Tesis sobre el tema "Naturel fiber"

Les effets du caoutchouc nitrile (NBR), du traitement de la surface des fibres et du noir de carbone sur les propriétés des composites à base de caoutchouc naturel renforcé par des fibres d'ananas (NR / PALF) ont été étudiés. L'incorporation de NBR et le traitement de surface de la fibre ont été utilisés pour améliorer les propriétés mécaniques des composites à faible déformation, alors que le noir de carbone a été utilisé pour améliorer ces propriétés à forte déformation. La teneur en fibres a été fixée à 10 phr. Les matériaux composites ont été préparés à l'aide d'un mélangeur à cylindres et ont été réticulés sous presse permettant ainsi le maintien de l'orientation des fibres. Ces composites ont été caractérisés à l’aide du rhéomètre à matrice mobile (MDR), par analyse thermique mécanique dynamique (DMTA) et par tests de traction. La morphologie après fracture cryogénique a été observée à l'aide de la microscopie électronique à balayage (MEB). L'effet du NBR dont la teneur varie de 0 à 20 phr par rapport à la teneur totale en caoutchouc, a été également étudié. Le NBR est utilisé afin d’encapsuler totalement les fibres d’ananas (PALF) ; ceci conduisant à un meilleur transfert de contraintes entre la matrice et les fibres. La méthode de mélange a également été étudiée. Plusieurs types de silanes tels que le propylsilane, l'allylsilane et le silane-69 ont été utilisés pour traiter les fibres pré-nettoyées à l’aide d’un traitement alcalin. Les fibres silanisées ont été caractérisées par spectroscopie infrarouge à transformée de Fourier (FTIR), par spectroscopie de photoélectrons aux rayons X (XPS) et par MEB. Le traitement de la fibre par le silane-69 a permis d’augmenter fortement le module du matériau composite à faible déformation. Ce traitement a été plus efficace que l'incorporation de NBR dans les composites NR / PALF. Ceci peut s’expliquer par une possible réticulation chimique entre le caoutchouc et la fibre traitée au silane-69 plutôt qu’une simple interaction physique du NR, du NBR et de la fibre. Cependant, le renforcement par fibre réduit la déformation à la rupture. Par conséquent, du noir de carbone a également été incorporé dans les composites NR/NBR/PALF et NR/ PALF traitée, afin d’améliorer leurs propriétés ultimes. En incorporant du noir de carbone à un taux de 30 phr dans les deux composites, les propriétés mécaniques des composites ont été améliorées et peuvent être contrôlées à la fois à des déformations faibles et hautes
The effects of nitrile rubber (NBR), fiber surface treatment and carbon black on properties of pineapple leaf fiber-reinforced natural rubber composites (NR/PALF) were studied. The incorporation of NBR and surface treatment of fiber were used to improve the mechanical properties of composites at low deformation, whereas carbon black was used to improve these properties at high deformation. The fiber content was fixed at 10 phr. The composites were prepared using two-roll mill and were cured using compression moulding with keeping the fiber orientation. These composites were characterized using moving die rheometer (MDR), dynamic mechanical thermal analysis (DMTA) and tensile testing. The morphology after cryogenic fracture was observed using scanning electron microscopy (SEM). The effect of NBR from 0 to 20 phr of total rubber content was investigated. NBR is proposed to encase PALF leading to higher stress transfer between matrix and PALF. The method of mixing was also studied. For the fiber surface treatment, propylsilane, allylsilane and silane-69 were treated on the alkali-treated fiber. Treated fibers were characterized using Fourier-Transform infrared spectroscopy (FTIR), x-ray photoelectron spectroscopy (XPS) and SEM. Silane-69 treatment of fiber increased the modulus at low deformation more than the incorporation of NBR of NR/PALF composites due to the chemical crosslinking between rubber and fiber from silane-69 treatment rather than the physical interaction of NR, NBR and fiber. However, reinforcement by fiber reduced the deformation at break. Hence, carbon black was also incorporated into NR/NBR/PALF and NR/surface-treated PALF composites to improve the ultimate properties. By incorporation of carbon black 30 phr in both composites, the mechanical properties of composites were improved and can be controlled at both low and high deformations

The material properties of fibre networks and fibre reinforced composites are strongly influenced by fibre-fibre interactions. Stress transfer between load bearing elements in such materials is often dictated by the nature of the fibre-fibre interface. Inter-fibre bonding is solely responsible for internal cohesion in paper, because all stresses transferred between fibres operate through fibre-fibre bonds. . The future development of cellulosic fibre materials will require an improved understanding of the fibre-fibre interface. Fluorescence resonance energy transfer (FRET) was proposed as a new tool for the study of fibre interfaces. A protocol for covalent linkage of fluorophores to natural and regenerated cellulosic fibres was developed and the absorptive and emissive properties of these dyes were characterized. The fluorescent response of these dyed fibres in paper sheets was studied using steady-state fluorescence spectroscopy. Fluorescence micrographs of fibre crossings on glass slides were analyzed using the FRETN correction algorithm. Energy transfer from coumarin dyed fibres to fluorescein dyed fibres at the interface was observed. The FRETN surfaces for spruce and viscose rayon fibre crossings were distinctly different. The FRET microscopy method was able to detect statistically significant differences in spruce fibre interface development when fibre fraction and wet pressing were varied. The coalescence of natural cellulosic fibre interfaces during drying was also observed with the technique. Polysaccharide films were employed as model systems for the natural and regenerated cellulose fibre interfaces. It was found that pressing cellulose films did not result in significantly increased FRETN either due to resistance to deformation or the inability to participate in interdiffusion. Conversely, xylan films demonstrated a drastic increase in the FRETN signal with increased wet pressing. These results support the previously observed differences between regenerated cellulose fibres and natural wood fibres. The results of the FRETN analysis of the polysaccharide film model systems suggest that lower molecular weight amorphous carbohydrates are likely to be significant contributors to fibre interface development.

L'utilisation des matériaux composites renforcés par des fibres végétales ne cesse de croitre dans divers secteurs tels que l'automobile et le packaging. Toutefois, le problème de leur sensibilité à l'humidité freine encore leur utilisation dans des applications exposées à des conditions environnementales extrêmes. Par conséquent, l'hybridation des fibres végétales avec des fibres synthétiques peut constituer une voie prometteuse pour améliorer certaines propriétés des composites à renfort végétal. C'est dans ce contexte que se situe le présent travail doctoral. Il présente une analyse expérimentale du comportement en fatigue par traction--traction et en fatigue par chocs à faible énergie de stratifiés non hybrides et hybrides lin-verre/époxyde. Une investigation de leur durabilité après un vieillissement hydrique jusqu'à la saturation est également présentée. À cette fin, plusieurs plaques des composites non hybrides et hybrides lin-verre/époxyde ont été élaborées par le procédé d'infusion sous vide. Dans un premier temps, nous avons réalisé une caractérisation en traction monotone des composites de l'étude et étudié la cinétique de diffusion de l'humidité au sein de ces matériaux. Les résultats de ces essais montrent que le remplacement de couches de lin par des couches de verre améliore nettement les propriétés mécaniques stratifié lin/époxyde et diminue également sa masse d'eau absorbée à saturation. Ensuite, des essais de fatigue cyclique ont été réalisés sur des éprouvettes composites non vieillies et vieillies. Ces essais de fatigue ont été couplés à la technique de l'émission acoustique afin d'identifier les mécanismes d'endommagement et leur chronologie d'apparition. Pour évaluer l'effet de la charge de fatigue sur la perte de rigidité, les boucles d'hystérésis et le facteur d'amortissement des composites non hybrides et hybrides ont été étudiées. L'analyse des signaux acoustique permet d'identifier trois classes de signaux acoustiques dans tous les composites étudiés. Ces trois classes sont attribuées aux principaux mécanismes d'endommagement comme la fissuration matricielle, la décohésion fibre--matrice et la rupture des fibres. Cette attribution est consolidée par des observations microscopiques obtenues à l'aide d'un microscope électronique à balayage. Enfin, des essais de fatigue par chocs à faible énergie ont été réalisés sur des échantillons composites non vieillis et vieillis. Les résultats obtenus montrent clairement que le composite lin/époxyde absorbe une grande partie de l'énergie d'impact en déformation élastique. Cependant, le stratifié verre/époxyde consomme cette énergie en endommagement et rupture. De plus, le vieillissement hydrique fragilise tous les composites étudiés et diminue leur résistance à la fatigue par chocs
The use of natural fibre-reinforced composite materials is growing in various sectors such as automotive and packaging. However, the problem of their sensitivity to humidity still hinders their use in applications exposed to extreme environmental conditions. Therefore, the hybridization of natural fibres with synthetic fibres can constitute a promising way to improve some properties of natural fibre-reinforced composites. It is in this context that the present doctoral work is situated. It presents an experimental analysis of the tensile-tensile fatigue and low-energy impact fatigue behaviour of non-hybrid and hybrid flax-glass/epoxy laminates. An investigation of their durability after water aging until saturation is also presented. To this end, several plates of non-hybrid and hybrid flax-glass/epoxy composites have been fabricated by the vacuum infusion process. First, we carried out a monotonic tensile characterization of the studied composites and evaluated the kinetics of moisture diffusion within these materials. The results of these tests show that the addition of glass layers to the flax/epoxy laminate improves its mechanical properties and also reduces its mass of water absorbed at saturation. Then, cyclic fatigue tests were performed on unaged and aged composite specimens. These fatigue tests were coupled with the acoustic emission technique in order to identify the damage mechanisms and their chronology of appearance. To evaluate the effect of fatigue loading on the loss of stiffness, hysteresis loops and the damping factor of non-hybrid and hybrid composites were investigated. The analysis of the acoustic signals makes it possible to identify three classes of acoustic signals in all the studied composites. These three classes are attributed to the main damage mechanisms such as matrix cracking, fibre/matrix decohesion and fibre breakage. This attribution is supported by microscopic observations obtained using a scanning electron microscope. Finally, low-energy impact fatigue tests were performed on unaged and aged composite samples. The obtained results clearly show that the flax/epoxy composite absorbs a large part of the impact energy and transforms it into elastic energy. However, the glass/epoxy laminate consumes this energy in damage and breakage. In addition, water aging weakens all the studied composites and reduces their resistance to impact fatigue

The objective of this thesis is to investigate the effects of adding natural fiber (kenaf fiber, retted kenaf fiber, and sugarcane fiber) into polymer materials. The effects are obtained by considering three main parts. 1. Performance in thermoplastic composites. The effect of fiber retting on polymer composite crystallization and mechanical performance was investigated. PHBV/PBAT in 80/20 blend ratio was modified using 5% by weight kenaf fiber. Dynamic mechanical analysis of the composites was done to investigate the glass transition and the modulus at sub-ambient and ambient temperatures. ESEM was conducted to analyze fiber topography which revealed smoother surfaces on the pectinase retted fibers. 2. Performance in thermoset composites. The effect of the incorporation of natural fibers of kenaf and of sugarcane combined with the polyester resin matrix is investigated. A comparison of mechanical properties of kenaf polyester composite, sugarcane polyester composite and pure polyester in tensile, bending, dynamic mechanical thermal analysis (DMA) and moisture test on performance is measured.. 3. Performance in sandwich composites. The comparison of the performance characteristics and mechanical properties of natural fiber composites panels with soft and rigid foam cores are evaluated. A thorough test of the mechanical behavior of composites sandwich materials in tensile, bending and DCB is presented here.

