In an effort to present more ‘green’ material for massive manufacturing that are both competitive in their properties and can be more environmental friendly, natural fibers are being considered for possible applications in the automotive industry. This paper shows an exploratory study of the effects of pressure and layup on a hybrid composite of randomly oriented woven kenaf fibers and fiberglass/polyester sheet molding compound (SMC). In addition to initial testing performed on their water absorption and other important properties, these hybrid composites were tested to determine the bending modulus of elasticity (MOE) and the bending modulus of rupture (MOR) as well as the tensile modulus of elasticity (MOE), ultimate tensile strength. Pictures are taken from a Spectral Electron Microscope to determine if the fiber mats were properly penetrated by the resin and if the structural integrity of the fibers was maintained during manufacture.

The use of wheat straw and other agricultural by-product fibers in polymer composite materials offers many economical and environmental benefits. Wheat straw has been recently commercialized as new filler for polypropylene thermoplastic composites in automotive applications. However, to expand its application in the automotive industry and other sectors where highly-engineered materials are needed, a systematic database and reliable composite property models are needed. For this purpose, this research was systematically conducted. A product design approach is used in studying wheat straw polypropylene (WS-PP) composite. A set of thermoplastic composite specifications relevant to several automotive parts was used as a basis for the customer needs which give the direction to the entire product design of thermoplastic composites based on polypropylene and straw. Straw fibers were produced by grinding and sieving (without any other treatment). These fibers were used in the formulation of polypropylene thermoplastic composites to understand the variable that can contribute to minimize production cost, maximize product performance and maximize wheat straw utilization (fraction of renewable material). The variation in chemical composition due to plant variety (parts of the plant, location of harvesting and seasonality), the bonding incompatibility between hydrophobic polypropylene matrix and hydrophilic straw fiber, along with the heterogeneity of fiber size and shape, has made wheat straw polypropylene composite a complex system. This complexity causes the mechanistic approach of composite modeling in the well-established composite theory difficult to be applied, since modeling the contribution of natural fibers to the performance of thermoplastic composites is not as straightforward like in the case of homogenous glass fiber (with same shape, diameter and narrow length distribution). Alternatively, a statistical approach of modeling by using designed experiments was used in this research. The Mixture and Process-Mixture Experimental Design methodologies were applied to develop response surface models that can be used to correlate input properties and formulation of these thermoplastic composites to the final properties of the product. The models obtained can then be inverted to predict the required properties and formulations using fiber (straw), matrix (polypropylene), and additives (coupling agent) as the main components for a specified product performance. The prediction includes the fiber grading (size and aspect ratio) and classification in order to maximize fiber utilization for different needs of composite products. The experiments were designed based on the analysis of the existing data provided by previous research works of wheat straw polypropylene composite system in our laboratory and by experimental data generated during this research. The focus of the analysis was the determination of the factor(s), i.e., the independent variables of the experiments and their acceptable levels. The response variables being measured were chosen based on the required specifications of targeted products. A constrained three-component mixture design of experiment was conducted to develop models for flexural properties of WS-PP composite. The three independent mixture variables in this experiment were the weight proportions of: straw (as fiber), polypropylene (as matrix), and maleic anhydride polypropylene (as coupling agent). Statistical analysis results showed that the obtained models have met standard requirements of response surface models with good predictive capability. One of the important finding of this study was the formulation for optimum coupling agent proportion which gives the best flexural properties of composite. The effect of straw fiber size on composite properties was investigated by using fiber length and aspect ratio as parameters to describe fiber size, instead of the size of sieves used in fiber preparation. Two-stage separation method was applied in the straw fiber