Effect of carbon fiber surface functionality on the moisture absorption behavior of carbon fiber/epoxy resin composites

Polyacrylonitrile (PAN)‐based carbon fibers were electrochemically oxidized in aqueous ammonium bicarbonate with increasing current density. The electrochemical treatment led to significant changes of surface physical properties and chemical structures. The oxidized fibers showed much cleaner surfaces and increased levels of oxygen functionalities. However, it was found that there was no correlation between surface roughness and the fiber/resin bond strength, i.e. mechanical interlocking did not play a major role in fiber/resin adhesion. Increases in surface chemical functionality resulted in improved fiber/resin bonding and increased interlaminar shear strength (ILSS) of carbon fiber reinforced epoxy composites. The relationship between fiber surface functionality and the hydrothermal aging behavior of carbon fiber/epoxy composites was investigated. The existence of free volume resulted from poor wetting of carbon fibers by the epoxy matrix and the interfacial chemical structure were the governing factors in the moisture absorption process of carbon fiber/epoxy composites. Copyright © 2016 John Wiley & Sons, Ltd.     

Improvement of interfacial adhesion for plasma‐treated aramid fiber‐reinforced poly(phthalazinone ether sulfone ketone) composite and fiber surface aging effects

Interfacial adhesion between the fiber and the matrix in a composite is a primary factor for stress transfer from the matrix to the fiber. In this study, oxygen plasma treatment method was applied to modify the fiber surface for improving interfacial adhesion of aramid fiber‐reinforced poly(phthalazinone ether sulfone ketone) (PPESK) composite. Composite interfacial adhesion properties were determined by interlaminar shear strength (ILSS) using a short‐beam bending test. The composite interfacial adhesion mechanism was discussed by SEM. The changes of chemical composition and wettability for plasma‐treated fiber surfaces stored in air as long as 10 days were investigated by XPS and dynamic contact angle analysis (DCAA), respectively. Results indicated that oxygen plasma treatment was an effective method for improving interfacial adhesion; plasma‐treated fiber surface suffered aging effects during storage in air. Copyright © 2008 John Wiley & Sons, Ltd.     

Study on the enhancement of the interface performance between CF and polyimide by triethylamine grafting nano-TiO2 particles

The TiO₂ is grafted by triethylamine and is introduced on the surface of the carbon fiber, which improves the wettability and activity of the carbon fiber surface and at the same time strengthens the carbon fiber/polyimide composite. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) confirmed the triethylamine grafting successfully on TiO₂. Scanning electron microscope (SEM) results show that when the trimethylamine concentration is 1.0%, a uniform coating is formed on the surface of the carbon fiber. The interlaminar shear strength (ILSS) and interfacial shear strength (IFSS) were increased by 32% and 69%, respectively.     

Effect of carbon fiber surface treatments on the flexural strength and tribological properties of short carbon fiber/polyimide composites

Pitch‐based short carbon fibers (CFs) were treated by air oxidation and cryogenic nitrogen, respectively. Thereafter the treated and untreated CFs were incorporated into polyimide (PI) matrix to form composites. The CFs before and after treatment were examined by XPS and SEM.The flexural strength of the specimen was determined in a three‐point test machine and the tribological properties of PI composites sliding against GCr15 steel rings were evaluated on an M‐2000 model ring‐on‐block test rig. The results show that the surface of the treated CFs became rougher. Lots of active groups formed on the CF surface after air oxidation.The treatment can effectively improve the mechanical and tribological properties in their PI composites due to the enhanced fiber‐matrix interfacial bonding. Copyright © 2008 John Wiley & Sons, Ltd.     

The mechanical properties of LDPE composite filled with CF coated by dimethylamine treated TiO2

In order to improve the surface wettability of carbon fiber and enhance its composite interface performance, dimethylamine treated TiO2 was coated on carbon fiber (CF). The surface morphology, surface chemical state, and surface wettability of CF were characterized by SEM, XPS, and TEM tests, and the interlaminar shear strength (ILSS) and cross-sectional morphology tests were used to test the performance of CF/Low density polyethylene (LDPE) composites. The interface bonding status was analyzed and characterized. The results show that after the surface treatment of CF by dimethylamine treated TiO2, the O/C (atomic ratio) of the surface of CF is increased, and a certain amount of nano-scale small convex micro-mechanical structure is given, which improves the surface wetting of CF. The surface of the CF modified by the TiO2 is rough; the contact area between modified CF and LDPE increases.     