Biocomposites made from biodegradable polymer as matrix and natural fiber as reinforcement are certainly environmentally friendly materials. Both constituent materials are fully biodegradable and do not leave any noxious components on Earth. The natural fibers have been used as reinforcement due to their advantages compared to glass fibers such as low cost, high specific strength and modulus, low density, renewability and biodegradability. Major aims of this work were to produce natural fibers and/or nanoparticles with polyethylene (PE), polypropylene (PP) and polylactide (PLA), poly(hydroxybutyrate-co-hydroxyvalerate)(PHBV) matrices and determine their structure-property relationships. Following abstracts of the present research work are manifold: BINARY COMPOSITES Polylactide (PLA)/flax mat composites The polylactide (PLA)/flax mat and modified PLA/flax mat composites were produced by hot press technique. Two additives of non-regulated wax/ethylene acrylate copolymer/butyl acrylate and acrylic were used as modifier for PLA. The dispersion of the flax mat in the composites was studied by scanning electron microscopy (SEM). The PLA composites were subjected to instrumented falling weight impact test. The mechanical and thermal properties of the composites were determined in tensile test, thermogravimetric analysis (TGA) and dynamic-mechanical thermal analysis (DMTA), respectively. It was found that the PLA based composites increased the impact resistance. The tensile strength value of modified PLA/flax mat composite decreased slightly compared to the PLA. The elongation at break data indicated that an improvement in ductility of modified PLA and its composites. Moreover, addition of thermal modifier enhanced thermal resistance below processing temperature of PLA and had a marginal effect on the glass transition temperature of PLA. The storage modulus master curves were constructed by applying the time-temperature superposition (TTS) principle. The principle of linear viscoelastic material was fairly applicable to convert from the modulus to the creep compliance for all systems studied. Polylactide (PLA)/woven flax textiles composites The polylactide (PLA)/woven flax textiles 2x2 twill and 4x4 hopsack composites were produced by interval hot press technique. Two weave styles of flax used to reinforce in PLA. The dispersion of the flax composite structures in the composites was inspected in scanning electron microscopy (SEM). The PLA composites were subjected to instrumented falling weight impact test. The mechanical properties (tensile, stiffness and strength) of the composites were determined in tensile and dynamic-mechanical thermal analysis (DMTA) tests, respectively. SEM observed that the interfacial gaps around pulled-out fibers were improved when produced by the interval hot press. It was also found that the both styles of flax composites increased the impact resistance compared to the neat PLA. The tensile strength and stiffness value of PLA/flax composites were markedly higher than that of the neat PLA and reflect the effects of composite structures. The calculated storage creep compliance was constructed by applying the time-temperature superposition (TTS) principle. The calculated creep response of these flax composites was much lower than that of the neat PLA. Polyethylene and polypropylene/nano-silicon dioxide/flax composites Composites composed of polylactide (PLA), modified PLA and woven flax fiber textiles (Flax weave style of 2x2 twill and 4x4 hopsack) were produced by hot press technique. Two structurally different additives used to modify PLA. The dispersion of the flax composite structures in the composites was studied by scanning electron microscopy (SEM) and computed microtomography system (µCT). The PLA composites were subjected to water absorption and instrumented falling weight impact tests. The thermomechanical and creep properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA)and short-time creep tests, respectively. It was found that the modified PLA and its composite increased the impact resistance compared to the unmodified PLA. Incorporation of flax decreased resistance to thermal degradation and increased water uptake. The impact energy and stiffness value of PLA/flax composites was markedly higher than that of PLA but reflect the effects of composite structures and flax content. The storage modulus master curves were constructed by applying the time-temperature superposition (TTS) principle. From the master curve data, the effect of modified PLA on the storage modulus was more pronounced in the low frequencies range. Polylactide (PLA)/woven flax fiber textiles/boehmite alumina (BA) composites The textile biocomposites made from woven and non-woven flax fibre reinforced poly(butylene adipate-co-terephthalate) (PBAT) were prepared by compression moulding using film stacking method. The mechanical properties (such as tensile strength and stiffness, flexural strength and modulus, and impact strength) of textile biocomposites were determined in tensile, flexural and impact tests, respectively. The PBAT-based composites were subjected to water absorption. The comparison of the mechanical properties was made between pure PBAT and textile composites. The influence of flax weave styles on the mechanical properties was also evaluated. The results showed that the strength of the textile biocomposites was increased according to weave types of fibers, especially in the stiffness was significantly increased with the higher densification of the fibers. The 4x4-plain woven fibers (4-yard-wrap and 4-yard-weft weave direction) reinforced biocomposite indicated the highest strength and stiffness compared to the other textile biocomposites and pure PBAT. This was considered to be as the result of the character of weave style of 4x4-plain woven fibers. The aminopropyltriethoxysilane affected the mechanical properties and water absorption of the resulting composites laminates due to the surface compatibility between flax fiber and PBAT. HYBRID COMPOSITES Polyethylene/nanoparticle, natural and animal composites Binary and ternary composites composed of high-density polyethylene (HDPE), boehmite alumina (BA) and different kinds of natural-, animal fibers, like flax, sponge gourd (SG), palm and pig hair (PH) were produced by hot press technique. Aqueous BA suspensions were sprayed on the HDPE/flax mat to prepare nanoparticle/natural fiber reinforced ternary polymer composites followed by drying. The dispersion of the natural-, animal fibers and BA particles in the composites was studied by scanning electron microscopy (SEM) and discussed. The thermomechanical and stress relaxation properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA) and short-time stress relaxation tests (performed at various temperatures), respectively. The HDPE based composites were subjected to water absorption and instrumented falling weight impact tests. It was found that the all composites systems increased the stiffness, stress relaxation and reduced the impact toughness. The stress relaxation modulus of natural-, animal fiber composites were higher compared to that of the neat HDPE. This modulus increased greatly with in corporation of BA. The relaxation master curves were constructed by applying the time-temperature superposition (TTS) principle. The inverse of Findley power law could fairly applicable to describe the relaxation modulus vs. time traces for all systems studied. Incorporation of BA particles enhanced the thermal resistance which started to degrade at higher temperature compared to the HDPE/flax mat composite. The HDPE/flax mat/BA composite could reduce the water uptake. Polyethylene/Flax/SiO2 Composites Composites composed of high-density polyethylene (HDPE), woven flax fiber textiles (Flax weave style of 2x2 twill and 4x4 hopsack) and silicon dioxide (SiO2) were produced by hot press with nano spraying technique. The SiO2 slurries were sprayed by a hand onto the both surface of the woven flax fiber. The HDPE /woven flax fibers composites with and without used nano-spraying technique were produced by hot pressing in a laboratory press. The dispersion of SiO2 particles and flax in the composites was studied by scanning electron microscopy (SEM). The related HDPE based composites were subjected to instrumented falling weight impact test. The thermal resistance, stiffness and tensile strength properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA) and tensile tests, respectively. It was found that the impact energy and stiffness value of HDPE/flax composites was markedly higher than that of HDPE but reflect the effects of composite structures and flax content. Incorporation of SiO2 particles enhanced resistance to thermal degradation. It was established that the linear viscoelastic material principle are fairly applicable to convert from the modulus to the creep compliance results. Un- and Modified Polylactide (PLA) /woven Flax Fiber composites Hybrid composites composed of polypropylene (PP) or high-density polyethylene (HDPE), different flax fibers (unidirectional-, biaxial and twill2x2) and silicon dioxide (SiO2) were produced by hot press technique. The ternary polymer composite was effectively fabricated by spraying SiO2 solvents onto the surface of flax fiber. The dispersion of SiO2 particles and flax in the composites was studied by scanning electron microscopy (SEM). The related PP and HDPE based composites were subjected to instrumented falling weight impact test. The thermal and mechanical properties of the composites were determined by thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA), creep and stress relaxation tests, respectively. It was found that thermal decomposition temperature of the PP or HDPE/flax composites increased by the addition of SiO2 particles. The impact energy, stiffness, creep resistance and relaxation modulus value of all flax composites increased markedly compared to the PP and HDPE matrix. Time–temperature superposition (TTS) was applied to estimate the creep and relaxation modulus of the composites as a function of time in the form of a master curve. The activation energies for the all PP and HDPE composites systems studied were also calculated by using the Arrhenius equation. The generalized Maxwell model was fairly applicable to the stress relaxation results. Polylactide (PLA)/woven flax fiber textiles/boehmite alumina (BA) composites Composites composed of polylactide (PLA), woven flax fiber textiles (weave style of 2x2 twill and 4x4 hopsack) and boehmite alumina (BA) were produced by hot press. The spraying technique served for the pre-dispersion of the alumina nanoparticles. The aqueous alumina slurry was produced by mixing the water with water dispersible alumina. The dispersion of the flax structures and alumina particles in the composites was studied by scanning electron microscopy (SEM). The PLA composites were subjected to water absorption and instrumented falling weight impact tests. The creep and thermomechanical properties of the composites were determined in short-time creep tests (performed at various temperatures), thermogravimetric analysis (TGA) and dynamic-mechanical thermal analysis (DMTA), respectively. It was found that the incorporation of alumina particles reduced the water uptake compared to the PLA/flax blends. The impact energy and stiffness value of PLA/flax blends was markedly higher than that of PLA but reflected the effects of composite structures. Incorporation of alumina particles enhanced storage modulus and the creep resistance compared to the PLA/flax blends but slightly incremented thermal resistance at high temperature. No clear trend in the flax weave style- effect was found in the thermal behaviour. The creep master curves were constructed by applying the time-temperature superposition (TTS) principle. The Findley power law could satisfactorily describe the creep compliance vs. time traces for all systems studied. Poly(hydroxybutyrate-co-hydroxyvalerate)/sisal natural fiber/clay composites Poly(hydroxybutyrate-co-hydroxyvalerate)(PHBV) biocomposites different sisal containing with the fiber length of 0.25 and 5 mm, and addition of clay particles were prepared by hot compression technique. Silane (Bis(triethoxysilylpropyl)tetrasulfide) treatment has been used to modify in order to enhance the properties of related hybrid composites. The all composites were subject to water absorption test. The mechanical properties of hybrid composites such as tensile stiffness and strength, toughness and hardness determined in tensile, impact and hardness tests, respectively. It was found that tensile strength, stiffness and impact strength of long sisal fiber improved with increasing fiber content. Hardness of short sisal fiber improved with increasing fiber content. Treated Silane of long fibers at 20 wt.% loading was found to enhance the tensile strength fiber by 10% and impact strength by 750% as compared to the neat PHBV. Note that this feature was also confirmed by the appearance of a scanning electron microscopy. Moreover, the hardness and water resistance of the PHBV/sisal composites increased by the addition of clay particles. The diffusion coefficient for the PHBV and hybrid composites systems studied were also calculated.
