Fracture and toughening behavior of aramid fiber/epoxy composites

The effect of short Aramid fibers on the fracture and toughening behavior of epoxy with high glass transition temperature has been studied. Fine dispersion of the fibers throughout the matrix is evidenced by optical microscopy. Compared with neat epoxy resin, the fracture toughness (K_IC) of the composites steadily increases with increasing fiber loading, indicating that addition of Aramid fibers has an effective toughening effect to the intrinsically brittle epoxy matrix. Scanning electron microscopy (SEM) indicates that formation of numerous step structures for fiber‐filled epoxy systems is responsible for the significant toughness improvement. SEM and transmitted optical microscopy show that fiber pullout and fiber breakage are the main toughening mechanisms for the Aramid fiber/epoxy composites. POLYM. COMPOS. 26:333–342, 2005. © 2005 Society of Plastics Engineers.     

Effect of surface treatments on the thermal behavior and tensile strength of piassava (Attalea funifera) fibers

Piassava (Attalea funifera) fibers subjected to several surface chemical treatments and as‐received raw fibers were compared with respect to their thermal and tensile behaviors. The thermal degradation of the raw fibers was characterized by three main stages that corresponded to water release at low temperatures, decomposition of hemicellulose, and decomposition of α cellulose. Mercerization acted mainly on hemicellulose removal, and there was no change in the hydrophilic behavior of the fibers. The removal of hemicellulose split the fibers into microfibrils and favored the thermal decomposition of α cellulose. The same behavior was observed when the fibers were subjected to mercerization and acetylation. The fibers subjected to only acetylation showed thermal behavior similar to that of the raw fibers. With the acetylation treatment, a minor decrease in the hydrophilic character of the fibers was noted. Despite some differences in the thermal behavior, the tensile strengths of the raw and treated fibers were statistically equal. Complementary Fourier transform infrared and scanning electron microscopy analysis corroborated the thermogravimetric analysis/differential thermogravimetry results. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Modification of eucalyptus pulp fiber using silane coupling agents with aliphatic side chains of different length

The objective of this work was to evaluate the effect of three silane coupling agents with different aliphatic chain lengths on the hydrophobicity of eucalyptus pulp fiber. The three silanes coupling agents used (isobutyltrimethoxysilane, methyltrimethoxysilane, and n‐octyltriethoxysilane [OTES]) were each tested at three concentrations. Scanning electron microscopy coupled with energy dispersive spectroscopy revealed that the silane coupling agents markedly increased the Si content of the treated fibers. The Si distribution was not completely homogenous but was abundant in the treated samples. The treated fibers had higher contact angles for water and lower moisture adsorption than the control. Of the coupling agents tested, OTES treated fibers had the highest moisture resistance. This was likely due to the greater chain length of the aliphatic side group coupled to OTES. The use of silane coupling agents with alkyl side chains could improve the functional properties of pulp fiber and increase its compatibility with hydrophobic polymers. POLYM. ENG. SCI., 55:1273?1280, 2015. © 2015 Society of Plastics Engineers     

Effect of acetylation on the properties of microfibrillated cellulose‐LDPE composites

Solvent‐free acetylation of microfibrillated cellulose was carried out in order to improve their hydrophobicity. All the samples were filled with low‐density polyethylene. The morphology, mechanical properties, and water uptake of the ensuing composites were investigated. An excessive reaction time leads to degradation of the fibers, which was observed by scanning electron microscopy and fiber quality analysis. The acetylation treatment did not improve the mechanical properties of composites but extensively decreased the moisture absorption of the composites. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44933.     

Study on the effect of woven sisal fiber mat on mechanical and viscoelastic properties of petroleum based epoxy and bioresin modified toughened epoxy network

Sisal fiber reinforced biocomposites are developed using both unmodified petrol based epoxy and bioresin modified epoxy as base matrix. Two bioresins, epoxidized soybean oil and epoxy methyl soyate (EMS) are used to modify the epoxy matrix for effective toughening and subsequently two layers of sisal fiber mat are incorporated to improve the mechanical and thermomechanical properties. Higher strength and modulus of the EMS modified epoxy composites reveals good interfacial bonding of matrix with the fibers. Fracture toughness parameters K_IC and G_IC are determined and found to be enhanced significantly. Notched impact strength is found to be higher for unmodified epoxy composite, whereas elongation at break is found to be much higher for modified epoxy blend. Dynamic mechanical analysis shows an improvement in the storage modulus for bioresin toughened composites on the account stiffness imparted by fibers. Loss modulus is found to be higher for EMS modified epoxy composite because of strong fiber–matrix interfacial bonding. Loss tangent curves show a strong influence of bioresin on damping behavior of epoxy composite. Strong fiber–matrix interface is found in modified epoxy composite by scanning electron microscopic analysis. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42699.     

