Interfacial adhesion and microfailure modes of electrodeposited carbon fiber/epoxy-PEI composites by microdroplet and surface wettability tests

Interfacial properties and microfailure modes of electrodeposition (ED)-treated carbon fiber-reinforced polyetherimide (PEI) toughened epoxy composite were investigated using microdroplet test and the measurement of surface wettability. ED was performed to improve the interfacial shear strength (IFSS). As PEI content increased, IFSS increased due to enhanced toughness and plastic deformation of PEI. In the untreated case, IFSS increased with adding PEI content, and the IFSS of the pure PEI matrix showed the highest. On the other hand, for the ED-treated case IFSS increased with PEI content with rather low improvement rate. In the untreated case, neat epoxy resin appeared brittle microfailure mode, whereas the pure PEI matrix exhibited a more likely ductile microfailure mode. In the ED-treated case, neat epoxy exhibited a more ductile fracture than that of the untreated case. Critical surface tension and polar surface free energy of ED-treated carbon fiber was higher than those of the untreated fiber. The work of adhesion between fiber and matrix was not directly proportional to IFSS for both the untreated and ED-treated cases. The matrix toughness might contribute to IFSS more likely than the surface wettability. Interfacial properties of the epoxy-PEI composite can be affected efficiently by both the control of matrix toughness and ED treatment.     

Comparison of interfacial properties of electrodeposited single carbon fiber/epoxy composites using tensile and compressive fragmentation tests and acoustic emission

Interfacial and microfailure properties of carbon fiber/epoxy composites were evaluated using both tensile fragmentation and compressive Broutman tests with an aid of acoustic emission (AE). A monomeric and two polymeric coupling agents were applied via the electrodeposition (ED) and the dipping applications. A monomeric and a polymeric coupling agent showed significant and comparable improvements in interfacial shear strength (IFSS) compared to the untreated case under both tensile and compressive tests. Typical microfailure modes including cone-shaped fiber break, matrix cracking, and partial interlayer failure were observed under tension, whereas the diagonal slipped failure at both ends of the fractured fiber exhibited under compression. Adsorption and shear displacement mechanisms at the interface were described in terms of electrical attraction and primary and secondary bonding forces. For both the untreated and the treated cases AE distributions were separated well in tension, whereas AE distributions were rather closely overlapped in compression. It might be because of the difference in molecular failure energies and failure mechanisms between tension and compression. The maximum AE voltage for the waveform of either carbon or large-diameter basalt fiber breakages in tension exhibited much larger than that in compression. AE could provide more likely the quantitative information on the interfacial adhesion and microfailure.     

Interfacial Aspects of Electrodeposited Carbon Fiber-Reinforced Epoxy Composites Using Monomeric and Polymeric Coupling Agents

Using a monomeric and two polymeric coupling agents, interfacial aspects of electrodeposited (ED) carbon fiber/epoxy composites were investigated by means of fragmentation techniques and acoustic emission (AE). ED results for dipped and untreated fibers under dry and wet conditions were compared. Multifiber-embedded composites (MFC) were prepared for direct comparison. Various treating conditions such as treating time, concentration of coupling agent, and treating temperature were optimized, respectively. The adsorption mechanisms of the coupling agents onto the carbon fiber were analyzed in terms of the electrolyte molecular interactions during ED process, due to chain mobility in the aqueous solution. The microfailure mechanisms occurring from fiber breaks, and matrix and interlayer cracks were examined by AE parameters. The interfacial shear strength (IFSS) of ED-treated carbon fibers was much higher than that of the other two cases under dry and wet conditions. Well-separated AE groups were found for the untreated, the dipped, and the ED-treated cases, and significantly more AE events occurred from the ED interlayer failure between fiber and matrix than from the untreated and even than from the dipping cases. AE events from different-type interlayers may be correlated with IFSS based on the differing mechanical and chemical roles of the interlayers. Copyright 2000 Academic Press.     

