Surface modification of boron fibres for improved strength in composite materials

When boron fibres are combined with an organic matrix, such as an epoxy resin, a high-performance composite structure is created. This study investigates the surface chemistry of plasma- and organosilane-treated boron fibres with the key aim to improving the adhesion properties between the boron fibre and the epoxy matrix. Optimisation of this interfacial region plays a critical role in influencing the mechanical behaviour of composite materials and has considerable industrial applications in the aerospace and manufacturing industries. The surface chemistry of a model boron surface and boron fibres was monitored using a combination of X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Initial investigation of the as-received fibres showed the presence of silicone contamination on the fibre surface, which would affect adhesion. Removal of this contaminant through solvent cleaning and plasma oxidation provided an ideal surface for attachment of the organosilane adhesion promoter. A model for the interaction of the organosilane with a boron surface is proposed. The pull-out strength of boron fibres, with different surface treatments, embedded in the epoxy resin was measured using a custom designed adhesiometer. Compared with as-received boron fibres, a 6-fold improvement in the apparent interfacial shear strength was achieved for the organosilane treated fibres. Optical microscopy was used to determine the failure mechanisms between the fibre and epoxy resin. Typically, as the surface treatment improved adhesion, the locus of failure changed from the boron–epoxy interface to failure within the epoxy and ultimately fibre breakage.     

Mechanical properties of maleic anhydride treated jute fibre/polypropylene composites

Abstract

The effect of maleic anhydride (MA) modification of jute fibre on the mechanical properties of jute/polypropylene (PP) composites was studied. Jute fibre, an environmental friendly, low-density renewable material was chemically modified with MA before the incorporation with PP to improve interfacial adhesion between them. Fourier transform infrared (FTIR) study showed that the C=C groups of MA attached to jute cellulose reacted with the PP matrix. Jute fibre/PP composite treated with MA displayed higher Young's modulus and dynamic storage modulus owing to the enhanced interfacial adhesion between the fibre and PP matrix. A scanning electron microscopy (SEM) study showed evidence of the enhanced adhesion and bridging in the interfacial region of the composite as the result of MA modification of jute fibre.     

Experimental characterization of interfacial adhesion of an optical fiber embedded in a composite material

The efficiency of an optical sensor embedded in a composite structure strongly depends on the interfacial adhesion between the optical fiber coating and the surrounding solid material. The present paper reports on the study of the interfacial adhesion of an optical fiber embedded in a composite material. A simple system composed of optical fibers embedded in an epoxy vinylester resin was first studied to evaluate the influence of embedded length, curing temperature and curing time. Pull-out tests on optical fibers bonded in epoxy vinylester/glass fiber composite material were carried out to measure the effect of glass concentration on the fiber bonding. The pull-out results showed no effect of both embedded length and curing temperature. However, an increase of the interfacial debonding stress is reported with increased curing time. For the optical fiber/composite system, a linear evolution of interfacial debonding stress with increasing glass fiber concentration is reported.     

Glass optical fibre sensors for detection of through thickness moisture diffusion in glass reinforced composites under hostile environments

A combination of evanescent wave optical sensors (EWOSs) and fibre Bragg gratings (FBGs) were embedded in an epoxy vinyl ester and an epoxy vinyl ester based glass reinforced polymer (GRP) composite to measure fluid ingress that would result in degradation under hostile conditions. Samples were subjected to accelerated aging in the form of single sided exposure to simulated sea water at 120°C in a pressurised stainless steel vessel. Low cost EWOSs were prepared from a standard multimode glass optical fibre and compared to commercially available FBGs. Both sensors were able to detect the early stage of moisture diffusion into the GRP matrix. The evanescent sensors showed a reduction in the transmitted signal intensity between 1500 and 1650?nm with an increasing exposure time due to a change in the optical properties of the polymer, whereas a peak shift was observed for the FBGs due to the swelling of the resin with the absorption of water. Additionally, the glass optical fibre sensors were embedded in a configuration that allowed the extent of diffusion through the thickness of the GRPs to be monitored, with the fibres in the closest position to the exposure face showing a greater signal change than those positioned further away.     

