Mechanical properties of thermally treated hemp fibers in inert atmosphere for potential composite reinforcement

Hemp (Cannabis Sativ L.) is an important lignocellulosic raw material for the manufacture of cost-effective environmentally friendly composite materials. From an earlier study it was found that when hemp bast fibers were heated above the glass transition temperature of lignin, there was a migration of lignin to the surface of the fiber. The preliminary observations showed that heat treatment in inert environment seemed to provide enough fiber opening without affecting the associated tissues of the fibers. Here, hemp fibers were given heat treatment in an enclosed vessel in air as well as inert environment and their mechanical properties were compared to the raw hemp fiber. It was found that there were openings of fibers upon heating, both along the length as well as along the diameter or the width directions. For the same weight of the fiber, the total count of fibers increased during heat treatment, with increment up to 32% for inert environment and 39% for air environment; the increment was mainly due to opening up of fibers into lesser diameters than the original fibers. The strength properties were strongly influenced by the diameter of the fibers, with the lesser fibers contributing to greater tensile strength and modulus. The overall tensile strength and modulus of fibers treated in inert environment were found to have increased, probably due to production of fibers of lesser diameters, presumably with less number of natural defects. The overall strength of fiber treated in air environment, however, decreased even though there was opening up of fibers in this case as well. This was due to oxidation of various constituents of fiber which contributes strength.     

The effect of heat treatment temperature and time on the microstructure and mechanical properties of PAN-based carbon fibers

The influence of heat treatment temperature from 1400 to 2840 °C and time from 1.2 to 12.0 min on the structure and mechanical properties of polyacrylonitrile carbon fibers was studied. It was observed that the Young’s modulus increased with increasing temperature and time, but the tensile strength exhibited different variation trends with the different processing methods. For a fixed time of 1.2 min, the strength dropped from 4.6 GPa at 1400 °C to 2.6 GPa at 2840 °C, (~43.5 %) as opposed to a 63.9 % increase in Young’s modulus. However, when the treatment time was increased to 6.0 min at 2500 °C, the tensile strength decreased only by 1.9 %, from 3.71 to 3.64 GPa, versus a nearly 20.0 % increase in Young’s modulus. The same situation was found for treatment at 2000 and 2700 °C. Raman spectroscopy and uniform stress model analysis show that the degree of covalent cross-linking between the graphene planes decreased as temperature increased, while it remained almost constant as treatment time was increased. It is believed that during heat treatment of a carbon fiber, the cross-linking collapses at the beginning but the crystalline size keeps growing with prolonging time, so the tensile strength decreases little with further heat treatment while tensile modulus keeps increasing.     

The strength of glass fibre reinforcement after exposure to elevated composite processing temperatures

The results of a study on the properties of glass fibres after thermal conditioning at typical engineering thermoplastic processing temperatures are presented. The mechanical performance of rovings and single fibres of well-defined silane- and water-sized E-glass fibre samples was investigated at room temperature after thermal conditioning at temperatures up to 400 °C. Thermal conditioning for 15 min led to strength degradation of >50 % at higher temperatures. The tensile strength of silane-coated fibres was relatively stable up to 300 °C but exhibited a precipitous drop at higher conditioning temperatures. The water-sized fibres exhibited an approximately linear decrease in strength with increasing conditioning temperature. The strength distribution of the water-sized fibres could be well represented by a unimodal three-parameter Weibull distribution. The strength distributions of the sized fibres were more complicated and required the use of a bimodal Weibull distribution. The results are discussed in terms of the changes in surface coating and bulk glass structure during heat conditioning.     

Polyimide fibers prepared by dry-spinning process: imidization degree and mechanical properties

Polyimide fibers were prepared by dry spinning a polyamic acid solution to get the precursor fibers and then the precursor fibers were transferred into the polyimide fiber by heat treatment. The imidization degree (ID) of the precursor fibers obtained at various spinning conditions was investigated using FTIR and TGA analysis. As a result, the IDs of the precursor fibers increased with elevating spinning temperature. Meanwhile, the IDs measured by FTIR and TGA were much higher than the values from our model prediction. The tensile strength of precursor fibers exhibited a slight dependency on IDs. On the other hand, the complete imidization and hot stretching led to a great improvement in the mechanical properties. Subglass transition and glass transition of the stretched polyimide fibers were observed in DMA, and the activation energy of these transitions was 346 and 981 kJ mol^?1, respectively.     