Improvement of surface wettability and interfacial adhesion ability of poly(p-phenylene benzobisoxazole) (PBO) fiber by incorporation of 2,5-dihydroxyterephthalic acid (DHTA)

By introducing 2,5-dihydroxyterephthalic acid (DHTA) into poly(p-phenylene benzoxazole) (PBO) macromolecular chains, dihydroxy poly(p-phenylene benzobisoxazole) (DHPBO) was synthesized and then DHPBO fibers were prepared by dry-jet wet-spinning method. Effects of hydroxyl polar groups on surface wettability and interfacial adhesion ability of PBO fiber were investigated. With the incorporation of double hydroxyl polar groups, contact angle on PBO fiber for water can decrease from 71.4° to 50.70°, and contact angle for ethanol can decrease from 37.2° to 27.40°. The wetting time on DHPBO fibers for water can be as short as 650 ms, which is half of that of PBO fibers. The interfacial shearing strength (IFSS) between DHPBO (10% mol content DHTA) fibers and epoxy resin is 18.87 MPa, 92.55% higher than that of PBO fibers. SEM images indicate that the PBO/epoxy composite failure mode may change from fiber/matrix adhesive failure to partially cohesive failure.     

Interfacial Aspects of Electrodeposited Conductive Fibers/Epoxy Composites using Electro-Micromechanical Technique and Nondestructive Evaluation

Interfacial adhesion and nondestructive behavior of the electrodeposited (ED) carbon fiber reinforced composites were evaluated using the electro-micromechanical technique and acoustic emission (AE). Interfacial shear strength (IFSS) of the ED carbon fiber/epoxy composites was higher than that of the untreated case. This might be expected because of the possible chemical and hydrogen bonding based on an electrically adsorbed polymeric interlayer. Logarithmic electrical resistivity of the untreated single-carbon fiber composite increased suddenly to infinity when the fiber fracture occurred, whereas that of the ED composite increased relatively broadly up to infinity. This may be due to the retarded fracture time as a result of the enhanced IFSS. In single- and 10-carbon fiber composites, the number of AE signals coming from the interlayer failure of the ED carbon fiber composite was much larger than that of the untreated composite. As the number of each first fiber fracture increased in the 10-carbon fiber composite, the electrical resistivity increased stepwise, and the slope of logarithmic electrical resistance increased. In the three-graphite filament composite with a narrow 1 time inter-filament distance, the total numbers of the filament fracture and the IFSS were smaller than those of the wider 5 times case. This might be because the interacting fracture energy caused by a filament break could affect the adjacent filaments. Copyright 2001 Academic Press.     

Surface modification of PBO fibers with 2,2-Bis (3-amino-4-hydroxyphenyl) hexafluoropropane in supercritical carbon dioxide for enhancing interfacial strength

PBO fiber is one of the most promising reinforcements in resin matrix composite because of its excellent mechanical properties. However, the inert and smooth surfaces make it the poor interface adhesion with resin matrix, which seriously limits the application in composites. In this article, we report a method to modify the surface of PBO fibers with 2,2-Bis (3-amino-4-hydroxyphenyl) hexafluoropropane（BisAPAF）in supercritical CO₂ to enhance interfacial properties. Chemical structures, surface elemental composition and functional groups, and surface morphology were characterized by FT-IR spectrometer, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM), respectively. The mechanical properties of the samples were tested by a tensile tester. Static contact angle and microdebonding tests were used to characterize the wetting ability and interfacial shear strength (IFSS) of the fiber and epoxy resin. The results showed that the BisAPAF could be solved in scCO₂ and introduced more groups, –NH₂, –OH, and –CF₃ on the fiber surface, resulting in the mechanical properties and the wettability of PBO fiber slightly improved. Moreover, the fiber surface roughness was also increased obviously. The IFSS between the modified PBO fiber and epoxy resin increased from 8.18 MPa to 31.4 MPa when the treating pressure was 14 MPa. In general, the method to modify PBO fibers surface using BisAPAF in scCO₂ can effectively improve their interfacial properties.     

提高PBO纤维/环氧树脂复合材料界面结合的研究

本文采用表面化学蚀刻与溶胀法结合、化学偶联法与氩气低温等离子体表面处理技术结合的方法对聚苯撑苯并二。唑（PBO）纤维进行表面改性。探讨了不同改性方法对纤维表面性能的影响。同时，采用FTIR和SEM等方法对处理前后纤维表面化学结构及形态进行了表征。     

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...     

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.     

