BOND STRENGTH MEASUREMENT BETWEEN GLASS FIBRES AND EPOXY RESIN AT ELEVATED TEMPERATURES USING THE PULL-OUT AND PUSH-OUT TECHNIQUES

Pull-out and push-out measurements were performed on glass fibres in an epoxy resin to determine the dependence of bond strength on test temperature and on fibre surface treatment. A comparative analysis of the two techniques was carried out to elucidate elementary processes of polymer-fibre debonding and to determine energy values for adhesional bonds. Differences in bond strength values for pull-out and push-out tests were attributed to failure mechanisms that were either interface-controlled or matrix-controlled. Evidence for the different failure mechanisms characteristic of the two test techniques was provided by an estimation of failure parameters, such as the activation energy for debonding. Failure mechanisms also were manifest in AFM images, showing differences in topography and roughness that depended on fibre surface treatment, test geometry, and test temperature.     

Oxidation effects on failure mechanism of plain-woven SiC/SiC Z-pinned joints subjected to push-out loading

Plain-woven SiC/SiC Z-pinned joints were prepared using chemical vapour infiltration. The oxidation behaviours and failure mechanism were investigated using push-out tests before and after oxidation. Microstructural analysis indicated that the degree of oxidation of the pin near the surface was more severe than that in the middle region. Internal damage was monitored using an acoustic emission (AE) system. Pattern recognition was introduced to study the evolution of failure during the test. Combined with the failure morphology, all AE signals were labelled as matrix cracking, fibre–matrix debonding, matrix peeling, and fibre break. The results suggest that the failure mechanism of the Z-pinned joints under axial loading is dominated by fibre–matrix debonding and matrix cracking.     

The Interfacial Bond Strength in Glass Fibre-Polyester Resin Composite Systems

The interfacial bond strength in glass fibre-polyester resin composites has been investigated using various experimental techniques. These included blocks of resin containing fibre (in which, depending on the geometry of the specimen, failure occurs in either a shear or tensile mode) the pullout of a fibre from a disc of resin and a short beam shear test for interlaminar shear strength determination.

Low power optical microscopy and optical retardation measurements of stress induced birefringence were used to detect the difference between intact and debonded fibre resin interfaces. The shear modulus and shear strength of the resin were obtained from torsion tests on cylindrical rods of the resin.

The single fibre shear debonding specimen and the short beam shear test are shown to be the most viable test methods but interpretation of the results is complicated by the various modes of failure possible and by the different stress states which exist in the area of the specimen where debonding starts. Stress concentration factors obtained by finite element analysis and photoelastic analysis have been applied to the results from these tests and the corrected interfacial bond strengths are in close agreement.

The real interfacial bond strengths of well bonded glass-fibre polyester resin systems is shown to be of the order of 70 MN m^-2.     

The Interfacial Bond Strength in Glass Fibre-Polyester Resin Composite Systems

The interfacial bond strength in glass fibre-polyester resin composites has been investigated using various experimental techniques. These included blocks of resin containing fibre (in which, depending on the geometry of the specimen, failure occurs in either a shear or tensile mode) the pullout of a fibre from a disc of resin and a short beam shear test for interlaminar shear strength determination.

Low power optical microscopy and optical retardation measurements of stress induced birefringence were used to detect the difference between intact and debonded fibre resin interfaces. The shear modulus and shear strength of the resin were obtained from torsion tests on cylindrical rods of the resin.

The single fibre shear debonding specimen and the short beam shear test are shown to be the most viable test methods but interpretation of the results is complicated by the various modes of failure possible and by the different stress states which exist in the area of the specimen where debonding starts. Stress concentration factors obtained by finite element analysis and photoelastic analysis have been applied to the results from these tests and the corrected interfacial bond strengths are in close agreement.

The real interfacial bond strengths of well bonded glass-fibre polyester resin systems is shown to be of the order of 70 MN m^?2.     

The Fiber/Matrix Bond Strength of CFRP Deduced from the Strength Transverse to the Fibers

The strength transverse to the fibre (or the transverse fracture strain) of CFRP is directly related to the fibre/matrix bond strength. This enables the determination of a fibre matrix bond strength based on transverse fracture data. In crossply laminates, the transverse ply usually fails many times, so that principally these experiments deliver a treasure of data. A method, developed to make use of these data, produces a Weibull distribution for transverse fracture based on the data of, basically, a single specimen. A model developed to separate the influences of defects, matrix ductility and constraint finally leads to a procedure to determine the strain at interphase(or interface) failure. The usefulness of the model and the determined strain at interface failure is demonstrated with several examples, such as the influence of constraint, of test temperature and of the fibre surface treatment on transverse cracking and the fibre/matrix bond strength.     

