Mechanical Properties of Regenerated Cellulose Fibres for Composites

Summary: A broad variety of regenerated cellulose fibres was subjected to single fibre tensile tests in order to determine the modulus of elasticity, tensile strength, and failure strain. The results were compared to glass fibres and flax fibres, which are considered the most important technical and natural fibres, respectively. With regard to their modulus of elasticity and tensile strength, regenerated cellulose fibres showed clearly lower values than glass fibres, even when their low density was taken into account. The average modulus of elasticity and tensile strength of regenerated cellulose fibres was also lower than the values measured for flax fibres, but when variability was considered, both fibres performed similarly. In terms of interfacial shear strength with polypropylene, lyocell fibres performed significantly less well than sized glass fibre and ramie fibre. The most important difference between regenerated cellulose fibres and both glass and flax fibres is their high failure strain and thus high work to fracture. The high work to fracture of regenerated cellulose fibres makes them particularly useful for composite applications where high fracture toughness is required.     

Synthesis and characterization of poly(arylene ether imidazole)s

Poly(arylene ether imidazole)s were prepared by the aromatic nucleophilic displacement reaction of a bisphenol imidazole with activated aromatic dihalides. The polymers had glass transition temperatures ranging from 230 to 318°C and number-average molecular weights as high as 82,000 g/mol. Thermogravimetric analysis showed a 5% weight loss occurring ～ 400°C in air and ～ 500°C in nitrogen. Typical neat resin mechanical properties obtained at room temperature included tensile strength and tensile modulus of 14.2 and 407 ksi and fracture energy (G_lc) of 23 in. lb/in.² Titanium-to-titanium tensile shear strengths measured at 23 and 200°C were 4800 and 3000 psi, respectively. In addition, preliminary data were obtained on carbon fiber laminates. The chemistry, physical, and mechanical properties of these polymers are discussed.     

Apparent shear strength of hybrid glass fibre reinforced composite joints

The incorporation of nano or micro ceramic particles into fibre reinforced composites (FRC) to enhance their stiffness and durability has been widely investigated. This mechanism has been attributed to the increase in stiffness of the polymeric matrix phase and shear strength of FRCs due to the presence of particles at the interlaminar regions. In order to elucidate such effect, hybrid single-lap joints consisted of ceramic particles and glass fibre reinforced composites were evaluated to better assess the mechanical interlocking effect provided by silica and cement inclusions. A full factorial design (2³) was performed to identify the effect of the type of particle (silica and cement), particle weight fraction (2.5 and 5 wt%) and glass fibre grammage (200 and 600 g/m²) on the apparent shear strength and adherent strength of single-lap joints under tensile loading. The ceramic particle inclusions led to increased apparent shear strength and adherent strength. The inclusion of 5 wt% ceramic particles into 600 g/m² cross-ply glass fibre composites enhanced both adherent and apparent shear strengths.     

Study of the carbon fiber–Poly(Ether–Ether–Ketone) (PEEK) interfaces, 4: influence of fiber–matrix adhesion on the mechanical properties of unidirectional composites

The aim of the last part of this general study is to analyze the influence of the interfacial properties and, more precisely, the adhesion energy, between carbon fibers and PEEK on the final performance of unidirectional composites. A set of mechanical properties, i.e. interlaminar shear strength, longitudinal tensile and compressive and transverse tensile properties, of different unidirectional laminates with the same content (60% by volume) of carbon fibers is determined. It is first shown that the interlaminar shear strength is constant, whatever the type of materials. Therefore, this test is not appropriate to characterize the strength of the fiber–matrix interface in PEEK-based composites. On the contrary, in agreement with previous work on other systems, it appears that the ultimate properties (longitudinal tensile and compressive as well as transverse tensile strengths and strains) of the laminates increase with the interfacial adhesion energy, whereas the stiffness of these composites remains unaffected in all cases.     

Mechanical properties of hybrid glass/sugar palm fibre reinforced unsaturated polyester composites

A research has been carried out to investigate the mechanical properties of composites made by hybridizing sugar palm fibre (Arenga pinnata) with glass fibre into an unsaturated polyester matrix. Hybrid composites of glass/sugar palm fibre were fabricated in different weight ratios of strand mat glass fibres: sugar palm fibres 4:0, 4:1, 4:2, 4:3, 4:4, and 0:4. The hybrid effects of glass and sugar palm fibre on tensile, flexural and impact properties of the composites were evaluated according to ASTM D5083, ASTM D790 and ASTM D256 respectively. Results have been established that properties of hybrid glass/sugar palm composites such as tensile strength, tensile modulus, elongation at break, toughness, flexural strength, flexural modulus and impact strength are a function of fibre content. The failure mechanism and the adhesion between fibres/matrix were studied by observing the scanning electron micrographs of impact fracture samples. In general, the incorporation of both fibres into unsaturated polyester matrix shows a regular trend of increase in the mechanical properties.     

