Effect of surface treatment on mode I interlaminar fracture behaviour of plain glass woven fabric composites: Part I. Report of the 2nd round-robin test results

A round-robin test programme has been carried out to characterise the mode I interlaminar fracture behaviour of E-glass woven fabric reinforced vinyl ester matrix composites. Special emphasis has been placed on the effect of silane coupling agent on the stability of interlaminar crack propagation and fracture toughness. Sixteen laboratories participated in this programme. Each laboratory was supplied with composite laminates of thicknesses of its own choice and conducted the tests according to its own procedures. The results showed that variations in interlaminar fracture toughness between laboratories were very large in spite of slight differences in the test procedures used, such as specimen dimensions, test speed and data reduction schemes. Nevertheless, the general trends were clearly identified with respect to different silane coupling agents. Other observations and the implications are discussed.     

Annealing effect in glass woven fabric composites,Part I. Mode I and mode II interlaminar fracture behavior

Mode I and mode II interlaminar fracture behavior of plain glass woven fabric composites with different silane concentration was investigated on the basis of a discussion of the effects of annealing on the fracture behavior. The fracture mode changed by annealing from stable to unstable manner in lower silane concentration and from unstable to stable manner in higher silane concentration specimens in mode I fracture. In the mode II fracture, the initiation values of fracture toughness increased by annealing without respect to silane concentration.     

Effect of surface treatment condition on interfacial degradation behavior in GFRP under acidic conditions

Interfacial degradation behavior of E-glass cloth reinforced vinyl ester resin under acidic conditions has been investigated. Specimens with different surface treatment conditions were prepared. Mode I fracture toughness tests were performed using DCB specimen, and the effect of surface treatment condition and immersion time on the crack propagation behavior is discussed. The crack propagation behavior changes as a function of the condition of the silane coupling agent and the immersion time due to the degradation of the interphase. A technique is proposed to evaluate the interfacial property. The change of fracture toughness of interphase and resin as a function of immersion time is studied by the crack propagation behavior and the fracture toughness of interphase and resin evaluated by this technique. The fracture toughness of interphase decreases rapidly with immersion in acidic solution.     

Mode I and Mode II interlaminar fracture toughness of CFRP/magnesium alloys hybrid laminates

The fiber metal laminates (FML), consisting of carbon fiber reinforced polymer prepregs and magnesium alloys sheets, were introduced, and the Mode I (peel) and Mode II (shear) interlaminar fracture toughness of the FMLs were investigated. The results show that the Mode I interlaminar toughness (0.23 kJ/m²) of the FMLs is much lower than the Mode II interlaminar toughness (5.81 kJ/m²), due to the fact that the effects of mechanical interlock to hinder crack propagates is smaller under Mode I loading conditions than under Mode II. The FMLs mainly show adhesive failure and interfacial failure under Mode I loading conditions, while for Mode II loading, it exhibits a degree of epoxy cohesive failure except the adhesive failure and interfacial failure.     

Roles of interfaces between carbon fibers and epoxy matrix on interlaminar fracture toughness of composites

The effect of atmospheric-pressure plasma treatment on high strength PAN-based carbon fibers had been studied in terms of fiber surface energetics and mode I and II interlaminar fracture toughness of unidirectional carbon fibers/epoxy matrix composites. The surface characterization of plasma treated carbon fibers was investigated by X-ray photoelectron spectroscopy (XPS) and contact angles. As a result, the plasma treatment changed the surface properties of the carbon fibers, mainly through formation of oxygen functional groups like hydroxyl, carbonyl, and carboxyl groups. According to contact angle measurements, it was observed that plasma treatment led to an increase in surface free energy of the fibers, mainly due to the increase of its specific component. Fracture toughness test results employing double-cantilever beam (DCB) and end notched flexure (ENF) specimens also showed that the increase in specific components or hydrogen bonding between the –OH groups on carbon fibers and the =O ring in epoxy matrix resins played an important role in improving the degree of adhesion at interfaces, resulting in an increase in the interfacial fracture toughness of the composites studied.     

Effects of fibre surface treatment on fracture-mechanical properties of sisal-fibre composites

Sisal fibre reinforced composites, one class of a broad range of eco-composite materials, were studied in connection with the effects of fibre surface treatment on their fracture-mechanical properties. Previous investigations on sisal fibre and its composites have been fully reviewed [1], which provided an impetus for this research. Two fibre surface treatment methods, chemical coupling based on silane and oxidization based on permanganate and dicumyl peroxide, together with untreated sisal fiber composites were used to set up different levels of interface bonding strength. The interface effects on the mechanical properties and fracture toughness of sisal fibre reinforced vinyl-ester composites were completely assessed based on the test results obtained and theoretical analyses. Many aspects of studies reported in this paper are original, such as single fiber pull-out tests and toughness evaluation of sisal composites aided by scanning electron microscopy. The results showed that fibre surface treatment could improve interfacial bonding properties between sisal fibre and vinylester resin. These in turn influenced the fracture-mechanical characteristics of this class of ecocomposites.     