Bioverbundwerkstoffe aus biologisch abbaubarem Polymer als Matrix und Naturfasern als Verstärkung sind ohne weiteres umweltfreundliche Materialien. Beide Bestandsmaterialien sind vollständig biologisch abbaubar und hinterlassen keine schädlichen Bestandteile auf der Erde zurück. Die als Verstärkung verwendeten Naturfasern wurden aufgrund ihrer Vorteile gegenüber Glasfasern, wie z.B. geringe Kosten, hohe spezifische Festigkeit und Steifigkeit, geringe Dichte, Erneuerbarkeit und Kompostierbarkeit ausgesucht. Der Hauptfokus dieser Arbeit lag darin Naturfasern und/oder Nanopartikel mit Polyethylen (PE), Polypropylen (PP) und Polylactid (PLA) herzustellen, sowie Poly-Hydroxybutyrat-Co-Hydroxyvalerat (PHBV) Matrizen und deren Struktur-Eigenschaft-Verhältnis zu bestimmen. Die folgenden Kurzfassungen der vorliegenden Forschungsarbeit sind vielfältig: BINÄRE VERBUNDWERKSTOFFE Polylactid (PLA)/ Flachsmatten-Verbundwerkstoffe Die Polylactid (PLA)/Flachsmatte und modifizierte PLA/Flachsmatten-Verbundwerkstoffe wurden im Pressverfahren hergestellt. Als Modifikator für das PLA wurden zwei nicht regulierte Wachs/Ethylen-Acrylat-Copolymer/Butyl-Acrylat und Acryl Additive verwendet. Die Verteilung der Flachsmatte in den Verbundwerkstoffen wurde mit dem Rasterelektronenmikroskop (SEM) untersucht. Die PLA-Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die mechanischen und thermischen Eigenschaften der Verbundwerkstoffe wurden im Zugversuch, der thermogravimetrische Analyse (TGA) und der dynamisch mechanischen Thermoanalyse (DMTA) jeweils bestimmt. Es zeigte sich, dass die PLA/Flachsmatten-basierten Verbundwerkstoffe eine erhöhte Schlagzähigkeit aufwiesen. Die Zähigkeitswerte der modifizierten PLA/Flachsmatten-Verbundwerkstoffe waren leicht verringert im Vergleich zum PLA. Die Bruchdehnungswerte zeigten eine Verbesserung der Verformbarkeit des modifizierten PLAs und dessen Verbundwerkstoffe. Nach Zugabe eines Wärme-Modifikators verbesserte sich der Wärmewiderstand auf unter Verarbeitungstemperatur des PLA und hatte nur einen unwesentlichen Einfluss auf die Glasübergangstemperatur des PLA. Die Hauptkurve des Speichermoduls wurde mit der Zeit-Temperatur-Überlagerung (TTS) aufgestellt. Auf alle untersuchten Systeme konnte das dafür gut geeignete Prinzip der linear viskoelastischen Werkstoffe angewendet werden um die Steifigkeit in die Kriechneigung umzuwandeln. Polylactid (PLA)/Flachstextilgewebe-Verbundwerkstoffe Die Polylactid (PLA)/Flachstextilgewebe 2x2 Körper und 4x4 Gewebe mit Leinwandbindung-Verbundwerkstoffe wurden im Intervall-Pressverfahren hergestellt. Das PLA wurde mit zwei Flachsgewebeformen verstärkt. Die Verteilung der Flachs-Verbundwerkstoffstrukturen in den Verbundwerkstoffen wurde mit dem Rasterelektronenmikroskop (SEM) untersucht. Die PLA Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die mechanischen Eigenschaften (Zugfestigkeit, Steifigkeit und Festigkeit) der jeweiligen Verbundwerkstoffe wurden in Zugversuchen und dynamisch mechanischen Thermoanalysen (DMTA) bestimmt. Das Rasterelektronenmikroskop zeigte auf, das der Grenzflächenzwischenraum von rausgezogenen Fasern sich durch das Herstellen im Intervall-Pressverfahren verbessert hat. Auch zeigte sich, dass beide Arten der Flachs-Verbundwerkstoffe die Schlagzähigkeit der Verbundwerkstoffe erhöht im Vergleich zum puren PLA. Die Zugfestigkeit- und Steifigkeitswerte der PLA/Flachs-Verbundwerkstoffe waren deutlich höher als die der puren PLA und spiegeln die Effekte von Verbundwerkstoffstrukturen wieder. Die berechnete Kriechneigung im Speichermodul wurde durch die Anwendung des Zeit-Temperatur-Überlagerung (TTS) Prinzips aufgestellt. Die errechnete Kriechgeschwindigkeit der Flachs-Verbundwerkstoffe war wesentlich geringer als im puren PLA. Polyethylen und Polypropylen/Nanosilikon Dioxid/Flachs-Verbundwerkstoffe Verbundwerkstoffe hergestellt aus Polylactid (PLA), modifiziertem PLA und Flachsfasertextilgewebe (Flachsgewebeform von 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) wurden im Pressverfahren hergestellt. Zwei strukturell unterschiedliche Additive wurden verwendet um das PLA zu modifizieren. Die Verteilung der Flachs-Verbundwerkstoffstruktur wurde unter dem Rasterelektronenmikroskop (SEM) und dem computergestütztes Computer-Tomography-System (µCT) untersucht. Die PLA Verbundwerkstoffe wurden dem Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die Kriech- und thermomechanischen Eigenschaften der respektiven Verbundwerkstoffe wurden in der thermogravimetrischen Analyse (TGA), der dynamisch mechanischen Thermoanalyse (DMTA) und dem Kurzzeit-Kriechversuch bestimmt. Das modifizierte PLA und dessen Verbundwerkstoffe zeigten eine Erhöhung der Schlagzähigkeit im Vergleich zum unmodifizierten PLA. Die Einbindung von Flachs verringerte den Widerstand gegenüber thermischer Degradierung und erhöhte die Wasseraufnahme. Die Schlagenergie- und Steifigkeitswerte der PLA/Flachs-Verbundwerkstoffe war deutlich höher als die der PLA aber spiegelt die Effekte von Verbundwerkstoffstrukturen mit Flachsinhalt wieder. Die Hauptkurve des Speichermoduls wurde mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Das Datenmaterial der Hauptkurve zeigte den Effekt des modifizierten PLAs auf dem Speichermodul deutlich ausgeprägter im Bereich der Niederfrequenz. Polylactide (PLA)/Flachfasertextilgewebe/Böhmit Aluminumoxid (BA)-Verbundwerkstoffe Die textilen Bioverbundwerkstoffe wurden aus flachsfaserverstärkten Poly(Butylen Adipat-Co-Terephtalat) (PBAT) Gewebe und Vlies im Formpressverfahren mit der Folien-Stapelmethode hergestellt. Die mechanischen Eigenschaften (wie Zugfestigkeit und Steifigkeit, Biegefestigkeit, Steifigkeit und Schlagzähigkeit) der jeweiligen textilen Bioverbundwerkstoffe wurde in Zug-, Biege-, und Schlagtests ermittelt. Die PBAT basierten Verbundwerkstoffe wurden dem Wasseraufnahmetest unterzogen. Der Vergleich der mechanischen Eigenschaften wurde zwischen reinem PBAT und textilen Verbundwerkstoffen durchgeführt. Der Einfluss der Flachsgewebeformen auf die mechanischen Eigenschaften wurde ebenfalls untersucht. Die Ergebnisse zeigten das die Festigkeit der textilen Bioverbundwerkstoffe mit der Webart der Fasern anstieg, signifikant in Bezug auf die Steifigkeit bei einer erhöhten Verdichtung der Fasern. Die 4x4 flachfasergewebten (4-Schussfaden-Windung und 4-Kettfaden-Windung) verstärkten Bioverbundwerkstoffe zeigten die höchste Festigkeit und Steifigkeit im Vergleich zu den anderen textilen Bioverbundwerkstoffen und dem puren PBAT. Dieses Resultat wurde der Beschaffenheit der 4x4-flachfasergewebten Webart zugewiesen. Das Aminopropyltriethoxysilan beeinträchtigte die mechanischen Eigenschaften und Wasseraufnahme der entstandenen Verbundlaminate durch Oberflächenkompatibilität zwischen der Flachsfaser und dem PBAT. HYBRIDE VERBUNDWERKSTOFFE Polyethylen/Nanopartikel, natürliche und tierische Verbundwerkstoffe Binäre und ternäre Verbundwerkstoffe, bestehend aus hoch dichtem Polyethylen (HDPE), Böhmit Aluminumoxid (BA) und verschiedenen natürlichen und tierischen Fasern wie Flachs, Schwammgurke (SG), Palmfaser und Schweinehaar (PH), wurden im Pressverfahren hergestellt. Vorbereitend wurden wasserhaltige BA-Suspensionen auf die HDPE/Flachsmatte gesprüht um nanopartikel/naturfaserverstärkte ternäre Polymer-Verbundwerkstoffe nach dem Trocknen zu erhalten. Die Verteilung der Natur-,Tierfasern und der BA-Partikel in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop untersucht und diskutiert. Die thermomechanischen und Spannungsrelaxation-Eigenschaften der jeweiligen Verbundwerkstoffe wurden in der thermogravimetrischen Analyse (TGA), der dynamisch mechanischen Thermoanalyse (DMTA) und dem Kurzzeit-Stressrelaxationstest (bei unterschiedlichen Temperaturen durchgeführt) bestimmt. Die HDPE-basierten Verbundwerkstoffe wurden Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstests unterzogen. Es wurde festgestellt, dass alle Verbundwerkstoffsysteme eine Erhöhung der Steifigkeit und Spannungsrelaxation und eine Verminderung der Kerbschlagzähigkeit aufzeigten. Die Spannungsrelaxations-Steifigkeit von Naturfaser-, Tierfaserverbundwerkstoffen war größer im Vergleich zu reinem HDPE. Diese Steifigkeit steig deutlich an mit der Einbindung von BA. Die Hauptkurven der Relaxation wurden mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Die Umkehrung des Findley Potenzgesetzes konnte gut für die Beschreibung der Relaxations-Steifigkeit vs. Zeitüberwachung in allen untersuchten Systemen angewendet werden. Die Einbindung der BA-Partikel erhöhte den Wärmewiderstand, welcher bei höherer Temperatur zu sinken begann im Vergleich zu HDPE/Flachsmatten-Verbundwerkstoff. Der HDPE/Flachsmatte/BA-Verbundwerkstoff konnte die Wasseraufnahme verringern. Polyethylen/Flachs/SiO Verbundwerkstoffe Verbundwerkstoffe bestehend aus hoch dichtem Polyethylen (HDPE), Flachsfasertextilgewebe (Flachsgewebeform 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) und Siliziumdioxid (SiO2) wurden im Pressverfahren mit Nanospritztechnik hergestellt. Die SiO2 Schlämme wurden auf beide Oberflächen des Flachsfasergewebes per Hand gesprüht. Die HDPE/ Flachsfasergewebe-Verbundwerkstoffe wurden in einer Laborpresse im Pressverfahren mit und ohne Nanospritztechnik hergestellt. Die Verteilung der SiO2-Partikel und des Flachs in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop (SEM) untersucht. Die ähnlichen HDPE-basierten Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Der Wärmewiderstand, Steifigkeit- und Zugfestigkeit-Eigenschaften der jeweiligen Verbundwerkstoffe wurden in thermogravimetrischen Analysen (TGA), dynamisch mechanischen Thermoanalysen (DMTA) und Zugversuchen bestimmt. Es zeigte sich, dass die Aufprallenergie und Steifigkeitswerte der HDPE/Flachs-Verbundwerkstoffe deutlich höher als die des HDPE waren aber die Effekte von Verbundwerkstoffen mit Flachsinhalt widerspiegeln. Die Einbindung von SiO2-Partikeln erhöhte den Widerstand von thermischer Degradierung. Es wurde bestimmt, das das Prinzip der linear viskoelastischen Werkstoffe gut anwendbar auf die Umwandlung der Steifigkeit zu Kriechneigungsergebnissen ist. Modifizierte und nicht modifizierte Polylactid (PLA)/Flachsfasergewebe-Verbundwerkstoffe Hybride Verbundwerkstoffe aus Polypropylen (PP) oder hoch-dichtem Polyethylen (HDPE), verschiedenen Flachsfasern (unidirektional, biaxial und 2x2 Körper) und Siliziumdioxid (SiO2) wurden im Pressverfahren hergestellt. Der ternäre Polymer-Verbundwerkstoff wurde wirkungsvoll durch das Aufbringen von SiO2 Lösemitteln auf die Oberfläche der Flachsfaser hergestellt. Die Verteilung der SiO2-Partikel und des Flachs in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop (SEM) untersucht. Die ähnlichen PP- und HDPE-basierten Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die thermischen und mechanischen Eigenschaften der respektiven Verbundwerkstoffe wurde in thermogravimetrischen Analysen (TGA), dynamisch mechanischen Thermoanalysen (DMTA), Kriech- und Spannungsrelaxations-Tests bestimmt. Es zeigte sich, dass die thermische Zersetzungstemperatur der PP oder HDPE/Flachs-Verbundwerkstoffe durch das Auftragen der SiO2-Partikel ansteigt. Die Aufprallenergie-, Steifigkeit-, Kriechbeständigkeit- und Relaxation-Steifigkeitn-Werte aller Flachs-Verbundwerkstoffe stiegen deutlich an im Vergleich zur PP und HDPE Matrix. Die Zeit-Temperatur-Überlagerung (TTS) wurde angewandt um die Kriech- und Relaxation-Steifigkeit für die Verbundwerkstoffe als Funktion der Zeit in Form einer Hauptkurve zu schätzen. Die Aktivierungsenergien aller untersuchten PP und HDPE-Verbundwerkstoffsysteme wurden mit der Arrhenius Gleichung errechnet. Das generalisierte Maxwell Model war gut auf die Spannungsrelaxationsergebnisse anwendbar. Polylactide (PLA)/Flachsfasertextilgewebe/Böhmit Aluminiumoxid (BA)-Verbundwerkstoffe Verbundwerkstoffe bestehend aus Polylactid (PLA), Flachfasertextilgewebe (Gewebeform 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) und Böhmit Aluminium (BA) wurden im Pressverfahren hergestellt. Für die Vordispergierung der Aluminiumoxid-Nanopartikel wurde die Spritztechnik angewendet. Die wasserhaltigen Aluminiumoxid-Schlämme wurden durch das Vermischen von Wasser mit wasserdispergierbarem Aluminiumoxid hergestellt. Die Verteilung der Flachsstrukturen und Aluminiumoxid-Partikeln in den Verbundwerkstoffen wurde mit einem Rasterelektronenmikroskop (SEM) untersucht. Die PLA-Verbundwerkstoffe wurden Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstests unterzogen. Die Kriech- und thermomechanischen Eigenschaften der jeweiligen Verbundwerkstoffe wurden in Kurzzeit-Kriechversuchen (bei unterschiedlichen Temperaturen durchgeführt), thermogravimetrischen Analysen (TGA) und dynamisch mechanischen Thermoanalysen (DMTA) bestimmt. Es zeigte sich, dass das Einbringen der Aluminiumoxid-Partikel die Wasseraufnahme im Vergleich zu PLA/Flachs-Gemischen reduziert. Die Aufprallenergie- und Steifigkeitswerte der PLA/Flachs-Gemische waren signifikant höher als die des PLA aber spiegelten die Effekte von Verbundwerkstoffstrukturen wieder. Das Einbringen von Aluminiumoxid-Partikeln verbesserte die Lagerungs-Steifigkeit und die Kriechbeständigkeit im Vergleich zu PLA/Flachs-Gemischen, erhöhte allerdings leicht den Wärmewiderstand bei hohen Temperaturen. Kein klarer Trend in der Flachswebart konnte dem Temperaturverhalten zugeordnet werden. Die Kriech-Hauptkurven wurden mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Das Findley Potenzgesetz konnte zufriedenstellend die Kriechneigung vs. Zeitüberwachung für alle untersuchten Systeme beschreiben. Poly(Hydroxybutyrat-Co-Hydroxyvalerat)/Natursisalfaser/Ton-Verbundwerkstoffe Poly(Hydroxybutyrat-Co-Hydroxyvalerat) (PHBV) Bioverbundwerkstoffe die Sisalfasern in Längen von 0,25 und 5 mm und Ton-Partikeln enthalten wurden im Heißpressverfahren hergestellt. Die Silan (Bis(Trithoxysilylpropyl)Tetrasulfide) Behandlung wurde für die Modifizierung verwendet um die Eigenschaften von ähnlichen hybriden Verbundwerkstoffen zu verbessern. Alle Verbundwerkstoffe wurden dem Wasseraufnahmetest unterzogen. Die mechanischen Eigenschaften der jeweiligen hybriden Verbundwerkstoffe wie Zugsteifigkeit und Festigkeit, Zähigkeit und Härte wurden in Zugversuchen, Schlagtests und Härteprüfungen bestimmt. Es zeigte sich, dass die Zugfestigkeit, Steifigkeit und Schlagzähigkeit von langen Sisalfasern sich mit der Erhöhung des Fasergehalts verbessert. Behandeltes Silan von langen Fasern mit 20 wt.% Belastung zeigte eine Verbesserung der Faser-Zugfestigkeit um 10% und Schlagzähigkeit von 750% im Vergleich zu reinem PHBV. Diese Besonderheit wurde auch von einem Rasterelektronenmikroskop bestätigt. Weiterhin ist die Härte und Wasserbeständigkeit in PHBV/Sisal-Verbundwerkstoffen durch das Einbringen von Ton-Partikeln angestiegen. Die Diffusionskoeffizienten für die untersuchten PHBV- und hybriden Verbundwerkstoffsysteme wurden auch errechnet.

