Sisal chemically modified with lignins: Correlation between fibers and phenolic composites properties

Sisal fibers have been chemically modified by reaction with lignins, extracted from sugarcane bagasse and Pinus-type wood and then hydroxymethylated, to increase adhesion in resol-type phenolic thermoset matrices. Inverse gas chromatography (IGC) results showed that acidic sites predominate for unmodified/modified sisal fibers and for phenolic thermoset, indicating that the phenolic matrix has properties that favor the interaction with sisal fibers. The IGC results also showed that the phenolic thermoset has a dispersive component closer to those of the modified fibers suggesting that thermoset interactions with the less polar modified fibers are favored. Surface SEM images of the modified fibers showed that the fiber bundle deaggregation increased after the treatment, making the interfibrillar structure less dense in comparison with that of unmodified fibers, which increased the contact area and encouraged microbial biodegradation in simulated soil. Water diffusion was observed to be faster for composites reinforced with modified fibers, since the phenolic resin penetrated better into modified fibers, thereby blocking water passage through their channels. Overall, composites` properties showed that modified fibers promote a significant reduction in the hydrophilic character, and consequently of the reinforced composite without a major effect on impact strength and with increased storage modulus. (c) 2008 Elsevier Ltd. All rights reserved.

Soda-Treated Sisal/Polypropylene Composites

Treated sisal fibers were used as reinforcement of polypropylene (PP) composites, with maleic anhydride-grafted PP (MAPP) as coupling agent. The composites were made by melting processing of PP with the fiber in a heated roller followed by multiple extrusions in a single-screw extruder. Injection molded specimens were produced for the characterization of the material. In order to improve the adhesion between fiber and matrix and to eliminate odorous substances, sisal fibers were treated with boiling water and with NaOH solutions at 3 and 10 wt.%. The mechanical properties of the composites were assessed by tensile, bend and impact tests. Additionally, the morphology of the composites and the adhesion at he fiber-matrix interface were analyzed by SEM. The fiber treatment led to very light and odorless materials, with yields of 95, 74 and 62 wt.% for treatments with hot water, 3 and 10 wt.% soda solution respectively. Fiber treatment caused an appreciable change in fiber characteristics, yet the mechanical properties under tensile and flexural tests were not influenced by that treatment. Only the impact strength increased in the composites with alkali-treated sisal fibers.

Phenolic matrices and sisal fibers modified with hydroxy terminated polybutadiene rubber: Impact strength, water absorption, and morphological aspects of thermosets and composites

The aim of the present work was to investigate the toughening of phenolic thermoset and its composites reinforced with sisal fibers, using hydroxyl-terminated polybutadiene rubber (HTPB) as both impact modifier and coupling agent. Substantial increase in the impact strength of the thermoset was achieved by the addition 10% of HTPB. Scanning electron microscopy (SEM) images of the material with 15% HTPB content revealed the formation of some rubber aggregates that reduced the efficiency of the toughening mechanism. In composites, the toughening effect was observed only when 2.5% of HTPB was added. The rubber aggregates were found located mainly at the matrix-fiber interface suggesting that HTPB could be used as coupling agent between the sisal fibers and the phenolic matrix. A composite reinforced with sisal fibers pre-impregnated with HTPB was then prepared; its SEM images showed the formation of a thin coating of HTPB on the surface of the fibers. The ability of HTBP as coupling agent between sisal fibers and phenolic matrix was then investigated by preparing a composite reinforced with sisal fibers pre-treated with HTPB. As revealed by its SEM images, the HTPB pre-treatment of the fibers resulted on the formation of a thin coating of HTPB on the surface of the fibers, which provided better compatibility between the fibers and the matrix at their interface, resulting in a material with low water absorption capacity and no loss of impact strength. (C) 2009 Elsevier B.V. All rights reserved.

Thermoset matrix reinforced with sisal fibers: Effect of the cure cycle on the properties of the biobased composite

Thermoset phenolic composites reinforced with sisal fibers were prepared to optimize the cure step. In the present study, processing parameters such as pressure, temperature, and time interval were varied to control the vaporization of the water generated as a byproduct during the crosslinking reaction. These molecules can vaporize forming voids, which in turn affect the final material properties. The set of results on impact strength revealed that the application of higher pressure before the gel point of the phenolic matrix produced composites with better properties. The SEM images showed that the cure cycle corresponding to the application of higher values of molding pressure at the gel point of the phenolic resin led to the reduction of voids in the matrix. In addition, the increase in the molding pressure during the cure step increased the resin interdiffusion. Better filling of the fiber channels decreased the possibility of water molecules diffusing through the internal spaces of the fibers. These molecules then diffused mainly through the bulk of the thermoset matrix, which led to a decrease in the water diffusion coefficient (D) at all three temperatures (25, 55 and 70 degrees C) considered in the experiments. (C) 2009 Elsevier Ltd. All rights reserved.