Effect of strain rate on the dynamic tensile behaviour of UHMWPE fibre laminates

Ultra-high molecular weight polyethylene (UHMWPE) fibre has great potential for strengthening structures against impact or blast loads. A quantitative characterization of the mechanical properties of UHMWPE fibres at varying strain rates is necessary to achieve reliable structural design. Quasi-static and high-speed tensile tests were performed to investigate the unidirectional tensile properties of UHMWPE fibre laminates over a wide range of strain rates from 0.0013 to 163.78 s⁻¹. Quasi-static tensile tests of UHMWPE fibre laminates were conducted at thicknesses ranging from 1.76 mm to 5.19 mm. Weibull analysis was conducted to investigate the scatter of the test data. The failure mechanism and modes of the UHMWPE fibre laminates observed during the test are discussed. The test results indicate that the mechanical properties of the UHMWPE fibre laminate are not sensitive to thickness, whereas the strength and the modulus of elasticity increase with strain rate. It is concluded that the distinct failure modes at low and high strain rates partially contribute to the tensile strength of the UHMWPE fibre laminates. A series of empirical formulae for the dynamic increase factor (DIF) of the material strength and modulus of elasticity are also derived for better representation of the effect of strain rate on the mechanical properties of UHMWPE fibre laminates.     

New soybean oil‐styrene‐divinylbenzene thermosetting copolymers. III. Tensile stress–strain behavior

The tensile stress–strain behavior and fracture properties of some new soybean oil based polymeric materials were investigated at room temperature. These materials were prepared by the cationic copolymerization of regular soybean oil, low saturation soybean oil (LoSatSoy oil), or conjugated LoSatSoy oil with styrene and the diene comonomers divinylbenzene, norbornadiene, or dicyclopentadiene in a process initiated by boron trifluoride diethyl etherate (BF₃ · OEt₂) or related modified initiators. These new polymeric materials exhibited tensile stress–strain behavior ranging from soft rubbers through ductile to relatively brittle plastics. The Young's moduli of these polymers varied from 3 to 615 MPa, the ultimate tensile strengths varied from 0.3 to 21 MPa, and the elongation at break varied from 1.6 to 300%. These properties are obviously related to their crosslink densities. The conjugated LoSatSoy oil polymers had higher mechanical properties than the corresponding LoSatSoy oil and regular soybean oil polymers with the same stoichiometry. Some conjugated LoSatSoy oil polymers with appropriate stoichiometries showed yielding behavior in the tensile test process. A variety of new polymer materials can thus be prepared by varying the stoichiometry, the type of soybean oil, and the crosslinking agent. These soybean oil based polymers possessed mechanical properties comparable to those of commercially available rubbery materials and conventional plastics and thus may serve as replacements in many applications. © 2000 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 39: 60–77, 2001     

Effect of temperature on weldline integrity of injection moulded short glass fibre and glass bead filled ABS hybrids

The present study investigated the effect of temperature on weldline strength of injection moulded ABS polymer reinforced with both short glass fibres (GF) and spherical glass beads (GB) over the temperature range 25 to 100 °C. It was noted that weld and non-weld tensile strength of ABS/GF/GB hybrids increased as the concentration of total glass in the hybrids increased. A linear increase in both weld and non-weld tensile strength was found with increasing the hybrid ratio of the glass fibre, χ. Results indicated that weld and non-weld tensile strength for the hybrid at a given temperature can be estimated from the rule of hybrid mixtures. Weld and non-weld tensile strength of the hybrid system decreased with increasing temperature in a linear manner. The rate at which weld and non-weld tensile strengths decreased with temperature was dependent upon the hybrid ratio of the glass fibre, χ, and the total concentration of glass in the hybrids. Weldline integrity factor for the hybrids decreased non-linearly with increasing χ, but increased linearly with increasing temperature.     

