Study on the interfacial properties of two‐dimensionally arranged glass fiber/epoxy resin model composites

The effect of interfiber distance on the interfacial properties in two dimensional multi‐E‐glass fiber/epoxy resin composites has been investigated using fragmentation test. In addition, the effect of the fiber surface treatment on the interfacial properties has been studied. We found that the interfacial shear strength decreased with the decreasing interfiber distance at the range of <50 μm and the extent of the decreasing was more serious as the increasing of the number of adjacent fiber. This is probably that the interface between the fiber and the resin was damaged by the breaking of adjacent fibers and the damage increased with minimizing the interfiber spacing and the number of adjacent fibers. We can guess that interfacial shear strength in real composites is much smaller than that of multifiber fragmentation sample with touched fiber. When the interfiber distance was >50 μm, the interfacial shear strengths were saturated regardless of fiber surface treatment and were in close agreement with those of the single fiber fragmentation test. Finally, the interfacial shear strength evaluated using two dimensional fragmentation tests are shown as real values in‐site regardless of fiber surface treatment, interfiber distance, and existing matrix cracks. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1541–1551, 2006     

Multiple fiber technique for the single fiber fragmentation test

The single fiber fragmentation test has been modified by embedding multiple fibers into matrix resin. During testing, we examined the interfacial shear strengths between the fibers and the matrix. In addition, the time-dependent nature of the fragmentation process was considered. In the fragmentation test, we examined the failure process of two fibers placed far from each other, and we found that the failure profile of the two fibers were similar to the failure profiles from tests done on single fibers. When we examined three fibers, we found that the measured interfacial shear strength values were much greater than the shear strength values from either the single or two fiber tests. However, when we used three fibers, we found it difficult to control the interfiber spacing. Consequently, whenever the interfiber spacing was too small, breaks in one fiber caused breaks in the adjacent fiber. In conclusion, using multiple fibers in a fragmentation test has many merits, such as saving time in testing, ease of comparing the effects of fiber surface treatment, and testing different fibers in the same matrix exposed to the same processing conditions. © 1998 John Wiley & Sons, Inc. J Appl Polm Sci 67:1701–1709, 1998     

Influence of processing rate and formulation on the interface strength of vinyl ester/E‐glass composites

The single fiber fragmentation test was used to investigate the effect of gelation time on interfacial shear properties of fast reacting resin systems. We developed a processing system capable of producing single fiber fragmentation samples with gelation times that ranged from 2 min to 45 min. The interfacial properties of E‐glass fibers in vinyl ester resin were measured with single fiber fragmentation tests using a manual and an automated testing machine. We found that vinyl ester resins catalyzed with methyl ethyl ketone peroxide and promoted with cobalt naphthenate and dimethylaniline gelled in less than two minutes and had an estimated interfacial shear strength of 105 MPa. Specimens cured without the promoter gelled in 45 min and had an interfacial shear strength of 72 MPa. Further curing of the unpromoted specimens resulted in an increase in shear strength to 96 MPa. We have demonstrated the ability to make and test rapidly cured specimens, thus expanding the range of materials that can be tested using the single fiber fragmentation testing technique.     

Effect of Atmospheric Plasma Treatment on Carbon Fiber/Epoxy Interfacial Adhesion

In this work the effect of atmospheric plasma treatment on carbon fiber has been studied. The carbon fibers were treated for 1, 3 and 5 min with a He/O₂ dielectric barrier discharge atmospheric pressure plasma. The fiber surface morphology, surface chemical composition and interfacial shear strength between the carbon fiber and epoxy resin were investigated using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and the single fiber composite fragmentation test. Compared to untreated carbon fibers, the plasma treated fiber surfaces exhibited surface morphological and surface composition changes. The fiber surfaces were found to be roughened, the oxygen content on the fiber surfaces increased, and the interfacial shear strength (IFSS) improved after the atmospheric pressure plasma treatment. The fiber strength showed no significant changes after the plasma treatment.     