Recyclable carbon fiber‐reinforced plastics (CFRP) containing degradable acetal linkages: Synthesis,properties, and chemical recycling

Two epoxy resins containing degradable acetal linkages were synthesized by the reaction of cresol novolak‐type phenolic resin (CN) with vinyl ethers containing a glycidyl group [cyclohexane dimethanol vinyl glycidyl ether (CHDMVG) and 4‐vinyloxybutyl glycidyl ether (VBGE). Carbon fiber‐reinforced plastics (CFRPs) were prepared by heating laminated prepreg sheets with CN‐CHDMVG resin (derived from CN and CHDMVG) and CN‐VBGE resin (derived from CN and VBGE), in which carbon fibers are impregnated with epoxy resins containing curing agents [dicyandiamide (DICY)] and curing accelerator [3‐(3,4‐dichlorophenyl)‐1,1‐dimethylurea (DCMU)]. CN‐CHDMVG‐based CFRPs and CN‐VBGE‐based CFRPs exhibited almost the same tensile strength as the conventional bisphenol‐A‐based CFRPs. CN‐CHDMVG‐based CFRPs and CN‐VBGE‐based CFRPs underwent smooth breakdown with the treatment of hydrochloric acid in tetrahydrofuran at room temperature for 24 h to regenerate strands of carbon fibers. The surface conditions of the recovered carbon fibers had little changes during degradation and recovery processes on the basis of scanning electron microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS). The recovered carbon fibers exhibited almost the same tensile strength as virgin carbon fibers and hence would be reused for the production of CFRPs. © 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015 , 53, 1052–1059     

The effect of surface modification with nitric acid on the mechanical and tribological properties of carbon fiber‐reinforced thermoplastic polyimide composite

Polyacrylamideacrylate (PAN)‐based carbon fibers were submitted to nitric acid oxidation treatments to improve the interfacial adhesion of the carbon fiber (CF)‐reinforced polyimide (CF/PI) composite. The carbon fiber surfaces were characterized by X‐ray photoelectron spectroscopy (XPS). Nitric acid oxidation not only affects the oxygen concentration but also produces an appreciable change in the nature of the chemical functions, namely the conversion of hydroxy‐type oxygen into carboxyl functions. Nitric acid oxidation treatment modifies the element constituting the fiber, the nitrogen concentration being about 1.2 times higher at the fiber external surface compared to the untreated one. The mechanical and tribological properties of the polymide (PI) composites reinforced by the carbon fibers treated with nitric acid oxidation were investigated. Results showed that the tensile strength of the CF/PI composites improved remarkably due to nitric acid treatment along with enhancement in friction and wear performance. Copyright © 2009 John Wiley & Sons, Ltd.     

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.     

Chemical modification on UHMWPE microparticles to improve the interfacial and tribological properties of UHMWPE/carbon fabric/phenolic laminate in water environment

Carbon fabric (CF)/phenolic laminates filled with pristine and chromic acid treated ultra high molecular weight polyethylene (UHMWPE) microparticles were fabricated. Their interfacial and tribological properties in water environment were comparatively investigated. The interlaminar shear strength (ILSS) of the laminates was tested on a universal testing machine (DY35), and the tribological properties were evaluated by a block‐on‐ring tribo‐tester. The worn surfaces and the interfaces of the laminates were respectively analyzed by scanning electron microscope (SEM) and field emission SEM (FESEM). The change of the chemical composition of UHMWPE microparticles after chromic acid etching was analyzed by Fourier transform infrared spectroscopy (FTIR). The chemical state of carbon fiber surface was examined using X‐ray photoelectron spectroscopy (XPS). The results revealed that the chromic acid treated UHMWPE microparticles had more remarkable effect than the pristine ones on improving not only ILSS and wear resistance of CF/phenolic laminate, but also its immunity to water environment. This should be attributed to the strengthened interfaces in treated UHMWPE/CF/phenolic laminate, which were characterized by the drawn dendritic UHMWPE fibrils firmly clinging on the surfaces of carbon fibers and resin in a Boston ivy‐like manner. Copyright © 2015 John Wiley & Sons, Ltd.     

Plasma treatment of carbon fiber on the tribological property of polyimide composite

The effect of different ratios of carbon fiber (CF) reinforcing polyimide (PI) and surface treatment of CF on the microstructure and wear resistance of surface layers was studied. The increase of CF content led to a gradual increase in the Interlaminar shear strength (ILSS) values, and the maximum ILSS value arises when the CF content is 15 vol%, with an improvement of 13.45% compared to virgin CF composites. The increased interfacial adhesion could be contributed mainly to the presence of branched PI at the interface region. SEM of the worn surface confirms that the plasma treatment efficiently improves the interfacial adhesion of CF/PI composite. Copyright © 2017 John Wiley & Sons, Ltd.     