基于NOL环的高性能纤维与环氧树脂的匹配性研究

纤维与树脂的界面对复合材料的整体力学性能有着显著的影响。基于NOL环的宏观力学测试一般被用来反映复合材料的界面粘结性能,因此适用于评价纤维与树脂之间的宏观力学性能匹配性。为了探究高性能碳纤维T700SC、T800HB及高强玻璃纤维与环氧树脂的宏观力学性能匹配性,本研究首先根据GB/T 1458—2008国家标准制备NOL环试样,再借助NOL环的拉伸和层间剪切强度测试分析了高性能纤维与环氧树脂不同匹配组合宏观力学性能差异的原因,并寻找出最佳匹配组合。结果表明:玻璃纤维与环氧树脂的界面存在最佳的粘结强度,而且不同粘结强度导致拉伸强度和破坏机理不同,而碳纤维复合材料界面性能较差,容易分层破坏;T800HB与环氧树脂的宏观力学匹配性优于T700SC,环氧树脂力学性能、碳纤维的表面微观结构与性质以及环氧树脂与碳纤维之间的相互作用关系是影响界面粘结性能的根本原因。该研究在高性能纤维单向复合材料的材料选择与设计方面具有现实意义。     

Effects of fiber surface chemistry and roughness on interfacial structures of electrospun fiber reinforced epoxy composite films

This work reported the effect of surface chemistry and roughness of electrospun fibers on fiber/matrix interfacial structures and the resultant macroscopical properties of composite films. Three types of fibrous mats composed of ultrafine fibers, that is, cellulose acetate (CANM), polyurethane (PUNM), and cellulose acetate/polyurethane composite (CAPUNM) were fabricated through electrospinning. CA fiber surfaces were rough with many hydroxyl groups; PU fiber surfaces were smooth, whereas CAPU composite fibers exhibited cocontiuous structure with rough surfaces. The fiber‐reinforced epoxy composite films were prepared by the solution impregnation method. The fractured surfaces of the composites were analyzed by scanning electron microscopy. Severe interfacial debonding and fiber pullouts were observed for PUNM/epoxy composites, while strong interfacial adhesion was formed for CANM/epoxy and CAPUNM/epoxy composites. The interfacial structure played important roles in the visible light transmittance of the composite films. For example, CANM/epoxy films showed the best optical property, whereas PUNM/epoxy films displayed the poorest light transmitting property and were translucent. The interfacial structure also affected the mechanical properties of the composites. The mechanical strength of fibrous mats followed an increasing order of CANM < CAPUNM < PUNM, but the mechanical strength of the composite films was in a reverse order, that is, CANM/epoxy > CAPUNM/epoxy > PUNM/epoxy. POLYM. COMPOS., 2011. © 2011 Society of Plastics Engineers     

The effect of fibre sizing and compatibilizer of polypropylene/poly(butylene terephthalate) blends on the mechanical and interphase properties of basalt fibre reinforced composites

The effect of basalt fibre sizing on the mechanical and interphase properties of fibre‐reinforced composites was studied. Two different chemical preparations of the fibre surface (PBT‐compliant and PP‐compliant) were used. The polymer matrix was prepared from polypropylene/poly(butylene terephthalate) (PP/PBT) immiscible polymer blend and the effect of different compatibilizers on the composite properties was evaluated. SEM hints at improved fibre adhesion to the polymer matrix when a PP‐compliant sizing is applied. SEM also reveals improved compatibilization effects when block copolymer instead of multiblock copolymer is used for the PP/PBT blend preparation. The pull‐out test was applied to quantitatively evaluate the interface adhesion between the fibres and matrices. It showed a high value of the interfacial shear strength between basalt fibres modified with PP‐compliant sizing and polymer blend compatibilized by block copolymer, thus confirming good adhesion. One possible explanation of such good mechanical properties can be related to the chemical interactions between functional groups, mainly maleic anhydride on basalt fibres and the polyolefin component (PP) of the polymer matrix. © 2017 Society of Chemical Industry     

Compressive behaviour of rigid rod polymer fibres and their adhesion to composite matrixes