Improvement of adhesion of Kevlar fiber to epoxy by chemical modification

Kevlar 149 fibers were surface-modified by chlorosulfonation and subsequent reaction of -SO₂O with some reagents (e.g. glycine, water, ethylenediamine, and 2-butanol) to improve the adhesion to epoxy resin. The mechanical properties and surface topography of the modified fibers were investigated at different reaction times and reagent concentrations. The surface functional groups introduced into the surface of the fibers were identified by X-ray photoelectron spectroscopy (XPS) and static secondary ion mass spectroscopy (SIMS). The interfacial shear strength (IFSS) between the fibers and epoxy resin was measured by the microbond test. The results showed that the IFSS was markedly improved (by a factor of 2.25) by the chlorosulfonation/glycine treatment and that the fiber strength was not affected. Scanning electron microscopy (SEM) was also used to study the surface topography of fibers pulled from the epoxy resin. Furthermore, energy dispersive X-ray (EDX) spectroscopy was used to qualitatively examine the amount of sulfur in the fiber surfaces and in the fracture surfaces of fibers from microbond pull-out specimens. The results of EDX examination were consistent with a change of the fracture mode from the interface between the fiber and the epoxy resin to a location within the fiber and/or epoxy resin as observed by SEM.     

Enzyme‐mediated surface modification of jute and its influence on the properties of jute/epoxy composites

Surface modification of jute fibers is necessary to improve the adhesion and interfacial compatibility between fibers and resin matrix before using fibers in polymer composites. In this study, dodecyl gallate (DG) was enzymatically grafted onto the jute fiber by laccase to endow the fiber with hydrophobicity. A hand lay‐up technique was then adopted to prepare jute/epoxy composites. Contact angle and wetting time measurements showed that the surface hydrophobicity of the jute fabric was increased after the enzymatic graft modification. The water absorption and thickness swelling of the DG‐grafted jute fabric/epoxy composite were lower than those of the other composites. The tensile and dynamic mechanical properties of the jute/epoxy composites were enhanced by the surface modification. Scanning electron microscopy images revealed stronger fiber–matrix adhesion in composites with modified fibers. Therefore, the enzymatic graft modification increased the fiber–matrix interface area. The fiber–matrix adhesion was enhanced, and the mechanical properties of the composites were improved. POLYM. COMPOS., 38:1327–1334, 2017. © 2015 Society of Plastics Engineers     

Surface ammonification of the mutual‐irradiated aramid fibers in 1,4‐dichlorobutane for improving interfacial properties with epoxy resin

The mutual irradiated aramid fibers in 1,4‐dichlorobutane was ammoniated by ammonia/alcohol solution, in an attempt to improve the interfacial properties between aramid fibers and epoxy matrix. Scanning electron microscopy (SEM), X‐ray photoelectron spectroscopy (XPS), dynamic contact angle analysis (DCA), interfacial shear strength (IFSS), and single fiber tensile testing were carried out to investigate the functionalization process of aramid fibers and the interfacial properties of the composites. Experimental results showed that the fiber surface elements content changed obviously as well as the roughness through the radiation and chemical reaction. The surface energy and IFSS of aramid fibers increased distinctly after the ammonification, respectively. The amino groups generated by ammonification enhanced the interfacial adhesion of composites effectively by participating in the epoxy resin curing. Moreover, benefited by the appropriate radiation, the tensile strength of aramid fibers was not affected at all. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44924.     

Grafting of poly (methyl acrylate) onto sulfite pulp fibers and its effect on water absorbance

To prepare super water absorbent hydrogels of wood cellulose fibers, poly (methyl acrylate) (PMA) was copolymerized onto softwood sulfite pulp fibers using free radical initiator followed by alkaline hydrolysis. Ceric ammonium nitrate (CAN) was used as the free radical initiator. Effects of various parameters such as fiber concentration, monomer/pulp (M/pulp) ratio, CAN concentration, and reaction time on the grafting yield and on other grafting parameters were investigated. The graft conversion was the same from low to medium fiber concentration. The amount of initiator required was found to be independent of fiber concentration to achieve maximum grafting yield. Different fiber fractions (classified based on their length) have no effect on the grafting yield. The evidence of graft copolymerization was determined by using ATR‐IR spectroscopy. The X‐ray diffraction (XRD) analysis shows that grafting takes place both in amorphous and crystalline regions of cellulose fibers and the decrease in crystallinity of the grafted fibers with an increase in grafting yield was confirmed. The surface morphology of the PMA‐g‐cellulose was characterized by scanning electron microscopy (SEM). The water retention value of the hydrolyzed grafted pulp was determined based on a centrifugation technique. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Activating pulp toward acetylation by chemical or mechanical means