Cassava bagasse cellulose nanofibrils reinforced thermoplastic cassava starch

Cellulose cassava bagasse nanofibrils (CBN) were directly extracted from a by-product of the cassava starch (CS) industry, viz. the cassava bagasse (CB), The morphological structure of the ensuing nanoparticles was investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), presence of other components such as sugars by high performance liquid chromatography (HPLC), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) experiments. The resulting nanofibrils display a relatively low crystallinity and were found to be around 2-11 nm thick and 360-1700 nm long. These nanofibrils were used as reinforcing nanoparticles in a thermoplastic cassava starch matrix plasticized using either glycerol or a mixture of glycerol/sorbitol (1:1) as plasticizer. Nanocomposite films were prepared by a melting process. The reinforcing effect of the filler evaluated by dynamical mechanical tests (DMA) and tensile tests was found to depend on the nature of the plasticizer employed. Thus, for the glycerol-plasticized matrix-based composites, it was limited especially due to additional plasticization by sugars originating from starch hydrolysis during the acid extraction. This effect was evidenced by the reduction of glass vitreous temperature of starch after the incorporation of nanofibrils in TPSG and by the increase of elongation at break in tensile test. On the other hand, for glycerol/sorbitol plasticized nanocomposites the transcrystallization of amylopectin in nanofibrils surface hindered good performances of CBN as reinforcing agent for thermoplastic cassava starch. The incorporation of cassava bagasse cellulose nanofibrils in the thermoplastic starch matrices has resulted in a decrease of its hydrophilic character especially for glycerol plasticized sample. (C) 2009 Elsevier Ltd. All rights reserved.

Extrusion and characterization of functionalized cellulose whiskers reinforced polyethylene nanocomposites

The surface of ramie cellulose whiskers has been chemically modified by grafting organic acid chlorides presenting different lengths of the aliphatic chain by an esterification reaction. The occurrence of the chemical modification was evaluated by FTIR and X-ray photoelectron spectroscopies, elemental analysis and contact angle measurements. The crystallinity of the particles was not altered by the chain grafting, but it was shown that covalently grafted chains were able to crystallize at the cellulose surface when using C18. Both unmodified and functionalized nanoparticles were extruded with low density polyethylene to prepare nanocomposite materials. The homogeneity of the ensuing nanocomposites was found to increase with the length of the grafted chains. The thermomechanical properties of processed nanocomposites were studied by differential scanning calorimetry (DSC), dynamical mechanical analysis (DMA) and tensile tests. A significant improvement in terms of elongation at break was observed when sufficiently long chains were grafted on the surface of the nanoparticles. It was ascribed to improved dispersion of the nanoparticles within the LDPE matrix. (C) 2009 Elsevier Ltd. All rights reserved.

Effect of the manufacturing process on the interlaminar fracture toughness of 2/2 twill weave fabric carbon/epoxy composites

A 2/2 twill weave fabric carbon fibre reinforced epoxy matrix composite MTM56/CF0300 was used to investigate the effect of different manufacturing processes on the interlaminar fracture toughness. Double cantilever beam tests were performed on composites manufactured by hot press, autoclave and 'Quickstep' processes. The 'Quickstep' process was recently developed in Perth, Western Australia for the manufacture of advanced composite components. The values of the mode I critical strain energy release rate (G1d were compared and the results showed that the composite specimens manufactured by the autoclave and the 'Quickstep' process had much higher interlaminar fracture toughness than the specimen produced by the hot press. When compared to specimens manufactured by the hot press, the interlaminar fracture toughness values of the Quickstep and autoclave samples were 38% and 49% higher respectively. The 'Quickstep' process produced composite specimens that had comparable interlaminar fracture toughness to autoclave manufactured composites. Scanning electron microscopy (SEM) was employed to study the topography of the mode I interlaminar fracture surface and dynamic mechanical analysis (DMA) was performed to investigate the fibre/matrix interphase. SEM micrography and DMA spectra indicated that autoclave and 'Quickstep' produced composites with stronger fibre/matrix adhesion than hot press.