Improvement of the interfacial shear strength of poly(p‐phenylene benzobisoxazole) fiber/epoxy resin composite via a novel surface coating agent

Poly(p‐phenylene benzobisoxazole) (PBO) fiber with a smooth surface exhibits limited interfacial interaction with resin matrix. One of the effective strategies to improve the adhesion between the fiber and resin matrix is through surface modification of the fiber. In this study, we have proposed a novel surface treatment agent based on phosphoester cross‐linked castor oil (PCCO) for effective surface treatment of PBO fibers. The surface treatment agent was prepared by a simple cross‐linking reaction between hydroxy phosphorylated castor oil (PCO) and epoxy resin, with alcohol as the solvent at 65°C. Once the PBO fiber was treated with this agent, the interfacial adhesion between the PBO fiber and the epoxy resin could then be improved. Systematic analyses suggest that the surface treatment with (PCO + epoxy)/alcohol solution improves the interaction of the PBO fiber with the epoxy resin matrix. The PCCO coated onto the surface of PBO fiber acts as a coupling agent, improving the interfacial shear strength (IFSS) of the PBO fiber/epoxy resin composite. Results indicate a 156% increase in IFSS without compromising the mechanical properties of the fiber. POLYM. COMPOS., 37:1198–1205, 2016. © 2014 Society of Plastics Engineers     

Improvement of the mechanical properties of an ultrahigh molecular weight polyethylene fiber/epoxy composite by corona‐discharge treatment

The interfacial shear strength of an ultrahigh molecular weight (UHMW) polyethylene (PE) fiber/epoxy‐resin system was greatly improved by the corona‐discharge treatment of the fiber. The UHMW PE‐fiber/epoxy‐resin composite was prepared with corona‐discharge‐treated UHMW PE fiber. The mechanical properties of the composite sheet were determined by tensile testing. The tensile strength of the composite was also very much improved. However, the tensile strength of the composite was about one‐half of the theoretical strength. This result was due to the molecular degradation of the PE‐fiber surface caused by surface modification. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 1162–1168, 2001     

Influence of fiber modification on interfacial adhesion and mechanical properties of pineapple leaf fiber‐epoxy composites

Three kinds of surface treatment, that is, the alkalization (5% w/v NaOH aqueous solution), the deposition of diglycidyl ether of bisphenol A (DGEBA) from toluene solution (1% w/v DGEBA), and the alkalization combined with the deposition of DGEBA (5% w/v NaOH/1% w/v DGEBA) were applied to modify interfacial bonding and to enhance mechanical properties of pineapple leaf fiber (PALF) reinforced epoxy composites. The fiber strength and strain were measured by single fiber test and the fiber strength variation was assessed using Weibull modulus. Furthermore, a fragmentation test was used to quantify the interfacial adhesion of PALF‐epoxy composite. It was verified that the interfacial shear strength of modified PALFs was substantially higher than that of untreated PALF by almost 2–2.7 times because of the greater interaction between the PALFs and epoxy resin matrix. The strongest interfacial adhesion was obtained from the fibers that had been received the alkalization combined with DGEBA deposition. Moreover, the flexural and impact properties of unidirectional PALF‐epoxy composites were greatly enhanced when reinforced with the modified PALFs due to an improvement in interfacial adhesion, particularly in the synergetic use of 5% NaOH and 5% NaOH/1% DGEBA. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Relationship Between Some Mechanical Strengths of CFRP and Interfacial Properties

The relationships between microscopic properties such as interfacial shear strength (IFSS) and macroscopic properties such as flexural strength were investigated for CFRP prepared from carbon fiber and epoxy resin. Flexural, tensile and impact strengths all went through maximum values when plotted against the surface treatment time of the carbon fiber. The flexural strength of CFRP as a function of the treatment time of the carbon fiber behaved similarly to the adhesive strength of the resin and carbon fiber. Also, the results indicated that the bahavior of tensile and impact strengths varied with the treatment time in much the same way as the interfacial shear strength did. The occurrence of these two types of macroscopic and microscopic property effects can be understood by taking into account the chemical activity and roughness of the carbon fiber surface.     

