Wettability of carbon fibers modified by acrylic acid and interface properties of carbon fiber/epoxy

The oxidation-reduction and pre-irradiation induced methods were employed to study the effect of acrylic acid modification on the wetting and adsorption ability of carbon fiber (CF) in epoxy solution and the interfacial properties of CF/epoxy. Systematic experimental work was conducted to determine the surface topography, surface energy, surface chemical composition, absorbability and tensile strength of carbon fibers and interfacial adhesion of CF/epoxy before and after modification. The roughness, surface energy, amount of containing-oxygen functional groups and wetting ability were all found to increase significantly after modifications. The tensile strength of carbon fibers was improved marginally by γ-ray pre-irradiation while was decreased little by oxidation-reduction modification. Consequently, the surface modifications of carbon fibers via both oxidation-reduction and pre-irradiation led to an improvement (more than 15%) of the interlaminar shear strength of CF/epoxy composites. The mechanisms of interfacial improvement of modified CF/epoxy composites are proposed.     

Improved interfacial properties of carbon fiber/UHMWPE composites through surface coating on carbon fiber surface

Carbon fibers were coated in an attempt to improve the interfacial properties between carbon fibers and ultra‐high molecular weight polyethylene resin matrix. Atomic force microscopy, scanning electron microscopy, and X‐ray photoelectron spectroscopy were performed to characterize the changes of carbon fiber surface. Atomic force microscopy results show that the coating of carbon fiber significantly increased the carbon fiber surface roughness. X‐ray photoelectron spectroscopy indicates that silicon containing functional groups obviously increased after modification. Interlaminar shear strength was used to characterize the interfacial properties of the composites.     

Surface modification of carbon fiber via electron‐beam irradiation grafting

In this paper, the surface properties of polyacrylonitrile‐based carbon fibers is improved by electron‐beam (EB) irradiation in maleic anhydride/acetone solution at 100, 150, 200 and 150 KGy. Experimental study of this paper is carried out to identify surface topography, surface chemical composition and functional groups, adsorption ability and interface properties of CF/epoxy composites. The results reveal that the roughness of carbon fiber surface is increased obviously after modification by EB irradiation grafting technology. The ratio value of O/C and the relative content of oxygen functional groups on fiber surface are improved effectively, comparing with the unmodified carbon fiber. Besides, adsorption of carbon fiber on epoxy and the mechanical performance of CF/epoxy composites are clearly enhanced after irradiation grafting modification. Copyright © 2012 John Wiley & Sons, Ltd.     

Multiscale carbon nanotube-carbon fiber reinforcement for advanced epoxy composites

We report an approach to the development of advanced structural composites based on engineered multiscale carbon nanotube-carbon fiber reinforcement. Electrophoresis was utilized for the selective deposition of multi- and single-walled carbon nanotubes (CNTs) on woven carbon fabric. The CNT-coated carbon fabric panels were subsequently infiltrated with epoxy resin using vacuum-assisted resin transfer molding (VARTM) to fabricate multiscale hybrid composites in which the nanotubes were completely integrated into the fiber bundles and reinforced the matrix-rich regions. The carbon nanotube/carbon fabric/epoxy composites showed approximately 30% enhancement of the interlaminar shear strength as compared to that of carbon fiber/epoxy composites without carbon nanotubes and demonstrate significantly improved out-of-plane electrical conductivity.     

Influence of surface properties of graphene oxide/carbon fiber hybrid fiber by oxidative treatments combined with electrophoretic deposition

An effective way to prepare graphene oxide/carbon fiber hybrid fiber was proposed by the treatment with hydrogen peroxide and concentrated nitric acid combined with electrophoretic deposition process. Surface functional group, surface roughness, and surface morphologies of carbon fibers were examined by Fourier transform infrared spectrometer, atomic force microscopy, and scanning electron microscopy. Results showed that a uniform and thick graphene oxide films were constructed on the surface of carbon fiber. Deposition density increased by introduction of pretreatment of the carbon fiber in the electrophoretic deposition process has been shown as a possible method. Dynamic contact angle analysis results indicated that the deposition of graphene oxide significantly improved surface free energy of carbon fiber by increasing surface area and polar groups. The introduction of graphene oxide in the carbon fiber‐reinforced epoxy composites results in a 55.6% enhancement in the interfacial shear strength and confirms the remarkable improvement in the interfacial adhesion strength of the composites, and the fracture mechanism was also analyzed. Copyright © 2016 John Wiley & Sons, Ltd.     

