EXPERIMENTAL RESULTS OF A PULL-OUT TEST PERFORMED WITH SINGLE- AND MULTI-FIBER SAMPLES

Widely-used methods for characterising the fibre/matrix interface in polymeric composites are the fragmentation test and the droplet test as a special kind of the single-fibre pull-out test. A severe disadvantage of these tests is that non-realistic model samples are investigated which contain only one fibre in the matrix. In order to obtain data about the effect of the different residual stress situations for fibres in such samples and in composites, pull-out tests of E-glass fibres in polystyrene and polycarbonate are performed using samples, where the investigated fibre is surrounded by 0 to 3 other near fibres. Neighbouring fibres can increase the pull-out forces by a factor of three and the interfacial toughness by a factor of four. This has to be taken into account, if the tests are performed not only for comparison reasons but for measuring interface properties.     

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.     

Mechanical properties of interfaces within a flax bundle – Part I: Experimental analysis

In order to model the tensile behaviour of flax fibre based composites, the properties of each of the constituents need to be determined. In addition to the fibres, the matrix and the fibre/matrix interface, the fibre/fibre interface present within a bundle of flax fibres is an element which is rather hard to characterize but whose properties also need to be taken into account to understand properly the deformation and rupture modes of the derived composites. In the first part of this study, the protocol used to determine these properties is described; the results of the mechanical tests and the microscopic observations carried out on pairs of fibres are given and exploited to lead to the fibre/fibre interface properties. In the second part, various cohesive zone models will be evaluated using these interface properties and numerical simulations will be performed for the purpose of validation.     

Effect of silane treatment on the Curaua fibre/polyester interface

ABSTRACT

Good adhesion at fibre/matrix interface of lignocellulosic fibres is crucial when substituting synthetic fibres in polymer composites. The great variability presented by those fibres requires diverse characterisation studies for better insights on fibre surface treatments and resin systems interactions. In this work, Curaua fibres were treated using silane coupling agents to improve their interfacial properties with polyester. The fibres were pre-treated using 4?wt% solution of NaOH and then treated with 5?wt% solution of (3-aminopropyl) trimethoxysilane (AMPTS) or triethoxymethylsilane (TEMS). Characterisation of the treated fibres was carried out using infrared spectroscopy, X-ray diffraction, thermogravimetric analysis and scanning electron microscopy. Fibre wettability and adhesion towards polyester was investigated using contact angle measurements and pull-out tests, respectively. The AMPTS treatment yielded a significant result of 20.2?MPa in interfacial shear strength (≈2.5 times that of the untreated fibre), attributed to the increase in availability of binding sites with polyester.     

Effect of PAN-based and pitch-based carbon fibres on microstructure and properties of continuous Cf/ZrB2-SiC UHTCMCs

In this paper the microstructure and mechanical properties of two different C_f/ZrB₂-SiC composites reinforced with continuous PyC coated PAN-derived fibres or uncoated pitch-derived fibres were compared.Pitch-derived carbon fibres showed a lower degree of reaction with the matrix phase during sintering compared to PyC/PAN-derived fibres. The reason lies in the different microstructure of the carbon. The presence of a coating for PAN-derived fibres was found to be essential to limit the reaction at the fibre/matrix interface during SPS. However, coated bundles were more difficult to infiltrate, resulting in a less homogeneous microstructure.As far as the mechanical properties are concerned, specimens reinforced with coated PAN-derived fibres provided higher strengths and damage tolerance than uncoated pitch-derived fibres, due to the higher degree of fibre pull-out. On the other hand, the weaker fibre/matrix interface resulted in lower interlaminar shear, off-axis strength and ablation resistance.     