Interfacial shear strength of flax fibers in thermoset resins evaluated via tensile tests of UD composites

A method of interfacial shear strength evaluation, based on the length distribution of fibers pulled out from the tensile fracture surface of an oriented flax-reinforced composite, is applied to composites with vinyl ester and acrylated epoxidized soy oil resin matrices. Two approaches for characterizing the strength of fibers with modified Weibull distribution, fiber fragmentation tests and fiber tension tests, are compared in the analysis of pull-out data. Interfacial shear strength is found to increase by a few percent when loading rate is increased from 1.33% to 8%/min.     

Application of the microbond technique. IV. Improved fiber–matrix adhesion by RF plasma treatment of organic fibers

The microbond technique is a modification of the single-fiber pullout test for measuring interfacial shear strength. Briefly, a cured microdroplet of material is debonded in shear from a single fiber. Ultra-high modulus polyethylene (Spectra) fibers and aramid fibers (Kevlar) were treated using a radio frequency plasma in order to increase the interfacial bond between the fibers and an epoxy resin. The treated fiber surface was subsequently analyzed by X-ray photoelectron spectroscopy (XPS). Plasma treatment resulted in an increased concentration of oxygen containing functionalities on the fiber surface. The interfacial shear strength as determined by the microbond test increased by 118% for the Spectra fibers and by 45% for the Kevlar fibers with the same epoxy resin. Scanning electron microscopy indicated little change of the surface topography of either fiber following plasma treatment. Effects of friction and surface composition of the plasma-treated fibers is discussed. © 1993 John Wiley & Sons, Inc.     

热致性液晶聚芳酯纤维表面的化学修饰

采用环氧氯丙烷作为处理试剂,通过傅-克化学反应来修饰热致性液晶聚芳酯(TLCP)纤维的表面,并通过傅里叶变换红外光谱仪(FTIR)、万能电子强力仪、单丝拔出试验(SFP)与扫描电子显微镜(SEM)系统研究了化学修饰对纤维表面的化学结构、纤维力学性能、复合材料的界面剪切强度及纤维的表面形态的影响。研究结果表明:通过傅-克化学反应修饰TLCP纤维的表面,可以有效地提高TLCP单纤维-环氧树脂复合材料的界面剪切强度,相对于未修饰的纤维约提高了52%,表面化学修饰的最佳反应时间为40 min。此外,经修饰的TLCP单纤维表面没有明显的刻蚀或受损现象,且纤维的力学性能不会受到明显影响。傅-克化学反应修饰TLCP纤维可有效提高TLCP纤维-环氧树脂复合材料的界面性能。     

Effects of silica surface treatment on the impregnation process of silica fiber/phenolics composites

Effects of silica surface treatment on the impregnation process of silica fiber/phenolics composites were studied. Micro‐Wilhelmy method was used to evaluate the surface characterization of silanized silica fibers. The interlaminar shear strength (ILSS) measurements and the void contents of the silica fiber/phenolics composites were also performed. The interactions occurring between silica fiber and the components of phenolic resin solution can affect the contact angle between silica fiber and phenolic solution and the dynamic adsorption behavior of phenolic resin onto silica fiber. There are competitive adsorptions to different extent for phenolic resin and solvent onto silica fibers. Silica fibers as reinforcement treated by silane‐coupling agent, such as γ‐aminopropyl‐triethoxysilane, γ‐glycidoxypropyl‐trimethoxysilane, trimethylchlorosilane, and γ‐methacryloxypropyl‐trimethoxysilane, influence the mechanical interfacial properties of silica fiber/phenolics composites and the uniformity of resin distribution. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Effect of silane coupling agents on basalt fiber–epoxidized vegetable oil matrix composite materials analyzed by the single fiber fragmentation technique

The fiber–matrix interfacial shear strength (IFSS) of biobased epoxy composites reinforced with basalt fiber was investigated by the fragmentation method. Basalt fibers were modified with four different silanes, (3‐aminopropyl)trimethoxysilane, [3‐(2‐aminoethylamino)propyl]‐trimethoxysilane, trimethoxy[2‐(7‐oxabicyclo[4.1.0]hept‐3‐yl)ethyl]silane and (3‐glycidyloxypropyl)trimethoxysilane to improve the adhesion between the basalt fiber and the resin. The analysis of the fiber tensile strength results was performed in terms of statistical parameters. The tensile strength of silane‐treated basalt fiber is higher than the tensile strength of the untreated basalt fiber; this behavior may be due to flaw healing effect on the defected fiber surfaces. The IFSS results on the composites confirm that the interaction between the fiber modified with coupling agents and the bio‐based epoxy resin was much stronger than that with the untreated basalt fiber. POLYM. COMPOS., 36:1205–1212, 2015. © 2014 Society of Plastics Engineers     

