbon fibers (CF) by triethylene-tetramine (TETA) treatment. Carbon fibers coated with triethylene-tetramine (TETA) were treated at 400°C for 30 s in an oxidizing furnace. Differential scanning calorimetry studies showed that the surface functional groups of CF reacted with TETA. The changes of the surface composition and structure of CF were tested by X-ray photoelectron spectrometry (XPS). The interfacial interaction between the resulting CF and an epoxy matrix was also characterized by scanning electron microscopy (SEM) and three-point short-beam shear testing. The XPS results indicate that the number of amino groups on the surface of the CF was significantly increased after being treated with TETA. The interlaminar shear strength (ILSS) of TETA-treated CF-reinforced resin composites (CFRP) was increased by 30% compared with untreated ones, and in the treated CF fracture sections, CFRP pores and carbon fiber pullout were seldom observed. The failure of composites reinforced by treated CF shows a cohesive failure effect in the interface layer.     

Supercritical fluid-assisted synthesis of a carbon nanotubes-grafted biocompatible polymer composite

A nanocomposite consisting of multi-wall nanotubes (MWNTs) grafted with a biocompatible polymer poly(2-hydroxyethyl methacrylate) was prepared by in situ polymerization in supercritical carbon dioxide. The surface of the MWNTs was first surface modified with hydroxyl groups in the solution of KMnO₄ and a phase-transfer catalyst. MWNT-OH was then functionalized with vinyl groups using a silane coupling agent, γ-methacryloxypropyltrimethoxysilane. The silane groups can improve the dipersion of MWNTs in supercritical carbon dioxide, while the terminal vinyl groups help fabricate polymer chains on the MWNT surface. The as-synthesized products were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and thermo-gravimetric analysis. The SEM and TEM images showed that the nanotubes were well coated with the polymer shell. The composite had higher thermal stability than the pure polymer and dispersed well in methanol. This biocompatible polymer composite was prepared using a green method and is expected to be useful as a biomaterial composite with potential applications in the biological field.     

Performance of glass woven fabric composites with admicellar-coated thin elastomeric interphase

Adequate stress transfer between the inorganic reinforcement and surrounding polymeric matrix is essential for achieving enhanced structural integrity and extended lifetime performance of fiber-reinforced composites. The insertion of an elastomeric interlayer helps increase the stress-transfer capabilities across the fiber/matrix interface and considerably reduces crack initiation phenomena at the fiber ends. In this study, admicellar polymerization is used to modify the fiber/matrix interface in glass woven fabric composites by forming thickness-controlled poly(styrene-co-isoprene) coatings. These admicellar interphases have distinct characteristics (e.g. topology and surface coverage) depending on the surfactant/monomer ratios used during the polymerization reaction. Overall, the admicellar coatings have a positive effect on the mechanical response of resin transfer molded, E-glass/epoxy parts. For instance, ultimate tensile strength of composites with admicellar sizings improved 50–55% over the control-desized samples. Interlaminar shear strength also showed increases ranging from 18 to 38% over the same control group. Interestingly, the flexural properties of these composites proved sensitive to the type of interphase formed for various admicellar polymerization conditions. Higher surface coverage and film connectedness in admicellar polymeric sizings are observed to enhance stress transfer at the interfacial region.     

The effect of interphase modification on carbon fiber/polyarylacetylene resin composites

Interfacial modification for carbon fiber (CF) reinforced polyarylacetylene (PAA) resin, a kind of non-polar, was investigated. The high carbon phenolic resin was used as coating to treat the surface of CF after oxidation. Atomic force microscopy (AFM) with force modulation mode was used to analyze the interphase of composite. The interlaminar shear strength (ILSS) and mechanical properties of CF/PAA composites were also measured. It was found that the CF/PAA composites treated with oxidation and coating after oxidation had transition area between carbon fiber and PAA resin. The existence of transition area led to the improvement of interfacial performance of composites. Specially, the thickness and stiffness of interphase of composite treated with coating after oxidation were more suitable for CF/PAA composites. Thus, the composite treated with coating after oxidation had the highest value of ILSS and the best mechanical properties.     