Improving the interfacial property of carbon fiber/PI resin composite by grafting modification of carbon fiber surface

The poor interfacial adhesion between carbon fibers (CFs) and polyimide (PI) resin has seriously hampered the application of CF/PI composites. In this work, the interfacial adhesion was efficiently enhanced by grafting on the CF surface. Surface morphology and surface composition of modified carbon fibers were characterized, which indicated that acrylamide was grafted successfully on the CF surface and the surface roughness was increased slightly. After grafting, the interface shear strength of modified carbon fibers/PI composites was significantly improved by 86.96%, and the interlaminar shear strength was enhanced by 55.61% due to the covalent bonds in interphase and the toughening effect of sizing agent. Moreover, the mechanical properties of composites with different interfacial adhesion were measured, which further confirmed the effect of the grafting modification.     

Preparation and characterization of functionalized graphene oxide/carbon fiber/epoxy nanocomposites

Graphene oxide (GO) was functionalized using three different diamines, namely ethylenediamine (EDA), 4,4′-diaminodiphenyl sulfone (DDS) and p-phenylenediamine (PPD) to reinforce an epoxy adhesive, with the aim of improving the bonding strength of carbon fiber/epoxy composite. The chemical structure of the functionalized GO (FGO) nanosheets was characterized by elemental analysis, FT-IR and XRD. Hand lay-up, as a simple method, was applied for 3-ply composite fabrication. In the sample preparation, the fiber-to-resin ratio of 40:60 (w:w) and fiber orientations of 0°, 90°, and 0° were used. The GO and FGO nanoparticles were first dispersed in the epoxy resin, and then the GO and FGO reinforced epoxy (GO- or FGO-epoxy) were directly introduced into the carbon fiber layers to improve the mechanical properties. The GO and FGO contents varied in the range of 0.1–0.5 wt%. Results showed that the mechanical properties, in terms of tensile and flexural properties, were mainly dependent on the type of GO functionalization followed by the percentage of modified GO. As a result, both the tensile and flexural strengths are effectively enhanced by the FGOs addition. The tensile and flexural moduli are also increased by the FGO filling in the epoxy resin due to the excellent elastic modulus of FGO. The optimal FGO content for effectively improving the overall composite mechanical performance was found to be 0.3 wt%. Scanning electron microscopy (SEM) revealed that the failure mechanism of carbon fibers pulled out from the epoxy matrix contributed to the enhancement of the mechanical performance of the epoxy. These results show that diamine FGOs can strengthen the interfacial bonding between the carbon fibers and the epoxy adhesive.     

Enhanced mechanical properties of carbon fiber composites by grafting different structural poly(amido amine) onto fiber surface

The mechanical properties of carbon fiber composites depend on the interfacial strength between fiber and epoxy matrix. Different poly (amido amine) (PAMAM) dendrimers were grafted onto carbon fiber to improve the interfacial strength of the resulting composites. Functional groups on the carbon fiber surface were examined by X-ray photoelectron spectroscopy. The surface morphology of the resulting materials was characterized by scanning electron microscopy and atomic force microscope. The characterization results revealed that PAMAM dendrimers were chemically grafted onto the surface of carbon fiber. More importantly, the mechanical properties of the resulting composites were enhanced owing to the presence of sufficient functional groups on the carbon fiber surface. In addition, after PAMAM containing chair conformations were grafted, the interlaminar shear strength had the highest increase of 53.13%, higher than that of the fiber grafted with PAMAM containing terminated linear amine. This work provides an alternative approach to enhance the mechanical properties of fiber composites by controlling the interface between fiber and epoxy matrix.     

Influence of coupling agent chain lengths on interfacial performances of carbon fiber and polyarylacetylene resin composites

The influence of chain lengths on interfacial performances of carbon fiber/polyarylacetylene composites was studied. For this purpose, four coupling agents, methyltrimethoxysilane, propyltrimethoxysilane, octyltrimethoxysilane and dodecyltrimethoxysilane, were grafted onto fiber surface to obtain different chain lengths. The resulting carbon fiber surface was characterized by XPS and dynamic contact angle test. Interfacial adhesion in the resulting fiber reinforced polyarylacetylene resin composites was also evaluated by fracture morphology analysis and interfacial shear strength test. It was found that the interfacial adhesion in composites greatly increased with chain lengths on fiber surface. The improvement of interfacial adhesion was attributed to the interaction between the chain of coupling agents on fiber surface and that of polyarylacetylene resin at the interface. Copyright © 2009 John Wiley & Sons, Ltd.     

