Elaboration and characterization of PET-Hemp fiber composites for thermoforming applications

An elaboration and characterization of the composites of polyethylene terephthalate (PET) reinforced with hemp fiber for thermoforming applications deal with significant challenges faced by the bio-composite industry vis-à-vis high temperature melting thermoplastics reinforced with vegetal fibers. The originality of this work includes processing such composite material while avoiding thermal degradation and using the resultant composite which is normally brittle for thermoforming, based on large deformations. Most of the previous works have only involved low temperature melting thermoplastics reinforced with natural fibers although high temperature melting thermoplastics have an important potential in numerous applications. During the past decades, the volume and types of natural fibers used as reinforcements for bio-composites applications have increased significantly. Such trend has been particularly observed in the group of vegetal fiber-reinforced composites, also known as ligno-cellulosic fiber-reinforced composites, which are found in construction, automobile, aerospace and bio-medicine to name a few. However, those applications are for the most part either made of polyolefin matrices or polymers whose highest melting points are close to 200°C. Despite its high melting point, Polyethylene terephthalate (PET), similar to other polyesters and highly polar matrices, shows good affinity for reinforcement by ligno-cellulosic or vegetal fibers such as hemp. This work aimed at achieving a dual objective: First to extend the elaboration of ligno-cellulosic fiber-reinforced composite materials to the range of higher temperature melting thermoplastics (Tm>200°C) and secondly to study the thermoformability of the processed PET-hemp fiber composites in order to determine the optimal formulation for thermoforming, as well as its optimal conditions. In the plastic industry, the thermoforming process is essentially based on heating extruded sheets to a temperature between the glass transition temperature (Tg) and the melting point, where large deformations occur. Both objectives are quite challenging: For the first objective, there is a risk of hemp fiber degradation due to the temperature gap between the melting point of PET (Tm~250°C) and the onset of thermal degradation of vegetal fibers (Td~190˚C) and concerning the second objective, thermoforming requires large deformations although bio-composites are generally brittle. The mentioned challenges were strategically overcome by modifying both the matrix and the fibers. Furthermore, five formulations with 1, 5, 10, 15 and 20% (w/w) fiber concentrations were investigated for their mechanical, thermal, structural and rheological properties; the best formulation was selected for numerical thermoforming. The fibers were modified by alkaline treatment to increase their thermal stability, while PET’s melting point was depressed by a ten of degree by compounding with polycaprolactone (PCL) using a torque based mixer. The numerical thermoforming was finally performed by an optimized application of the ThermoForm© code to the previously determined composite parameters. The following major observations were made in different sections of this research. The mechanical properties of PET-hemp fiber composites showed similar variations with those of other natural fiber reinforced composite materials reported in the literature. \n•In the presence of the applicable additives such as pyromellitic dianhydride (PMDA), glycidyl methacrylate (GMA) and clay, the elastic modulus of PET-5% (w/w) PCL-Additives increased by 10 to 20% with respect to the unreinforced formulation and 2 to 10% with respect to the reinforced formulation without additives. However, all the formulations were significantly brittle and their strain at break decreased from over 40 to about 4%. Their maximum force was also lowered by up to 4% with respect to virgin PET. \n•In the absence of additives, the elastic modulus and the maximum force of PET-5% (w/w) PCL-5% (w/w) - (1, 5, 10, 15 and 20% (w/w)) hemp fibers increased logarithmically with the fiber concentration, while the strain at break dropped below 5%. An improved interface quality without additives is an indication of the possible hydrogen bonding between the carbonyl groups of PET and the hydroxyl groups of hemp fibers. The remaining investigation was then performed without additives. \nAll the composite formulations proved to be thermally stable until 315°C as an indication for their ability to undergo multistage processing. Two thermo-degradation ranges were observed from 290 to 385°C and from 385 to 490°C respectively. They were respectively described by the Sestak-Berggren and the truncated Sestak-Berggren models. Similar observations were made for the formulations compounded with the mixing chamber heated at 240, 250 and 250°C. Consequently, the numerical thermoforming process was restricted to the group compounded