preparation process. In this method, width-based separation was followed by length-based separation to obtain fiber fractions with distinct fiber length and aspect ratio. Samples of thermoplastic composites for measurement of physical properties were produced from each fiber factions at two different levels of fiber loading. The samples were compounded by twin-screw extrusion and specimens were prepared by injection molding. The fibers were then extracted from the samples after injection molding (using solvent) and their sizes were measured to investigate the fiber size reduction during the compounding and molding process. A comprehensive analysis was then performed to study the responses of stiffness, impact resistance and specific properties of these composites by including initial fiber sizes, fiber chemical compositions (measured as cellulose, hemi-cellulose and lignin), fiber size reduction during compounding/molding process, and fiber loading as factors. One of the important contributions of this study is fiber grading in terms of their sizes and their respective contributions to the final composite product properties. Based on the previous results, a mixture design of experiment was performed on wheat straw – polypropylene / impact copolymer polypropylene (WS-PP/ICP) composite system. The objective of the experiment was to obtain response surface models that can be used to estimate some important properties required by a set of automotive product specifications. The optimum formulation of coupling agent obtained in the previous study was used to determine the fixed recipe of coupling agent; simplifying the composite system into a three-component mixture, i.e. straw (as fiber) and polypropylene (homopolymer and impact copolymer (polypropylene blend as matrix). Simulation of the models shows the superiority of using a blend of polypropylenes to balance the stiffness and impact strength of the composites and being able to reach three targeted product specifications. A case study was also performed to demonstrate that the models can be used to find optimum formulations to minimize material cost while meeting specifications of all targeted products. Finally, a framework for wheat straw polypropylene product design and development is presented in this thesis. The framework can be used for designing polypropylene-straw thermoplastic composites with various combinations of fiber - polymer matrix - additive systems with different product attributes and specifications suitable for several applications in the automotive industry.

Natural fibers, such as hemp and flax, are emerging as cheaper reinforcing fibers for polymer composites. Renew-ability, comparable specific properties, and biodegradability make natural fibers more attractive than glass fibers. Vacuum Assisted Resin Transfer Molding (VARTM) is widely used to manufacture medium-to-large sized composites. The non-woven mats used in VARTM must meet manufacturing (permeability) and structural (volume fraction (Vf), thickness, fiber orientation, properties) requirements. Unlike glass mats, natural fiber mats are not available commercially. Design and development of natural fiber mats require knowledge on the relationship among manufacturing, structure and properties of these mats and their composites. Developing this knowledge is the objective of this thesis. Effect of needle punch density on hemp fiber mat structure (areal density, Vf, fiber orientation distribution (FOD), thickness, permeability) was systematically studied. The FOD was characterized non-destructively using X-ray tomography. The Effect of consolidation pressure during composite manufacturing on its structure (Vf, thickness, FOD) was studied. The modulus and strength of needle-punched hemp mat – thermoset polyester composites, manufactured using VARTM and compression molding, were measured. A predictive model for these properties and a modeling approach for the evolution of FOD and thickness during mat manufacturing were developed and validated. The results of these studies were used to understand the relationship. The modulus and the strength of the composites were significantly influenced by the Vf and the FOD, the evolution of which during composite manufacturing depended on the consolidation pressure and the mat structure. The latter depended on mat manufacturing parameters, namely the punch density used to bind the fibers together and the areal density of the web of fibers formed during air laying, and the FOD in the web. The permeability of the mat decreased with increasing the punch density and was found to be a function of both the Vf and the FOD. Despite this, the manufacturing of composite was not adversely affected, and the tensile modulus increased with punch density. The mat composite was modeled as an equivalent laminate, whose lay-up was determined using its FOD. The properties of equivalent laminate that was predicted using lamination theory compared well with the experimental results.