Interfacial adhesion and shear behaviors of aramid fiber/polyamide 6 composites under different thermal treatments

Aramid fiber (AF) reinforced by polyamide (PA) composites are excepted to have good interfacial matching due to their similar chemical interactions of hydrogen bonding. Thus, polarizing optical microscope (POM), transverse fiber bundle (TFB) test, and droplet micro-debonding technique were respectively performed to characterize interfacial crystallization, adhesion and shear behaviors of AF/PA6 composites with different thermal treatments. Both interface adhesion and AF fibrillation are enhanced with decreasing cooling rate or increasing annealing temperature due to the increased interfacial transcrystallization interaction. However, fast cooled interface also presents a high interfacial shear strength (IFSS) due to favorable normal residual stress. The apparent IFSS is believed to be a result of competition between crystallization enhancing interfacial interaction, interfacial mismatching aggravating debonding, and an uncertain residual stress positive or negative for load transfer. TFB failure mechanism including AF fibrillation and kinking are schematically presented. Fibrillation strength of AF is found to follow Weibull distribution evaluated by droplet micro-debonding technique.     

Effect of chemical treatment of Kevlar fibers on mechanical interfacial properties of composites

In this work, the effects of chemical treatment on Kevlar 29 fibers have been studied in a composite system. The surface characteristics of Kevlar 29 fibers were characterized by pH, acid-base value, X-ray photoelectron spectroscopy (XPS), and FT-IR. The mechanical interfacial properties of the final composites were studied by interlaminar shear strength (ILSS), critical stress intensity factor (K(IC)), and specific fracture energy (G(IC)). Also, impact properties of the composites were investigated in the context of differentiating between initiation and propagation energies and ductile index (DI) along with maximum force and total energy. As a result, it was found that chemical treatment with phosphoric acid solution significantly affected the degree of adhesion at interfaces between fibers and resin matrix, resulting in improved mechanical interfacial strength in the composites. This was probably due to the presence of chemical polar groups on Kevlar surfaces, leading to an increment of interfacial binding force between fibers and matrix in a composite system.     

New strategy to reinforce and toughen composites via introducing thorns-like micro/nanofibers

In this work, we report a new strategy of introducing thorns-like fiber into composites, so that the resultant composites substantially benefit from strong fiber–matrix interface adhesion. Specifically, the “thorns” could increase in interlocking molecules chains and entangle with the surrounding matrix resin, which could impede the mobility of polymer chains, as like the roots with uplift capacity. Strong interfacial adhesion between fibers and matrices is suggested by the SEM images and the DMA studies. After the thorns-like fibers are embedded into epoxy resin, the glass transition temperature (T_g) and the storage modulus (E′) are higher than these of neat epoxy and untreated fibers-reinforced epoxy, respectively, and the flexural properties of the composites reinforced with thorns-like fibers are significantly increased. Therefore these novel three dimensional thorns-like fibers will be applicable for composite materials based upon its unique architecture, making it an attractive alternative to increase the performance of any matrix resin.     

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.     

Influence of compatibilizing agent molecular structure on the mechanical properties of phosphate glass fiber‐reinforced PLA composites

Eight compatibilizing agents were studied to investigate their effect on the quality of the interface between a phosphate glass fiber and a poly(lactic acid) (PLA) matrix. After application of the agents via dip‐coating, the fibers were Soxhlet extracted to remove any unreacted compatibilizer. To assess the interface quality, single fiber tensile tests of treated fibers and interfacial shear strengths (IFSS) of single fiber composites (SFC) were assessed. Of the agents tested, Glycerol‐2‐phosphate disodium pentahydrate (GP) and low molecular weight PLA with a sodium salt terminal group (PLA‐Na) showed the highest IFSS values, which were significantly higher than those of the control. Oligomeric PLA with a carboxylic acid end group and alendronate sodium trihydrate also showed an improvement over the control fibers. The hydrolytic degradation of these single fiber composites was studied over 7 days in water at 37 °C and a significant decrease in IFSS was observed in all cases, with the treated samples dropping to the level of the control. TGA and XPS analysis of the sized fibers showed that GP and PLA‐Na had been applied successfully to the fiber surface. © 2010 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 3082–3094, 2010     

Studies on PAN-based carbon fibers irradiated by Ar+ ion beams

In this work, the effects of Ar+ ion beam irradiation on carbon fibers were studied using tensile and surface analytical techniques. The single-fiber pull-out test was executed in order to characterize the fiber/epoxy matrix interfacial adhesion. The Ar+ ion beam was irradiated using an ion-assisted reaction (IAR) method in reactive gas conditions under an oxygen environment with 1 x 10(16) ions/cm(2) Ar+ ion dose (ID), 6 sccm blown gas flow rate, and different ion beam energy intensities. From the experimental results, both the interfacial shear strength (IFSS) and fracture toughness (Gi) were found to increase with increasing Ar+ ion irradiation intensity. This was probably due to the fact that Ar+ ion beam irradiation on carbon fibers was effective in altering their surface physical chemistry and structural morphology, resulting in improved interfacial adhesion in the fiber/epoxy matrix. The reliability of single-fiber pull-out test data could be improved by statistical analysis using the Weibull distribution, which served to predict the variation of the mechanical interfacial properties in a composite system.     