Abstract

The deformation behaviour of the new high performance polymer fibres, poly(p-phenylene benzobisoxazole) (PBO) and polypyridobisimidazole (PIPD) and their adhesion to an epoxy composite matrix have been investigated. Both fibres give well defined Raman spectra, and the deformation micromechanics of PBO and PIPD single fibres and composites were studied from stress induced Raman band shifts. Single fibre stress-strain curves were determined in both tension and compression, thus providing an estimate of the compressive strength of these fibres. It was found that the PIPD fibre has a higher compressive strength (~1 GPa) than PBO (~0·3 GPa) and other high performance polymer fibres, because hydrogen bond formation is possible between PIPD molecules. It has been shown that when PBO and PIPD fibres are incorporated into an epoxy resin matrix, the resulting composites show very different interfacial failure mechanisms. The fibre strain distribution in the PBO-epoxy composites follows that predicted by the full bonding, shear lag model at low matrix strains, but deviations occur at higher matrix strains due to debonding at the fibre/matrix interface. For PIPD-epoxy composites, however, no debonding was observed before fibre fragmentation, indicating better adhesion than for PBO as a result of reactive groups on the PIPD fibre surface.     

Interfacial studies on the surface modified aramid fiber reinforced epoxy composites

In this work, solutions of rare earth modifier (RES) and epoxy chloropropane (ECP) grafting modification method were used for the surface treatment of aramid fiber. The effect of chemical treatment on aramid fiber has been studied in a composite system. The surface characteristics of aramid fibers were characterized by Fourier transform infrared spectroscopy (FTIR). The interfacial properties of aramid/epoxy composites were investigated by means of the single fiber pull‐out tests. The mechanical properties of the aramid/epoxy composites were studied by interlaminar shear strength (ILSS). As a result, it was found that RES surface treatment is superior to ECP grafting treatment in promoting the interfacial adhesion between aramid fiber and epoxy matrix, resulting in the improved mechanical properties of the composites. Meanwhile, the tensile strengths of single fibers were almost not affected by RES treatment. This was probably due to the presence of reactive functional groups on the aramid fiber surface, leading to an increment of interfacial binding force between fibers and matrix in a composite system. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:4165–4170, 2006     

Effect of alkali treatment on properties of unidirectional isora fibre reinforced epoxy composites

Abstract

Unidirectional isora fibre reinforced epoxy composites were prepared by compression moulding. Isora is a natural bast fibre separated from Helicteres isora plant by retting process. The effect of alkali treatment on the properties of the fibre was studied by scanning electron microscopy (SEM), IR, thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Mechanical properties such as tensile strength, Young's modulus, flexural strength, flexural modulus and impact strength of the composites containing untreated and alkali treated fibres have been studied as a function of fibre loading. The optimum fibre loading for tensile properties of the untreated fibre composite was found to be 49% by volume and for flexural properties the loading was optimised at ～45%. Impact strength of the composite increased with increase in fibre loading and remained constant at a fibre loading of 54·5%. Alkali treated fibre composite showed improved thermal and mechanical properties compared to untreated fibre composite. From dynamic mechanical analysis (DMA) studies it was observed that the alkali treated fibre composites have higher E' and low tan δ maximum values compared to untreated fibre composites. From swelling studies in methyl ethyl ketone it was observed that the mole percentage of uptake of the solvent by the treated fibre composites is less than that by the untreated fibre composites. From these results it can be concluded that in composites containing alkalised fibres there is enhanced interfacial adhesion between the fibre and the matrix leading to better properties, compared to untreated fibre composites.     

碳纤维复合材料发动机壳体用高性能树脂基体的研制

在综合考虑树脂黏度、力学性能、耐热性能的基础上。开发了适用于碳纤维复合材料火箭发动机壳体温法缠绕成型工艺用耐高温和韧性环氧树脂基体。用差示扫描式量热法(DSC)、傅里叶红外光谱FT—IR等分析技术对该韧性树脂基体的固化反应动力学参数、树脂基体固化物的性能和复合材料的性能进行了系统的研究。结果表明，该韧性树脂基体黏度低，适用期长，韧性好，与碳纤维界面粘接强度高，所制得的复合材料火箭发动机壳体纤维强度转化率高。为今后相关方面的研究指明了方向。     

Application of the microbond technique: Characterization of carbon fiber-epoxy interfaces

Microbonding has been applied to measure the interfacial shear strength, τ, between single carbon fiber and microdroplets of epoxy resins. The effect of thermoset cure and resin modification on this initial parameter for composite performance have been studied. The interfacial shear strength for the host fiber/epoxy system (T-300/Epos 828) increased 3 fold from a B-stage to a fully cured material. The addition of a toughening agent called “Fortifier P” to the host resin system increased T by 40%. Residual thermal stresses were calculated and their contribution to mechanical adhesion were related to friction components.     