Experimental study on mechanical properties of aramid fibres reinforced natural rubber/SBR composite for large deformation – quasi-static mechanical properties

Quasi-static mechanical properties of aramid fibres reinforced natural rubber/SBR composites are comprehensively investigated via scanning electron microscopy (SEM), uniaxial tensile tests, multi-step stress relaxation, and the Mullins experiment. The strength, stiffness, viscoelasticity, and Mullins effect of composites are analysed, and the micro failure mechanism is also explored. It is shown that the samples appear similar to a laminate plate with random short fibres in a plane. The results of the uniaxial tensile tests indicate that the tensile strength and elongation at failure decrease, while the stiffness increases following the addition of a small amount of aramid fibres into the rubber matrix. The multi-step relaxation and Mullins experiments reveal that the aramid-short-fibres weaken the viscoelasticity of rubber composites. Finally, the strain energy of the composite is divided into four parts, and one part is considered with respect to its application to the study of interface destruction between the matrix and fibre.     

Microstructure and damage evolution of SiCf/PyC/SiC and SiCf/BN/SiC mini-composites: A synchrotron X-ray computed microtomography study

SiC_f/PyC/SiC and SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapor deposited PyC or BN interface layers are fabricated. The microstructure evolutions of the mini-composite samples as the oxidation temperature increases (oxidation at 1000, 1200, 1400, and 1600?°C in air for 2?h) are observed by scanning electron microscopy, energy dispersive spectrometry, and X-ray diffraction characterization methods. The damage evolution for each component of the as-fabricated SiC_f/SiC composites (SiC fibre, PyC/BN interface, SiC matrix, and mesophase) is mapped as a three-dimensional (3D) image and quantified with X-ray computed tomography. The mechanical performance of the composites is investigated via tensile tests.The results reveal that tensile failure occurs after the delamination and fibre pull-out in the SiC_f/PyC/SiC composites due to the volatilization of the PyC interface at high temperatures in the air environment. Meanwhile, the gaps between the fibres and matrix lead to rapid oxidation and crack propagation from the SiC matrix to SiC fibre, resulting in the failure of the SiC_f/PyC/SiC composites as the oxidation temperature increases to 1600?°C. On the other hand, the oxidation products of B₂O₃ molten compounds (reacted from the BN interface) fill up the fracture, cracks, and voids in the SiC matrix, providing excellent strength retention at elevated oxidation temperatures. Moreover, under the protection of B₂O₃, the SiC_f/BN/SiC mini-composites show a nearly intact microstructure of the SiC fibre, a low void growth rate from the matrix to fibre, and inhibition of new void formation and the SiO₂ grain growth from room to high temperatures. This work provides guidance for predicting the service life of SiC_f/PyC/SiC and SiC_f/BN/SiC composite materials, and is fundamental for establishing multiscale damage models on a local scale.     

Characterising the time-dependant behaviour on the single fibre level of SHCC: Part 2: The rate effects on fibre pull-out tests

This paper is the second part of a two paper series about the time-dependant behaviour of Strain Hardening Cement-based Composite (SHCC) on the single fibre level. Having dealt with mechanisms of creep in SHCC in the first part, this paper reports single fibre pull-out tests that were done to investigate the effect of the pull-out rate on the mechanical response of the interface between the fibre and the matrix. It was found that not only the pull-out resistance increased with an increase of the pull-out rate but the probability of fibre rupture during pull-out as well. Another important finding was that the interfacial shear resistance and slip-hardening coefficient are not only dependant on the pull-out rate, but also the embedment length.     

Adhesion of polymers to reinforcing fibres

A single fibre pull out technique is presented which makes it possible to measure the strength in the interface between fibre and polymer with high precision even if the embedded length of the fibre is short. The method allows measurements for all kinds of fibres in thermoplastic or thermosetting polymers. The effect of fibre surface treatment can be investigated as well as the effect of morphology or internal stresses in the polymer. Examples are given. The shear strength results are compared with results of tensile shear tests performed on symmetrically notched unidirectional reinforced composite samples. The correlation is good and it is shown that the new single fibre pull out method is able to give a better discrimination between the composites than other methods. An analysis of mechanical stress induced during the pull out demonstrates the use and limitation of this method.     