Interfacial improvement of carbon fiber/epoxy composites using a simple process for depositing commercially functionalized carbon nanotubes on the fibers

An aqueous suspension deposition method was used to coat the sized carbon fibers T700SC and T300B with commercially carboxylic acid-functionalized and hydroxyl-functionalized carbon nanotubes (CNTs). The CNTs on the fiber surfaces were expected to improve the interfacial strength between the fibers and the epoxy. The factors affecting the deposition, especially the fiber sizing, were studied. According to single fiber-composite fragmentation tests, the deposition process results in improved fiber/matrix interfacial adhesion. Using carboxylic acid-functionalized CNTs, the interfacial shear strength was increased 43% for the T700SC composite and 12% for the T300B composite. The relationship between surface functional groups of the CNTs and the interfacial improvement was discussed. The interfacial reinforcing mechanism was explored by analyzing the surface morphology of the carbon fibers, the wettability between the carbon fibers and the epoxy resin, the chemical bonding between the fiber sizing and the CNTs, and fractographic observation of cross-sections of the composites. Results indicate that interfacial friction, chemical bonding and resin toughening are responsible for the interfacial improvement of nanostructured carbon fiber/epoxy composites. The mechanical properties of the CNT-deposited composite laminate were further measured to confirm the effectiveness of this strategy.     

Adhesion characteristics of oxygen plasma-treated rayon fibers

The effect of oxygen plasma treatment of fiber on the adhesion between regenerated cellulose fiber and polyethylene (PE) was investigated using the single-fiber fragmentation test. In addition to allowing the determination of the interfacial shear strength, the fragmentation test provided a great deal of useful information on shear stress transfer and failure mechanisms in the systems. It was found that oxygen plasma treatment considerably enhanced the interfacial adhesion, as established by both the shear strength values that were measured and the birefringence patterns observed. The influence of the duration of treatment on adhesion was studied and found to be a very important parameter. The roles of surface chemistry, surface energetics, and surface topography of fiber in the interaction balance were investigated using electron spectroscopy for chemical analysis (ESCA), contact angle measurements, and scanning electron microscopy (SEM). It was seen that neither the plasma-induced changes in the surface energetics nor those in the surface topography could have exerted a positive effect on adhesion. Instead, the improved adhesion was ascribed to covalent bonds formed between the fiber and the matrix, as hydroperoxides, which were created on the fiber surface by the plasma treatment, decomposed during the fabrication of single-fiber specimens.     

Improvement of adhesion between polyethylene and regenerated cellulose fibers by surface fibrillation

Regenerated cellulose fibers spun from straw pulp using the N-methylmorpholine N-oxide (NMMO) process were evaluated as a reinforcement for low-density polyethylene (LDPE). Surface fibrillation was carried out by a mechanical treatment to improve interfacial adhesion. Surface fibrillation resulted in a gradual change in surface topography, as detected by SEM. Long and numerous twisted fibrils were observed on the surface of the treated fibers. The fiber perimeters, determined by the Wilhelmy plate method, increased with an extended degree of fibrillation, while the strength of the fiber was not affected by the surface treatment. Model composites were prepared by embedding untreated and surface-fibrillated single fibers into an LDPE matrix, and the single fiber fragmentation (SEF) test was carried out to determine the critical fiber length. The interfacial shear strength (τ) was then calculated by applying a modified form of the Kelly-Tyson equation. It was found that the interfacial shear strength increased significantly as a result of surface fibrillation. The proposed mechanism for the improvement of interfacial adhesion is a mechanical anchoring between the matrix and the fiber.     