A novel surface treatment process for enhanced adhesion of ultra-high modulus polyethylene fibres to epoxy resins

Ultra-high modulus polyethylene (UHMPE) fibres have been treated using a novel 'non-plasma' treatment allowing the incorporation of various chemical functional groups onto the polymer surface. The process comprises two steps: corona discharge treatment, followed by silanization of the polymer surface by a solution of an organo-functional silane. Corona discharge treatment incorporates oxygen-containing functionalities, e.g. reactive hydroxyl groups, onto the polymer surface. The presence of reactive -OH groups provides the possibility of covalent linkage of any organo-functional silane to the corona discharge-treated polymer in the form of a fibre, film, sheet, or powder. The effectiveness of the process was assessed by examining the interlaminar fracture energy and flexural modulus and by SEM analysis of the fracture surfaces of composites fabricated from the untreated, corona discharge-treated, ammonia plasma-treated, and the amine-grafted (using the novel process) UHMPE fabric. A significant improvement in interfacial adhesion was confirmed by increases in the interlaminar fracture energies and flexural moduli. The effectiveness of the process investigated is similar to the ammonia plasma treatment. SEM analysis of the fracture surfaces indicated a change in the fracture mode from purely adhesive for unmodified fibres, through to mixed failure mode for corona-treated material, to highly cohesive-in-fibre surface for amine-grafted UHMPE fibres. XPS analysis confirmed the incorporation of the amine groups onto the surface of polyethylene treated using the novel method.     

The measurement of cohesive and interfacial toughness for bonded metal joints with epoxy adhesives

The types of crack growth in adhesive joints are reviewed and three are identified, namely central cohesive, asymmetric cohesive and interfacial. Test methods for measuring fracture toughness associated with these cracks are then outlined and include a Tapered Double Cantilever Beam (TDCB) test for a central cohesive crack and peel tests on flexible laminates for the other types of crack. In particular, fixed arm and mandrel peel tests are used. Two aerospace adhesives are used to prepare test specimens in order to conduct these tests. For one of these adhesives, all three types of crack growth were recorded and this provided an opportunity to make detailed comparisons of the three associated fracture toughness values. Of particular interest was the use of the mandrel peel method because it enabled a fracture transition (asymmetric cohesive to interfacial fracture) to be observed during the test. The fracture toughness value associated with a central cohesive crack was similar in magnitude to that for an asymmetric cohesive crack. However, the fracture toughness for interfacial fracture was much lower, but similar in magnitude to the expected value of half the fracture toughness from a TDCB test.     

Enhanced interlaminar fracture toughness of unidirectional carbon fiber/epoxy composites modified with sprayed multi-walled carbon nanotubes

A recently reported solvent spraying technique was used herein for incorporation of multi-walled carbon nanotubes (MWCNTs) on unidirectional carbon fiber/epoxy prepregs. The role of the agglomerates reduction of oxidized MWCNTs on Mode-I interlaminar fracture toughness (G_IC) of laminated composites was investigated using double cantilever beam tests. Multiscale laminate composites were fabricated using MWCNTs without and with an acid oxidation, agglomerates reduction (AR) and a sequential treatment based on oxidation and AR. For comparison, specimens without MWCNTs were also prepared and tested. Fourier transform infrared analysis shows evidence of an important amount of oxygenated functional groups on the surface of as-received and oxidized MWCNTs. The results also show Mode-I fracture toughness improvements for all the laminated composites compared to reference samples. A substantial 52% increase in the average G_IC initiation was achieved for laminated composites reinforced with oxidized AR-MWCNTs prepared with only 0.05 wt.% MWCNTs.     

Preparation and Characterization of Nano-Calcium Carbonate/Silane Coupling Agent Master Batch and Its Effect on Epoxy Resin

A nano-calcium carbonate (CaCO₃)/silane coupling agent (NCC/SCA) master batch was prepared by the reaction of SCA (γ-aminopropyl triethoxy silane, trade name KH550) with the hydroxyl groups of nano-CaCO₃. Both Fourier transform infrared spectroscopy and thermal gravimetric analysis indicated that the nanoparticles were grafted by SCA. An epoxy resin was modified by adding the NCC/SCA master batch. A simple dipping test suggested that a better dispersion of the treated NCC in epoxy could be obtained than that of the untreated NCC. Then samples of epoxy nano-composites were prepared by a hot press process. The compressive property of epoxy nano-composites was investigated; the results of these mechanical property tests revealed that the compressive strength, elastic modulus, and the total fracture work of the epoxy matrix filled with the treated NCC were significantly improved relative to that filled with the untreated NCC.     