Natural fibers, such as hemp and flax, are emerging as cheaper reinforcing fibers for polymer composites. Renew-ability, comparable specific properties, and biodegradability make natural fibers more attractive than glass fibers. Vacuum Assisted Resin Transfer Molding (VARTM) is widely used to manufacture medium-to-large sized composites. The non-woven mats used in VARTM must meet manufacturing (permeability) and structural (volume fraction (Vf), thickness, fiber orientation, properties) requirements. Unlike glass mats, natural fiber mats are not available commercially. Design and development of natural fiber mats require knowledge on the relationship among manufacturing, structure and properties of these mats and their composites. Developing this knowledge is the objective of this thesis. Effect of needle punch density on hemp fiber mat structure (areal density, Vf, fiber orientation distribution (FOD), thickness, permeability) was systematically studied. The FOD was characterized non-destructively using X-ray tomography. The Effect of consolidation pressure during composite manufacturing on its structure (Vf, thickness, FOD) was studied. The modulus and strength of needle-punched hemp mat – thermoset polyester composites, manufactured using VARTM and compression molding, were measured. A predictive model for these properties and a modeling approach for the evolution of FOD and thickness during mat manufacturing were developed and validated. The results of these studies were used to understand the relationship. The modulus and the strength of the composites were significantly influenced by the Vf and the FOD, the evolution of which during composite manufacturing depended on the consolidation pressure and the mat structure. The latter depended on mat manufacturing parameters, namely the punch density used to bind the fibers together and the areal density of the web of fibers formed during air laying, and the FOD in the web. The permeability of the mat decreased with increasing the punch density and was found to be a function of both the Vf and the FOD. Despite this, the manufacturing of composite was not adversely affected, and the tensile modulus increased with punch density. The mat composite was modeled as an equivalent laminate, whose lay-up was determined using its FOD. The properties of equivalent laminate that was predicted using lamination theory compared well with the experimental results.

The use of wheat straw and other agricultural by-product fibers in polymer composite materials offers many economical and environmental benefits. Wheat straw has been recently commercialized as new filler for polypropylene thermoplastic composites in automotive applications. However, to expand its application in the automotive industry and other sectors where highly-engineered materials are needed, a systematic database and reliable composite property models are needed. For this purpose, this research was systematically conducted. A product design approach is used in studying wheat straw polypropylene (WS-PP) composite. A set of thermoplastic composite specifications relevant to several automotive parts was used as a basis for the customer needs which give the direction to the entire product design of thermoplastic composites based on polypropylene and straw. Straw fibers were produced by grinding and sieving (without any other treatment). These fibers were used in the formulation of polypropylene thermoplastic composites to understand the variable that can contribute to minimize production cost, maximize product performance and maximize wheat straw utilization (fraction of renewable material). The variation in chemical composition due to plant variety (parts of the plant, location of harvesting and seasonality), the bonding incompatibility between hydrophobic polypropylene matrix and hydrophilic straw fiber, along with the heterogeneity of fiber size and shape, has made wheat straw polypropylene composite a complex system. This complexity causes the mechanistic approach of composite modeling in the well-established composite theory difficult to be applied, since modeling the contribution of natural fibers to the performance of thermoplastic composites is not as straightforward like in the case of homogenous glass fiber (with same shape, diameter and narrow length distribution). Alternatively, a statistical approach of modeling by using designed experiments was used in this research. The Mixture and Process-Mixture Experimental Design methodologies were applied to develop response surface models that can be used to correlate input properties and formulation of these thermoplastic composites to the final properties of the product. The models obtained can then be inverted to predict the required properties and formulations using fiber (straw), matrix (polypropylene), and additives (coupling agent) as the main components for a specified product performance. The prediction includes the fiber grading (size and aspect ratio) and classification in order to maximize fiber utilization for different needs of composite products. The experiments were designed based on the analysis of the existing data provided by previous research works of wheat straw polypropylene composite system in our laboratory and by experimental data generated during this research. The focus of the analysis was the determination of the factor(s), i.e., the independent variables of the experiments and their acceptable levels. The response variables being measured were chosen based on the required specifications of targeted products. A constrained three-component