Strain-rate dependence of the tensile strength of glass fibers

It is well known that the strength of glass fibers increases with increasing strain rate. Consequently, impact strength of glass fiber is competitive with that of carbon fiber. This strengthening phenomenon is well recognized for bulk glass. Strain-rate dependence of the strength for bulk glass was described by considering slow crack growth in glass. The analytical model that considered the slow crack growth of glass is proposed to predict the strength of glass fibers. The proposed model considered the stress corrosion limit and a constant crack velocity region. Calculations showed almost same results with the previous model, however, some differences were confirmed. To discuss the validity of the analysis, tensile tests of E-glass fiber bundles were conducted at various strain rates. It was observed that the fracture behaviors differ with the strain rates. Experimental results showed that the strength of E-glass fibers increased with increasing strain rate. Furthermore, we confirmed that the analytical results were in good agreement with the experimental results. The strain-rate dependence of the strength of glass fibers was successfully predicted by considering the slow crack growth in glass.     

Surface modification of fiber reinforced polymer composites and their attachment to bone simulating material

The purpose of this study was to investigate the effect of fiber orientation of a fiber-reinforced composite (FRC) made of poly-methyl-methacrylate (PMMA) and E-glass to the surface fabrication process by solvent dissolution. Intention of the dissolution process was to expose the fibers and create a macroporous surface onto the FRC to enhance bone bonding of the material. The effect of dissolution and fiber direction to the bone bonding capability of the FRC material was also tested. Three groups of FRC specimens (n = 18/group) were made of PMMA and E-glass fiber reinforcement: (a) group with continuous fibers parallel to the surface of the specimen, (b) continuous fibers oriented perpendicularly to the surface, (c) randomly oriented short (discontinuous) fibers. Fourth specimen group (n = 18) made of plain PMMA served as controls. The specimens were subjected to a solvent treatment by tetrahydrofuran (THF) of either 5, 15 or 30 min of time (n = 6/time point), and the advancement of the dissolution (front) was measured. The solvent treatment also exposed the fibers and created a surface roughness on to the specimens. The solvent treated specimens were embedded into plaster of Paris to simulate bone bonding by mechanical locking and a pull-out test was undertaken to determine the strength of the attachment. All the FRC specimens dissolved as function of time, as the control group showed no marked dissolution during the study period. The specimens with fibers along the direction of long axis of specimen began to dissolve significantly faster than specimens in other groups, but the test specimens with randomly oriented short fibers showed the greatest depth of dissolution after 30 min. The pull-out test showed that the PMMA specimens with fibers were retained better by the plaster of Paris than specimens without fibers. However, direction of the fibers considerably influenced the force of attachment. The fiber reinforcement increases significantly the dissolution speed, and the orientation of the glass fibers has great effect on the dissolving depth of the polymer matrix of the composite, and thus on the exposure of fibers. The glass fibers exposed by the solvent treatment enhanced effectively the attachment of the specimen to the bone modeling material.     

Effects of SWCNTs on mechanical and thermal performance of epoxy at elevated temperatures

A property which limits the breadth of application of thermoset polymers and their composites is their relatively low maximum operating temperatures. This work investigates the potential application of both functionalized single-walled carbon nanotubes (f-SWCNTs) based on negative charging, and unfunctionalized SWCNTs (u-SWCNTs) to increase the mechanical and thermal performance of a high-temperature aerospace-grade epoxy with a glass transition temperature of approximately 270 °C. Thermal and mechanical properties of the baseline epoxy and nanocomposites containing a low content of SWCNTs (0.2 % by weight) were characterized through thermogravimetric analyses, tensile tests, and dynamic mechanical analyses. Tensile tests were performed both at room temperature and at 80 °C. Further, room temperature tensile tests were performed on untreated and heat-treated specimens. The heat treatment was performed at 300 °C, slightly above the resin glass transition temperature. Results demonstrate that f-SWCNTs are effective in improving the mechanical and thermal performance of the epoxy. No significant improvement was observed for u-SWCNT nanocomposites. For the nanocomposite with f-SWCNTs, the ultimate tensile strength and strain to failure at room temperature (80 °C) increased by 20 % (8 %) and 71 % (77 %), respectively, as compared to the baseline epoxy. The f-SWCNT nanocomposite, unlike other examined materials, exhibited a stress–strain necking behavior at 80 °C, an indication of increased ductility. After heat treatment, these properties further improved relative to the neat epoxy (160 % increase in ultimate tensile strength and 270 % increase in strain to failure). This work suggests the potential to utilize f-SWCNTs based on negative charging to enhance high-temperature thermoset performance.     