Biocomposites made from biodegradable polymer as matrix and natural fiber as reinforcement are certainly environmentally friendly materials. Both constituent materials are fully biodegradable and do not leave any noxious components on Earth. The natural fibers have been used as reinforcement due to their advantages compared to glass fibers such as low cost, high specific strength and modulus, low density, renewability and biodegradability. Major aims of this work were to produce natural fibers and/or nanoparticles with polyethylene (PE), polypropylene (PP) and polylactide (PLA), poly(hydroxybutyrate-co-hydroxyvalerate)(PHBV) matrices and determine their structure-property relationships. Following abstracts of the present research work are manifold: BINARY COMPOSITES Polylactide (PLA)/flax mat composites The polylactide (PLA)/flax mat and modified PLA/flax mat composites were produced by hot press technique. Two additives of non-regulated wax/ethylene acrylate copolymer/butyl acrylate and acrylic were used as modifier for PLA. The dispersion of the flax mat in the composites was studied by scanning electron microscopy (SEM). The PLA composites were subjected to instrumented falling weight impact test. The mechanical and thermal properties of the composites were determined in tensile test, thermogravimetric analysis (TGA) and dynamic-mechanical thermal analysis (DMTA), respectively. It was found that the PLA based composites increased the impact resistance. The tensile strength value of modified PLA/flax mat composite decreased slightly compared to the PLA. The elongation at break data indicated that an improvement in ductility of modified PLA and its composites. Moreover, addition of thermal modifier enhanced thermal resistance below processing temperature of PLA and had a marginal effect on the glass transition temperature of PLA. The storage modulus master curves were constructed by applying the time-temperature superposition (TTS) principle. The principle of linear viscoelastic material was fairly applicable to convert from the modulus to the creep compliance for all systems studied. Polylactide (PLA)/woven flax textiles composites The polylactide (PLA)/woven flax textiles 2x2 twill and 4x4 hopsack composites were produced by interval hot press technique. Two weave styles of flax used to reinforce in PLA. The dispersion of the flax composite structures in the composites was inspected in scanning electron microscopy (SEM). The PLA composites were subjected to instrumented falling weight impact test. The mechanical properties (tensile, stiffness and strength) of the composites were determined in tensile and dynamic-mechanical thermal analysis (DMTA) tests, respectively. SEM observed that the interfacial gaps around pulled-out fibers were improved when produced by the interval hot press. It was also found that the both styles of flax composites increased the impact resistance compared to the neat PLA. The tensile strength and stiffness value of PLA/flax composites were markedly higher than that of the neat PLA and reflect the effects of composite structures. The calculated storage creep compliance was constructed by applying the time-temperature superposition (TTS) principle. The calculated creep response of these flax composites was much lower than that of the neat PLA. Polyethylene and polypropylene/nano-silicon dioxide/flax composites Composites composed of polylactide (PLA), modified PLA and woven flax fiber textiles (Flax weave style of 2x2 twill and 4x4 hopsack) were produced by hot press technique. Two structurally different additives used to modify PLA. The dispersion of the flax composite structures in the composites was studied by scanning electron microscopy (SEM) and computed microtomography system (µCT). The PLA composites were subjected to water absorption and instrumented falling weight impact tests. The thermomechanical and creep properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA)and short-time creep tests, respectively. It was found that the modified PLA and its composite increased the impact resistance compared to the unmodified PLA. Incorporation of flax decreased resistance to thermal degradation and increased water uptake. The impact energy and stiffness value of PLA/flax composites was markedly higher than that of PLA but reflect the effects of composite structures and flax content. The storage modulus master curves were constructed by applying the time-temperature superposition (TTS) principle. From the master curve data, the effect of modified PLA on the storage modulus was more pronounced in the low frequencies range. Polylactide (PLA)/woven flax fiber textiles/boehmite alumina (BA) composites The textile biocomposites made from woven and non-woven flax fibre reinforced poly(butylene adipate-co-terephthalate) (PBAT) were prepared by compression moulding using film stacking method. The mechanical properties (such as tensile strength and stiffness, flexural strength and modulus, and impact strength) of textile biocomposites were determined in tensile, flexural and impact tests, respectively. The PBAT-based composites were subjected to water absorption. The comparison of the mechanical properties was made between pure PBAT and textile composites. The influence of flax weave styles on the mechanical properties was also evaluated. The results showed that the strength of the textile biocomposites was increased according to weave types of fibers, especially in the stiffness was significantly increased with the higher densification of the fibers. The 4x4-plain woven fibers (4-yard-wrap and 4-yard-weft weave direction) reinforced biocomposite indicated the highest strength and stiffness compared to the other textile biocomposites and pure PBAT. This was considered to be as the result of the character of weave style of 4x4-plain woven fibers. The aminopropyltriethoxysilane affected the mechanical properties and water absorption of the resulting composites laminates due to the surface compatibility between flax fiber and PBAT. HYBRID COMPOSITES Polyethylene/nanoparticle, natural and animal composites Binary and ternary composites composed of high-density polyethylene (HDPE), boehmite alumina (BA) and different kinds of natural-, animal fibers, like flax, sponge gourd (SG), palm and pig hair (PH) were produced by hot press technique. Aqueous BA suspensions were sprayed on the HDPE/flax mat to prepare nanoparticle/natural fiber reinforced ternary polymer composites followed by drying. The dispersion of the natural-, animal fibers and BA particles in the composites was studied by scanning electron microscopy (SEM) and discussed. The thermomechanical and stress relaxation properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA) and short-time stress relaxation tests (performed at various temperatures), respectively. The HDPE based composites were subjected to water absorption and instrumented falling weight impact tests. It was found that the all composites systems increased the stiffness, stress relaxation and reduced the impact toughness. The stress relaxation modulus of natural-, animal fiber composites were higher compared to that of the neat HDPE. This modulus increased greatly with in corporation of BA. The relaxation master curves were constructed by applying the time-temperature superposition (TTS) principle. The inverse of Findley power law could fairly applicable to describe the relaxation modulus vs. time traces for all systems studied. Incorporation of BA particles enhanced the thermal resistance which started to degrade at higher temperature compared to the HDPE/flax mat composite. The HDPE/flax mat/BA composite could reduce the water uptake. Polyethylene/Flax/SiO2 Composites Composites composed of high-density polyethylene (HDPE), woven flax fiber textiles (Flax weave style of 2x2 twill and 4x4 hopsack) and silicon dioxide (SiO2) were produced by hot press with nano spraying technique. The SiO2 slurries were sprayed by a hand onto the both surface of the woven flax fiber. The HDPE /woven flax fibers composites with and without used nano-spraying technique were produced by hot pressing in a laboratory press. The dispersion of SiO2 particles and flax in the composites was studied by scanning electron microscopy (SEM). The related HDPE based composites were subjected to instrumented falling weight impact test. The thermal resistance, stiffness and tensile strength properties of the composites were determined in thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA) and tensile tests, respectively. It was found that the impact energy and stiffness value of HDPE/flax composites was markedly higher than that of HDPE but reflect the effects of composite structures and flax content. Incorporation of SiO2 particles enhanced resistance to thermal degradation. It was established that the linear viscoelastic material principle are fairly applicable to convert from the modulus to the creep compliance results. Un- and Modified Polylactide (PLA) /woven Flax Fiber composites Hybrid composites composed of polypropylene (PP) or high-density polyethylene (HDPE), different flax fibers (unidirectional-, biaxial and twill2x2) and silicon dioxide (SiO2) were produced by hot press technique. The ternary polymer composite was effectively fabricated by spraying SiO2 solvents onto the surface of flax fiber. The dispersion of SiO2 particles and flax in the composites was studied by scanning electron microscopy (SEM). The related PP and HDPE based composites were subjected to instrumented falling weight impact test. The thermal and mechanical properties of the composites were determined by thermogravimetric analysis (TGA), dynamic-mechanical thermal analysis (DMTA), creep and stress relaxation tests, respectively. It was found that thermal decomposition temperature of the PP or HDPE/flax composites increased by the addition of SiO2 particles. The impact energy, stiffness, creep resistance and relaxation modulus value of all flax composites increased markedly compared to the PP and HDPE matrix. Time–temperature superposition (TTS) was applied to estimate the creep and relaxation modulus of the composites as a function of time in the form of a master curve. The activation energies for the all PP and HDPE composites systems studied were also calculated by using the Arrhenius equation. The generalized Maxwell model was fairly applicable to the stress relaxation results. Polylactide (PLA)/woven flax fiber textiles/boehmite alumina (BA) composites Composites composed of polylactide (PLA), woven flax fiber textiles (weave style of 2x2 twill and 4x4 hopsack) and boehmite alumina (BA) were produced by hot press. The spraying technique served for the pre-dispersion of the alumina nanoparticles. The aqueous alumina slurry was produced by mixing the water with water dispersible alumina. The dispersion of the flax structures and alumina particles in the composites was studied by scanning electron microscopy (SEM). The PLA composites were subjected to water absorption and instrumented falling weight impact tests. The creep and thermomechanical properties of the composites were determined in short-time creep tests (performed at various temperatures), thermogravimetric analysis (TGA) and dynamic-mechanical thermal analysis (DMTA), respectively. It was found that the incorporation of alumina particles reduced the water uptake compared to the PLA/flax blends. The impact energy and stiffness value of PLA/flax blends was markedly higher than that of PLA but reflected the effects of composite structures. Incorporation of alumina particles enhanced storage modulus and the creep resistance compared to the PLA/flax blends but slightly incremented thermal resistance at high temperature. No clear trend in the flax weave style- effect was found in the thermal behaviour. The creep master curves were constructed by applying the time-temperature superposition (TTS) principle. The Findley power law could satisfactorily describe the creep compliance vs. time traces for all systems studied. Poly(hydroxybutyrate-co-hydroxyvalerate)/sisal natural fiber/clay composites Poly(hydroxybutyrate-co-hydroxyvalerate)(PHBV) biocomposites different sisal containing with the fiber length of 0.25 and 5 mm, and addition of clay particles were prepared by hot compression technique. Silane (Bis(triethoxysilylpropyl)tetrasulfide) treatment has been used to modify in order to enhance the properties of related hybrid composites. The all composites were subject to water absorption test. The mechanical properties of hybrid composites such as tensile stiffness and strength, toughness and hardness determined in tensile, impact and hardness tests, respectively. It was found that tensile strength, stiffness and impact strength of long sisal fiber improved with increasing fiber content. Hardness of short sisal fiber improved with increasing fiber content. Treated Silane of long fibers at 20 wt.% loading was found to enhance the tensile strength fiber by 10% and impact strength by 750% as compared to the neat PHBV. Note that this feature was also confirmed by the appearance of a scanning electron microscopy. Moreover, the hardness and water resistance of the PHBV/sisal composites increased by the addition of clay particles. The diffusion coefficient for the PHBV and hybrid composites systems studied were also calculated