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.     

Effect of Chemical Modifications of Fibers on Tensile Properties of Epoxy Hybrid Composites

Treatment of oil palm empty fruit bunch (EFB) and jute fibers is carried out by using 2-hydroxy ethyl acrylate (2-HEA) to increase the interfacial bonding of fibers with the epoxy matrix. Fourier transform-infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM) were used to measure the change of surface composition of the fibers after treatment. Modified oil palm and jute fibers were used as reinforcements for epoxy matrix to fabricate hybrid composites by the hand lay-up technique. Tensile and morphological properties of hybrid composites were studied, and tensile properties of hybrid composites prepared from chemically treated oil palm/jute fibers were found to be better than those of untreated hybrid composites. SEM micrographs disclose that interfacial bonding between fiber and matrix significantly improved in the hybrid composites. Developed hybrid composites can be exploited as alternative materials for development of automotive and structural components instead of synthetic fiber–reinforced polymer composites.     

Effect of Chemical Treatment and Fiber Loading on Mechanical Properties of Borassus (Toddy Palm) Fiber/Epoxy Composites

The aim of the present study was to investigate and compare the mechanical properties of untreated and chemically modified Borassus fiber–reinforced epoxy composites. Composites were prepared by the hand lay-up process by reinforcing Borassus fibers with epoxy matrix. To improve the fiber-matrix adhesion properties, alkali (NaOH) and alkali combined with silane (3-aminopropyltriethoxysilane) treatment of the fiber surface was carried out. Examinations through Fourier transform-infrared spectroscopy and scanning electron microscopy (SEM) were conducted to investigate the structural and physical properties of the Borassus fibers. Tensile properties such as modulus and strength of the composites made with chemically modified and untreated Borassus fibers were studied using a universal testing machine. Based on the experimental results, it was found that the tensile properties of the Borassus-reinforced epoxy composites were significantly improved as compared with the neat epoxy. It was also found that the fiber treated with a combination of alkali and silane exhibited superior mechanical properties to alkali-treated and untreated fiber composites. The nature of the fiber/matrix interface was examined through SEM of cryo-fractured samples. Chemical resistance of composites was also found to be improved with chemically modified fiber composites.     

Effect of Oil Palm and Jute Fiber Treatment on Mechanical Performance of Epoxy Hybrid Composites

In this work, oil palm empty fruit bunch (EFB) and jute fibers were treated with 2-hydroxy ethyl acrylate (2-HEA) to improve interfacial bonding of oil palm EFB and jute fibers with epoxy matrix. Hybrid composites were fabricated by incorporation of modified oil palm EFB and jute fibers into an epoxy matrix by the hand lay-up technique. Mechanical (flexural and impact) and morphological properties of modified hybrid composites were measured. Results indicated that flexural and impact properties of modified fiber–reinforced hybrid composites improved as compared to untreated hybrid composites due to better fiber/matrix interfacial bonding, which was confirmed by scanning electron microscopy. We confirmed that treated oil palm/jute hybrid composite may be fabricated by advanced techniques such as resin transfer molding, extrusion, and injection molding for industrial applications in the automotive sector.     

Acid treatment for functionalizing polyethylene fiber surfaces for enhanced adhesion to epoxy resins

The utility of high-strength, high-modulus polyethylene fibers in fiber-reinforced composites is limited due to its poor interfacial adhesion to various polymeric matrices. One way to overcome this limitation is to introduce reactive functionalities on the fiber surface capable of covalently bonding to matrix resins. Ultra high-strength polyethylene (UHSPE) fibers were treated with chlorosulfonic acid. The surface acid groups were found to considerably improve the interfacial adhesion between polyethylene fibers and epoxy resins as shown by the microbond test. These surface functionalities were found to improve the fiber wettability, as shown by contact angle measurements using the Wilhelmy balance method. Colorimetric measurements of methylene blue absorption were used to quantify the surface concentrations of the acid groups. It was possible to functionalize the UHSPE fiber surfaces using this method to obtain fibers that formed a stronger adhesive bond with epoxy resins; this was achievable without sacrificing other fiber mechanical properties.