The crosslinking of epoxy resins at interfaces. V. Amine-cured resins at carbon and graphite surfaces

The effects of carbon blacks, chopped carbon fibers, and crushed carbon fibers on the crosslinking chemistry of a diglycidyl epoxy resin/m-phenylenediamine system were examined by infrared (IR) spectroscopy and differential scanning calorimetry (DSC). The carbon and graphite surfaces were given oxidizing and reducing treatment to simulate the surface treatment of carbon fibers used in the manufacture of composites. The oxidized carbon surfaces initially accelerated epoxy–amine reactions but inhibited the later stages of the reaction such that the final extent of cure was reduced. The oxidized carbons also preferentially adsorbed the amine curing agent, resulting in a stoichiometric imbalance at the interface.     

Modification of the surface of carbon fibers with multi-walled carbon nanotubes and its effect on mechanical characteristics of composites with epoxy resin

Effect of the catalyst composition on the structure of nanotubes layers obtained on the surface of carbon nanofibers was studied. We found the preliminary functionalization of the surface of carbon fibers to affect the coating uniformity and the thickness of synthesized nanotube layer. We determined the optimal surface concentration of the catalyst (Fe–Co) which provides uniform layer of nanotubes on the surface of carbon fibers. The effect of modification of the surface of carbon fibers with multi-walled carbon nanotubes on the mechanical properties of carbon fiber–epoxy resin composites was examined. The modification of the carbon fibers with multi-walled carbon nanotubes were shown to increase the flexural modulus and the flexural strength.     

Surface modification of carbon fiber for improving the interfacial adhesion between carbon fiber and polymer matrix

In this study, the reinforcing mechanism of amine functionalized on carbon fibers (CFs) has been precisely discussed, and the differences between aliphatic and aromatic compounds have been illustrated. Polyacrylonitrile‐based CFs were functionalized with ethylenediamine, 4,4‐diaminodiphenyl sulphone, and p‐aminobenzoic acid (PAB), and CF‐reinforced epoxy composites were prepared. The structural and surface characteristics of the functionalized CFs were investigated using X‐ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FT‐IR), and scanning electron microscopy (SEM). Mechanical properties in terms of tensile and flexural strengths and moduli were studied. The FT‐IR results confirm the success in bonding amines on the CF surface. After treatment of CFs, the oxygen and nitrogen contents as well as the N/C ratio showed an increase. XPS results provided evidence of the chemical reaction during functionalization, rather than being physically coated on the CF surface. Chemical modification of CF with diamines led to considerable enhancement in compatibility of CF filaments and epoxy resin, and remarkable improvements were seen in both tensile and flexural properties of the reinforced composites. SEM micrographs also confirmed the improvement of interface adhesion between the modified CFs and epoxy matrix. Finally, it can be concluded that PAB is a promising candidate to functionalize CF in order to improve interfacial properties of CF/epoxy composites. Copyright © 2015 John Wiley & Sons, Ltd.     

超临界正丁醇对回收碳纤维复合材料的降解及表征

采用响应面分析方法设计超临界正丁醇降解废弃的碳纤维/环氧树脂(CF/EP)复合材料降解实验,用以回收碳纤维.通过Design-Expert V8.0建立环氧树脂降解率和工艺参数之间的数学模型,获得了最优工艺参数;通过图形优化研究了工艺参数对环氧树脂基体降解率的影响规律;通过场发射电子扫描显微镜、原子力显微镜、X射线光电子能谱仪、显微共焦激光拉曼光谱仪及单丝拉伸等分析最优工艺参数下回收的碳纤维的表面形貌、表面化学、石墨化程度及力学性能.结果表明,建立的数学模型拟合误差范围为±5.5%,实现了回收工艺参数的预估;单因素对环氧树脂基体降解率的影响程度为:反应温度保温时间添加剂浓度正丁醇含量;最优工艺参数为:反应温度330℃,保温时间60 min,添加剂浓度0.0538 mol/L,投料比0.024g/mL.回收的碳纤维表面无残留树脂,没有发生明显的石墨化,且表面平均粗糙度与原碳纤维相近;与原始碳纤维相比,回收的碳纤维的拉伸强度约为原碳纤维的93.58%,杨氏模量约为原碳纤维的94.87%.     