at 250°C. The rheological properties fitted with the ThermoForm® code indicated the suitability of the Christensen model to describe the visco-elastic behavior of the investigated composite formulations. The numerical variations of various forming parameters indicated a partition of the formulations into two groups reinforced by 0, 1 and 5% (w/w) for the first, and 10 and 15% (w/w) for the second. The first group was better suited for both the free forming and the thermoforming process. However, a more powerful air flow is needed for forming of PET -1% (w/w) hemp, leaving PET-5% (w/w) hemp as the best thermoformable alternative with respect to the process cost and in-service performance. The second group showed a relatively poor performance which can be attributed to the fiber’s partial thermo-degradation resulting from processing larger fiber volume with respect to the limited available matrix. \nAlthough PET-hemp fiber composites have been successfully formulated and their behavior towards the thermoforming process numerically investigated, a fine tuning of the processing conditions will be the object of future work alongside the valorization of higher fiber loads through targeted applications requiring woven reinforcements. \n \nL’élaboration et la caractérisation des composites de polyéthylène téréphtalate (PET) renforcés de fibres de chanvre pour des applications en thermoformage adresse des défis majeurs auxquels est confrontée l’industrie des bio-composites concernant le renforcement des polymères ayant des hauts points de fusion avec des fibres d’origine végétale. La contribution originale de ce travail a un impact significatif sur l’industrie des plastiques. En outre il concerne le renforcement d’un polymère thermoplastique ayant un point de fusion élevé avec des fibres naturelles tout en évitant la thermo-dégradation, et procède à la mise en forme du produit qui est normalement cassant, par le thermoformage basé sur les grandes déformations. Durant les dernières décennies, on a assisté à une augmentation significative du volume et des types de fibre naturelle comme renforts des bio-composites utilisés dans divers secteurs d’activité. L’on retrouve les composites dont les renforts sont des fibres naturelles, encore appelés bio-composites dans divers domaines à l’exemple de la construction, la biomédecine, l’aérospatial, et l’automobile; cependant ces applications sont pour la plupart soit restreints aux matrices de type polyoléfine ou des polymères dont le point de fusion maximal est proche de 200°C. Le PET, tout comme d’autres matrices de type polyester ou de grande polarité ayant des hauts points de fusion, présente une plus haute affinité de renfort avec des fibres lignocellulosiques ou fibres naturelles à l’exemple des fibres de chanvre. Ce travail vise deux objectifs principaux, à savoir étendre l’élaboration des matériaux bio-composites au groupe de matrices qui fondent à haute température (Tm>200°C), ensuite faire une mise en œuvre des applications de ce type de composite par thermoformage. Le thermoformage des plastiques-composites est un procédé de mise en forme basé essentiellement sur le chauffage des feuilles extrudées entre le point de transition vitreuse (Tg) et le point de fusion, suivi d’une grande déformation. Les deux objectifs présentent beaucoup de défis, à savoir dans un cas éviter la dégradation thermique des fibres de chanvre causée par la différence entre le point de fusion du PET (Tm~250°C) et la température initiale de dégradation des fibres naturelles (Td~190°C), et faire le thermoformage d’un matériau cassant alors que le processus est basé sur les grandes déformations. Les défis rencontrés ont été stratégiquement relevés en combinant la modification des fibres et de la matrice. Ensuite, des formulations de composites renforcés de 1, 5, 10, 15 et 20% (w/w) de fibres ont été mises en forme, testées au point de vue mécanique, thermique, structural, et rhéologique. La stabilité thermique des fibres a été améliorée par traitement alcalin et la température de fusion du PET a été abaissée d’une dizaine de degré par mélange avec le polycaprolactone (PCL) dans un mélangeur à torque. Finalement, le thermoformage numérique a été réalisé en appliquant le code ThermoForm® aux paramètres des composites déterminés initialement. Les observations suivantes ont été faites dans diverses sections de cette recherche. Les variations des propriétés mécaniques des composites de PET renforcés de fibres de chanvre sont similaires aux comportements d’autres composites renforcés de fibres naturelles que l’on trouve dans la littérature. \n• En présence des additifs tels que le dianhydride pyromellitique (PMDA), le méthacrylate de glycidyle (GMA) et l’argile, le module d’élasticité de PET-5% (w/w) PCL-Additifs augmente de 10 à 20 % par rapport à la formulation sans renfort et de 2 à 10% par rapport à la formulation renforcée sans additifs. Cependant, toutes ces formulations étaient fragiles et leu

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