Annealing effect in glass woven fabric composites,Part II. Bending properties

Effects of annealing on bending properties of composites reinforced with plain glass woven fabrics that were treated with different concentrations of silane coupling agent were investigated in this paper. Bending strength increased by annealing in the specimen treated with lower silane concentration. Higher annealing temperature in a range from 80°C to 150°C led to higher bending strength. Then, the fracture mode changed from a micro-crack type (low strength type) to a branched matrix crack type (high strength type) by annealing.     

Enhancing indium tin oxide (ITO) thin film adhesiveness using the coupling agent silane

The coupling agent γ-mercapto propyl trimethoxy silane (WD-80) was used to enhance the adhesiveness of the indium tin oxide (ITO) thin film, which was prepared on a glass substrate using the sol-gel method. The nano-scratching test, XRD, TEM, SEM, and UV-vis spectrophotometer were employed to examine film adhesion, crystal structure, surface morphology, and transmittance. The results indicated that silane coupling agent, used in low concentration, did not change the film structure but increased the critical load of the film by 49%, from 4.16 mN to 6.20 mN, when the film was peeled off from the substrate. The principle by which the coupling agent works is discussed. In addition to increasing with the light wavelength, the average transmittance of the film in the visible range varied from 78.9% to 83.6%. Moreover, as a function of the WD-80 silane coupling agent, the film exhibited a high smoothness and density due to the orderly arrangement of particles.     

Microcellular and Solid Polylactide–Flax Fiber Composites

Polylactide–flax fiber composites with 1, 10 and 20 wt% fiber were melt-compounded and subsequently molded via the conventional and microcellular injection-molding processes. Silane was used as a coupling agent. The effects of fiber and silane content on cell morphology, static and dynamic mechanical properties, and crystallization properties have been studied. The average cell size decreased while the cell density increased with the fiber content. The degree of crystallinity increased with the fiber content. Silane treatment of fibers affected neither the cell morphology nor the degree of crystallinity. The toughness and strain-at-break of solid samples decreased with the fiber content while silane treatment increased both properties; however, neither fiber content nor silane treatment had much influence on the toughness and strain-at-break of microcellular samples. The specific modulus of both solid and microcellular samples increased with the fiber content. The specific strength of the solid and microcellular PLA–flax composites were only slightly lower than that of their solid and microcellular pure PLA counterparts. Overall, the toughness, strain-at-break, and specific strength of microcellular samples were found to be lower than that of their solid counterparts. The storage modulus of the PLA–flax composites with 10 and 20% fiber contents was higher than that of pure PLA.     

INVESTIGATION OF STATIC AND DYNAMIC FRACTURE TOUGHNESS OF SHORT CERAMIC FIBER REINFORCED POLYPROPYLENE COMPOSITES

Short ceramic fiber reinforced polypropylene composites have been investigated to determine their static and dynamic fracture toughness for different reinforcing fiber contents. The composites were reinforced with fibers produced by a carding technique combined with needle-punching. Static fracture toughness (K _c) was measured on single-edge notched tensile (SEN-T) specimens, while dynamic fracture toughness (K _d) was tested by impact strength Charpy specimens. Specimens in both cases were cut transverse (T) and in longitudinal (L) directions. Test results show that dynamic fracture toughness is larger than the static one. During loading of SEN-T specimens the burst-type acoustic emission (AE) signals were monitored. From AE signals it can be concluded that the main damage form is the pull-out in the T specimens, and debonding in L ones. These results were supported by scanning electron microscopy micrographs taken from fracture surfaces.     

Deformation and Fracture Behavior of PP/Ash Composites

In the present work, the deformation and fracture behavior of PP/ash composites with different ash content was investigated. The effect of a silane coupling agent was also analyzed. From uniaxial tensile tests, an increase in the stiffness with ash content was found as a result of the incorporation of the stiffer filler within the PP matrix. On the other hand, a decrease in tensile strength and strain at break with filler loading was observed. This result was attributed to the increased number of debonded large particles with filler content, which subsequently led to the formation of critical-size flaws. On the other side, the composites displayed higher values of fracture parameters than the matrix as a result of the development of a particle induced toughening mechanism. However, fracture properties were also found to decrease with ash content. This could be attributed to the increase in the number of critical-size flaws that induced premature failure. The incorporation of a silane coupling agent in the formulations led to composites with slightly improved tensile and fracture properties. This was probably due to improved interaction between PP and ash in the first case and a better dispersion of ash particles in the matrix and/or changes in the crystallization behavior of PP, in the latter case.     