Interfacial studies on the ozone and air‐oxidation‐modified carbon fiber reinforced PEEK composites

In this work, ozone modification method and air‐oxidationwere used for the surface treatment of polyacrylonitrile(PAN)‐based carbon fiber. The surface characteristics of carbon fibers were characterized by XPS. The interfacial properties of carbon fiber‐reinforced (polyetheretherketone) PEEK (CF/PEEK) composites were investigated by means of the single fiber pull‐out tests. As a result, it was found that IFSS (interfacial shear strength) values of the composites with ozone‐treated carbon fiber are increased by 60% compared to that without treatment. XPS results show that ozone treatment increases the amount of carboxyl groups on carbon fiber surface, thus the interfacial adhesion between carbon fiber and PEEK matrix is effectively promoted. The effect of surface treatment of carbon fibers on the tribological properties of CF/PEEKcomposites was comparativelyinvestigated. Experimental results revealed that surface treatment can effectively improve the interfacial adhesion between carbon fiber and PEEK matrix. Thus the wear resistance was significantly improved. Copyright © 2009 John Wiley & Sons, Ltd.     

Improving the interfacial property of carbon fibre/epoxy resin composites by grafting amine-capped cross-linked poly-itaconic acid

To improve the interfacial properties of carbon fibre-reinforced polymer composites, a surface treatment was used to cap cross-linked poly-itaconic acid onto carbon fibres via in-situ polymerization after itaconic acid grafting. The chemical composition of the modified carbon fiber (CF) surface was characterized by X-ray photoelectron spectral and Fourier-transform infrared spectroscopy. Scanning electron microscopy and atomic force microscopy images showed that the poly-itaconic acid protective sheath was uniformly capped onto the CF surface and that the surface roughness was obviously enhanced. Chemical bonds also played a key role in the interfacial enhancement. The results showed that the interfacial shear strength of the composites with poly-itaconic acid on the carbon fibres (72.2 MPa) was significantly increased by 89.5% compared with that of the composites with pristine CF (38.1 MPa). Moreover, the poly-itaconic acid sheath promoted a slight increase in mono-fibre tensile strength. In addition, the interfacial mechanisms were also discussed. Meanwhile, the mechanical property of the functionalized CF/epoxy resin composites was also significantly improved.     

The mechanical properties of plasma‐treated carbon fiber reinforced PA6 composites with CNT

The aim of this work is the evaluation of the effects of plasma treatment and the addition of CNT on the mechanical properties of carbon fibre/PA6 composite. A powder impregnation process with integrated inline continuous plasma of carbon fibers was used to produce CF/PA6 composite. CF/PA6 composite was processed into test laminates by compression moulding, and interface dominated composite properties were studied. The tensile and impact strength of composites containing CNT and plasma‐treated carbon fibres improved obviously. The tensile strength of nanocomposite largely increases with the increasing of the CNT content and then decreases when the CNT content is over 2%. The hydroxyl groups of the fibers surface are in favor of the wettability of carbon fibers by the polar matrix resin, which is resulting in a further interaction of the fiber surface with the curing system of the matrix resin.     

Interlaminar and ductile characteristics of carbon fibers-reinforced plastics produced by nanoscaled electroless nickel plating on carbon fiber surfaces

In this work, a new method based on nanoscaled Ni-P alloy coating on carbon fiber surfaces is proposed for the improvement of interfacial properties between fibers and epoxy matrix in a composite system. Fiber surfaces and the mechanical interfacial properties of composites were characterized by atomic absorption spectrophotometer (AAS), scanning electron microscopy (SEM), X-ray photoelectron spectrometry (XPS), interlaminar shear strength (ILSS), and impact strength. Experimental results showed that the O(1s)/C(1s) ratio or Ni and P amounts had been increased as the electroless nickel plating proceeded; the ILSS had also been slightly improved. The impact properties were significantly improved in the presence of Ni-P alloy on carbon fiber surfaces, increasing the ductility of the composites. This was probably due to the effect of substituted Ni-P alloy, leading to an increase of the resistance to the deformation and the crack initiation of the epoxy system.     