Activation of pulps during acetylation, by prior mechanical or chemical treatment, has been investigated. The effect of degree of beating on the acetylation rate of wood and bagasse pulps has been studied. It is found that the acetylation rate of pulps increases when the degree of beating of pulps is increased to a definite degree, after which it slows down. The maximum reactivity of bagasse pulp is obtained at 50°SR, while that of wood pulp is observed at 30°SR. The effect of grafting of acrylonitrile onto bagasse and wood pulps on their reactivity during acetylation has been also studied. The results indicate that grafting of acrylonitrile onto pulps has a favorable effect on their acetylation rate. This is dependent on the degree of grafting as well as the origin of pulp fibers. The most suitable method of activation during acetylation reaction is dependent on the origin of the pulp. The reactivity of bagasse pulp during acetylation is influenced more by beating of pulp, prior to the reaction, than by the grafting of acrylonitrile onto pulp. On the other hand, the acetylation reaction of wood pulp is activated by grafting rather than by beating. Also the effect of the activation process, mechanical or chemical, on the strength properties of the paper sheets produced from acetylated pulps has been investigated. Chemical activation of wood pulp prior to acetylation resulted in pulp with slightly higher strength properties than that activated by mechanical means. But, in the case of bagasse pulp, mechanical activation resulted in a pulp with strength superior to that produced by chemical activation.     

Unsaturated polyester‐toughened epoxy composites: Effect of sisal fiber on thermal and dynamic mechanical properties

In the present study, the mechanical and thermal properties of sisal fiber‐reinforced unsaturated polyester (UP)‐toughened epoxy composites were investigated. The sisal fibers were chemically treated with alkali (NaOH) and silane solutions in order to improve the interfacial interaction between fibers and matrix. The chemical composition of resins and fibers was identified by using Fourier‐transform infrared spectroscopy. The UP‐toughened epoxy blends were obtained by mixing UP (5, 10, and 15 wt%) into the epoxy resin. The fiber‐reinforced composites were prepared by incorporating sisal fibers (10, 20, and 30 wt%) within the optimized UP‐toughened epoxy blend. Scanning electron microscopy was used to analyze the morphological changes of the fibers and the adhesion between the fibers and the UP‐toughened epoxy system. The results showed that the tensile and flexural strength of (alkali‐silane)‐treated fiber (30 wt%) ‐reinforced composites increased by 83% and 55%, respectively, as compared with that of UP‐toughened epoxy blend. Moreover, thermogravimetric analysis revealed that the (alkali‐silane)‐treated fiber and its composite exhibited higher thermal stability than the untreated and alkali‐treated fiber systems. An increase in storage modulus and glass transition temperature was observed for the UP‐toughened epoxy matrix on reinforcement with treated fibers. The water uptake behavior of both alkali and alkali‐silane‐treated fiber‐reinforced composites is found to be less as compared with the untreated fiber‐reinforced composite. J. VINYL ADDIT. TECHNOL., 23:188–199, 2017. © 2015 Society of Plastics Engineers     

Concentration-dependent diffusion of dye in reactive dyeing systems

The cure of a tetrafunctional epoxy resin (largely tetraglycidyldiaminodiphenylmethane, TGDDM), cross-linked with diaminodiphenylsulphone (DDS) and boron trifluoride/ethylamine (BF₃EA) catalyst, is affected in a complex fashion by the presence of an oxidized carbon fiber surface. If the fiber is aged in a humid environment (25°C, 95% humidity) before coating with the matrix, the affinity of the oxidized fiber surface for water leads to destruction of the catalyst and retardation of the cure. This retardation is noticeable at lower humidities if the polymer content of the composite is reduced to > 20%. For oxidized fibers that are stored under ambient conditions (40% humidity), the retarding effect of water is overwhelmed by the catalytic effect of the acidic fiber surface. This activates the latent catalyst, increasing the rate of epoxy consumption and the proportion of the epoxy–epoxy reaction relative to the epoxy–amine reaction. For the low-humidity case, even though the rate of chemical reaction is increased, vitrification of the matrix is retarded, implying that there is less cross-linking and more extended epoxy–epoxy sequences in the network. The proposed chemical changes in epoxy/carbon fiber composites were confirmed by analysis of model reactions in solution. © 1992 John Wiley & Sons, Inc.     