Investigation of effective material properties in composites with internal defect or reinforcement particles

This paper is concerned with the investigation of the effective material properties of internally defective or particle-reinforced composites. An analysis was carried out with a novel method using the two-dimensional special finite element method mixing the concept of equivalent homogeneous materials. A formulation has been developed for a series of special finite elements containing an internal defect or reinforcement in order to assure the high accuracy especially in the vicinity of defects or reinforcements. The adoption of the special finite element can greatly simplify numerical modeling of particle-composites. The numerical result provides the effective material properties of particle-reinforced composite and explains that the size of particles has great influence on the material properties. Numerical examples also demonstrate the validity and versatility of the proposed method by comparing with existing results from literatures.

Equal channel angular pressing of metal matrix composites: effect on particle distribution and fracture toughness

An Al6061-20%Al₂O₃ powder metallurgy (PM) metal matrix composite (MMC) with a strongly clustered particle distribution is subjected to equal channel angular pressing (ECAP) at a temperature of 370 °C. The evolution of the homogeneity of the particle distribution in the material during ECAP is investigated by the quadrat method. The model proposed by Tan and Zhang [Mater Sci Eng 1998;244:80] for estimating the critical particle size which is required for a homogeneous particle distribution in PM MMCs is extended to the case of a combination of extrusion and ECAP. The applicability of the model to predict a homogeneity of the particle distribution after extrusion and ECAP is discussed. It is shown that ECAP leads to an increase of the  uniformity of the particle distribution and the fracture toughness.

Influence of helium atmospheric plasma treatment on surface and fracture-mechanical behaviour of quickstepTM cured bio-composites

This work investigated the potential of improving flexural properties of natural fiber (jute) reinforced biocomposites by atmospheric pressure helium plasma treatment. Composites were made by the use of combined hand lay-up and vacuum bagging technique followed by newly developed Australia patented Quickstep^TM curing. The physical properties of helium plasma modified fibers were investigated by means of wettability time, coefficient of friction (COF), atomic force microscopy (AFM) and chemical nature of the surface with ATR-FTIR and XPS. There was found a logical correlation between physical and chemical characteristics of the surface of fiber with the fracture mechanical behavior of their resulting biocomposites. In addition, the use of helium atmospheric plasma treatment prior to Quickstep^TM process has proved to be a potential way to positively alter the fracture-mechanical behavior of biocomposites. This study will lead to new commercial applications of natural fiber jute for the composite industry that go beyond wrapping and packaging.

Tensile behaviour of non-uniform fibres and fibrous composites

This work investigates the tensile behaviour of non-uniform fibres and fibrous composites. Wool fibres are used as an example of non-uniform fibres because they're physical, morphological and geometrical properties vary greatly not only between fibres but also within a fibre. The focus of this work is on the effect of both between-fibre and within-fibre diameter variations on fibre tensile behaviour. In addition, fit to the Weibull distribution by the non-brittle and non-uniform visco-elastic wool fibres is examined, and the Weibull model is developed further for non-uniform fibres with diameter variation along the fibre length. A novel model fibre composite is introduced to facilitate the investigation into the tensile behaviour of fibre-reinforced composites. This work first confirms that for processed wool, its coefficient of variation in break force can be predicted from that of minimum fibre diameters, and the prediction is better for longer fibres. This implies that even for processed wool, fibre breakage is closely associated with the occurrence of thin sections along a fibre, and damage to fibres during processing is not the main cause of fibre breakage. The effect of along-fibre diameter variation on fibre tensile behaviour of scoured wool and mohair is examined next. Only wet wool samples were examined in the past. The extensions of individual segments of single non-uniform fibres are measured at different strain levels. An important finding is the maximum extension (%) (Normally at the thinnest section) equals the average fibre extension (%) plus the diameter variation (CV %) among the fibre segments. This relationship has not been reported before. During a tensile test, it is only the average fibre extension that is measured. The third part of this work is on the applicability of Weibull distribution to the strength of non-uniform visco-elastic wool fibres. Little work has been done for wool fibres in this area, even though the Weibull model has been widely applied to many brittle fibres. An improved Weibull model incorporating within-fibre diameter variations has been developed for non-uniform fibres. This model predicts the gauge length effect more accurately than the conventional Weibull model. In studies of fibre-reinforced composites, ideal composite specimens are usually prepared and used in the experiments. Sample preparation has been a tedious process. A novel fibre reinforced composite is developed and used in this work to investigate the tensile behaviour of fibre-reinforced composites. The results obtained from the novel composite specimen are consistent with that obtained from the normal specimens.