Stress Transfer Function for Interface Assessment in Composites with Plasma Copolymer Functionalized Carbon Fibres

Radio-frequency-induced plasma copolymerization of acrylic acid/1,7-octadiene was used to produce a range of functionalized plasma copolymer coatings with controlled degree of adhesion. The single-fibre fragmentation test was used to characterize the adhesion of plasma copolymer coated fibres to epoxy resin. The cumulative stress transfer function (CSTF) and Kelly-Tyson approaches were used to evaluate the degree of adhesion. By continuous monitoring of the fragmentation process, it was found that the mechanical performance of a composite material could be evaluated using the CSTF methodology at strain well below saturation. The degree of debonding was a good measure of relative interface/interphase adhesive strength. The trend in the CSTF is consistent with the propagation of interfacial debonds during the test. For a completely debonded fibre a normalized CSTF value, referred as stress transfer efficiency (STE), was found to provide a more consistent analysis that was able to differentiate between fibres with similar degrees of debonding. The calculated values of interfacial shear strength (IFSS) were only valid for a fully debonded fibre (1,7-octadiene plasma homopolymer coating) where the assumption of a constant shear stress, as in the Kelly-Tyson model, applied. However, IFSS did not provide the same ranking. Where debonding does not occur, the stress transfer efficiency also provides a sensitive measure of the interface/interphase performance. Improved adhesion over the untreated-unsized carbon fibre was observed for both of the plasma copolymer-coated and commercially treated carbon fibres. Since there is a concentration dependence of carboxyl groups on adhesion, the mechanism appears to relate to covalent bond formation with the epoxy group. Plasma copolymer coatings on carbon fibres also causes an increased tensile strength and Weibull modulus.     

Stress Transfer Function for Interface Assessment in Composites with Plasma Copolymer Functionalized Carbon Fibres

Radio-frequency-induced plasma copolymerization of acrylic acid/1,7-octadiene was used to produce a range of functionalized plasma copolymer coatings with controlled degree of adhesion. The single-fibre fragmentation test was used to characterize the adhesion of plasma copolymer coated fibres to epoxy resin. The cumulative stress transfer function (CSTF) and Kelly-Tyson approaches were used to evaluate the degree of adhesion. By continuous monitoring of the fragmentation process, it was found that the mechanical performance of a composite material could be evaluated using the CSTF methodology at strain well below saturation. The degree of debonding was a good measure of relative interface/interphase adhesive strength. The trend in the CSTF is consistent with the propagation of interfacial debonds during the test. For a completely debonded fibre a normalized CSTF value, referred as stress transfer efficiency (STE), was found to provide a more consistent analysis that was able to differentiate between fibres with similar degrees of debonding. The calculated values of interfacial shear strength (IFSS) were only valid for a fully debonded fibre (1,7-octadiene plasma homopolymer coating) where the assumption of a constant shear stress, as in the Kelly-Tyson model, applied. However, IFSS did not provide the same ranking. Where debonding does not occur, the stress transfer efficiency also provides a sensitive measure of the interface/interphase performance. Improved adhesion over the untreated-unsized carbon fibre was observed for both of the plasma copolymer-coated and commercially treated carbon fibres. Since there is a concentration dependence of carboxyl groups on adhesion, the mechanism appears to relate to covalent bond formation with the epoxy group. Plasma copolymer coatings on carbon fibres also causes an increased tensile strength and Weibull modulus.     