A microdebonding test for in situ assessment of fibre/matrix bond strength in composite materials

A test technique which gives a quantitative measure of the in situ fibre/matrix bond strength in fibre-reinforced composite materials is described. The test involves the compressive loading of a fibre or region of fibres on a polished specimen surface to produce debonding. Results are presented for the debonding load for glass/epoxy, aramid/epoxy and graphite/epoxy composites. The change in debonding load is also followed as the interface degrades during moisture conditioning at different points through the thickness of the material. It is concluded that refinements to the technique are needed to simplify interpretation of the debonding force in terms of interface shear strength, and to make the test more reproducible.     

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.     

The effects of chelation on the adhesion of two different root canal sealers

Objective: This study aims to evaluate alterations in the root canal dentin after irrigation with EDTA, HEBP, and Chitosan in order to determine the push-out bond strengths of the different root canal sealers on altered dentin surfaces. Materials And Methods: Crowns of 70 maxillary single-rooted teeth were removed to obtain a standardized length of 16 mm. The canals were instrumented using rotary files and the step back technique. The master apical file used in this study was #40. The subgroups were determined based on the chelation agent and the material of the root canal sealer that was used (17% EDTA, 18% HEPB, 0.2% Chitosan, Well Root ST (WRST) or AH Plus). Three slices with 1 mm thickness were cut from the root thirds of each tooth and subjected to a push-out test. The data (MPa) were analyzed using a one-way ANOVA and a Duncan’s multiple comparison test at a level of α = 0.05. Finally, scanning electron microscope (SEM) photographs were taken. Results: Groups that used WRST exhibited significantly higher push-out bond strength values in all subgroups independent of the irrigant that was used (ANOVA, p < 0.05). Group 1 showed higher push-out bond strength than the other AH Plus subgroups. Conclusion: The EDTA improved the push-out bond strength of the AH Plus. The WRST root canal sealer had the highest push-out bond strength and did not depend on the irrigant used.     

Mechanical properties of flared root canals restored with fiber post and chemically activated resin: study using push-out bond strength and fracture load tests

This study aimed to evaluate the fracture load and push-out bond strength of flared root canals restored with different procedures, including a technique with a fiber post and a chemically activated resin composite. Eighty human canines were selected and treated endodontically. Two methodologies were used: push-out and fracture load. The teeth were divided into four groups: Cast metal core (CMC); PAN (direct anatomic post); PAC (fiber post and accessory posts); and PE (fiber post with chemically activated resin composite). For the fracture load test, the samples were submitted to load application in a universal testing machine. The fracture mode was evaluated visually. Forty other samples were submitted to the push-out test. The fracture load (n = 10) and the bond strength (n = 10) were analyzed by analysis of variance and Tukey tests (α < 0.05). CMC presented the highest fracture load (p < 0.05), and no significant differences were observed in the fracture load values for Groups PAN, PAC, and PE. CMC presented 90% of unfavorable failures; PAN and PAC, the remaining 10% of these failures. PE presented only favorable failures. PAC presented lower push-out bond strength values. The fracture load for CMC procedure was higher than that of the others, but presented 90% unfavorable fractures, indicating the use of any of the glass fiber post techniques evaluated for restoring flared root canals due to favorable fracture modes.     

Effects of mixing techniques and dentin moisture conditions on push-out bond strength of ProRoot MTA and Biodentine

Objective: To evaluate the influence of manual and mechanical mixing techniques as well as the effects of moisture on the push-out bond strength of ProRoot MTA (Dentsply Tulsa Dental, Tulsa, OK, USA) and Biodentine (Septodont, Saint Maur des Fosses, France) to radicular dentin.

Material and methods: Two hundred and forty dentin discs were assigned into three groups with respect to the moisture condition tested: (1) dry, (2) paper points, (3) wet. The discs were further divided into four subgroups according to the calcium silicate cements (CSCs) and mixing techniques used: (1) ProRoot MTA mixed manually, (2) ProRoot MTA mixed mechanically, (3) Biodentine mixed manually, and (4) Biodentine mixed mechanically. Bond strengths of the cements to root canal dentin were measured using a push-out test setup. The data were statistically analyzed using three-way ANOVA and Bonferroni post hoc test p = 0.05.

Results: The data indicated that the push-out bond strength values were significantly affected by CSCs, mixing techniques, and moisture conditions (p < 0.001). Dry conditions caused a significant decrease in bond strength values for both CSCs (p < 0.001). The mean bond strength of Biodentine was significantly higher than that of ProRoot MTA, regardless of the mixing techniques and moisture conditions (p < 0.001). Mechanical mixing favored bond strength values statistically compared to manual mixing (p < .001).

Conclusion: The mixing techniques and moisture conditions have an effect on the push-out bond strengths of ProRoot MTA and Biodentine. Dry samples and manual mixing of cements deteriorate the push-out bond strengths values.     