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 characterisation of flax fibre-thermoplastic polymer composites by the pull-out test

The interface between flax fibres and thermoplastic polymer matrices has been investigated. Two types of flax fibres have been used: dew retted and upgraded Duralin fibres. The latter fibres have been treated by a novel treatment process for improved moisture and rot sensitivity. The apparent shear strength of dew-retted and upgraded Duralin fibres embedded in high and low density polyethylene, polypropylene and maleic anhydride modified polypropylene, respectively, has been calculated from the maximum force measured from the pull-out test using the Kelly-Tyson equation. Higher apparent shear strength values have been measured in the case of high density polyethylene. An improvement in the interfacial shear strength by the use of upgraded flax fibres has not been clearly observed. The curves of pull-out force versus displacement for all samples are typical of a brittle fracture mixed mode interface behaviour. The pull-out test of flax fibre-polymer matrices exhibit similar characteristics with the pull-out test of synthetic fibre-polymer systems.     

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.     

Uniaxial tensile and creep behaviour of an alumina fibre-reinforced ceramic matrix composite: I. Experimental study

The uniaxial tensile and creep behaviour of an alumina fibre-reinforced silicon carbide composite is studied. The damage mechanisms during tensile loading are identified on the basis of the elastic response and in-situ morphological analysis. Tensile tests show that the composite presents a pseudoductile behaviour due to matrix microcracking and fibre-matrix debonding. Temperature induces changes in the tensile behaviour because of variations in load transfer conditions and in the axial residual stress borne by the fibres and the matrix. The creep curves at 1100°C under vacuum present an extended tertiary part, especially at low creep stress. The unloading-reloading loops periodically performed during creep show a progressive decrease in longitudinal stiffness. Progressive interface debonding during creep is invoked to explain: (i) the strain rate increase during tertiary creep, (ii) the decrease of the elastic modulus and (iii) the large fibre pull-out observed on the creep fracture surface. The different creep rupture modes at low and high stresses are related to the capability of the remaining intact fibres to support the overload failure of the first fibres.     

Short PET and PA fibre composites based on LDPE and HDPE matrices. Morphology-behaviour relationship

The effect of unmodified and azide-modified short poly(ethylene terephthalate) (PET) and polyamide 66 (PA) fibres on the mechanical properties of thermoplastic composites based on low density (LDPE) and high density polyethylene (HDPE) matrices was investigated. The results have shown that both organic fibres are suitable reinforcements for LDPE and HDPE matrices. The weakest the matrix the strongest is the reinforcing effect of the fibres, so, the reinforcing effect of the fibres is more sensible in the LDPE matrix. p-(Azidosulfonyl)benzoyl azide is an adequate coupling agent for both fibres, especially for PET fibres. A better adhesion at the fibre/matrix interface of the composites has been observed by scanning electron microscopy, mainly in the PET-filled LDPE.     

Silane coupling agents in basalt-reinforced polyester composites

A new reinforcing mineral fibre, comparable in strength (3 MPa) and modulus (90 MPa) with E-glass fibres, has recently been produced from naturally-occurring basalt rock. Following earlier studies of basalt fibre/polymer matrix interactions by single fibre pull-out tests, the interfacial interaction in basalt/polyester composite systems has now been investigated. The effect of silane coupling agents applied under various conditions is reported here. The controlling effects of silane hydrolysis, condensation, orientation on the basalt surface and chemical bonding on the surface are revealed in corresponding variations in flexural strengths.     

Interfacial adhesion in short-fibre composites

For the evaluation of the interfacial adhesion in short-fibre composites, a simple method based on fibre pull-out length distribution was proposed. The experiments with three composites of isotactic polypropylene with 32 wt.-% of short-glass fibres confirm the potentials of the method for a sensitive determination of differences in the interfacial adhesion. The effects of temperature, crystallinity and fibre orientation angle on the interfacial adhesion were investigated.     