Influence of pulp bleaching and compatibilizer selection on performance of pulp fiber reinforced PLA biocomposites

This article focuses on the effect of pulp bleaching and emerging commercial compatibilizers on physical performance of pulp fiber reinforced poly(lactic acid) (PLA) biocomposites. Industrially bleached and unbleached hardwood kraft pulp fibers are treated with several additive types, and compounded with PLA to fiber content of 30 wt %. After injection molding, the produced biocomposites are evaluated by their mechanical performance and fiber–matrix adhesion. For selected materials, fiber surface and fiber properties are reflected to composite performance by analyzing the compositions, dimensions, and lignin coverage of original fibers, as well as fiber dispersion and dimensions after melt processing. As a conclusion, unbleached kraft pulp fibers provide significant improvement in physical properties of PLA/pulp fiber composites. Of the screened compatibilizers, epoxidated linseed oil has a clear positive effect on performance when bleached kraft pulp fibers are used. The improvements correspond to enhanced fiber–matrix adhesion and differences in remaining fiber length distributions. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47955.     

Adhesive joints between carbon fiber and aluminum foam reinforced by surface‐treated aramid fibers

Short aramid fibers have been successfully used to reinforce the interface adhesive property between carbon fiber/epoxy composites and aluminum foam, and to form aramid‐fiber “composite adhesive joints.” In this study, to further improve the reinforcing effect of the aramid‐fiber‐reinforced adhesive joints, aramid fibers were ultrasonic treated to conduct different surface conditions. Critical energy release rate of the carbon fiber/aluminum foam sandwich beams with as‐received and treated interfacial aramid fibers were measured to study the influence of the surface treatment on aramid fibers. It was found that reinforcements in critical energy release rate were achieved for all samples with treated aramid fiber as measured under double cantilever beam condition. The interfacial characteristics of the short aramid fibers with different surface condition were investigated and discussed based on scanning electron microscopy observations. It is suggested that advanced bonding between aramid fibers and epoxy resin was conducted after surface treatment, and more energy was therefore absorbed through fiber bridging during crack opening and extension process. POLYM. COMPOS., 36:192–197, 2015. © 2014 Society of Plastics Engineers     

Effect of cloisite 30B clay and sisal fiber on dynamic mechanical and fracture behavior of unsaturated polyester toughened epoxy network

This study examined the dynamic mechanical properties of sisal fiber reinforced unsaturated polyester (UP) toughened epoxy nanocomposites. The chemical structures changes in Epoxy, UP and UP toughened epoxy (Epoxy/UP) systems were characterized by Proton Nuclear magnetic resonance (¹HNMR) spectroscopy. The morphological alterations of the nanocomposites were analyzed by X‐ray diffraction (XRD) and transmission electron microscopy (TEM). The untreated, chemically treated fibers, nanoclays, and the fiber reinforced Epoxy/UP nanocomposites were confirmed by FTIR spectrometer. The obtained mechanical results showed that alkali‐silane treated fibers improve the tensile strength (96%) and flexural strength (60%) of the Epoxy/UP nanocomposite than that of Epoxy/UP blend due to the strong interfacial bonding between the sisal fiber and matrix. The fracture toughness (K_IC) and fracture energy (G_IC) of treated sisal fiber reinforced DGEBA/UP/C30B nanocomposites found to be higher than that of untreated sisal fiber nanocomposites. The dynamic mechanical analysis (DMA) reveals that the fiber reinforced Epoxy/UP nanocomposites contains 30 wt% treated fiber and 1 wt% nanoclays, exhibits the highest storage modulus and better glass transition temperature (T_g) among the other kind of systems. The surface morphology of the fibers, fractured surface of the resins and composites were confirmed by scanning electron microscope (SEM). POLYM. COMPOS., 37:2832–2846, 2016. © 2015 Society of Plastics Engineers     