型钢与地聚合物混凝土粘结滑移性能研究

为了研究型钢与地聚合物混凝土之间的粘结滑移规律,对9个型钢地聚合物混凝土柱试件进行推出试验,研究地聚合物混凝土抗压强度、型钢的保护层厚度、型钢的锚固长度以及配箍率四个参数对型钢地聚合物混凝土试件荷载-滑移曲线、破坏形态以及粘结滑移性能的影响。结果表明:试件的荷载-滑移曲线具有相同的发展趋势,可将其划分为无滑移段、荷载上升段、荷载下降段和水平残余段四个阶段;试件的破坏模式为混凝土劈裂破坏,劈裂裂缝从加载端型钢翼缘产生,并向自由端发展;随着地聚合物混凝土抗压强度、型钢的保护层厚度和配箍率的提高,试件的特征粘结强度呈上升趋势;与普通水泥型钢混凝土不同,型钢的锚固长度增大也会使试件的特征粘结强度提高。根据试验结果,建立了特征粘结强度的计算公式,提出了型钢地聚合物混凝土的粘结-滑移本构模型,采用该模型计算得到的型钢地聚合物混凝土粘结-滑移曲线与试验曲线吻合度较高。     

A study of the influence of controlled corona treatment on UHMWPE fibres in reinforced vinylester composites

In order to illuminate the mechanisms of corona discharge treatment on ultra‐high molecular weight polyethylene (UHMWPE) fibre, the effects of corona treatment power and time are discussed in detail. The surface‐roughness and tensile‐failure characteristics of the polyethylene fibre were determined by a scanning electron microscope (SEM). The photos from the SEM showed that the size and number of the micro‐pits on the fibre surface increase with increase of corona power. The oxygen‐containing groups on the fibre surface could be detected by Fourier‐transform infrared attenuated total reflectance and also increased gradually with increase of corona power. The T‐peel strength of composites increased from the corona treatment, and then showed a maximum value at a corona treatment time about 0.1 s with increase of treatment time. However, the tensile strength of the fibre was reduced with increase of corona power and the failure mechanism obviously changed after the treatment. The ballistic impact energy absorption of UHMWPE fibre/vinylester composite was obtained after fragment simulating projectiles (FSP) impact tests. After 6‐kW corona treatment for 0.075 s, the impact energy absorbed by the laminate reached a maximum value. Copyright © 2003 Society of Chemical Industry     

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.     

Wilhelmy Technique and Solidification Front Technique to Study the Wettability of Fibres

The strength of fibre-reinforced materials depends heavily on the adhesion between the fibre and the resin. To predict the bond strength of the adhesion, it is desirable for the surface tension of the fibre to be known. Two independent methods, the Wilhelmy balance method and the solidification front method, were investigated. The fibres used for this investigation included a carbon fibre, Thornel 300®, and an aromatic poiyamide fibre, Kevlar.

In the Wilhelmy experiments three liquids, ethylene glycol, glycerol and distilled water were employed to measure the surface tensions of the test fibres. They were found to be 42.4 mJ/m² and 43.7 mJ/m² for the carbon fibre and Kevlar, respectively. These values agreed very well with the results obtained from the solidification front method, from which the carbon fibre was found to have a surface tension value of 41.8 mJ/m² while that for Kevlar was 46.4 mJ/m². Furthermore, error analysis has shown that the error limits of the experiments are within 5% of the resulting values. The reproducibility and accuracy of these two techniques indicate that they are viable for determining the surface tension of small diameter fibres.     

The Effect of Fibre Surface Treatment on the Failure of Continuous Carbon Fibre/Epoxy Resin Composites

The failure mechanisms of a composite, consisting of continuous, aligned, high strength, polyacrylonitrile (PAN) based carbon fibre in an epoxy resin, under uniaxial tension, have been studied. In order to study the effect of the interphase/interface strength, six different levels of an electrochemical fibre surface treatment were used. Single tows containing approximately 12,000 treated carbon fibres were impregnated to produce composite rods with a fibre volume fraction of 0.55. Lengths of this impregnated tow were also set in the centre of glass-fibre/epoxy resin composite coupons which were used to study the mechanisms of failure of the embedded tows. Acoustic emission was used to monitor all samples and bundle failure was found to occur after a build-up of sub-critical damage events as previously modelled.¹ Microdebond tests demonstrated an initial increase of interfacial strength which levelled out at the higher levels. In impregnated samples with high surface treatments, catastrophic failure occurred with the crack propagating approximately perpendicular to the fibre direction. However, in samples with lower fibre surface treatments, longitudinal splitting (not accounted for in current models), occurred, meaning that a greater length of composite was involved in the final failure process. Acoustic emission has been shown to have an approximately direct relation with the predicted number of single fibre breaks in composite test-pieces; however, there was no significant difference attributable to the different surface treatments. The hybrid test coupons allow a detailed assessment of the failure mechanisms within the impregnated carbon tow. The failure strains of the embedded tow is some 5% higher than that of unsupported tow. The Weibull modulus is of the same order.     