Quantitative evaluation of interfacial adhesion between fiber and resin in carbon fiber/epoxy composite cured by semiconductor microwave device

Interfacial adhesion between carbon fiber (CF) and epoxy resin in carbon fiber-reinforced epoxy composite, which was prepared by different heating process such as semiconductor microwave (MW) device and conventional electric oven, has been evaluated quantitatively. The interfacial shear strength (IFSS) between CF and epoxy resin, which was an indicator of adhesion on the interface, was measured by a single fiber fragmentation test. The single fiber fragmentation test showed that the IFSSs of the prepared specimens were different by heating methods. In the case of MW process, the curing reaction of epoxy resin on the CF interface would be progressed preferentially due to the selective heating of CF, resulting that the IFSSs of specimens prepared by MW irradiation were increased by enhancing the output power of MW. However, the IFSSs of the specimens were decreased by excessively high output power because the matrix resin on the CF interface was thermally degraded. As results, by optimizing the MW conditions of output power and irradiation time, the IFSS of the sample cured by MW was increased by 21% as compared to oven-heated one. It was found that the interfacial adhesion between CF and epoxy resin would be improved by the MW-assisted curing reaction on the surface of CF.     

Plasma treatment of carbon fibers: Non-equilibrium dynamic adsorption and its effect on the mechanical properties of RTM fabricated composites

The effect of oxygen plasma treatment on the non-equilibrium dynamic adsorption of the carbon fabric reinforcements in RTM process was studied. 5-Dimethylamino-1-naphthalene-sulfonylchloride (DNS-Cl) was attached to the curing agent to study the change of curing agent content in the epoxy resin matrix. Steady state fluorescence spectroscopy (FS) analysis was used to study this changes in the epoxy resin at the inlet and outlet of the RTM mould, and XPS was used to study the chemical changes on the carbon fiber surfaces introduced by plasma treatment. The interlaminar shear strength (ILSS) and flexural strength were also measured to study the effects of this non-equilibrium dynamic adsorption progress on the mechanical properties of the end products. FS analysis shows that the curing agent adsorbed onto the fiber surface preferentially for untreated carbon fiber, the curing agent content in the resin matrix maintain unchanged after plasma treatment for 3 min and 5 min, but after oxygen plasma treatment for 7 min, the epoxy resin adsorbed onto the fiber surface preferentially. XPS analysis indicated that the oxygen plasma treatment successfully increased some polar functional groups concentration on the carbon fiber surfaces, this changes on the carbon fiber surfaces can change the adsorption ability of carbon fiber to the resin and curing agent. The mechanical properties of the composites were correlated to this results.     

Effects of γ-ray radiation grafting on aramid fibers and its composites

Armos fiber was modified by Co⁶⁰ γ-ray radiation in the different concentrations’ mixtures of phenol-formaldehyde and ethanol. Interlaminar shear strength (ILSS) was examined to characterize the effects of the treatment upon the interfacial bonding properties of Armos fibers/epoxy resin composites. The results showed that the ILSS of the composite, whose fibers were treated by 500 kGy radiation in 1.5 wt% PF, was improved by 25.4%. Nanoindentation technique analysis showed that the nanohardnesses of the various phases (the fiber, the interface and the matrix) in the composite, whose fibers were treated, were correspondingly higher than those in the composite, whose fibers were untreated. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) spectrum confirmed the increase in the polar groups at the fibers’ surface. Atomic force microscopy (AFM) results revealed that the surface of the fibers treated was rougher than that of the fibers untreated. The wettability of the fibers’ surface was also enhanced by the treatment. The conclusion that γ-ray irradiation grafting significantly improved the surface properties of Armos fibers could be drawn.     

Multiwalled carbon nanotubes mass-produced by dc arc discharge in He–H2 gas mixture

Uniform cathode deposits (longer than 15 mm), containing multiwalled carbon nanotubes (MWNTs) inside, were produced by dc arc discharge evaporation with a computer-controlled feeder of a pure-carbon electrode without a metal catalyst in a He–H₂ gas mixture. The purification of MWNTs was carried out to remove amorphous carbon and carbon nanoparticles. High-resolution transmission electron microscopy observations and Raman scattering studies show that the MWNTs possess a high crystallinity and a mean outermost diameter of ∼ ∼10 nm. It has been confirmed that the current density in the electron field emission from a purified MWNT mat can reach 77.92 mA/cm², indicating that the purified MWNTs are a promising candidate electron source in a super high-luminance light-source tube or a miniature X-ray source.     