The effect of a doubly modified carbon nanotube derivative on the microstructure of epoxy resin

The surface of multi wall carbon nanotubes (MWCNTs) was first covalently functionalized with oleyl amine and then non-covalently wrapped with polycarbosilane (PCS). The hybrid functional groups were chosen to introduce different features in the MWCNTs properties. For covalent functionalization a long chain unsaturated aliphatic amine was used to simultaneously achieve the dissociation of MWCNT bundles along with the dispersion and interaction with the host matrix using the amide functionality and double bond. On the other hand, a thermally stable polymer was selected which can interact with both resin and glass fabric to promote interfacial adhesion. This hybrid doubly modified MWCNT is thus possesses duel advantages in glass fiber based epoxy composite. The pristine, covalent, noncovalent and covalent-noncovalent doubly modified MWCNT systems were used to study the viscoelastic behavior and interactions of functionalized MWCNTs in the matrix above and below the glass transition temperature of the matrix. The PCS coating on the MWCNTs is amorphous and thermally insulating whereas the nanotube is highly graphitized and thermally conducting. This contrasting behavior provides us to insight into the temperature dependant resin microstructure and curing thermodynamics of epoxy resin in the presence of MWCNTs.     

The effect of irradiation surface treatment of UHMWPE fibre on the interfacial properties of PVC composite

Irradiation surface modification method was used for the surface treatment of ultrahigh molecular weight polyethylene (UHMWPE) fibre to improve the interfacial adhesion of the UHMWPE fibre reinforced PVC composite. The surface characteristics of untreated and treated UHMWPE fibre were characterised by XPS and Fourier transform infra-red spectroscope. The friction and wear properties of the PVC composites filled with differently surface-treated UHMWPE fibres (20?vol.-%), were investigated on a ring-on-block tribometer. Experimental results revealed that irradiation treatment largely increased the mechanical properties of UHMWPE fibre/neoprene/PVC (UF/N/PVC) composites. Scanning electron microscope investigation of worn surfaces of PVC composites showed that surface-treated UF/N/PVC composite had the strongest interfacial adhesion.     

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     

A comparative investigation of interfacial adhesion behaviour of polyamide based self-reinforced polymer composites by single fibre and multiple fibre pull-out tests

Abstract

Interfacial adhesion of composite materials plays an important role in their mechanical properties and performance. In the present investigation, analysis of the interfacial properties of self-reinforced polyamide composites by using microbond multiple fibre pull-out test is emphasised. Microbond specimens prepared through thermal processing are tested for their interfacial properties by multiple fibre bundle pull-out tests and compared with that of traditional single fibre pull-out test specimens. Multiple fibre pull-out addresses the volume fraction as well as eliminates the possibility of fibre breakage before matrix shear. Higher scatter in the data in the samples is addressed in the present studies. FTIR and Fractographic studies are carried out for deep understanding of the post pull-out interfacial adhesion.     

A highly fluorinated epoxy resin. III. Behavior in composite and fiber-coating applications

The behavior of a highly fluorinated epoxy resin used as a composite matrix material with AS-4 fibers and as an AS-4 fiber coating was studied. The composite mechanical properties were obtained, and the adhesion of the matrix to the fibers was evaluated. Comparisons of uncoated and fluoropolymer coated AS-4 fibers using single fibers embedded in an Epon 828 matrix were made. Substantial improvement in fiber critical length, and therefore fiber-matrix adhesion, was observed.     

Experimental and numerical investigation into fatigue damage mechanisms in multifibre microcomposites

Abstract

Polarised light microscopy has been used to investigate the influence of stress level, interfibre spacing, and fibre–matrix adhesion on the fatigue micromechanisms in carbon–epoxy model composites consisting of a planar array of five intermediate modulus carbon fibres. It was found that an increase in fatigue stress results in an increase in the number of fibre breaks, a more coordinated fibre fracture pattern as a result of fibre–fibre interaction, and extensive interfacial damage. In addition, it was shown that a smaller interfibre spacing results in a higher level of fibre–fibre interaction. Finally, in the case of surface treated carbon fibres (good fibre–matrix adhesion), a more coordinated fibre failure pattern was observed owing to stronger fibre–fibre interaction, whereas in the case of untreated carbon fibres (poor fibre–matrix adhesion), extensive debonding was observed which resulted in a more random fibre failure pattern. Finally, the experimental results were validated by means of a three-dimensional finite element analysis.