The Effect of Fibre Surface Treatment on the Failure of Continuous Carbon Fibre/Epoxy Resin Composites

The failure mechanisms of a composite, consisting of continuous, aligned, high strength, polyacrylonitrile (PAN) based carbon fibre in an epoxy resin, under uniaxial tension, have been studied. In order to study the effect of the interphase/interface strength, six different levels of an electrochemical fibre surface treatment were used. Single tows containing approximately 12,000 treated carbon fibres were impregnated to produce composite rods with a fibre volume fraction of 0.55. Lengths of this impregnated tow were also set in the centre of glass-fibre/epoxy resin composite coupons which were used to study the mechanisms of failure of the embedded tows. Acoustic emission was used to monitor all samples and bundle failure was found to occur after a build-up of sub-critical damage events as previously modelled.¹ Microdebond tests demonstrated an initial increase of interfacial strength which levelled out at the higher levels. In impregnated samples with high surface treatments, catastrophic failure occurred with the crack propagating approximately perpendicular to the fibre direction. However, in samples with lower fibre surface treatments, longitudinal splitting (not accounted for in current models), occurred, meaning that a greater length of composite was involved in the final failure process. Acoustic emission has been shown to have an approximately direct relation with the predicted number of single fibre breaks in composite test-pieces; however, there was no significant difference attributable to the different surface treatments. The hybrid test coupons allow a detailed assessment of the failure mechanisms within the impregnated carbon tow. The failure strains of the embedded tow is some 5% higher than that of unsupported tow. The Weibull modulus is of the same order.     

微脱粘法研究等离子处理的高模量聚乙烯纤维的粘结性

对等离子处理后的高模量聚乙烯纤维的表面形态、表面官能团和与环氧树脂的粘结性进行了研究。相关参数是平均界面剪切应力和临界嵌入长度。微粘法固有的数据分散是纤维结构和表面缺陷造成的。实验结果表明 ,等离子处理后 ,纤维表面出现了明显的刻痕 ,官能团含量增加 ,界面剪切强度随等离子处理时间而增加。     

The influence of endodontic sealer dentine penetration on fibreglass post retention

This study aimed to evaluate the influence of endodontic sealer inside dentinal tubules on the retention of fibreglass posts. One hundred eighty extracted teeth were instrumented with rotary instruments and divided into two groups (n = 90) according to their filling technique: (LC) lateral condensation and (CT) controlled technique, and subdivided into three subgroups according to the endodontic sealer used: (A) epoxy resin sealer, (B) zinc-oxide and eugenol sealer, and (C) bioceramic endodontic sealer. After root preparation, each subgroup received a fibreglass posts cemented with (1) adhesive resin cement, (2) self-adhesive resin cement, and (3) glass ionomer cement. After stored for 15 days at 37 °C and 100% humidity, the teeth were sectioned transversely into 1-mm thick slices and subjected to laser confocal scanning microscopy and push-out test. The failure mode was analyzed by stereo microscope, and scanning electron microscopy images of representative fractures were made. Although there were no significant differences in the dislocation resistance among the filling techniques (p > 0.05), the type of sealer used affected bond strengths on the cervical and middle thirds. Fibreglass posts cemented with glass ionomer cement presented higher values for the push-out test than those cemented with resin cements (p < 0.05). Mix failure modes were predominant and occurred in all experimental groups. The use of bioceramic endodontic sealer was able to reduce the bond strength, mainly when the fibreglass posts was cemented by resin cement.     

Finite element analysis of load transfer at a fibre–matrix interface during pull-out loading

Load transfer ability of the fibre–matrix interface is well known to mainly control the mechanical behaviour of fibre-reinforced materials. This load transfer phenomenon is of great importance in dentistry when a post is used for fixing a ceramic crown on the tooth. The pull-out test has been well accepted as the most important micromechanical test for evaluating the interaction properties between the fibre and matrix. In this study, a finite element model is developed to analyse the pull-out process of a steel fibre from an epoxy matrix. Based on the pull-out force–displacement curves, developed in our previous experimental work, specific load transfer laws at the fibre–matrix interface have been proposed for each stage of the pull-out process, i.e., before and after fibre–matrix debonding. Predicted initial extraction forces for different implantation lengths were fitted to experimental values and an initial interference fit of 4 μm was determined. An interfacial shear strength of 21 MPa was then determined by fitting the predicted debonding forces for different implantation lengths to the experimental values. According to the load transfer laws considered, analysis of the interfacial shear stress indicates that fibre–matrix debonding initiates simultaneously at both the lower and upper extremities of the interface.