Influence of surface properties on the interfacial adhesion in carbon fiber/epoxy composites

A polyacrylonitrile‐based carbon fiber was electrochemically oxidized in an aqueous ammonium bicarbonate solution with current density of up to 2.76 A/m² at room temperature. X‐ray photoelectron spectroscopy revealed that the oxygen content increased with increasing current density before approaching saturation. The increase can be divided into two regions, the rapid increase region (0–1.78 A/m²) and a plateau region (1.78–2.76 A/m²). The surface chemistry analysis showed that the interlaminar shear strength (ILSS) value of the carbon fiber/epoxy composite could be improved by 24.7%. The carbon structure was examined using Raman spectroscopy in terms of order/disorder in the graphite structure and the results indicated that the relative percentage of graphite carbon in the form of sp² hybridization increased above a current density of 1.39 A/m². The increasing non‐polar graphite carbon on the carbon fiber surface decreased the surface energy. As a result, both the surface free energy () and its polar component () decreased when current density increased above 1.78 A/m². The ILSS value had no direct relationship with the nature and surface density of the oxygen‐containing functional groups nor with the carbon structure. It is the surface free energy (), especially the polar component (), which played a critical role in affecting the interfacial adhesion of carbon fiber/epoxy composites. The ILSS value changed with increasing current density and could be divided into three distinct regions, as chemical interaction region (I), anchor force region (II) and matrix damage region (III). Copyright © 2013 John Wiley & Sons, Ltd.     

连续纤维增强含二氮杂萘酮联苯结构聚芳醚砜酮树脂基复合材料的界面

利用射频感性耦合冷等离子体(ICP)处理技术改性连续纤维表面,分别采用X射线光电子能谱(XPS)、原子力显微镜(AFM)及动态接触角分析(DCA)系统研究了等离子体处理时间、放电气压、放电功率等工艺参数对连续碳纤维、芳纶纤维和对亚苯基苯并二噁唑(PBO)纤维的表面化学成分、表面形貌、表面粗糙度及表面自由能的影响.研究结...     

Influence of an oxidation of the carbon fiber surface by boiling nitric acid on the adhesion strength in carbon fiber‐acrylate composites cured by electron beam

A time‐dependent oxidation of carbon fibers in boiling nitric acid was used to investigate the influence of a modification of the fiber surface properties on the adhesion strength with an acrylate resin cured by electron beam (EB). For each time of treatment, a characterization of the surface topography and the surface chemistry was done (topography at a micrometric and nanometric scale, specific surface area, temperature programmed desorption, X‐ray photoelectron spectroscopy analysis). The oxidation of the fiber surface in boiling nitric acid created a rough surface, which significantly increased the specific surface area, and also generated a high density of hydroxyl groups, carboxylic acids and lactones in comparison to untreated fibers. The adhesion strength with the acrylate resin cured by EB was measured by a pull‐out test. For comparison, an isothermal ultraviolet curing of the matrix was also investigated. The value of the interfacial shear strength, determined by the Greszczuk's model, was increased by the oxidation of the carbon fiber surface for both curing processes, but lower values were systemically obtained with EB curing. Copyright © 2012 John Wiley & Sons, Ltd.     

Friction and wear properties of combined surface modified carbon fabric reinforced phenolic composites

Carbon fabric (CF) was surface treated with silane-coupling agent modification, HNO₃ oxidation, combined surface treatment, respectively. The friction and wear properties of the carbon fabric reinforced phenolic composites (CFP), sliding against GCr15 steel rings, were investigated on an M-2000 model ring-on-block test rig. Experimental results revealed that combined surface treatment largely reduced the friction and wear of the CFP composites. Scanning electron microscope (SEM) investigation of the worn surfaces of the CFP composites showed that combined surface modified CFP composite had the strongest interfacial adhesion and the smoothest worn surface under given load and sliding rate. SEM and X-ray photoelectron spectroscopy (XPS) study of carbon fiber surface showed that the fiber surface became rougher and the oxygen concentration increased greatly after combined surface treatment, which improved the adhesion between the fiber and the phenolic resin matrix and hence to improve the friction-reduction and anti-wear properties of the CFP composite.     