Continuous Atmospheric Plasma Oxidation of Carbon Fibres: Influence on the Fibre Surface and Bulk Properties and Adhesion to Polyamide 12

Continuous atmospheric plasma oxidation (APO) was used to introduce oxygen functionalities to the surface of carbon fibres in an attempt to enhance interfacial adhesion between carbon fibres and polyamide-12 (PA-12). APO only affects the surface properties of the fibres while their bulk properties remained unchanged. Contact angle and ζ-potential measurements demonstrated that APO-treated fibres became significantly more hydrophilic due to the introduction of polar oxygen-containing groups on the fibre surface, which also resulted in an increase of surface energy on the carbon fibres. The interfacial shear strength of single carbon fibre/PA-12 model composites, determined by single fibre fragmentation tests, showed an increase from 40 to 83 MPa with up to 4 min of APO treatment time which confirms that the fibre/matrix interfacial adhesion was enhanced. This highlights that the incorporation of APO into composite manufacturing will allow tailoring of the fibre/matrix interface.     

High-strength fire- and heat-resistant imide resins containing cyclotriphosphazene and hexafluoroisopropylidene groups

High-strength fire- and heat-resistant polymers were obtained by the thermally induced melt-polymerization of maleimido-phenoxy cyclotriphosphazenes linked by hexafluoroisopropyliden-ediphthalimide groups. These polymers show good thermal stability and high char yields: 78–80% at 800°C in nitrogen and 60–68% in air at 700°C. Graphite-fabric laminates did not burn in pure oxygen, even at 300°C (LOI = 100%), and were tested for shear, flexural, and tensile strengths. Two monomers were synthesized by reacting tris(4-aminophenoxy)-tris(phenoxy) cyclotriphosphazene with maleic anhydride and hexafluoroisopropylidenediphthalic anhydride. The triamine was synthesized by a stepwise reaction of hexachlorocyclotriphosphazene with phenol and 4-nitrophenol to give tris(4-nitrophenoxy)-tris(phenoxy)cyclotriphosphazene and reducing the nitro groups. The structures of cyclic phosphazene-trimeric precursors and the polymers were characterized by FT-IR, ¹H-NMR, ³¹P-NMR, and mass spectroscopy. The curing behaviors of polymer precursors were evaluated by differential scanning calorimetry and thermogravimetric analyses.     

Influence of plasma treatment on the adhesion between a polymeric matrix and natural fibres

The aim of this work is to study the influence of low-pressure plasma treatment on cellulose fibres to improve the adhesion between a polymeric matrix and natural fibres used as reinforcement. To evaluate fibre wettability, contact angle measurements were carried out on flax fibres after treatment with plasma under several conditions. Similarly, contact angle measurements were performed without plasma treatment. A comparison between all the samples led to the definition of the optimal plasma treatment conditions. Once the latter were determined, composite materials were prepared with treated and untreated flax fibres and a low-density polyethylene matrix. Composites, with different fibre contents (5 and 40%) and different fibre lengths (1 and 10 mm), were manufactured using a mixer and a hot plate press. The tensile strengths of the composites were assessed to determine optimal fibre content and length, and the plasma treatment effect was also quantified. It was found that the higher the fibre content, the higher the tensile strength, and the higher the Young’s modulus; however, fibre length did not affect tensile strength. Regarding plasma treatment, composites with treated fibres exhibited a considerably improved tensile strength and Young’s modulus. Plasma treatment effects were also studied by X-ray photoelectron spectroscopy and by differential scanning calorimetric. Finally, an analysis of the fibre surface and an interaction study between the matrix and the fibres was conducted with scanning electron microscopy.     

Effect of stress on the fire reaction properties of polymer composite laminates

A small-scale loading frame was used to apply tensile and compressive stresses to glass vinyl ester and glass polyester laminates in a cone calorimeter under a heat flux of 75 kW m⁻². It was found, for the first time, that stress has a small but significant effect on the fire reaction properties. Increasing tensile stress increased heat release rate and smoke production while shortening the time-to-ignition. Compressive stress had the reverse effect. This was attributed to the fact that tensile stress promotes the formation of matrix microcracks, facilitating the evolution of flammable volatiles. This hypothesis is further supported by the observation that stress has the greatest effect on the early heat and smoke release peaks, with a lower effect on the final ‘run-out’ values.Stress rupture (time-to-failure) curves were produced for tension and compression. In tension, the behaviour was fibre dominated, with times-to-failure being roughly 10 times those in compression. Compressive failure involved resin dominated local fibre kinking, initiated near to the rear face of the specimen. The failure time was determined by a significant proportion of the specimen reaching its glass transition temperature.     