Bioverbundwerkstoffe aus biologisch abbaubarem Polymer als Matrix und Naturfasern als Verstärkung sind ohne weiteres umweltfreundliche Materialien. Beide Bestandsmaterialien sind vollständig biologisch abbaubar und hinterlassen keine schädlichen Bestandteile auf der Erde zurück. Die als Verstärkung verwendeten Naturfasern wurden aufgrund ihrer Vorteile gegenüber Glasfasern, wie z.B. geringe Kosten, hohe spezifische Festigkeit und Steifigkeit, geringe Dichte, Erneuerbarkeit und Kompostierbarkeit ausgesucht. Der Hauptfokus dieser Arbeit lag darin Naturfasern und/oder Nanopartikel mit Polyethylen (PE), Polypropylen (PP) und Polylactid (PLA) herzustellen, sowie Poly-Hydroxybutyrat-Co-Hydroxyvalerat (PHBV) Matrizen und deren Struktur-Eigenschaft-Verhältnis zu bestimmen. Die folgenden Kurzfassungen der vorliegenden Forschungsarbeit sind vielfältig: BINÄRE VERBUNDWERKSTOFFE Polylactid (PLA)/ Flachsmatten-Verbundwerkstoffe Die Polylactid (PLA)/Flachsmatte und modifizierte PLA/Flachsmatten-Verbundwerkstoffe wurden im Pressverfahren hergestellt. Als Modifikator für das PLA wurden zwei nicht regulierte Wachs/Ethylen-Acrylat-Copolymer/Butyl-Acrylat und Acryl Additive verwendet. Die Verteilung der Flachsmatte in den Verbundwerkstoffen wurde mit dem Rasterelektronenmikroskop (SEM) untersucht. Die PLA-Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die mechanischen und thermischen Eigenschaften der Verbundwerkstoffe wurden im Zugversuch, der thermogravimetrische Analyse (TGA) und der dynamisch mechanischen Thermoanalyse (DMTA) jeweils bestimmt. Es zeigte sich, dass die PLA/Flachsmatten-basierten Verbundwerkstoffe eine erhöhte Schlagzähigkeit aufwiesen. Die Zähigkeitswerte der modifizierten PLA/Flachsmatten-Verbundwerkstoffe waren leicht verringert im Vergleich zum PLA. Die Bruchdehnungswerte zeigten eine Verbesserung der Verformbarkeit des modifizierten PLAs und dessen Verbundwerkstoffe. Nach Zugabe eines Wärme-Modifikators verbesserte sich der Wärmewiderstand auf unter Verarbeitungstemperatur des PLA und hatte nur einen unwesentlichen Einfluss auf die Glasübergangstemperatur des PLA. Die Hauptkurve des Speichermoduls wurde mit der Zeit-Temperatur-Überlagerung (TTS) aufgestellt. Auf alle untersuchten Systeme konnte das dafür gut geeignete Prinzip der linear viskoelastischen Werkstoffe angewendet werden um die Steifigkeit in die Kriechneigung umzuwandeln. Polylactid (PLA)/Flachstextilgewebe-Verbundwerkstoffe Die Polylactid (PLA)/Flachstextilgewebe 2x2 Körper und 4x4 Gewebe mit Leinwandbindung-Verbundwerkstoffe wurden im Intervall-Pressverfahren hergestellt. Das PLA wurde mit zwei Flachsgewebeformen verstärkt. Die Verteilung der Flachs-Verbundwerkstoffstrukturen in den Verbundwerkstoffen wurde mit dem Rasterelektronenmikroskop (SEM) untersucht. Die PLA Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die mechanischen Eigenschaften (Zugfestigkeit, Steifigkeit und Festigkeit) der jeweiligen Verbundwerkstoffe wurden in Zugversuchen und dynamisch mechanischen Thermoanalysen (DMTA) bestimmt. Das Rasterelektronenmikroskop zeigte auf, das der Grenzflächenzwischenraum von rausgezogenen Fasern sich durch das Herstellen im Intervall-Pressverfahren verbessert hat. Auch zeigte sich, dass beide Arten der Flachs-Verbundwerkstoffe die Schlagzähigkeit der Verbundwerkstoffe erhöht im Vergleich zum puren PLA. Die Zugfestigkeit- und Steifigkeitswerte der PLA/Flachs-Verbundwerkstoffe waren deutlich höher als die der puren PLA und spiegeln die Effekte von Verbundwerkstoffstrukturen wieder. Die berechnete Kriechneigung im Speichermodul wurde durch die Anwendung des Zeit-Temperatur-Überlagerung (TTS) Prinzips aufgestellt. Die errechnete Kriechgeschwindigkeit der Flachs-Verbundwerkstoffe war wesentlich geringer als im puren PLA. Polyethylen und Polypropylen/Nanosilikon Dioxid/Flachs-Verbundwerkstoffe Verbundwerkstoffe hergestellt aus Polylactid (PLA), modifiziertem PLA und Flachsfasertextilgewebe (Flachsgewebeform von 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) wurden im Pressverfahren hergestellt. Zwei strukturell unterschiedliche Additive wurden verwendet um das PLA zu modifizieren. Die Verteilung der Flachs-Verbundwerkstoffstruktur wurde unter dem Rasterelektronenmikroskop (SEM) und dem computergestütztes Computer-Tomography-System (µCT) untersucht. Die PLA Verbundwerkstoffe wurden dem Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die Kriech- und thermomechanischen Eigenschaften der respektiven Verbundwerkstoffe wurden in der thermogravimetrischen Analyse (TGA), der dynamisch mechanischen Thermoanalyse (DMTA) und dem Kurzzeit-Kriechversuch bestimmt. Das modifizierte PLA und dessen Verbundwerkstoffe zeigten eine Erhöhung der Schlagzähigkeit im Vergleich zum unmodifizierten PLA. Die Einbindung von Flachs verringerte den Widerstand gegenüber thermischer Degradierung und erhöhte die Wasseraufnahme. Die Schlagenergie- und Steifigkeitswerte der PLA/Flachs-Verbundwerkstoffe war deutlich höher als die der PLA aber spiegelt die Effekte von Verbundwerkstoffstrukturen mit Flachsinhalt wieder. Die Hauptkurve des Speichermoduls wurde mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Das Datenmaterial der Hauptkurve zeigte den Effekt des modifizierten PLAs auf dem Speichermodul deutlich ausgeprägter im Bereich der Niederfrequenz. Polylactide (PLA)/Flachfasertextilgewebe/Böhmit Aluminumoxid (BA)-Verbundwerkstoffe Die textilen Bioverbundwerkstoffe wurden aus flachsfaserverstärkten Poly(Butylen Adipat-Co-Terephtalat) (PBAT) Gewebe und Vlies im Formpressverfahren mit der Folien-Stapelmethode hergestellt. Die mechanischen Eigenschaften (wie Zugfestigkeit und Steifigkeit, Biegefestigkeit, Steifigkeit und Schlagzähigkeit) der jeweiligen textilen Bioverbundwerkstoffe wurde in Zug-, Biege-, und Schlagtests ermittelt. Die PBAT basierten Verbundwerkstoffe wurden dem Wasseraufnahmetest unterzogen. Der Vergleich der mechanischen Eigenschaften wurde zwischen reinem PBAT und textilen Verbundwerkstoffen durchgeführt. Der Einfluss der Flachsgewebeformen auf die mechanischen Eigenschaften wurde ebenfalls untersucht. Die Ergebnisse zeigten das die Festigkeit der textilen Bioverbundwerkstoffe mit der Webart der Fasern anstieg, signifikant in Bezug auf die Steifigkeit bei einer erhöhten Verdichtung der Fasern. Die 4x4 flachfasergewebten (4-Schussfaden-Windung und 4-Kettfaden-Windung) verstärkten Bioverbundwerkstoffe zeigten die höchste Festigkeit und Steifigkeit im Vergleich zu den anderen textilen Bioverbundwerkstoffen und dem puren PBAT. Dieses Resultat wurde der Beschaffenheit der 4x4-flachfasergewebten Webart zugewiesen. Das Aminopropyltriethoxysilan beeinträchtigte die mechanischen Eigenschaften und Wasseraufnahme der entstandenen Verbundlaminate durch Oberflächenkompatibilität zwischen der Flachsfaser und dem PBAT. HYBRIDE VERBUNDWERKSTOFFE Polyethylen/Nanopartikel, natürliche und tierische Verbundwerkstoffe Binäre und ternäre Verbundwerkstoffe, bestehend aus hoch dichtem Polyethylen (HDPE), Böhmit Aluminumoxid (BA) und verschiedenen natürlichen und tierischen Fasern wie Flachs, Schwammgurke (SG), Palmfaser und Schweinehaar (PH), wurden im Pressverfahren hergestellt. Vorbereitend wurden wasserhaltige BA-Suspensionen auf die HDPE/Flachsmatte gesprüht um nanopartikel/naturfaserverstärkte ternäre Polymer-Verbundwerkstoffe nach dem Trocknen zu erhalten. Die Verteilung der Natur-,Tierfasern und der BA-Partikel in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop untersucht und diskutiert. Die thermomechanischen und Spannungsrelaxation-Eigenschaften der jeweiligen Verbundwerkstoffe wurden in der thermogravimetrischen Analyse (TGA), der dynamisch mechanischen Thermoanalyse (DMTA) und dem Kurzzeit-Stressrelaxationstest (bei unterschiedlichen Temperaturen durchgeführt) bestimmt. Die HDPE-basierten Verbundwerkstoffe wurden Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstests unterzogen. Es wurde festgestellt, dass alle Verbundwerkstoffsysteme eine Erhöhung der Steifigkeit und Spannungsrelaxation und eine Verminderung der Kerbschlagzähigkeit aufzeigten. Die Spannungsrelaxations-Steifigkeit von Naturfaser-, Tierfaserverbundwerkstoffen war größer im Vergleich zu reinem HDPE. Diese Steifigkeit steig deutlich an mit der Einbindung von BA. Die Hauptkurven der Relaxation wurden mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Die Umkehrung des Findley Potenzgesetzes konnte gut für die Beschreibung der Relaxations-Steifigkeit vs. Zeitüberwachung in allen untersuchten Systemen angewendet werden. Die Einbindung der BA-Partikel erhöhte den Wärmewiderstand, welcher bei höherer Temperatur zu sinken begann im Vergleich zu HDPE/Flachsmatten-Verbundwerkstoff. Der HDPE/Flachsmatte/BA-Verbundwerkstoff konnte die Wasseraufnahme verringern. Polyethylen/Flachs/SiO Verbundwerkstoffe Verbundwerkstoffe bestehend aus hoch dichtem Polyethylen (HDPE), Flachsfasertextilgewebe (Flachsgewebeform 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) und Siliziumdioxid (SiO2) wurden im Pressverfahren mit Nanospritztechnik hergestellt. Die SiO2 Schlämme wurden auf beide Oberflächen des Flachsfasergewebes per Hand gesprüht. Die HDPE/ Flachsfasergewebe-Verbundwerkstoffe wurden in einer Laborpresse im Pressverfahren mit und ohne Nanospritztechnik hergestellt. Die Verteilung der SiO2-Partikel und des Flachs in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop (SEM) untersucht. Die ähnlichen HDPE-basierten Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Der Wärmewiderstand, Steifigkeit- und Zugfestigkeit-Eigenschaften der jeweiligen Verbundwerkstoffe wurden in thermogravimetrischen Analysen (TGA), dynamisch mechanischen Thermoanalysen (DMTA) und Zugversuchen bestimmt. Es zeigte sich, dass die Aufprallenergie und Steifigkeitswerte der HDPE/Flachs-Verbundwerkstoffe deutlich höher als die des HDPE waren aber die Effekte von Verbundwerkstoffen mit Flachsinhalt widerspiegeln. Die Einbindung von SiO2-Partikeln erhöhte den Widerstand von thermischer Degradierung. Es wurde bestimmt, das das Prinzip der linear viskoelastischen Werkstoffe gut anwendbar auf die Umwandlung der Steifigkeit zu Kriechneigungsergebnissen ist. Modifizierte und nicht modifizierte Polylactid (PLA)/Flachsfasergewebe-Verbundwerkstoffe Hybride Verbundwerkstoffe aus Polypropylen (PP) oder hoch-dichtem Polyethylen (HDPE), verschiedenen Flachsfasern (unidirektional, biaxial und 2x2 Körper) und Siliziumdioxid (SiO2) wurden im Pressverfahren hergestellt. Der ternäre Polymer-Verbundwerkstoff wurde wirkungsvoll durch das Aufbringen von SiO2 Lösemitteln auf die Oberfläche der Flachsfaser hergestellt. Die Verteilung der SiO2-Partikel und des Flachs in den Verbundwerkstoffen wurde unter dem Rasterelektronenmikroskop (SEM) untersucht. Die ähnlichen PP- und HDPE-basierten Verbundwerkstoffe wurden dem instrumentalisierten Fallgewichtsschlagzähigkeitstest unterzogen. Die thermischen und mechanischen Eigenschaften der respektiven Verbundwerkstoffe wurde in thermogravimetrischen Analysen (TGA), dynamisch mechanischen Thermoanalysen (DMTA), Kriech- und Spannungsrelaxations-Tests bestimmt. Es zeigte sich, dass die thermische Zersetzungstemperatur der PP oder HDPE/Flachs-Verbundwerkstoffe durch das Auftragen der SiO2-Partikel ansteigt. Die Aufprallenergie-, Steifigkeit-, Kriechbeständigkeit- und Relaxation-Steifigkeitn-Werte aller Flachs-Verbundwerkstoffe stiegen deutlich an im Vergleich zur PP und HDPE Matrix. Die Zeit-Temperatur-Überlagerung (TTS) wurde angewandt um die Kriech- und Relaxation-Steifigkeit für die Verbundwerkstoffe als Funktion der Zeit in Form einer Hauptkurve zu schätzen. Die Aktivierungsenergien aller untersuchten PP und HDPE-Verbundwerkstoffsysteme wurden mit der Arrhenius Gleichung errechnet. Das generalisierte Maxwell Model war gut auf die Spannungsrelaxationsergebnisse anwendbar. Polylactide (PLA)/Flachsfasertextilgewebe/Böhmit Aluminiumoxid (BA)-Verbundwerkstoffe Verbundwerkstoffe bestehend aus Polylactid (PLA), Flachfasertextilgewebe (Gewebeform 2x2 Körper und 4x4 Gewebe mit Leinwandbindung) und Böhmit Aluminium (BA) wurden im Pressverfahren hergestellt. Für die Vordispergierung der Aluminiumoxid-Nanopartikel wurde die Spritztechnik angewendet. Die wasserhaltigen Aluminiumoxid-Schlämme wurden durch das Vermischen von Wasser mit wasserdispergierbarem Aluminiumoxid hergestellt. Die Verteilung der Flachsstrukturen und Aluminiumoxid-Partikeln in den Verbundwerkstoffen wurde mit einem Rasterelektronenmikroskop (SEM) untersucht. Die PLA-Verbundwerkstoffe wurden Wasseraufnahme- und instrumentalisierten Fallgewichtsschlagzähigkeitstests unterzogen. Die Kriech- und thermomechanischen Eigenschaften der jeweiligen Verbundwerkstoffe wurden in Kurzzeit-Kriechversuchen (bei unterschiedlichen Temperaturen durchgeführt), thermogravimetrischen Analysen (TGA) und dynamisch mechanischen Thermoanalysen (DMTA) bestimmt. Es zeigte sich, dass das Einbringen der Aluminiumoxid-Partikel die Wasseraufnahme im Vergleich zu PLA/Flachs-Gemischen reduziert. Die Aufprallenergie- und Steifigkeitswerte der PLA/Flachs-Gemische waren signifikant höher als die des PLA aber spiegelten die Effekte von Verbundwerkstoffstrukturen wieder. Das Einbringen von Aluminiumoxid-Partikeln verbesserte die Lagerungs-Steifigkeit und die Kriechbeständigkeit im Vergleich zu PLA/Flachs-Gemischen, erhöhte allerdings leicht den Wärmewiderstand bei hohen Temperaturen. Kein klarer Trend in der Flachswebart konnte dem Temperaturverhalten zugeordnet werden. Die Kriech-Hauptkurven wurden mit dem Zeit-Temperatur-Überlagerung (TTS) Prinzip aufgestellt. Das Findley Potenzgesetz konnte zufriedenstellend die Kriechneigung vs. Zeitüberwachung für alle untersuchten Systeme beschreiben. Poly(Hydroxybutyrat-Co-Hydroxyvalerat)/Natursisalfaser/Ton-Verbundwerkstoffe Poly(Hydroxybutyrat-Co-Hydroxyvalerat) (PHBV) Bioverbundwerkstoffe die Sisalfasern in Längen von 0,25 und 5 mm und Ton-Partikeln enthalten wurden im Heißpressverfahren hergestellt. Die Silan (Bis(Trithoxysilylpropyl)Tetrasulfide) Behandlung wurde für die Modifizierung verwendet um die Eigenschaften von ähnlichen hybriden Verbundwerkstoffen zu verbessern. Alle Verbundwerkstoffe wurden dem Wasseraufnahmetest unterzogen. Die mechanischen Eigenschaften der jeweiligen hybriden Verbundwerkstoffe wie Zugsteifigkeit und Festigkeit, Zähigkeit und Härte wurden in Zugversuchen, Schlagtests und Härteprüfungen bestimmt. Es zeigte sich, dass die Zugfestigkeit, Steifigkeit und Schlagzähigkeit von langen Sisalfasern sich mit der Erhöhung des Fasergehalts verbessert. Behandeltes Silan von langen Fasern mit 20 wt.% Belastung zeigte eine Verbesserung der Faser-Zugfestigkeit um 10% und Schlagzähigkeit von 750% im Vergleich zu reinem PHBV. Diese Besonderheit wurde auch von einem Rasterelektronenmikroskop bestätigt. Weiterhin ist die Härte und Wasserbeständigkeit in PHBV/Sisal-Verbundwerkstoffen durch das Einbringen von Ton-Partikeln angestiegen. Die Diffusionskoeffizienten für die untersuchten PHBV- und hybriden Verbundwerkstoffsysteme wurden auch errechnet