Microstructural development in Al/MgAl2O4 in situ metal matrix composite using value-added silica sources

Al/MgAl2O4 in situ metal matrix composites have been synthesized using value-added silica sources (microsilica and rice husk ash) containing ~97% SiO2 in Al-5 wt.% Mg alloy. The thermodynamics and kinetics of MgAl2O4 formation are discussed in detail. The MgO and MgAl2O4 phases were found to dominate in microsilica (MS) and rice husk ash (RHA) value-added composites, respectively, during the initial stage of holding the composites at 750 °C. A transition phase between MgO and MgAl2O4 was detected by the scanning electron microscopy and energy-dispersive spectroscopy (SEM–EDS) analysis of the particles extracted from the composite using 25% NaOH solution. This confirms that MgO is gradually transformed to MgAl2O4 by the reaction 3SiO2(s)+2MgO(s)+4Al(l)→2MgAl2O4(s)+3Si(l). The stoichiometry of MgAl2O4, n, computed by a new methodology is between 0.79 and 1.18. The reaction between the silica sources and the molten metal stopped after 55% of the silica source was consumed. A gradual increase in mean MgAl2O4 crystallite size, D, from 24 to 36 nm was observed in the samples held for 10 h.

A study on the thermodynamics of in situ MgAl2O4/Al MMC formation using amorphous silica sources

MgAl₂O₄ (spinel) is considered as a commercially important ceramic reinforcement in MMC fabrication because of the possible tailorable properties imparted with Al for many applications. Generally, any oxygen source, i.e., the dissolved oxygen, or pure oxygen atmosphere or atmospheric oxygen is sufficient for the formation of MgAl₂O₄ in Al–Mg alloy. Among all the reactive oxygen sources, the reactivity of SiO₂ with Al alloy is found to be higher. Amorphous silica is highly reactive in nature compared to crystalline silica. The present study has examined the thermodynamics of MgAl₂O₄ formation in Al–Mg alloy by amorphous silica sources with the aid of differential thermal analyzer (DTA) and the simulated experiments. The dissolution of Si and the formation of MgAl₂O₄ are detected as the endothermic peak and the immediate exothermic peak respectively in DTA curves and the presence of MgAl₂O₄ is confirmed by the XRD of the simulated sample. The MgO formed due to the oxidation of Mg in Al–Mg alloy has been found to influence the MgAl₂O₄ formation.

Synthesis of an Al/MgAl2O4 in situ metal matrix composite from silica gel

An aluminum/MgAl2O4 in situ metal matrix composite has been synthesized using silica gel containing B98% SiO2 in an Al–5Mg alloy. The thermodynamics and kinetics of MgAl2O4 formation have been discussed in detail. A transition phase of composition between MgO and MgAl2O4 has been detected in the SEM-EDS analysis of the particles extracted from the composite by a 25% NaOH solution. This confirms the gradual transformation of MgO to MgAl2O4 by the reaction 3SiO2(s)12MgO(s)14Al(l)-2MgAl2O4(s)13Si(l). The stoichiometry, n, of MgAl2O4 has been found to sustain close to 1 and the crystallite growth of MgAl2O4 has been stopped at DB30 nm in the composites held at 7501C up to 10 h.

Thermodynamics and kinetics of the formation of Al2 O3/ MgAl2O4/MgO in Al-Silica metal matrix composite

The formation of Al₂O₃, MgAl₂O₄, and MgO has been widely studied in different Al base metal matrix composites, but the studies on thermodynamic aspects of the Al₂O₃/ MgAl₂O₄/MgO phase equilibria have been limited to few systems such as Al/Al₂O₃ and Al/SiC. The present study analyzes the Al₂O₃/MgAl₂O₄ and MgAl₂O₄/MgO equilibria with respect to the temperature and the Mg content in Al/SiO2 system using an extended Miedema model. There is a linear and parabolic variation in Mg with respect to the temperature for MgAl₂O₄/MgO and Al₂O₃/MgAl₂O₄ equilibria, respectively, and the influence of Si and Cu in the two equilibria is not appreciable. The experimental verification has been limited to MgAl₂O₄/MgO equilibria due to the high Mg content (≥0.5 wt pct) required for composite processing. The study has been carried out on two varieties of Al/SiO₂ composites, i.e., Al/Silica gel and Al/Micro silica processed by liquid metallurgy route (stir casting route). MgO is found to be more stable compared to MgAl₂O₄ at Mg levels ≥5 and 1 wt pct in Al/Silica gel and Al/Micro silica composites, respectively, at 1073 K. MgO is also found to be more stable at lower Mg content (3 wt pct) in Al/Silica gel composite with decreasing particle size of silica gel from 180 micron to submicron and nanolevels. The MgO to MgAl₂O₄ transformation has taken place through a series of transition phases influenced by the different thermodynamic and kinetic parameters such as holding temperature, Mg concentration in the alloy, holding time, and silica particle size.