Fabrication of high-performance supercapacitors based on transversely oriented carbon nanotubes

High-performance supercapacitors with organic electrolyte 1 M TEABF₄ (tetraethyl ammonium tetrafluoroborate) in PC (propylene carbonate) were fabricated and tested, based on multiwall carbon nanotubes (MWNTs) deposited by electrophoresis on three types of alternative substrates: aluminium foil, ITO (indium tin oxide) coated PET (polyethylene terephthalate) film and PET film. In all cases, SEM (scanning electron microscopy) and STEM (scanning transmission electron microscopy) micrographs demonstrated that protruding, transversely oriented MWNT structures were formed, which should increase the transverse conductivity of these MWNT electrodes. The best supercapacitor cell of MWNT electrodes deposited on aluminium foil displayed good transverse orientation of the MWNT structures as well as an in-plane MWNT network at the feet of the protruding structures, which ensured good in-plane conductivity. Capacitor cells with MWNT electrodes deposited either on ITO-coated PET film or on PET film demonstrated lower but still very good performance due to the high density of transversely oriented MWNT structures (good transverse conductivity) but some in-plane inhomogeneities. Capacitor cells with drop-printed MWNTs on aluminium foil, without any transverse orientation, had 16–30 times lower specific capacitance and 5–40 times lower power density than the capacitor cells with the electrophoretically deposited MWNT electrodes.     

Steady Shear Rheological Behavior,Mechanical Properties,and Morphology of the Polypropylene/Carbon Nanotube Nanocomposites

Nanocomposites based on polypropylene (PP) and multiwall carbon nanotubes (MWNT) have been prepared through melt blending. Scanning electron microscopy (SEM) observations indicate that nanotubes were dispersed almost homogeneously throughout the matrix; however, some aggregates were also observed at high nanotubes loading. Rheological studies showed that at low shear rates, there is an increase in steady shear viscosity and shear stress of samples with increasing of nanotubes concentration. However, at high shear rates nanocomposites behave like pure PP. The activation energy of flow showed an increasing trend and has a maximum at 1wt% MWNT content. It was found that incorporation of nanotubes causes a remarkable decrease in surface and volume resistivity values of the polymeric matrix. The presence of CNTs improved the tensile and flexural properties of the polymeric matrix.     

Micromechanical Behavior of Carbon Nanotube-Covered SiC Fibers in Polymer Matrix Composites

The incorporation of nanotube-covered fibers in continuous fiber/epoxy composites has been shown to influence the mechanical, electrical, and thermal properties of the composite. Increased interlaminar shear stress, flexural strength and modulus have been reported in such composites over composites containing bare fibers. In this study, the microstructure and interfacial shear strength (ISS) of continuous silicon carbide fiber/epoxy composites with and without nanotubes grown from the SiC fiber surface were investigated with micro-Raman spectroscopy (MRS) and microscopy. The fibers with nanotubes grown from the surface were found to have a reduced ISS compared with the bare fibers. Electron microscopy showed good wetting of epoxy in the nanotube forests, but poor attachment of the nanotube forests to the fibers. These results suggest that the mechanism leading to improvements in bulk composite properties is not due to an improvement in the fiber/matrix ISS.     

Synthesis and characterization of polycaprolactone-grafted carbon nanotubes via click reaction

Polycaprolactone (PCL) was covalently grafted on the surface of carbon nanotubes by a simple click reaction of propargyl-terminated PCL (propargyl-PCL) and carbon nanotubes (CNTs) containing azide groups (MWNT-N₃). Propargyl-PCL was synthesized by the ring-opening polymerization of ε-caprolactone using propargyl alcohol and stannous octoate. MWNT-N₃ was prepared from MWNT having 2-bromoisobutyryl groups (MWNT-Br) with sodium azide by azidation. The melting temperature of propargyl-PCL was shifted to the high temperature in PCL-grafted MWNT. The thermal stability of PCL-grafted MWNT was enhanced as compared to that of propargyl-PCL. PCL was coated on the surface of MWNT with a high density of PCL chains, which showed good solubility of PCL-grafted MWNT in organic solvents. PCL-grafted MWNT was characterized with FT-IR, ¹H NMR, Raman, differential scanning calorimetry, thermogravimetric analysis, and scanning electron microscopy.     