The relationship between zeta-potential and pull-out shear strength on modified UHMWPE fiber reinforced epoxy composites

UHMWPE fiber exhibits high performance, featuring high tensile strength and modulus, because of its extended chain structure. However, this fiber demonstrates some defects, such as low melting point, creep, and poor interfacial bonding with resin. Therefore, it is still not widely applied in composites. This research attempted to improve the performance by applying interfacial treatment to the fiber, using polypyrrole (PPy) synthesized through oxidation. The interfacial shear strength was evaluated using the results of a pull-out test and a Zeta Potential. The UHMWPE fiber was exposed to PPy treatment at various temperatures. The PPy-modified fiber was then impregnated with epoxy to generate the composites. The effects of the modification were also examined. The performance of the composites was determined by the Zeta Potentials of the fiber and resin, using an EKA electrokinetic analyzer. The interfacial shear strength was determined by the pull-out test. The morphology of fiber was observed by SEM. Results show that the shear strength of the interface between the PPy-treated UHMWPE fiber and epoxy increased 215%. The correlation between the Zeta Potential and the interfacial shear strength was also observed.     

Effects of functional groups and surface roughness on interfacial shear strength in ultrahigh molecular weight polyethylene fiber/polyethylene system

Corona discharge treatment was conducted for ultrahigh molecular weight polyethylene (UHMWPE) fiber. The functional groups and surface roughness of the polyethylene fiber surface were determined by an X‐ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). The interfacial shear strength of UHMWPE fiber with HDPE film was determined by microbond pullout method. The interfacial shear strength increased by corona treatment. Then, the effect of the chemical and physical factors on the interfacial shear strength was discussed based on the results of multivariate regression analysis. The results indicated that the contribution of functional groups and surface roughness to the interfacial shear strength was expressed as 50 and 50%, respectively. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 243–249, 1999     

Carbon nanotubes grafting PBO fiber: A study on the interfacial properties of epoxy composites

To improve the interfacial performance of poly[p‐phenylene benzobisoxazole] (PBO) fiber and epoxy resin, a modified multiwalled carbon nanotubes (MWCNTs‐Ecp) were used to achieve this purpose through grafting onto PBO fiber surface using a gamma ray radiation method. Experimental results indicated that the equilibrium wetting rate and equilibrium adsorption amount of the modified PBO fiber for epoxy resin and acetone were all higher than that of as received PBO fiber. The interfacial shear strength (IFSS) of single fiber composite increased from 31.4 to 77.5 MPa after modification. The fracture models of composites are changed from pure interfacial failure to combination failure of interface and resin interlayer. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

Characterization of ramie fiber/soy protein concentrate (SPC) resin interface

Ramie fiber/soy protein concentrate (SPC) polymer (resin) interfacial shear strength (IFSS) was measured using the microbond technique. To characterize the effect of plasticization, SPC resin was mixed with glycerin. Fibers were also treated with ethylene plasma polymer to reduce fiber surface roughness and polar nature to control the IFSS. Fiber surfaces after ethylene plasma polymerization, and fracture surfaces of specimens before and after the microbond tests were characterized using a scanning electron microscope (SEM). Some specimens were also characterized using electron microprobe analyzer (EMPA) to map the residual resin on the fiber surface after the microbond test. Effects of glycerin concentration in SPC and ethylene plasma fiber surface treatment time on the IFSS were investigated. Preparation of SPC resin requires a large amount of water. As expected, during drying of SPC resin, the microdrops shrank significantly. The high IFSS values indicate strong interfacial interaction in the ramie fiber/SPC resin system. This strong interfacial interaction is a result of a highly polar nature of both the ramie fiber and the SPC resin and rough fiber surface. Ethylene plasma polymerization was used to control the IFSS. The plasma polymer imparted a polyethylene-like, non-polar polymer coating on the fiber surface. As a result, the fiber surface became smoother compared to the untreated fiber. Both fiber smoothness and non-polar nature of the coating reduced the ramie fiber/SPC resin IFSS. Plasticization of the SPC resin by glycerin also decreased the adhesion strength of the ramie fibers with the SPC resin. The load-displacement plots for IFSS tests obtained for different resin and fiber combinations indicate different interfacial failure modes.