Nanoclay plating of cellulosic fiber surfaces

A basic problem in making cellulose‐reinforced composites is achieving a dispersion of cellulosic fibers in an often olephinic polymer matrix. Drying cellulosic fibers results in the formation of fiber flocs/nodules because of their strong interfiber bonding, and this makes the hydrophilic cellulosic fibers difficult to disperse in a hydrophobic matrix material. One common approach to alleviate floc formation is to adsorb cationic surfactant onto anionically charged cellulose, which reduces the interfiber bonding, decreases floc formation and gives better compatibility with the matrix. In this report, a different approach is taken, namely to adsorb nanoclays onto the cellulosic fibers, and thereby reduce the natural hydrogen‐bonding affinity between fibers. In a second report, the same technology will be shown to be advantageous to decrease floc formation in oleophinic composites reinforced with cellulosic fibers. This article summarizes experiments aimed at optimizing the chemistry of deposition of montmorillonite clay onto fiber surfaces. The aim was to optimize the chemical conditions for the heterodeposition of the anionic clay onto cationically charged fluff pulp. The experiments were designed to provide a theoretical framework for the deposition of the nanoclay onto the pulp fibers. High M_w p‐DADMAC and an exfoliated clay (achieved by passing the clay through a homogenizer) were used. As expected, a certain degree of charge overcompensation by adding an electrolyte was necessary to bring about deposition. The adsorbed amount of clay could be calculated from the charge balance between the overcompensated charge and the net clay charge, constituting the theoretical framework for nanoclay heterodeposition. As expected, montmorillonite clay greatly destroyed the joint strength between fibers (determined by evaluating the strength of paper made from treated fibers). The surface coverage (determined by ESCA) was shown to be a linear function of the attached amount of clay, and ～3% clay was required to fully cover the fiber surfaces. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Bleached extruder chemi‐mechanical pulp fiber‐PLA composites: Comparison of mechanical,thermal, and rheological properties with those of wood flour‐PLA bio‐composites

An environmentally friendly bleached extruder chemi‐mechanical pulp fiber or wood flour was melt compounded with poly(lactic acid) (PLA) into a biocomposite and hot compression molded. The mechanical, thermal, and rheological properties were determined. The chemical composition, scanning electron microscopy, and Fourier transform infrared spectroscopy results showed that the hemicellulose in the pulp fiber raw material was almost completely removed after the pulp treatment. The mechanical tests indicated that the pulp fiber increased the tensile and flexural moduli and decreased the tensile, flexural, and impact strengths of the biocomposites. However, pulp fiber strongly reinforced the PLA matrix because the mechanical properties of pulp fiber‐PLA composites (especially the tensile and flexural strengths) were better than those of wood flour‐PLA composites. Differential scanning calorimetry analysis confirmed that both pulp fiber and wood flour accelerated the cold crystallization rate and increased the degree of crystallinity of PLA, and that this effect was greater with 40% pulp fiber. The addition of pulp fiber and wood flour modified the rheological behavior because the composite viscosity increased in the presence of fibers and decreased as the test frequency increased. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 44241.     

Influence of new thermoplastic sizing agents on the mechanical behavior of poly(ether ketone ketone)/carbon fiber composites

In this study, unidirectional poly(ether ether ketone)/carbon fiber (CF) composite sheets were elaborated with unsized, epoxy‐sized, and thermoplastic‐sized CFs by hot‐press molding. The thermoplastic sizings that we used were poly(ether imide) (PEI) and poly(ether ketone ketone) oligomer aqueous dispersions. Scanning electron microscopy observation of the composites freeze fractures showed that unlike unsized or epoxy‐sized CFs, the thermoplastic sizings improved the interaction between the fibers and the matrix. A comparative study of the mechanical relaxations by dynamic mechanical analysis was carried out on the different composites before and after immersion in kerosene. At low temperature, the PEI sizing had a significant influence on the β relaxation, particularly after kerosene immersion. The thermoplastic sizings did not modify the glass‐transition temperature but improved the kerosene resistance on the composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42550.     

Studies on thermal degradation and flame retardant behavior of the sisal fiber reinforced unsaturated polyester toughened epoxy nanocomposites

Unsaturated polyester (UP) toughened nanocomposites were prepared using both sisal fibers and montmorillonite clays. The effect of fibers and Cloisite 30B (C30B) nanoclays on the mechanical properties, thermal stability, flame retardant, and morphological behavior of the UP toughened epoxy (Epoxy/UP) were systematically studied. The chemical structures of Epoxy, UP, and Epoxy/UP systems were characterized using Proton Nuclear magnetic resonance (¹HNMR) and Fourier transform infrared (FTIR) spectra. The homogeneous dispersion of nanoclay within the polymer matrix was analyzed using transmission electron microscopy (TEM) and X‐ray diffraction (XRD) analysis. Incorporation of sisal fibers and C30B nanoclays within Epoxy/UP system resulted in an increase in the mechanical, thermal, and flame retardance properties. Thermogravimetric analysis (TGA) has been employed to evaluate the thermal degradation kinetic parameters of the composites using Kissinger and Flynn‐Wall‐Ozawa methods. Cone calorimeter, UL‐94, and LOI tests revealed a reduction in the burning rate of the matrix with the addition of fibers and nanoclays. The results showed that the treated fiber reinforced nanocomposites had higher thermal stability and better flame retardant properties than the treated fiber reinforced composites. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42068.