mixture design of experiment was conducted to develop models for flexural properties of WS-PP composite. The three independent mixture variables in this experiment were the weight proportions of: straw (as fiber), polypropylene (as matrix), and maleic anhydride polypropylene (as coupling agent). Statistical analysis results showed that the obtained models have met standard requirements of response surface models with good predictive capability. One of the important finding of this study was the formulation for optimum coupling agent proportion which gives the best flexural properties of composite. The effect of straw fiber size on composite properties was investigated by using fiber length and aspect ratio as parameters to describe fiber size, instead of the size of sieves used in fiber preparation. Two-stage separation method was applied in the straw fiber preparation process. In this method, width-based separation was followed by length-based separation to obtain fiber fractions with distinct fiber length and aspect ratio. Samples of thermoplastic composites for measurement of physical properties were produced from each fiber factions at two different levels of fiber loading. The samples were compounded by twin-screw extrusion and specimens were prepared by injection molding. The fibers were then extracted from the samples after injection molding (using solvent) and their sizes were measured to investigate the fiber size reduction during the compounding and molding process. A comprehensive analysis was then performed to study the responses of stiffness, impact resistance and specific properties of these composites by including initial fiber sizes, fiber chemical compositions (measured as cellulose, hemi-cellulose and lignin), fiber size reduction during compounding/molding process, and fiber loading as factors. One of the important contributions of this study is fiber grading in terms of their sizes and their respective contributions to the final composite product properties. Based on the previous results, a mixture design of experiment was performed on wheat straw – polypropylene / impact copolymer polypropylene (WS-PP/ICP) composite system. The objective of the experiment was to obtain response surface models that can be used to estimate some important properties required by a set of automotive product specifications. The optimum formulation of coupling agent obtained in the previous study was used to determine the fixed recipe of coupling agent; simplifying the composite system into a three-component mixture, i.e. straw (as fiber) and polypropylene (homopolymer and impact copolymer (polypropylene blend as matrix). Simulation of the models shows the superiority of using a blend of polypropylenes to balance the stiffness and impact strength of the composites and being able to reach three targeted product specifications. A case study was also performed to demonstrate that the models can be used to find optimum formulations to minimize material cost while meeting specifications of all targeted products. Finally, a framework for wheat straw polypropylene product design and development is presented in this thesis. The framework can be used for designing polypropylene-straw thermoplastic composites with various combinations of fiber - polymer matrix - additive systems with different product attributes and specifications suitable for several applications in the automotive industry.

abstract: This study investigates the fabrication and mechanical properties of semicontinuous, hemp fiber reinforced thermoset composites. This research determines if off-the-shelf refined woven hemp fabric is suitable as composite reinforcement using resin pre-impregnated method. Industrial hemp was chosen for its low cost, low resource input as a crop, supply chain from raw product to refined textile and biodegradability potential. Detail is placed on specimen fabrication considerations. Lab testing of tension and compression is conducted and optimization considerations are examined. The resulting composite is limited in mechanical properties as tested. This research shows it is possible to use woven hemp reinforcement in pre-impregnated processed composites, but optimization in mechanical properties is required to make the process commercially practical outside niche markets. / Dissertation/Thesis / M.S.Tech Engineering 2012

A micromechanical analysis of the representative volume element (RVE) of a unidirectional flax/jute fiber reinforced epoxy composite is performed using finite element analysis (FEA). To do so, first effective mechanical properties of flax fiber and jute fiber are evaluated numerically and then used in evaluating the effective properties of ax/jute/epoxy hybrid composite. Mechanics of Structure Genome (MSG), a new homogenization tool developed in Purdue University, is used to calculate the homogenized effective properties. Numerical results are compared with analytical solution based on rule of mixture, Halpin-Tsai as well as Tsai-Hahn equations. The effect of the volume fraction of the two different fibers is studied. Mechanical performance of hybrid composite is compared with the mechanical performance of single fiber composites. Synergistic effect due to hybridization is studied using analytical method given in literature, finite element method based MSG and Classical Lamination Theory (CLT). It is found that, when Poisson ratio is taken into consideration, elastic modulus shows synergy due to hybridization. Finally, impact properties of ax/jute/epoxy hybrid composite material are studied using Charpy impact testing.