Effect of Seawater and Warm Environment on Glass/Epoxy and Glass/Polyurethane Composites

A study of the durability of fiber reinforced polymer (FRP) materials in seawater and warm environment is presented in this paper. The major objective of the study is to evaluate the effects of seawater and temperature on the structural properties of glass/epoxy and glass/polyurethane composite materials. These effects were studied in terms of seawater absorption, permeation of salt and contaminants, chemical and physical bonds at the interface, degradation in mechanical properties, and failure mechanisms. Test parameters included immersion time, ranging from 3 months to 1 year, and temperature including room temperature and 65°C. Seawater absorption increased with immersion time and with temperature. The matrix in both composites was efficient in protecting the fibers from corrosive elements in seawater; however moisture creates a dual mechanism of stress relaxation—swelling—mechanical adhesion, and breakdown of chemical bonds between fiber and matrix at the interface. It is observed that high temperature accelerates the degradation mechanism in the glass/polyurethane composite. No significant changes were observed in tensile strength of glass/epoxy and in the modulus of both glass/epoxy and glass/polyurethane composites. However, the tensile strength of the glass/polyurethane composite decreased by 19% after 1 year of exposure to seawater at room temperature and by 31% after 1 year of exposure at 65°C. Plasticization due to moisture absorption leads to ductile failure in the matrix, but this can be reversed in glass/polyurethane composites after extended exposure to seawater at high temperature where brittle failure of matrix and fiber were observed.     

Acid corrosion resistance and mechanism of E-glass fibers: boron factor

Acid corrosion and stress corrosion characteristics of E-glass fibers with and without boron (B₂O₃ or B) were carefully studied, using 1 N H₂SO₄ acid at 96 °C and room temperature, respectively. The effect of boron on glass resistance to the acid attack is elucidated in conjunction with structural roles of B, Al, and Ca in the glass. Scanning electron microscopy with energy dispersive spectrometer (SEM/EDS) characterization was performed on the selective fiber samples before and after the acid leaching. For high boron-containing fibers, the results showed the formation of alteration layer enriched in Si as a result of depletion of both Ca and Al. Chemical analysis of the high boron fibers before and after 24 h acid leaching and the solution after 24 h test further confirmed that B, Ca, and Al in the glass fibers preferentially dissolved in the acid solution. Glass fiber dissolution mechanisms were discussed with a proposal that acid corrosion attack in boron-containing E-glass is controlled by hydrolysis of aluminoborate complex species (less than 10 nm) separated from the silicate glass network, whereas the acid corrosion attack in boron-free E-glass is controlled by hydrolysis of the silicate network, where 4-coordinated aluminum in the network is locally charge compensated by Ca.     

Chlorinated polyethylene nanocomposites: thermal and mechanical behavior

Chlorinated polyethylene (CPE) nanocomposites prepared with natural and organically treated montmorillonite (MMT) clays by solution intercalation method were investigated. X-ray diffraction and transmission electron microscopy techniques showed separation of organically modified clay MMT layers and indicated formation of exfoliated nanocomposites. Fourier transform infrared spectroscopy results showed interaction between the CPE matrix and the clay intercalants of Cloisite^® 30B and Cloisite^® 15A (natural MMT modified with quaternary ammonium salts). Organically treated MMT clays were found to be better dispersed in CPE in comparison to natural MMT clay. Mechanical testing showed enhanced tensile strength, Young’s modulus, and storage modulus of chlorinated-polymers/organically treated MMT clay nanocomposites. Significant improvements in the above properties were obtained with Cloisite^® 15A nanoclay. The temperature, at which maximum degradation occurred, was higher for the nanocomposite having 5 wt% Cloisite 15A than that of neat CPE. Differential scanning calorimetric results revealed that the same composition also absorbed more heat during the heating, indicating better thermal stability. CPE rubber nanocomposite could be a promising heat resistant polymeric material.     