原位合成纳米SiO2增强阴离子聚酯型上浆剂及其对碳纤维复合材料层间剪切强度的影响

采用溶胶-凝胶法, 在侧链带有羧基的线性不饱和聚酯中加入正硅酸乙酯(TEOS), 使TEOS在酸性条件下发生水解反应, 原位合成纳米SiO₂增强阴离子型聚酯乳液(SEAPE). 利用傅里叶变换红外光谱(FTIR)仪、 激光粒度分析仪和冷冻扫描电子显微镜(Cryo-SEM)对SEAPE进行分析与表征. 将SEAPE与聚乙二醇单油酸酯润滑剂、 非离子型表面活性剂FC-4430及抗氧剂1010进行复配, 原位制备纳米SiO₂增强阴离子型聚酯乳液上浆剂(SEAPEs), 用扫描电子显微镜(SEM)、 视频动态接触角测量仪、 X射线能谱(EDS)仪和纤维强力仪对SEAPEs上浆后碳纤维的表面形貌、 表面能、 碳纤维(CF)表面元素及碳纤维增强不饱和聚酯(UPR)复合材料(CF/UPR)的层间剪切强度(ILSS)进行测试与表征. 结果表明, 当TEOS添加质量分数为5%时, SEAPEs上浆后的碳纤维有效增强了其与UPR的结合强度, CF/UPR复合材料的ILSS达到40.03 MPa, 与市售环氧树脂型上浆剂上浆后碳纤维增强UPR复合材料相比, ILSS提高90.1%. SEAPEs中原位生成的纳米SiO₂分散均匀, 乳液储存稳定, 上浆后SiO₂均匀吸附在碳纤维表面, 增加碳纤维表面能, 改善碳纤维与树脂间的浸润性, 可有效提高碳纤维增强不饱和聚酯树脂复合材料的ILSS.     

Effect of low current density electrochemical oxidation on the properties of carbon fiber‐reinforced epoxy resin composites

Changes in surface physicochemical structures of polyacrylonitrile‐based carbon fibers resulted from low current density electrochemical oxidation were monitored by scanning electron microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS). The relationship between the interlaminar shear strength (ILSS) values of carbon fiber‐reinforced polymers (CFRPs) and carbon fiber surface chemistry including elemental ratios and the relative content of oxygen‐containing functional groups were researched. SEM results revealed that the electrochemical oxidation got rid of surface contaminants generated during the production process. XPS analysis showed that the relative contents of oxygen and nitrogen increased by 446% and 202%, respectively, after the electrochemical oxidation. Carbon fiber surface chemistry was of paramount importance to the interfacial properties of CFRPs. The higher the carbon fiber surface activity, the better the interfacial bonding was, and an increase in the acidic‐group contents was responsible for a higher ILSS value. However, when the current density increased to 1.0 A/m², the interfacial bonding between carbon fiber and the epoxy resin became weak which led to the decline in ILSS values. Copyright © 2012 John Wiley & Sons, Ltd.     

Interfacial and wetting properties of carbon fiber reinforced epoxy composites with different hardeners by electrical resistance measurement

In this research, interfacial and wetting properties of N,N,N,N-tetraglycidyl-4,4-diaminodiphenylmethane (TGDDM) epoxy resin with two hardeners with different chemical structure were evaluated by electrical resistance (ER) measurement. The heat of reaction of TGDDM epoxy with the two different hardeners, 33 and 44 di-amino di-phenyl sulphone (DDS), was analyzed by differential scanning calorimetry (DSC). The TGDDM epoxy exhibited different mechanical properties with the two different DDS hardeners. Combined ER, wetting measurements and the microdroplet test were used for evaluating the spreading effect and interfacial shear strength (IFSS) of carbon fiber (CF) reinforced TGDDM epoxy composites with these different hardeners. The heat of reaction and mechanical properties of TGDDM/DDS were influenced by the chemical structure and different free volumes of the epoxy resins. The relationships between the ER-wetting results and the IFSS were internally consistent. Ultimately it was demonstrated that ER measurements makes it possible to estimate the interfacial and wetting properties of CF reinforced epoxy composites.