Lactic acid based thermoset were synthesised by reacting lactic acid with glycerol andfunctionalizing lactic acid branches by methacrylic anhydride. Resins with different chainlength were prepared and their thermo mechanical properties were examined through DMAanalysis and their molecular structures were analyzed by NMR method and their viscositywere investigated through rheometry analysis and three monomers were selected as the bestchain length. Degree of reaction in different reaction times was evaluated by a modifiedtitration method and bulk preparation of resin was performed by optimal process condition.DSC analysis was conducted in order to evaluate curing behaviour of resin with benzoylperoxide as cross-linking initiator. TGA analysis was performed to check thermo stability ofthe resin. Bio composites by viscose unidirectional and bidirectional knitted fabrics and alsonon woven viscose fiber with different fiber loads were prepared by ordinary hand layupimpregnation followed by compress moulding and their mechanical and thermo mechanicalproperties were characterized by tensile, flexural, charpy and DMA analysis and optimumfiber loads were identified for each fiber type. Ageing properties of prepared composites wereexamined by placing samples in climate chamber to simulate long time ageing and ageingexperiment was followed by tensile and flexural test to evaluate mechanical properties afterageing simulation. Composite`s swelling properties for water and some other solvents wereinvestigated and also their chemical resistance were evaluated by immersing them in 1M HCland KOH. The resin was also compared with a commercial oil based thermoset by preparingglass fiber reinforced composites and also effect of adding styrene to the resin were evaluated.Results of this work demonstrated that the novel synthesised have very high mechanical andthermo mechanical properties surpassing commercial oil based poly esters but ageingbehaviour is not very good however adding styrene can improve ageing properties. Also theresin is compatible with cellulosic natural fibers and forms strong composites. / Program: Masterutbildning i energi- och material

The first part of the thesis investigates the enhancement of fly ash-based geopolymer with alkali pretreated sweet sorghum fiber. The unconfined compression, splitting tensile and flexural tests were conducted to investigate the mechanical properties of geopolymer composite. The results indicate that the inclusion of sweet sorghum fiber slightly decreases the unconfined compressive strength (UCS), however, the splitting tensile and flexural strengths as well as the post-peak toughness increase with the fiber content up to 2% and then decrease thereafter. A durability test program containing 10 wet/dry cycles was performed to evaluate the long-term performance of the geopolymer composite related to wet/dry cycling. The results indicate that both the UCS and the splitting tensile strength of the geopolymer composite progressively decrease with the number of wet/dry cycles. The second part of the thesis investigates the utilization of biopolymers to stabilize MT for dust control. First, a fall cone method was adopted to evaluate the Atterberg limits and undrained shear strength of MT stabilized with biopolymers. The results indicate that the inclusion of biopolymers increases both the liquid limit and the undriained shear strength of MT. Two new equations are proposed for predicting the undrained shear strength of MT based on liquid limit and water content, and liquidity index. Second, an experimental program including moisture retention, wind tunnel and surface strength tests was performed to evaluate the effectiveness of biopolymer stabilization for dust control. The results indicate that biopolymers are effective in enhancing the moisture retention capacity, improving the dust resistance, and increasing the surface strength of MT. Third, a durability test program containing 10 wet/dry cycles was applied to MT samples treated with biopolymer solutions of different concentrations. The results show that the dust resistance of MT samples progressively decreases with the number of wet/dry cycles. Finally, experimental and numerical studies on the unconfined compressive strength (UCS) of MT stabilized with biopolymer were carried out. It is found that inclusion of biopolymer into MT favors the increase of adhesion between MT particles and thus the increase of the UCS of MT.