The effect of high-temperature vapor deposition polymerization of polyimide coating on tensile properties of polyacrylonitrile- and pitch-based carbon fibers

Carbon fibers are widely used as a reinforcement in composite materials because of their high-specific strength and modulus. Current trends toward the development of carbon fibers have been driven in two directions; ultrahigh tensile strength fiber with a fairly high strain to failure (~2 %), and ultrahigh modulus fiber with high-thermal conductivity. Today, a number of ultrahigh strength polyacrylonitrile (PAN)-based (more than 6 GPa), and ultrahigh modulus pitch-based (more than 900 GPa) carbon fibers have been commercially available. In the present work, the tensile properties of polyimide-coated PAN-based (T1000GB, T300, and M60JB) and pitch-based (K13D and XN-05) carbon fibers have been investigated using a single-filament tensile test. The pyromellitic dianhydride/4-4′-oxydianiline polyimide coating was deposited on the carbon fiber surface using high-temperature vapor deposition polymerization (VDP_H). The Weibull statistical distributions of the tensile strength were characterized. The results clearly show that the VDP_H polyimide coating improves the tensile strength and the Weibull modulus of PAN- and pitch-based carbon fibers.     

High-temperature behavior and degradation mechanism of SiC fibers annealed in Ar and N<Subscript>2</Subscript> atmospheres

The thermal and mechanical stability of SiC fibers at elevated temperature is an important property for the practical application of SiC fiber-reinforced ceramic matrix composites and is related to the heat-treating atmosphere. In this study, the high-temperature behavior of KD SiC fibers with low oxygen content was investigated in both Ar and N₂ at temperatures from 1400 to 1800 °C through scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Auger electron spectroscopy, resistivity measurements, and tensile tests in order to understand the effects of atmospheres on the degradation of the fibers. The results show that high-temperature treatment caused more severe strength degradation in Ar than in N₂. In particular, the fibers heat treated in N₂ at 1700 °C retained a relatively high strength of 1.52 GPa, 60 % of their original strength, while the fiber strength was completely lost after heat treatment in Ar. Fiber strength degradation was mainly caused by a combination of crystal growth and surface flaws. The formation of huge grains and porosity in the fiber surfaces, owing to the thermal decomposition of the SiC _x O _y N _z and SiC _x O _y phases, significantly degraded the strength for fibers heat treated in Ar. However, the suppressing effect of N₂ on the decomposition of the SiC _x O _y N _z phase in the fiber surfaces and nitrided case on the decomposition of the SiC _x O _y phase in the fiber cores, led to higher SiC fiber temperature stability in N₂ rather than Ar.     

Determining the mechanism controlling glass fibre strength loss during thermal recycling of waste composites

This paper presents an experimental investigation into the large reductions to the tensile fracture stress and the associated strength loss mechanism of E-glass fibres during thermal recycling. Fractographic analysis reveals the fracture process is controlled by surface flaws, irrespective of heat treatment temperature and duration. The fracture toughness is an important material property in order to understand possible changes in the strength–flaw relationship during heat treatment. Focussed ion beam (FIB) milling is used to artificially create a single nano-sized deep notch (between 30 and 1000 nm) in glass fibres. The strength loss, fracture toughness, fracture mirror constant and fracture mechanism observed for nano-notched and thermally recycled fibres are identical, indicating bulk property changes do not occur during thermal recycling. The study proves conclusively that surface flaw growth is the controlling mechanism reducing fibreglass strength during thermal recycling of waste polymer composites.     