Effect of on-line ultrasonic treatment on the properties of carbon fiber reinforced plastic composites

The strength, performance, and application of carbon fiber reinforced plastic (CFRP) composites are directly affected by the interfacial bonding between fiber and resin. Wet winding technology is a commonly used composite productive process, and improving interfacial bonding of composites by on-line treatment has always been the focus of attention. In this paper, an on-line ultrasonic treatment system is designed and realized, the resin content of prepregs is determined by the dissolution method; standard deviation and dispersion coefficient are also calculated. The surface morphology, internal structure of prepregs, and the component of resin are observed and analyzed using a Metallurgical Microscope, scanning electron microscope (SEM), and near infrared radiation spectra (NIRS). The strength and performance of prepregs [(tensile strength, bending strength, tensile modulus of elasticity, bending modulus of elasticity, and interlaminar shear strength (ILSS)] are also tested. The results show the on-line ultrasonic treatment system can effectively improve the interfacial bonding of CFRP composites and enhance the strength and performance of CFRP composites.     

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.     

The oxidation‐treated interface on tribological properties of carbon fibers‐reinforced PTFE composite under oil‐lubricated condition

The effect of air oxidation and ozone surface treatment of carbon fibers (CF) on tribological properties of CF reinforced polytetrafluoroethylene (PTFE) composites under oil‐lubricated condition was investigated. Experimental results revealed that ozone treated CF reinforced PTFE (CF–PTFE) composite had the lowest friction coefficient and wear under various applied loads and sliding speeds compared with untreated and air‐oxidated composites. X‐ray photoelectron spectroscopy (XPS) study of carbon fiber surface showed that, after ozone treatment, oxygen concentration was obviously increased, and the amount of oxygen‐containing groups on CF surfaces was largely increased. The increase in the amount of oxygen‐containing groups enhanced interfacial adhesion between CF and PTFE matrix. With strong interfacial adhesion of the composite, stress could be effectively transmitted to carbon fibers; carbon fibers were strongly bonded with PTFE matrix and large scale rubbing‐off of PTFE was prevented, therefore, the tribological properties of the composite were improved. Copyright © 2009 John Wiley & Sons, Ltd.     

Improvement of PBO fiber surface and PBO/PPESK composite interface properties with air DBD plasma treatment

The interface of fibrous composites is a key factor to the whole properties of the composites. In this study, the effects of air dielectric barrier discharge (DBD) plasma discharge power density on surface properties of poly(p‐phenylene benzobisoxazole) (PBO) fiber and the interfacial adhesion of PBO fiber reinforced poly(phthalazinone ether sulfone ketone) (PPESK) composite were investigated by several characterization methods, including XPS, SEM, signal fiber tensile strength, interlaminar shear strength, and water absorption. After the air DBD plasma treatment at a power density of 41.4 W/cm³, XPS analysis showed that some polar functional groups were introduced on the PBO fiber surface, especially the emergence of a new oxygen‐containing group (?O–C = O group). SEM observations revealed that the air DBD plasma treatment had a great influence on surface morphologies of the PBO fiber, while the signal fiber tensile strength results showed only a small decline of 5.9% for the plasma‐treated fiber. Meanwhile, interlaminar shear strength value of PBO/PPESK composite was increased to 44.71 MPa by 34.5% and water absorption of the composite decreased from 0.46% for the untreated specimen to 0.27%. The results showed that the air DBD plasma treatment can effectively improve the properties of the PBO fiber surface and the PBO/PPESK composite interface. Results obtained from the above analyses also showed that both the fiber surface and the composite interface performance would be reduced when an undue plasma discharge power density was applied. Copyright © 2011 John Wiley & Sons, Ltd.     

液态氧化法处理超高分子量聚乙烯纤维

用液态氧化法对超高分子量聚乙烯纤维进行了表面处理,研究了处理介质、处理时间对超高分子量聚乙烯／环氧复合材料层间剪切强度的影响,用扫描电子显微镜、ＸＰＳ表面元素分析、毛细浸润法测接触角等方法探讨了纤维表面性能处理前后的变化,以及纤维与树脂的界面结合情况。     

The interfacial feature of thermoplastic polystyrene composite filled with nitric acid oxidized carbon fiber

The quality of interfacial interaction is dictated by the surface chemistry of the carbon fibers and the composition of the matrix. The composition of polystyrene was modified by the addition of maleic anhydride (MAH) grafted polystyrene. The surface properties of the various matrix formulations were characterized by contact angle. Carbon fibers were modified by oxidation in nitric acid. The surface composition of the carbon fibers was characterized. The interaction between modified polystyrene and the carbon fibers was studied by single fiber pull‐out tests. The best adhesion behavior was achieved between polystyrene containing grafted MAH and nitric acid oxidation carbon fibers. The addition of MAH‐grafted polystyrene to the unmodified polystyrene caused the interfacial shear strength (IFSS) to increase. The IFSS of this fiber‐matrix combination allowed for the full utilization of the tensile strength of polystyrene. Copyright © 2009 John Wiley & Sons, Ltd.