Les matériaux composites constituent aujourd’hui un domaine très dynamique tant au niveau de l’industrie que de la recherche. Dans ce cadre, les renforts d’origines naturelles représentent une alternative intéressante aux fibres synthétiques de par leurs propriétés mécaniques élevées, leur faible densité et leur caractère biosourcé, afin de répondre à l’accroissement des niveaux de performances ciblés ainsi qu’aux exigences économiques et écologiques actuelles.Ces travaux s’inscrivent dans un projet regroupant laboratoires de recherche, fournisseurs et end-users, visant à développer un matériau composite unidirectionnel structural à base de fibre de lin pour une application sport et loisirs. Ainsi, les objectifs initiaux incluent le développement de différents traitements chimiques des fibres, afin de les laver, d’homogénéiser leurs propriétés mécaniques et d’améliorer l’adhésion fibre-matrice. Une stratégie originale a pour cela été élaborée, basée sur la réactivité et les propriétés physico-chimiques d’un agent de couplage biosourcé. Ce produit a montré un potentiel prometteur d’additif de renforcement des matériaux cellulosiques, notamment à l’état humide. De plus, sa réactivité avec des molécules compatibilisantes a permis de le fonctionnaliser pour promouvoir l’adhésion fibre-matrice.Les caractérisations menées aux différentes échelles de la fibre de lin ont ensuite montré la pertinence de ces traitements, qui renforcent les interfaces fibre-matrice et les fibres techniques à l’état humide. Les études mécaniques ont cependant soulevé de nombreuses problématiques expérimentales, et ont démontré que les spécificités morphologiques de ces objets et leur caractère naturel ne permettaient pas l’exploitation directe des mesures dans le cadre d’un tel projet de développement. Les axes de recherche se sont alors avant tout focalisés sur l’étude des matériaux composites. Ainsi, plusieurs verrous structuraux ont pu être identifiés. La qualité de l’imprégnation de ces renforts naturels, qui peut être influencée par la formulation des traitements et la mise en œuvre, est déterminante dans le développement du matériau à cause de la morphologie multi-échelles des fibres. L’orientation des fibres au sein des plis unidirectionnels s’est également avéré être un paramètre prépondérant, étroitement lié à l’architecture des renforts et aux procédés de traitements industriels.Les développements menés à la fois sur les traitements et sur la structure des composites ont ainsi permis de doubler les propriétés mécaniques des systèmes initiaux pour atteindre un module de rigidité de 30 GPa et une contrainte ultime d’environ 370 MPa en traction tout en limitant grandement la perte de résistance après vieillissement dans l’eau et en garantissant une déformation en flexion répondant au cahier des charges. Les évolutions réalisées ne permettent pas pour le moment d’envisager l’industrialisation de ce matériau, mais vont permettre le prototypage de produits finis. / Nowadays, composite materials are a challenging and dynamic thematic for both industry and academic research. In this context, natural fibres are an interesting alternative to synthetic fibres thanks to their high mechanical properties, low density and biosourced origins in order to meet the requirements in terms of performance, costs and durability.This work take part into an industrial project that include research laboratories, suppliers and end-users. It aims at developing a unidirectional flax fibre composite material for sport and recreation application. The initial objectives of development focused on the surface optimization and the reinforcement, and the improvement of fibre-matrix adhesion. An original strategy has been set, based on the reactivity and the physico-chemical properties of métapériodate oxidized xyloglucan. This molecule has shown a promising effect of reinforcement on cellulosic materials, particularly in wet conditions. Besides, its reactivity with compatibilization agents allows different functionalization possibilities to increase fibre-matrix adhesion, encouraging its use as a coupling agent.The characterizations led on the different scales of flax fibre validated this strategy, as micro-mechanical tests showed adhesion improvement and mechanical properties of wet fibres had significantly increased. However, further mechanical investigations rose numerous experimental issues, and demonstrated that the specific morphology of these objects as well as their natural origins were major obstacles to measures exploitation in this kind of development project. So, the main research axis then focused on directly composite materials.Different structural problematics has been thus identified. Natural fibre impregnation, which can be influenced by treatments composition and elaboration process, has revealed itself has an important parameter linked to the multi-scale organization of flax. The fibre orientation in the unidirectional ply has been also identified as a key parameter that is affected by reinforcement architecture and industrial process of treatment.Those developments on treatments and composite structure led to a great increase of the material tensile properties to reach 30 GPa modulus and 370 MPa in strength, also improving its water ageing behaviour and its flexion ultimate strain. These promising enhancements are not sufficient in terms of overall mechanical performance and elaboration process to envisage an industrialization phase, but the prototyping of finished products will be realized.