Functional multi-walled carbon nanotube/polyaniline composite films as supports of platinum for formic acid electrooxidation

Embedding of carbon nanotubes in conducting polymeric matrices for various nanocomposites material is now a popular area. In this article, a concise chemical method has been described for the preparation of homogeneous nanocomposite of multi-walled carbon nanotube (MWNT)/polyaniline (PANI) by electrochemical codeposition. For this we functionalized the MWNTs via the diazotization reaction. This helped to disperse the nanotubes in aniline. The composite films were dispersed Pt by electrodeposition technique. The presence of MWNTs and platinum in the composite films was confirmed by XRD analysis and transmission electron microscopy (TEM). Four-point probe investigations revealed that the MWNT/PANI composite films exhibited a good conductivity. Cyclic voltammograms (CV) showed that Pt-modified MWNT/PANI composite films perform higher electrocatalytic activity and better long-term stability than Pt-modified pure PANI film toward formic acid oxidation. The results imply that the MWNT/PANI composite films as a promising support material improves the electrocatalytic activity for formic acid oxidation greatly.     

磁场辅助热处理金属化碳纳米管场发射性能

利用化学镀方法对多壁碳纳米管(multi-walled carbon nanotubes,MWNTs)表面金属化镀镍(MWNTs/Ni),采用丝网印刷制备MWNTs/Ni场发射阴极,并在磁场辅助下热处理所得阴极,研究磁场辅助热处理对MWNTs/Ni阴极的场发射性能的影响,经300mT磁场辅助热处理的MWNTs/Ni的场发射阴极开启场强约为0.80V·μm~(-1),场增强因子β约为16068,对单根MWNTs/Ni在磁场中的受力情况进行建模分析,实验结果表明:磁场辅助热处理有助于提高MWNTs/Ni在阴极表面的直立分布,提高了MWNTs/Ni的场发射性能。     

Influence of γ-ray radiation grafting on interfacial properties of aramid fibers and epoxy resin composites

This research used Co⁶⁰ γ-ray radiation to modify Armos fibers in 1,2-epoxy-3-chloropropane. After the treatment, the interlaminar shear strength (ILSS) values of aramid/epoxy composites were improved by about 20%. Surface elements of Armos fibers were determined by XPS analysis, which indicated that the oxygen/carbon ratio was increased. The surface of the fibers treated was rougher than that of the untreated fibers when examined by atomic force microscopy (AFM) and scanning electron microscopy (SEM). Fourier transform infrared (FT-IR) spectra confirmed that the epoxy group was grafted onto the fibers. The wettability of the fibers' surface was also enhanced by the treatment. Nanoindentation technique analysis showed that the nanohardnesses of the various phases (the fiber, the interface and the matrix) in the composite, whose fibers were treated, were correspondingly higher than those in the composite, whose fibers were untreated. The results indicate that γ-ray irradiation grafting technique, which is a suitable batch process for industrialization, can modify the physicochemical properties of Armos fibers and improve the interfacial adhesion of its composite.     

Study on the Structure and Properties of UHMWPE/Epoxy Resin Composite Fiber

The preparation, crystallization behavior, and fiber structure and properties of ultrahigh molecular weight polyethylene (UHMWPE) epoxy resin composite fiber were studied by means of differential scanning calorimeter (DSC), X‐ray diffraction (XRD), Scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and tensile testing. The morphology showed a different behavior from pure polyethylene (PE) fiber. The fiber mechanical properties, creep behavior, and thermal properties of UHMWPE fiber can be improved by adding epoxy resin. It's believed that the epoxy can serve as a physical cross‐linking agent to limit the motion or migration of PE molecules and consequently improve the fiber creep property. However, when the content of epoxy resin is higher than 5 wt%, all of the behavior and properties deteriorate.     

真空紫外辐射对碳/环氧复合材料性能的影响

 介绍了真空紫外线的模拟和射流式真空紫外辐射模拟设备的工作原理、技术参数及特点,并利用该设备及其它分析手段对环氧树脂浇铸体(EP648)和碳/环氧复合材料(C/E648)在真空紫外线辐照作用下的出气、质量损失率、层间剪切强度和表面状态的变化进行了研究。试验结果表明：真空紫外线辐照导致材料产生明显的出气效应,质量损失率呈现先递增后趋于平缓的趋势;17 280esh辐照剂量下,EP648的质量损失是C/E648的3.4倍,C/E648的层间剪切强度与辐照前相比下降了13.3%;环氧树脂破损较重,而碳纤维表面状态基本完好,并对内部的环氧树脂起到一定的保护作用。