Effects of preparation conditions on properties of rigid polyurethane foam composites based on liquefied bagasse and jute fibre

Rigid polyurethane foams based on liquefied bagasse and reinforced with jute fibre were prepared. The effects of preparation conditions were investigated using a paper cup with a small horizontal section area as a mould. They were reflected in the foam height, which acted as a sensitive indicator. Density gradient existed in the foam rise direction and decreased from the bottom to top. Although the amount of blowing agent water was fixed, the foam height increased with stirring time after the addition of diphenyl methane diisocyanate, the isocyanate index and the catalyst content. This was partly due to the released heat that also contributed to the foam expansion. The relative intensity of the C─N stretching band at 1510 cm⁻¹ and the N─H out-of-plane bending band at 1527 cm⁻¹ in the FTIR spectrum reflected isocyanate reactions, which had a close relationship with the crosslink density. The normalized compressive strength was essentially attributed to the combined effects of the crosslink density and the thickness of cell walls and struts. Jute fibre enhanced the compressive strength only slightly due to poor interfacial adhesion between some fibres and the matrix.     

Determination of dynamic properties of flax fibres reinforced laminate using vibration measurements

Experimental and numerical methods to identify the linear viscoelastic properties of flax fibre reinforced polymer (FFRP) composite are presented in this study. The method relies on the evolution of storage modulus and loss factor as observed through the frequency response. Free-free symmetrically guided beams were excited in the dynamic range of 10 Hz to 4 kHz with a swept sine excitation focused around their first modes. A fractional derivative Zener model has been identified to predict the complex moduli. A modified ply constitutive law has been then implemented in a classical laminates theory calculation (CLT) routine. Overall, the Zener model fitted the experimental results well. The storage modulus was not frequency dependant, while the loss factor increased with frequency and reached a maximum value for a fibre orientation of 70°. The damping of FFRP was, respectively, 5 and 2 times higher than for equivalent carbon and glass fibres reinforced epoxy composites.     

The mechanical properties of plasma‐treated carbon fiber reinforced PA6 composites with CNT

The aim of this work is the evaluation of the effects of plasma treatment and the addition of CNT on the mechanical properties of carbon fibre/PA6 composite. A powder impregnation process with integrated inline continuous plasma of carbon fibers was used to produce CF/PA6 composite. CF/PA6 composite was processed into test laminates by compression moulding, and interface dominated composite properties were studied. The tensile and impact strength of composites containing CNT and plasma‐treated carbon fibres improved obviously. The tensile strength of nanocomposite largely increases with the increasing of the CNT content and then decreases when the CNT content is over 2%. The hydroxyl groups of the fibers surface are in favor of the wettability of carbon fibers by the polar matrix resin, which is resulting in a further interaction of the fiber surface with the curing system of the matrix resin.     

On the strain measurement and stiffness calculation of carbon fibre reinforced composites under quasi-static tensile and tension-tension fatigue loads

The applicability of different strain measurement techniques for carbon/epoxy laminates under quasi-static tensile and tension-tension fatigue loads was studied. Strain gauges, mechanical extensometers, digital image correlation and 2 D camera systems were applied on laminates tested at angles of 0°, 45°, 60°, 90° and ±45°. In addition, displacements recorded by the servo-hydraulic piston were monitored and compared to local strain measurement techniques. Representative examples that illustrate characteristics and limits of each technique in quasi-static and fatigue tests are discussed. Influences of the respective method of strain measurement, the specimen surface, fibre direction and processes in the specimens during tests on the recorded stress-strain behaviour and on the calculated stiffness are presented. Recommendations for accurate strain measurement of anisotropic laminates based on the results are made.     

Topologically interpenetrating elastomeric networks

Several partially interpenetrating polymeric networks (IPN) were made by combining chemically different linear elastomers. The polymer combinations were deposited as films from aqueous emulsions made by mixing the individual emulsions in equal proportions. The films were crosslinked to form two superimposed networks. In two cases, the networks were cleanly separated by hydrolysis of one of the component networks to demonstrate that there was no chemical interaction between the polymers. Measurement of crosslink density showed that, in most cases, partial interpenetration does occur as evidenced by an effective crosslink density of the IPN's greater than the arithmetic mean of the crosslink densities of the component networks. The swelling ratios, densities, and stress–strain properties were determined. For one of the network combinations, a poly(urethane–urea) and a poly(butadiene–acrylonitrile), a series of IPN's varying in polymer composition was made. The swelling ratios and densities are close to the arithmetic means; however, both the tensile strength and crosslink density exhibit a maximum at about 70% poly(butadiene-acrylonitrile). The maximum tensile strength is actually significantly higher than that of either of the component polymers. The elongations all approach that of the poly(urethane–urea), the more extensible material, except for compositions approaching 100% poly(butadiene–acrylonitrile), which exhibit a very low extensibility.     