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

La régularité de masse linéique (titre) des structures textiles linéaires produites en filature constitue le critère de qualité le plus important. En se basant sur les théories stochastiques classiques de l'étirage en grappes des fibres textiles individualisées, l'auteur a proposé une modélisation originale et très générale applicable à toutes les fibres, individualisées ou agglomérées sous forme de faisceaux fibreux ; cette théorie concerne tout particulièrement les fibres libériennes telles que le jute et le lin qui se présentent toujours sous forme de «faisceaux techniques» dissociables au cours du processus de filature. Les développements théoriques ont été totalement validés par une expérimentation industrielle approfondie réalisée dans le centre d'essais N. Schlumberger, premier constructeur français de matériel de filature. Enfin, la limite de filabilité a été discutée

Natural fibre composites (NFCs) possess relatively good specific strength and stiffness properties. However, natural fibres (NFs) often show relatively poor interfacial adhesion with respect to polymeric matrices, may contain relatively high levels of moisture and have variable mechanical properties due to the route by which they have been harvested and manufactured. These aspects may result in inconsistent mechanical properties of such composites, especially evident in a poor interlaminar fracture toughness. Thus, the present work investigates the mode I interlaminar fracture toughness, of NFCs based upon an anhydride-cured diglycidyl ether of bisphenol-A (DGEBA) epoxy matrix. Further, this matrix was used as a ‘control’ or modified with silica nanoparticles and/or rubbery microparticles. Two types of natural fibres were employed: unidirectional flax fibre (FF) and plain-woven regenerated cellulose fibre (CeF). Two very different routes were explored for the production of the NFCs based upon these materials. One route was via a resin infusion under flexible tooling (RIFT) process and a second route employed a resin transfer moulding (RTM) process. A very low value of the interlaminar fracture energy of about 20 J/m2 was measured for the flax fibre-reinforced plastics (FFRPs), using the ‘control epoxy matrix, produced by the RIFT manufacturing process which was initially employed. However, such composite manufactured via the RTM process possessed fracture energy of about 963 J/m2. Further, this value was found to increase to 1264 J/m2 when the epoxy matrix was modified using a combination of silica nanoparticles and rubbery microparticles. Hence, optimization studies using the RIFT manufacturing process were undertaken which led to a simple modification of this manufacturing route whereby the natural fibres were first oven-dried. This resulted in the final RIFT process giving values of the fracture toughness of the same order as those obtained from the RTM process. Also of note was the observation that the FFRPs manufactured via the RTM or the final RIFT process had similar values of toughness as those measured for glass fibre-reinforced plastics (GFRPs) made using the equivalent type of epoxy matrix. Similar observations were recorded in the case of the cellulose fibre-reinforced plastics (CeFFRPs). The present study has also considered the underlying mechanisms for the above observations and used analytical models to predict the toughening mechanisms and a good agreement between the predictions and the experimental data for the NFCs was obtained.

The different topics of this thesis include high-temperaturestable fiber Bragg gratings, photosensitivity and fiber basedcomponents. Fiber Bragg gratings (FBG) are wavelength dispersiverefractive index structures manufactured through UV exposure ofoptical fibers. Their applications range from WDM filters,dispersion compensators and fiber laser resonators fortelecommunication applications to different types of point ordistributed sensors for a variety of applications. One aim of this thesis has been to study a new type of FBGreferred to as chemical composition grating. These gratingsdiffer from other types of FBG in that their refractive indexstructure is attributed to a change in the chemicalcomposition. Chemical composition gratings have shown to beextremely temperature stable surviving temperatures in excessof 1000 oC. Photosensitivity of pure silica and germanium-dopedcore fibers in the presence of hydroxyl groups has also beenstudied and different types of fiber based components have beendeveloped. The main result of the thesis is a better understanding ofthe underlying mechanism of the formation of chemicalcomposition gratings and their decay behavior at elevatedtemperatures. The refractive index modulation is caused by aperiodic change in the fluorine concentration, which has beenverified through time-of-flight secondary-ion-mass spectrometryand through studies of the decay behavior of chemicalcomposition gratings. A model based on diffusion of dopants hasbeen developed, which successfully predicts the thermal decayat elevated temperatures. Studies of the dynamics of chemicalcomposition grating formation have resulted in a manufacturingtechnique that allows for reproducible gratingfabrication. The main results regarding photosensitivity is a method tosignificantly increase the effect of UV radiation on standardtelecommunications fiber. The method, referred to asOH-flooding, has also been applied to pure-silica core fibersresulting in the first report of strong grating formation insuch fibers. Finally, research into different schemes for developingfiber-based components has resulted in two types of singlefiber integrated Mach-Zehnder interferometers; one passiveinterferometer that can be used as an optical filter and oneactive interferometer controlled with internal metalelectrodes. Keywords:optical fibers, fiber Bragg gratings,photosensitivity, thermal stability, fiber sensors, chemicalcomposition gratings, fiber components, Mach-Zehnderinterferometer, optical switch, optical modulator.
QC 20100607

Thesis (M. Eng.)--Massachusetts Institute of Technology, Dept. of Civil and Environmental Engineering, 2013.
Cataloged from PDF version of thesis.
Includes bibliographical references (p. 51-52).
The purpose of this study is to compare existing research with aerated concrete and fiber reinforcement to original experiments completed investigating the benefits of adding natural fiber tensile reinforcement to aerated concrete. Concrete is a great composite material which can be created in various proportions and with various materials to alter its strength, density and porosity, amongst other properties. Concrete which is used commonly in construction of columns, beams, and slabs acts well in compression but fails under tension. The common solution is to reinforce the structure in areas where it experiences tension with steel. There are other materials besides steel which also take tension well. Natural fibers for example come in various strengths and types and would create lighter and perhaps more sustainable beam designs. Natural fibers have been used for their availability, workability, and high tensile strengths for centuries. This research discovers that the compressive strength of this cellular material can support the construction of a small structure, assuming accuracy of previous experimental results. These previous experiments discover how the natural fibers distribute within the mixture and how they affect the aeration of the concrete, as well as how they affect the strength. Multiple samples are cured with different fiber types and in different proportions within the mixture. Furthermore, similar experimentation is conducted to discover an ideal ratio of aggregate to aerated concrete mix. The aggregate gives the concrete greater strength and economy, but could negatively affect the aeration. The various concrete mixes are poured and allowed to cure to maximum strength before indirect tensile tests and compression tests are conducted. The effects of creating smooth aerated concrete molds are also investigated. All experiments conducted are precursory to an ultimate tensile reinforced aerated concrete beam design with an aggregate mix and smooth surfaces.
by Leonidia Maria Garbis.
M.Eng.

Natural fibers like kenaf, hemp, flax and sisal fiber are becoming alternatives to conventional petroleum fibers for many applications. One such applications is the use of Non-woven bio-fiber mats in the automobile and construction industries. Non-woven hemp fiber mats were used to manufacture plywood in order to optimize the plywood structure. Hemp fiber mats possess strong mechanical properties that comparable to synthetic fibers which include tensile strength and tensile modulus. This study focuses on the use of hemp fiber mat as a core layer in plywood sandwich composite. The optimization of fiber mat plywood was done by performing a three factor experiment. The three factors selected for this experiment were number of hemp mat layers in the core, mat treatment of the hemp mat, and the glue content in the core. From the analysis of all treatments it was determined that single hemp mat had the highest effect on improving the properties of the plywood structure.

The use of asbestos fibres in construction products has been banned in European countries for about two decades due to its effect on human health. At present, many developing countries use asbestos cement board as one of the most important construction products for roofing, cladding and partition walls. The Hatschek process is the most commonly used method to produce asbestos Fibre Cement Board (FCB). There are two major problems for the asbestos FCB manufacturers in replacing their products with non-asbestos FCB. The first one is finding materials and fibres that are available and competitive in price compared to asbestos fibres, and the second is providing inexpensive machines and equipment to produce non-asbestos FCB. In this research, an effort has been made to solve these two major problems. After the initial laboratory investigations on several natural and synthetic fibres some of the fibres with potential use in FCB were chosen for the further investigations. A slurry vacuum dewatering process was then designed and made for the laboratory use. The performance of material selections and mix designs selected from the laboratory studies were subsequently verified with factory Hatschek process in a factory site trial. Many specimens with natural and synthetic fibres incorporating silica fume and limestone powder were made and tested in the laboratory. Silica fume and limestone powder were used for enhancing flexural strength and suppression of alkalinity to reduce breakdown of the cellulose fibres. The results of mechanical, physical and II durability tests were analysed. The microstructure of the fibres and composites was also studied by SEM (Scanning Electron Microscopy). At some stages, mix design optimization was carried out to gain the highest flexural strength. The most suitable mixes were chosen for the factory site trials. A number of full-scale non-asbestos trial boards were made successfully in an asbestos FCB factory and tested in accordance with the current national and international standards. The results indicated that the trial boards fulfilled the requirements of the relevant standards. Based on the outcome of this research, a combination of acrylic fibres and waste cardboard in a mix incorporating silica fume and limestone powder in addition to Portland cement can be used to replace asbestos fibres. Although broadly compatible with the asbestos cement production process, this formulation change will necessitate some changes to the existing production lines in asbestos cement factories to produce non-asbestos FCB.

It is believed, that due to the large surface areas provided by the nano scale materials, various composite properties could be enhanced when such particles are incorporated into a polymer matrix. There is also a trend of utilizing natural resources or reusing and recycling materials that are already available for the fabrication of the new composite materials. Cellulose is the most abundant natural polymer on the planet, and therefore it is not surprising to be of interest for composite fabrication. Basic structures of cellulose, comprised of long polysaccharide chains, are the building blocks of cellulose nano fibers. Nano fibers are further bound into micro fibrils and macro fibers. Theoretically pure cellulose nano fibers have tremendous strengths, and therefore are some of the most sought after nano particles. The fiber extraction however is a complex task. The ultrasound, which creates pressure variation in the medium, was employed to extract nano-size cellulose particles from microcrystalline cellulose (MCC). The length and the intensity of the cavitations were evaluated. Electron microscopy studies revealed that cellulose nanoparticles were successfully obtained from the MCC after ultrasound treatment of just 30 minutes. Structure of the fractionated cellulose was also analyzed with the help of X-ray diffraction, and its thermal properties were evaluated with the help of differential scanning calorimetry (DSC). Ultrasound treatment performed on the wheat straw, kenaf, and miscanthus particles altered fiber structure as a result of the cavitation. The micro fibers were generated from these materials after they were subjected to NaOH treatment followed by the ultrasound processing. The potential of larger than nano-sized natural fibers to be used for composite fabrication was also explored. The agricultural byproducts, such as wheat or rice straw, as well as other fast growing crops as miscanthus or kenaf, are comprised of three basic polymers. Just like in wood the polymers are: cellulose, hemicelluloses, and lignin. When subjected to elevated pressures and temperatures, we are able to get access to some of these natural polymers and use them as a matrix material for composite fabrication. Therefore, fabrication of composite materials without addition of synthetic polymers is possible. Thermal and mechanical properties of such composites are evaluated with the help of electron microscopy, differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), thermogravimetric analysis (TGA), and flexural strength measurements. The chemical changes in the composites are also probed with the help of Fourier transform infrared (FTIR) analysis. Various additives introduced into composite materials provide different properties. The addition of small amounts of synthetic polymers further enhances the properties of natural fiber composites and do not require high fabrication pressures. Calcium sulfite crystals, which are one of the coal combustion products, were combined with the natural fibers and recycled HDPE polymer to form wood substitute composites. The introduction of these additives resulted in composites with the properties similar to those of the natural wood. Coal combustion products, often used in composite material fabrication, contain mercury which may be rereleased during composite fabrication. Mercury behavior under composite fabrication conditions, such as elevated pressures and temperatures were evaluated. Sulfite rich scrubber material, generated during the flue gas desulphurization process was the main target of the study. It was observed that the release of the mercury is highly dependent on the composite fabrication pressure as well as the temperature.