Graphite Fibre-Epoxy Matrix Interface Interactions

Studies of fibre-epoxy resin matrix model composites show that the “tensile debond” test is not applicable to carbon or graphite fibres. Fibre fracture occurs under the compression strains involved relieving interface stresses and precluding subsequent debond. Calculated minimum bond strengths for pitch-based graphite fibres are similar to results for boron and glass fibres. Interfacial failure is obtained with the “shear debond” test for low and intermediate modulus graphite fibres, but compression fracture also occurs first with high modulus fibres. Pitch-based graphite fibres show a decreasing adhesive interaction with epoxy resin the more oriented the fibre, but results compare favorably with those of other fibres. Surface characterisation shows that all pitch-based graphite fibres exhibit a surface-oriented skin, although surface roughness increases with fibre modulus. The fibres all exhibit similar apparent surface energy characteristics which suggests that wettability does not play a significant role in determining interfacial bond strengths.     

Thermal conversion of carbon fibres/polysiloxane composites to carbon fibres/ceramic composites

The aim of this work is to investigate the thermal conversion of carbon fibres/polysiloxane composites to carbon fibres/ceramic composites. The conversion mechanism of four different resins to the ceramic phase in the presence of carbon fibres is investigated. The experiments were conducted in three temperature ranges, corresponding to composite manufacturing stages, namely up to 160 °C, 1000 °C and finally 1700 °C.The study reveals that the thermal conversion mechanism of pure resins in the presence of carbon fibres is similar to that without fibres up to 1000 °C. Above 1000 °C thermal decomposition occurs in both solid (composite matrix) and gas phases, and the presence of carbon fibres in resin matrix produces higher mass losses and higher porosity of the resulting composite samples in comparison to ceramic residue obtained from pure resin samples. XRD analysis shows that at temperature of 1700 °C composite matrices contain nanosized silicon carbide. SEM and EDS analyses indicate that due to the secondary decomposition of gaseous compounds released during pyrolysis a silicon carbide protective layer is created on the fibre surface and fibre–matrix interface. Moreover, nanosized silicon carbide filaments crystallize in composite pores.Owing to the presence of the protective silicon carbide layer created from the gas phase on the fibre–matrix interface, highly porous C/SiC composites show significantly high oxidation resistance.     

Adhesion of RFL-coated aramid fibres to elastomers: The role of elastomer–latex compatibility

The performance of fibre-reinforced composites is strongly dependent on the nature and the strength of the fibre–matrix interface. Good interfacial bonding is required to ensure load transfer from matrix to reinforcing fibres. For rubber-reinforced composites, resorcinol formaldehyde latex (RFL) is known as a fibre surface coating which is able to provide good adhesion between rubber and fibres. In the present study, aramid fibres are investigated, because of their significantly higher modulus and strength, compared to other commercial fibres. Their adhesion after being coated with RFL, in compounds based on natural rubber (NR) and in NR blended with a small amount of styrene butadiene rubber (SBR) is investigated. It is shown that though having very similar tensile properties, the latter compound has much better adhesion to RFL which is also less sensitive to RFL ageing, compared to the pure NR compound. It is argued that an interphase region is formed between RFL and the elastomer, which is stronger for the compound containing SBR due to its enhanced compatibility with the latex part of the RFL.     

Effect of intermediate heat treatment on mechanical properties of SiCf/SiC composites with BN interphase prepared by ICVI

SiC_f/SiC composites with BN interface were prepared through isothermal-isobaric chemical vapour infiltration process. Room temperature mechanical properties such as tensile, flexural, inter-laminar shear strength and fracture toughness (K_IC) were studied for the composites. The tensile strength of the SiC_f/SiC composites with stabilised BN interface was almost 3.5 times higher than that of SiC_f/SiC composites with un-stabilised BN interphase. The fracture toughness is similarly enhanced to 23 MPa m^1/2 by stabilisation treatment. Fibre push-through test results showed that the interfacial bond strength between fibre and matrix for the composite with un-stabilised BN interface was too strong (>48 MPa) and it has been modified to a weaker bond (10 MPa) due to intermediate heat treatment. In the case of composite in which BN interface was subjected to thermal treatment soon after the interface coating, the interfacial bond strength between fibre and matrix was relatively stronger (29 MPa) and facilitated limited fibre pull-out.