Tensile strength and fracture surface characterisation of sized and unsized glass fibers

The tensile strength of commercial glass fibers is examined by single fiber tensile tests. The fibers are analysed as received from the manufacturer (sized) and after a heat treatment at 500C (unsized). Weibull plots of the two series are used for comparison of the strengths of the sized and unsized fibers. It is shown that large sample sizes (over 60 tests) are required to lead to a reliable two-parameter Weibull distribution. The experimental tests clearly indicated that the unsized fibers were weaker in the low strength range, but had similar strength in the high strength range. An investigation of the fracture surfaces in the SEM showed distinct differences in the fracture patterns for high and low strength fibers. Fracture mechanics were applied to estimate the original flaw size and relate the observed fracture mirror surface to the fiber strength. Based on the observation of surface flaws, a healing mechanism by the sizing is considered likely for this type of fiber and sizing, thereby effectively increasing the strength of the fiber in the presence of larger surface flaws.     

Effect of hot stretching graphitization on the structure and mechanical properties of rayon-based carbon fibers

The influence of hot stretching graphitization on the structure and mechanical properties of rayon-based carbon fibers was studied. It was observed that the Young’s modulus of the treated fibers increased with heat treatment temperature (HTT) and hot stretching stress, to 173 GPa by 158.2 % through hot stretching at 2700 °C under stress of 270 MPa compared to that of the as-received carbon fiber. Meanwhile the tensile strength increased to 1.75 GPa by 73.3 % through hot stretching at 2700 °C under 252 MPa. The field emission scanning electron images showed markedly increased roughness on the external surface and bigger and more compacted granular morphologies on the cross section of the treated fibers with increasing HTT. The preferred orientation of graphitic layers was improved by hot stretching, and the higher the HTT, the stronger the effectiveness of the hot stretching. The crystallite sizes grew and the crystallite interlayer spacing decreased obviously with increasing HTT but changed just slightly with increasing stretching stress. The analysis based on uniform stress model and shear fracture theory proposed that the improvement of tensile strength and Young’s modulus for rayon-based carbon fiber was mainly due to the increased preferred orientation and nearly unchanged shear modulus between planes with increasing HTT during hot stretching graphitization, which was much different from polyacrylonitrile-based carbon fibers.     

Evaluation of mechanical properties of banana and sisal fiber reinforced epoxy composites: Influence of glass fiber hybridization

In this work, the effect of glass fiber hybridization with the randomly oriented natural fibers has been analyzed. The banana (B), sisal (S) fibers were chopped and woven E-glass (G) synthetic fibers were reinforced with epoxy matrix. Nine different kinds of laminates were prepared in the following stacking sequence of B, S, BS, G/B/G, G/S/G, G/BS/G, G/B/G/B/G, G/S/G/S/G and G/BS/G/BS/G. Mechanical properties like tensile strength, flexural strength and impact strength were evaluated and compared. Interfacial analysis was also carried out with the help of Scanning Electron Microscope (SEM) to study the micro structural behavior of the tested specimen. It was observed that the addition of two and three layer of glass fiber can improve the tensile strength by a factor of 2.34 and 4.13 respectively. The flexural properties were enhanced on banana–sisal fiber with two layers of glass fibers rather than three layers and the laminate with sisal and three glass ply offers better impact strength.     

Fatigue of a 3D Orthogonal Non-crimp Woven Polymer Matrix Composite at Elevated Temperature

Tension-tension fatigue behavior of two polymer matrix composites (PMCs) was studied at elevated temperature. The two PMCs consist of the NRPE polyimide matrix reinforced with carbon fibers, but have different fiber architectures: the 3D PMC is a singly-ply non-crimp 3D orthogonal weave composite and the 2D PMC, a laminated composite reinforced with 15 plies of an eight harness satin weave (8HSW) fabric. In order to assess the performance and suitability of the two composites for use in aerospace components designed to contain high-temperature environments, mechanical tests were performed under temperature conditions simulating the actual operating conditions. In all elevated temperature tests performed in this work, one side of the test specimen was at 329 °C while the other side was open to ambient laboratory air. The tensile stress-strain behavior of the two composites was investigated and the tensile properties measured for both on-axis (0/90) and off-axis (±45) fiber orientations. Elevated temperature had little effect on the on-axis tensile properties of the two composites. The off-axis tensile strength of both PMCs decreased slightly at elevated temperature. Tension-tension fatigue tests were conducted at elevated temperature at a frequency of 1.0 Hz with a ratio of minimum stress to maximum stress of R = 0.05. Fatigue run-out was defined as 2 × 10⁵ cycles. Both strain accumulation and modulus evolution during cycling were analyzed for each fatigue test. The laminated 2D PMC exhibited better fatigue resistance than the 3D composite. Specimens that achieved fatigue run-out were subjected to tensile tests to failure to characterize the retained tensile properties. Post-test examination under optical microscope revealed severe delamination in the laminated 2D PMC. The non-crimp 3D orthogonal weave composite offered improved delamination resistance.     