Natural fiber composites, (NFC) are defined in this work as a group of materials where at least the fibers originates from renewable and CO2 neutral resources. NFC consists of a polymer matrix and a natural fiber. The fibers which originate from wood or plants can replace non-renewable fibers or fillers or simply replace part of the plastic. If plastics from renewable resources are used, NFC is a 100% renewable material. Even though there is very large variety of fibers, matrices and manufacturing techniques used to produce NFC, these materials are often separated as its own material class. However, the variety of constituents and processing methods result in completely different materials with very diverse properties. NFC could thus be suitable for an extremely wide area of applications. We believe that it is important to distinguish different types of NFC and classify them based on matrix (thermoplastic or thermoset), fiber (long or short/orientation) and manufacturing techniques. For instance compression molded composites are very different from injection molded materials. Therefore it is important to find the limits of their performance in connection to the processing parameters. The focus of this work is on the compounding and injection molding techniques. Although extensive research has been done on injection molded NFC, this is one area where the natural fibers still have not made a market breakthrough. We believe that the reason for the limited use of natural fiber compound in injection molded products is partly due to uncertainties about the influence of different constituents on the final properties and lack of defined framework for product design and manufacturing in order to optimize the material and assure consistent quality. Although deep knowledge about these materials have been accumulated among producers and researchers in this area, guidelines or simple rules of thumb for NFC development and processing are quite hard to find in literature. Thus, in order to make natural fiber compounds a more interesting alternative for the injection molding industry, this work is focused on finding limitations on important properties and giving general guidelines for material optimization and processing of natural fiber composites.

Godkänd; 2007; 20070523 (ysko)

The automotive and construction industries are actively involved in substituting natural fibre composites (NFCs) for other engineering materials in motor vehicles and buildings. In this work, emphasis has been placed on evaluating agave fibre composites containing well aligned, closely packed straight fibre bundles and focussing on the development of different types of practical joints for NFCs in composite structures. Two novel co-cured joints were proposed and evaluated, based on laminated and intermingled configurations.

Pipeline natural gas is the primary fuel of choice for distributed fuel cell-based applications. The concentration of sulfur in odorized natural gas is about 30 ppm, with acceptable levels being <1 ppm for catalyst stability in such applications. Packed bed technology for desulfurization suffers from several disadvantages including high pressure drop and slow regeneration rates that require large unit sizes. We describe a novel Rapid Temperature Swing Adsorption (RTSA) system utilizing hollow fibers with polymer 'binder', impregnated with high loadings of sulfur selective sorbent 'fillers'. Steam and cooling water can be utilized to thermally swing the sorbent during the regeneration cycles. An impermeable, thin polymer barrier layer on the outside of fiber sorbents allows only thermal interactions with the regeneration media, thereby promoting consistent sorption capacity over repeated cycles. A simplified flow pattern minimizes pressure drop, porous core morphology maximizes sorption efficiencies, while small fiber dimensions allows for rapid thermal cycles.

Compared to the conventional amine adsorption process to separate CO₂ from natural gas, the membrane separation technology has exhibited advantages in easy operation and lower capital cost. However, the high CO₂ partial pressure in natural gas can plasticize the membranes, which can lead to the loss of CH₄ and low CO₂/CH₄ separation efficiency. Crosslinking of polymer membranes have been proven effective to increase the CO₂ induced plasticization resistance by controlling the degree of swelling and segmental chain mobility in the polymer. This thesis focuses on extending the success of crosslinking to more productive asymmetric hollow fibers. In this work, the productivity of asymmetric hollow fibers was optimized by reducing the effective selective skin layer thickness. Thermal crosslinking and catalyst assisted crosslinking were performed on the defect-free thin skin hollow fibers to stabilize the fibers against plasticization. The natural gas separation performance of hollow fibers was evaluated by feeding CO₂/CH₄ gas mixture with high CO₂ content and pressure.

Robust industrially relevant membranes for CO₂ removal from aggressive natural gas feed streams were developed and characterized. Asymmetric hollow fiber membranes with defect-free selective skin layers on an optimized porous support substructure were successfully spun and subsequently stabilized by covalent crosslinking within the economical membrane formation process. Thermal treatment conditions, which promote sufficient crosslinking without introducing defects or undesired substructure resistance, were identified. It was found that crosslinking improves membrane efficiency and plasticization resistance as well as mechanical strength of fibers. The capability to maintain attractive separation performance under realistic operating conditions and durability against deleterious impurities suggests that the crosslinked fibers have great potential for use in diverse aggressive applications, even beyond the CO₂/CH₄ example explored in this work.

Thesis (S.B.)--Massachusetts Institute of Technology, Dept. of Architecture, 2013.
Cataloged from PDF version of thesis.
Includes bibliographical references (p. 34).
The purpose of this study is to investigate the benefits of adding natural fiber tensile reinforcement to aerated concrete. Concrete is a great composite material which can be created in various proportions and with various materials to alter its strength, density and porosity, amongst other properties. Concrete which is used commonly in construction of columns, beams, and slabs acts well in compression but fails under tension. The common solution is to reinforce the structure in areas where it experiences tension with steel. There are other materials besides steel which also take tension well. Natural fibers for example come in various strengths and types and would create lighter and perhaps more sustainable beam designs. Natural fibers have been used for their availability, workability, and high tensile strengths for centuries. This research discovers how the natural fibers distribute within the mixture and how they affect the aeration of the concrete, as well as how they affect the strength. Multiple samples are cured with different fiber types and in different proportions within the mixture. Furthermore, similar experimentation is conducted to discover an ideal ratio of aggregate to aerated concrete mix. The aggregate gives the concrete greater strength and economy, but could negatively affect the aeration. The various concrete mixes are poured and allowed to cure to maximum strength before indirect tensile tests and compression tests are conducted. The effects of creating smooth aerated concrete molds are also investigated. All experiments conducted are precursory to an ultimate tensile reinforced aerated concrete beam design with an aggregate mix and smooth surfaces.
by Leonidia Maria Garbis.
S.B.

Interest in natural fiber reinforced composites (NFRCs) is increasing rapidly thanks to their numerous advantages such as low cost, biodegradability, eco-friendly nature, relatively good mechanical properties, and a growing emphasis on the environmental and sustainability aspects of engineering materials. However, large scale use of NFRCs is still considered as challenging due to the difficulties in manufacturing, limited knowledge of its machinability and appropriate parameter settings, and being prone to machining-induced defects. These materials are known as hard-to-machine materials due to their heterogeneous structure, mechanical anisotropy and tendency to damage while exposed to mechanical stresses. High rejection rate of composite parts at the assembly stage because of poor quality hole due to several vital drilling induced damages such as matrix cracking, fiber pull-out, delamination, fiber and matrix separation and thermal degradation is a serious concern for manufacturing industries. Among all these defects, delamination was found to be the most vital life-limiting factor which affects the mechanical strength and structural integrity of the component significantly in terms of dimensional tolerances and load carrying capability. Therefore, the main objective of this research is investigating the influence of drilling process parameters on the machinability of flax/poly(lactic acid) bio-composites along with characterization, modelling, and condition monitoring of drilling operation through extensive experimental and analytical investigations. The effect of key drilling parameters and tool geometry such as cutting speed, feed rate, drill diameter, drill material and point angle at different levels were studied experimentally to analyse the relations between resultant quality of the produced holes, cutting forces and size of delamination. Damages and defects associated with the drilling process such as delamination, fiber breakage, fiber pull-out, and matrix cracking were studied through qualitative measurements, optical microscopy and scanning electron microscopy examination. Experimental results revealed that the choice of drill bit in terms of diameter, material and point angle has a considerable effect on the machinability and hole performance. Drilling with HSS drills resulted in nearly 60% lower thrust force and better hole quality compared to that with carbide drills. In addition, the analysis of variance (ANOVA) was applied to identify the significance of each individual cutting parameter. Analytical model was developed to predict the critical thrust force related to the onset of delamination propagation during drilling FF/PLA laminates. The delamination zone was modelled as an elliptical plate, with clamped edge and the analytical model developed based on theory of virtual work, LEFM methodology and theory of plate bending. An experimental investigation was carried out, in addition to the analytical model, through a punching test on different configurations of blind hole to characterize the critical thrust force at the onset of delamination. The developed model has been verified by experimental data and compared with the results of existing models and the presented model considering the effect chisel edge and cutting edges. Based on the results, the predicted values by the proposed model present better correlation with the experimental values than those predicted by other models. A relationship exists between cutting variables (thrust and cutting forces), tool wear and the final quality of the drilled hole. Accordingly, the quality of drilled holes can be improved by in-process monitoring in order to record the whole process status through measuring the thrust force and other indicators. An experimental investigation on online monitoring and non-destructive evaluation of drilling operation using vibration, acoustic emission and thrust force signals was conducted and the correlation between the cutting parameters, delamination, cutting thrust force and the pattern of the signals was detected. The response of material through acceleration, force and AE signals were analysed using different signal analysis tools and statistical parameters to derive the features of signals that can express the key characteristics of machining condition. It is observed that the AE rms values are affected by variation in the cutting parameters and it follows a similar trend as observed in the case of drilling thrust force by varying cutting conditions. The variation of vibration and acoustic emission signals were in correlation with delamination factor and damage severity. Four major damage mechanisms have been identified generally as the main sources of AE energy wave in drilling of FF/PLA composites namely fiber breakage, delamination, matrix cracking and friction. A process for detection and discrimination of various damage mechanisms can be correlated to the frequency of damages. Furthermore, among several statistical parameters applied on the effective segment of the time signals, Kurtosis was found the most competent statistical parameter for condition monitoring of the drilling process to to differentiate between poor and good quality of the drilled holes and enhance the quality of composite component. The findings from this research concluded that damage severity can be assessed through AE parameter analysis and it has a considerable potential for the application of in-process monitoring.
Thesis (PhD Doctorate)
Doctor of Philosophy (PhD)
School of Eng & Built Env
Science, Environment, Engineering and Technology
Full Text

Composite materials based on natural bast fibres offer potential commercial and environmental benefits due to the low cost, availiability, and biodegradability of the fibres. However, such benefits cannot be realised without a comprehensive evaluation of processing and properties. This thesis involved a comprehensive evaluation of composites based on two types of natural bast fibre (hemp and flax), and two types of matrix - synthetic (epoxy), and biodegradable (Novamont Mater-Si). The experimental work involved four strands: the effects of growing conditions and fibre processing on the properties of raw bast fibres; the optimisation of a pultrusion process for epoxy-matrix composites; development of a film stacking process for Mater-Bi composites, and a detailed evaluation of the mechanical properties of the composites themselves. Fibre bundles and individual fibre cells were investigated to characterise their structure, with particular focus on compressive kink defects. The kink bands were sectioned using a novel technique of focused ion beam milling, and kinking was found to induce delamination and voiding of the lamellar fibre structure. The defect concentration per unit length was assessed for conventionally-processed fibres and for hemp fibres from plants grown under controlled conditions to assess the effect of wind shear and stem flexure on fibre defect concentration. No effect was found for plant flexure, while industrially processed fibre was found to have increased defect concentration. The loading behaviour of both types of composite was seen to be initially linear with a yield point at 20 - 30 MPa and a transition to nonlinear deformation dominated by damage mechanisms as a result of fibre kinks. Epoxy composites possessed an inital modulus of 30 GPa with a 30 - 60% reduction in modulus after yield. Flax reinforcement was found to increase the modulus of Mater-Bi from 0.1 to 20 GPa and strength from 24 to 169 MPa. Fibre addition was also found to significantly embrittle the polymers.

Improving the thermal performance of existing domestic buildings can have multiple benefits: reducing greenhouse gas emissions, reducing the cost of heating and therefore fuel poverty, improving comfort and health. Solid wall buildings constitute around 30% of UK housing stock, and are among the least efficient. However, the installation of solid wall insulation, while improving thermal performance can significantly affect the moisture balance of the building. This can result in mould growth, which can cause structural damage and lead to health problems for the occupants. This thesis explores the use of Natural Fibre Insulation (NFI) materials for internal solid wall insulation. The hygrothermal properties of a range of NFI materials are characterised in order to assess their potential for retrofit applications. This is followed by large-scale testing, which compares three solid wall insulation systems in controlled conditions, the results of which are used to validate a heat and moisture transfer model to further assess performance. Experimental results showed that the risk of interstitial condensation is significantly reduced by the application of natural fibre insulation in comparison to a conventional rigid foam system. Simulation of a solid wall exposed to climatic conditions for the UK revealed that the relative humidity at the interface between the masonry and insulation layers remained at 69% when internally insulated with hemp-lime and 96% with rigid foam insulation, while average moisture content of the masonry was 48% lower when hemp-lime was used. Field tests were also conducted to determine the thermal performance of two solid walls internally insulated with 80 mm of hemp-lime when exposed to real weather conditions. The thermal conductivity of the hemp-lime was found to be 30% higher than when measured in dry stead-state laboratory conditions due to the high moisture content of the masonry. However, its application still resulted in 66% and 68% reductions in the U-value compared to the uninsulated wall from 2.73 and 2.65 W/m2K to 0.93 and 0.86 W/m2K.