PBX材料宏细观断裂行为的数字散斑相关法实验研究

 采用半圆盘弯曲实验和数字散斑相关方法,对高聚物粘结炸药（PBX）的宏、细观断裂行为进行了实验研究。宏观上,带有预制裂纹的半圆盘试样发生拉伸破坏,利用数字散斑相关技术得到了试样的应变场和位移矢量场分布,定量分析了试样全场的变形特征,并测得了PBX材料的平面应变断裂韧性;细观上,用配有加载装置的扫描电子显微镜对含预制裂纹的半圆盘试样间接拉伸下的损伤演化和破坏过程进行了实时原位观察,借助于数字散斑相关方法,定量分析了试样损伤局部化特征。结果表明,将数字散斑相关方法用于研究PBX材料宏、细观尺度上的变形破坏问题是有效的。     

Effects of reactive gas on shear and fracture behaviors of plasma-treated polyethylene/steel joints

For this study, we investigated the effects of reactive gases (oxygen, nitrogen, and argon) on the shear behavior and fracture toughness of HDPE/steel joints by treating high-density polyethylene (HDPE) with plasma using a microwave method. We also investigated the effect of plasma treatment on the physical and chemical changes on the surface of HDPE. HDPE/steel joints were fabricated using a secondary bonding process. The results showed that the shear strength and fracture toughness of HDPE/steel joints treated with different reactive gases were ordered as follows, oxygen > nitrogen > argon. Specifically, the shear strength and fracture toughness of oxygen plasma-treated HDPE/steel joints were approximately 7600% and 2400% greater, respectively, than that of untreated HDPE/steel joints. The improvements in shear strength and fracture toughness are attributed to increase in surface roughness and the creation of carbonyl functional groups on the HDPE surface via plasma treatment.     

Small-scale fracture toughness of ceramic thin films: the effects of specimen geometry,ion beam notching and high temperature on chromium nitride toughness evaluation

For the implementation of thin ceramic hard coatings into intensive application environments, the fracture toughness is a particularly important material design parameter. Characterisation of the fracture toughness of small-scale specimens has been a topic of great debate, due to size effects, plasticity, residual stress effects and the influence of ion penetration from the sample fabrication process. In this work, several different small-scale fracture toughness geometries (single-beam cantilever, double-beam cantilever and micro-pillar splitting) were compared, fabricated from a thin physical vapour-deposited ceramic film using a focused ion beam source, and then the effect of the gallium-milled notch on mode I toughness quantification investigated. It was found that notching using a focused gallium source influences small-scale toughness measurements and can lead to an overestimation of the fracture toughness values for chromium nitride (CrN) thin films. The effects of gallium ion irradiation were further studied by performing the first small-scale high-temperature toughness measurements within the scanning electron microscope, with the consequence that annealing at high temperatures allows for diffusion of the gallium to grain boundaries promoting embrittlement in small-scale CrN samples. This work highlights the sensitivity of some materials to gallium ion penetration effects, and the profound effect that it can have on fracture toughness evaluation.     

Influence of Cell Topology on Mode I Fracture Toughness of Cellular Structures

A cellular structure is made up by an interconnected network of beams or plates which forms the edges and faces of cells. This paper proposes three different micromechanical models to determine the fracture toughness values of cellular materials such as rigid polyurethane foams using the finite element micromechanical analysis and Abaqus software. This study was carried out for mode I fracture and fracture toughness was predicted based on linear elastic fracture mechanics. Models of two-dimensional cellular solids with square, hexagonal and circular cells were generated for five different relative densities (0.077, 0.105, 0.133, 0.182 and 0.333). A study of the influence of geometrical parameters on fracture toughness was also conducted. Based on the finite-element simulations, three linear correlations are proposed which could be useful for estimation of fracture toughness values if relative densities are in the considered range of 0.077 (90 kg/m³ density) and 0.333 (390 kg/m³ density). Finally, the authors validate their proposed micromechanical models presenting a comparison of analytical, numerical and experimental results of fracture toughness of cellular materials. It was found that at low relative densities (between 0.077 and 0.333), the proposed micromechanical models predict the fracture toughness values similar to experimental and numerical ones, but they must be used according with the real cellular structure.     

Effect of the molecular weight of sizing agent on the surface of carbon fibres and interface of its composites

The influence of different molecular weight sizing agent on the performances of carbon fibres and carbon fibres composites were studied. Three different kinds of molecular weight sizing were used. Surface composition of the fibres modified with aqueous sizing and topographies of carbon fibres surface were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and scanning electron microscope (SEM). The interlaminar shear strength and hygrothermal ageing test have been used to study the effect of fibres coatings on the adhesion of surface. The results of the study indicate that the molecular weight of sizing agent has an important influence to the carbon fibres and carbon fibres composites. The high and low molecular weight sizing agent decreased the interfacial shear strengths and hygrothermal ageing of carbon fibres composite. The moderate molecular weight of sizing agent showed an improvement of the interfacial adhesion and hygrothermal ageing.