Tensile and creep performance of a novel mullite fiber at high temperatures

The novel fiber CeraFib75 with a composition near to pure mullite was analyzed with respect to its potential for high-temperature applications. This mullite fiber free of glass phase was aimed to overcome the strength of commercial oxide fibers at high-temperatures. Tensile tests at room and high temperatures ranging from 900 to 1400 °C and creep tests were performed. Nextel™720, another crystalline mullite-alumina fiber, was tested as a reference. Microstructure and crystal phase analysis of the new fiber revealed mullite grains with traces of γ- and α-alumina in-between; it contains occasionally defects causing a reduced strength at room-temperature. Remarkably, at temperatures beyond 1200 °C, CeraFib75 presented a higher tensile strength than Nextel™720. During tensile tests at 1400 °C, an extended region of inelastic deformation was observed for CeraFib fibers only, which was related to a grain boundary sliding mechanism. Creep rates were of the same order of magnitude for both fibers.     

Effects of fiber surface treatments on mechanical properties of epoxy composites reinforced with glass fabric

In this study, effects of fiber surface treatments on mechanical behavior and fracture mechanism of glass fiber/epoxy composites were investigated experimentally. To change the composition of the glass and regenerate to the hydroxyl groups, activation pretreatment of heat cleaned woven glass fabric was performed using (v/v) HCl aqueous solution at different concentrations before silane treatment. The treatment of silanization of heat cleaned and acid activated glass fibers with γ-glycidoxypropyltrimethoxysilane were performed. In this work, short beam shear test has been conducted to determine the performance of the acid treatment and the silane treatment in terms of the interlaminar shear strength. The silane coating on the heat cleaned glass fibers increased the interlaminar shear strength of the composite. However, the silane coating on the acid activated glass fibers did not improve the interlaminar shear strength of the composite. In addition, the strengths of the glass fabric specimens in tension and flexure were investigated. When the glass fibers are first treated with HCl solution and then with silane coupling agent, the tensile strengths of the composites decreased significantly. Scanning electron photomicrographs of fractured surfaces of composites were performed to explain the failure mechanisms in the composite laminates broken in tension.     

An amorphous ceramic Al32.4Er7.6O60 fiber with large viscous flow deformation and a high-strength nanocrystallized ceramic fiber

An amorphous ceramic Al_32.4Er_7.6O₆₀ continuous fiber with a diameter of about 20 m could be made successfully by using the melt extraction method. This fiber shows large viscous flow deformation at the supercooled liquid state (about 1273 K). The fiber's tensile strength is about 900 MPa and this strength is maintained up to around 1100 K. A high-strength continuous ceramic fiber with a uniform Er₃Al₅O₁₂ nanocrystalline phase in an amorphous matrix can also be obtained with suitable crystallization from the amorphous state by heat treatment. The heat resistance, Young's modulus, and other properties are therefore improved. The nanocrystallized fiber which was heat-treated at 1373 K for 2 hours in an air atmosphere has a maximum room temperature tensile strength of 1.9 GPa, around twice that of an as-extracted amorphous fiber. The amorphous continuous ceramic fiber is promising as a ceramic that can be easily shaped at relatively low temperatures (about 1273 K), and as a reinforcing fiber for composites that can undergo secondary processing. Furthermore, this fiber can be considered as more superior to glass fibers because of its greater high-temperature strength and its high Young's modulus.