Curing of epoxy resins with metal(II)4,4′,4″,4‴-tetraamino phthalocyanines-modification with elastomers

The use of metal phthalocyanine tetraamines in curing epoxy resins to form high-temperature-resistant matrix polymers for composites has been reported earlier. The effect of adding carboxy-terminated butadiene-acrylonitrile (CTBN) elastomer is now described; preliminary measurements of tensile, flexural, and short-beam shear strengths, dynamic moduli, resin content, and moisture absorption are presented, and the results of dynamic thermogravimetric analyses are given. In addition to their high char yield (86–87.5% at 800°C in a nitrogen atmosphere) and limiting oxygen index (48.3–50.3), the laminates showed good mechanical properties.     

In-situ fracture investigations of MgLi-carbon fibre composite materials by AES and data analysis by means of factor and cluster analysis

Uncoated and 300 nm pyrocarbon coated polyacrylonitril (PAN) based T300 type carbon fibres were pressure infiltrated with molten Mg8Li and Mg12Li alloys at 903 K and 963 K, respectively, and at contact times of 4 s and 30 s. The fracture surfaces were characterized by in-situ Auger electron spectroscopy (AES) to investigate the reason for differences in mechanical properties, which were obtained by tensile strength experiments. Pressure increase occurred during the fracture of all the MgLi samples under ultra high vacuum conditions in the analyzer chamber of the AES apparatus, indicating porosity probably due to poor wetting of the fibres during the infiltration process. As visible in the scanning electron micrographs, the pyrocarbon coated carbon fibres were less attacked by the molten MgLi than the uncoated fibres. The damage seemed to increase, the higher the Li contents, the higher the contact time and the higher the temperature were chosen, whereas pyrocarbon coating may retard this affection. Characteristic objects of the sample fracture surfaces (fibre fracture surface, fibre jacket surface, fibre impression surface and matrix) were investigated by laterally high resolution Auger electron spectroscopy. Oxygen was found to be distributed all over the fracture surfaces of the as-fractured samples, and Mg/Li were identified in a chemically bound form. On all the characteristic objects carbide (Li₂C₂) formation has been detected. Factor analysis was performed to exctract the principal components from the whole set of differentiated Auger electron spectra in the Mg/Li, C and O spectral regions, respectively. Cluster analysis of the weighting factors (the factor loadings) of the most important principal components lead to a separation of the data set into two main groups due to the presence or absence of a strong carbide C (KVV) peak as result of Ar⁺ sputter removal of the covering oxide layer; no separation of the objects concerning the reaction conditions was found. Received: 18 June 1996 / Revised: 26 July 1996 / Accepted: 30 July 1996     

The ageing phenomenon of polyethersulphone hollow fibre membranes for gas separation and their characteristics

We have studied the ageing behaviour of PES/NMP (polyethersulphone/N-methyl pyrrolidone) hollow fibres for gas separation that were prepared from 35% and 37% dope. The effect of ageing on hollow fibres spun from low and high shear rate (103 vs. 862 s⁻¹) has also been investigated, in terms of their transport properties (permeation flux and separation performance), thermal, mechanical and tensile properties. Hollow fibres in this study were aged for around four months in ambient air at room temperature prior to testing.In general, the gas permeation flux drops steeply during the 40 days following fabrication and levels off thereafter. The O₂/N₂ selectivity decreases slightly over time. Hollow fibres spun with high shear rate seem to age faster than those spun with low shear rate. The gas fluxes of both membranes were found to follow a log–log relationship with ageing time. For almost all the gases used in this study, the gas flux decay rate, calculated from the slope of the log–log plot of gas flux vs. ageing, is higher for membranes spun with high shear rate. The effect of shear rate on ageing is less significant for smaller gas molecules that travel faster such as He and H₂. No significant effect of ageing on gas selectivity was observed. Experimental results also indicate that the storage modulus and loss modulus of the hollow fibres increase with ageing. Hollow fibres spun with high shear rates give a slightly higher increase in these moduli than those spun at low shear rates. Surprisingly, tangent δ (energy dissipation) and glass transitional temperature are not sensitive to ageing. We also found that the tensile yield strength and Young's modulus of the hollow fibres increase slightly with ageing. The hollow fibre membranes spun at high shear rates also show a higher increment in tensile yield stress. However, the change in Young's modulus due to ageing was similar for fibres spun with high and low shear rates.