Thesis (MScEng)--Stellenbosch University, 2013.
ENGLISH ABSTRACT: Natural fibre reinforced concrete (NFRC) is a type of concrete that has become of particular interest in recent years, due to its potential for being used as a sustainable and economically viable building material. Natural fibres are often cheap and widely available in developing nations. Sisal is one such fibre predominantly grown in Brazil and has been identified as having the potential to be commercially cultivated in Southern Africa. The durability of sisal fibres in a cementitious environment tends to be adversely affected due to the high alkalinity of pore water and the presence of calcium hydroxide. This research dealt with the use of sisal fibre reinforced concrete (SFRC) blocks. It focused on the mechanical and volumetric properties of blocks with varying fibre and condensed silica fume content (CSF). Two different SFRC blocks were produced (solid and hollow) using an average fibre length of 10 mm. Two matrix types were used: one using a 70:30 cement:fly-ash ratio and another using a 60:30:10 cement:fly-ash:CSF ratio by weight. Samples of each matrix type were prepared with 0, 0.5 and 1% fibre content by volume. Hollow blocks were tested for compressive strength and capillary water absorption, while solid blocks were tested for compressive strength, flexural strength, capillary water absorption, dimensional stability, drying shrinkage, density, total water absorption and void content. All tests were performed on samples with an age of 28 days. Solid block compressive tests were also performed on samples with an age of 7 days. The hollow blocks had significantly lower average compression strength than the solids, but an increase in fibre content caused a slight increase in strength. For solid blocks, it was found that the addition of natural fibres decreases the strength, although a partial substitution of cement with CSF, in conjunction with fibres, did increase the strength relative to blocks without CSF. The flexure strength was also lowered somewhat by the addition of fibres, but an increase in ductility was noted, although not quantified. The addition of CSF to fibre-containing blocks led to an increase in capillary water absorption, but a decrease in absorption through immersion. This shows that the addition of CSF does significantly alter the pore system of a cementitious matrix reinforced with natural fibres. Also, the dimensional stability increased with the addition of CSF and fibres. The same can be said for drying shrinkage. Even though an increase in fibre and CSF caused samples to shrink more under drying, they were more stable under cycles of wetting and drying. It was concluded that the addition of fibres to a matrix had a detrimental effect on strength, although ductility did increase. The volumetric properties of concrete were also adversely affected by the addition of fibres, although dimensional stability was improved. The partial substitution of cement with CSF did improve many of the mechanical and volumetric properties of samples containing sisal fibre.
AFRIKAANSE OPSOMMING: Natuurlike vesel bewapende beton (NVBB) is ’n tipe beton wat onlangs heelwat belangstelling ontlok het weens die potensiaal om gebruik te word as ‘n volhoubare en ekonomiese haalbare boumateriaal. Natuurlike vesels is dikwels baie goedkoop en wyd beskikbaar in ontwikkelende lande. Sisal is een so ‘n vesel wat verkry word vanaf die blare van ’n garingboom. Die plant word hoofsaaklik in Brasilië verbou en is al uitgewys weens sy potensiaal om op kommersiële skaal in Suidelike Afrika verbou te word. Die duursaamheid van sisal vesels is geneig om nadelig geaffekteer te word in die teenwoordigheid van kalsium hidroksied en ’n hoë-alkali omgewing, soos gevind in die porie-water van beton. Hierdie navorsing handel oor die gebruik van sisal vesel bewapende beton (SVBB) boublokke. Dit fokus op die meganiese- en duursaamheids eienskappe van blokke met verkillende inhoude van vesel en gekondenseerde silika dampe (GSD). Twee verskillende SVBB blokke is geproduseer (solied en hol) deur gebruik te maak van 10 mm vesels. Twee matriks tipes is gebruik: een met ’n 70:30 sement:vliegas verhouding en een met ’n 60:30:10 sement:vliegas:GSD verhouding, volgens gewig. Blokke van elke matriks tipe is geproduseer met 0, 0.5 en 1% vesel inhoud, volgens volume. Hol blokke is getoets vir druksterkte en kapillêre water absorpsie, terwyl soliede blokke getoets is vir druksterkte, buigsterkte, kapillêre water absorpsie, dimensionele stabiliteit, krimp onder uitdroging, digtheid, totale water absorpsie en luginhoud. Alle toetse is gedoen op blokke met ’n ouderdom van 28 dae. Druktoetse is ook gedoen op soliede blokke met ’n ouderdom van 7 dae. Die hol blokke het ’n aansienlike laer gemiddelde druksterkte as die soliede blokke gehad, maar ’n toename in veselinhoud het gelei tot ’n effense verhoging in druksterkte. ’n Toename in veselinhoud van soliede blokke het gelei tot ’n afname in druksterkte, alhoewel ’n gedeeltelike vervanging van sement met GSD gelei het tot ’n hoër druksterkte vir blokke met vesels. Die buigsterkte van soliede blokke het ook afgeneem met ’n verhoging in veselinhoud. ’n Verhoging in duktiliteit is waargeneem met ’n toename in veselinhoud, alhoewel dit nie gekwantifiseer is nie. Die toevoeging van GSD tot blokke bevattende vesels het gelei tot ’n verhoging in kapillêre water absorpsie, maar ’n verlaging in totale water absorpsie. Dit kan daarop wys dat die toevoeging van GSD die poriestelsel van NVBB noemenswaardig verander. Beide die dimensionele stabiliteit en krimp onder uitdroging het toegeneem met die toevoeging van GSD en vesels tot die blokke. Dus, die toevoeging het gelei tot ’n hoër krimpvervorming tydens uitdroging en ’n hoër stabiliteit tydens nat/droog siklusse. Daar is tot die gevolgtrekking gekom dat die toevoeging van sisal vesels tot ’n beton blok oor die algemeen ’n negatiewe effek het op sterkte, alhoewel duktiliteit toeneem. Die volumetriese eienskappe van beton word ook negatief geaffekteer met die toevoeging van sisal vesels, alhoewel dimensionele stabiliteit verbeter. Die gedeeltelike vervanging van sement met GSD lei tot die verbetering van beide meganiese en volumetriese eienskappe van beton blokke wat sisal vesels bevat.

Mixed matrix membranes offer an attractive route to the development of high performance and efficiency membranes required for demanding gas separations. Such membranes combine the advantageous processing characteristics of polymers with the excellent separation productivity and efficiency of molecular sieving materials. This research explores the development of mixed matrix membranes, namely in the form of asymmetric hollow fiber membranes using zeolites as the molecular sieving phase and commercially available high performance polymers as the continuous matrix. Lack of adhesion between the typically hydrophobic polymer and the hydrophilic native zeolite surface is a major hurdle impeding the development of mixed matrix membranes. Silane coupling agents have been used successfully to graft polymer chains to the surface of the zeolite to increase compatibility with the bulk polymer in dense films. However, transitioning from a dense film to an asymmetric structure typically involves significant processing changes, the most important among them being the use of phase separation to form the asymmetric porous structure. During the phase separation, it is believed that hydrophilic sieves can act as nucleating agents for the hydrophilic polymer lean phase. Such nucleation tendencies are believed to lead to the formation of gaps between the polymer and sieve resulting in poor mixed matrix performance. This research focuses on defining procedures and parameters to form successful mixed matrix hollow fiber membranes. The first part of this dissertation describes dope mixing procedures and unsuccessful results obtained using a silane coupling agent to enhance polymer-zeolite adhesion. The next section follows the development of a highly successful surface modification technique, discovered by the author, employing the use of a Grignard reagent. As a test case, two zeolites of different silicon-to-aluminum ratios are successfully modified and used to develop mixed matrix membranes with greatly increased gas separation efficiencies. The broad applicability of the surface treatment is also demonstrated by the successful incorporation of the modified zeolites in a second polymer matrix. The final section of the work describes the novel occurrence of large defects (macrovoids) caused by the presence of large zeolite particles proposing a particle size effect in the formation of such defects.

Thesis (Ph.D)--Chemical Engineering, Georgia Institute of Technology, 2009.
Committee Chair: Dr. William J. Koros; Committee Member: Dr. Amyn Teja; Committee Member: Dr. Christopher W. Jones; Committee Member: Dr. Haskell W. Beckham; Committee Member: Dr. Stephen J. Miller. Part of the SMARTech Electronic Thesis and Dissertation Collection.

Les fibres naturelles ont réussi à acquérir un grand intérêt à l'échelle académique et industrielle. Ces fibres sont résistantes, possèdent des densités relativement basses, ont de faibles coûts et proviennent de ressources renouvelables abondantes. Les mêmes techniques classiques peuvent être utilisées pour la mise en œuvre des composites à base de fibres naturelles. Tous ces avantages ont fait que des constructeurs automobiles, par exemple, s'intéressent massivement à intégrer des pièces en ce type de composite dans plusieurs modèles de leurs véhicules. Cependant, les problèmes de compatibilité entre les fibres lignocellulosiques et les thermoplastiques limitent le transfert de charge entre fibre et matrice et ainsi les propriétés mécaniques des composites. La durabilité de ces matériaux en présence d'eau ou d'humidité est aussi problématique à cause de la haute hydrophilie des fibres naturelles. Le but de ce travail est de mieux comprendre les phénomènes relatifs à la mise en œuvre et à la l'utilisation de matériaux composites à base de polypropylène renforcé par des fibres de chanvre. L'influence d'un séchage préalable des fibres et d'une nouvelle technique de pré-imprégnation à sec, appelée Fibroline, ont été particulièrement étudiées. Cette dernière consiste à soumettre une poudre et un substrat fibreux à imprégner à un champ électrique de haute tension. Celui-ci provoque l'accélération des grains et crée une parfaite répartition de la résine dans le support fibreux. Au cours de ce traitement, des modifications chimiques et physiques peuvent se produire et entraîner l'amélioration de l'adhésion fibre/matrice. L'influence des techniques de préparation et de mise en œuvre sur les propriétés morphologiques, chimiques et mécaniques des fibres a été analysée. Des observations MEB ont permis de mettre en évidence des modifications de la surface par apparition de micro-craquelures après séchage, application du champ électrique et surtout après double traitement (séchage et Fibroline). Des analyses chimiques par XPS (spectroscopie photo-électronique aux rayons X) des fibres ont montré aussi des modifications de la chimie des surfaces. Principalement des phénomènes d'oxydation sont apparus. D'autre part, la caractérisation mécanique par traction sur mono-filaments dans différents états, a montré une dégradation des propriétés des fibres lors de leur préparation et lors de la phase d'imprégnation en utilisant la technique Fibroline, comparé au cas brut de réception. Les propriétés interfaciales ont été analysées en utilisant trois techniques. D'une part mécaniquement en utilisant le test de fragmentation et le test de déchaussement de micro-goutte, et d'autre part, par suivit de cristallisation isotherme à l'aide de platine chauffante et microscopie optique en lumière polarisée. Les essais mécaniques ont montré l'amélioration de la résistance interfaciale des fibres pré-séchées et celles traitées par la technique Fibroline. Celles doublement traitées ont vu leurs propriétés interfaciales chuter. L'analyse sous conditions isothermes des phénomènes de cristallisation ont permis d'observer l'apparition de zones transcristallines uniformes dans les deux cas ayant été imprégnés par la technique Fibroline. Ceci peut être expliqué par les modifications apportées par cette technique au niveau des surfaces des fibres. [...]

I materiali compositi possiedono proprietà funzionali e di resistenza sempre più performanti grazie alla natura dei rinforzanti in fibra di carbonio, i quali però sono caratterizzati da criticità relative al processo di trasformazione altamente energivoro e dispendioso, all’inquinamento collegato alla produzione delle fibre e al trattamento di sizing, nonché alla difficoltà nello stadio di separazione dei costituenti del manufatto composito e del conseguente riciclo. A causa di queste problematiche sono stati introdotti in produzione materiali a matrice epossidica rinforzata con fibre di lino. Lo studio è stato indirizzato verso la caratterizzazione delle materie prime che compongono i manufatti, quindi fibre e semilavorati, mediante analisi termiche dinamiche in DSC e TGA con il fine di determinare la composizione e resistenza dei singoli componenti e la misura della variazione nel comportamento quando sono uniti per comporre i prepreg. Sono state eseguite delle prove di igroscopicità, umidità e densità per ottenere una panoramica precisa sulle differenze nella struttura delle fibre in carbonio e lino che le differenzia in modo apprezzabile. Sono stati laminati compositi reticolati secondo tecnologia in autoclave, le cui proprietà sono state definite mediante prove termiche dinamiche in DSC, TGA, DMA, prove alla fiamma mediante conocalorimetro, prove fisiche di igroscopicità, umidità e densità, prove ottiche al SEM in seguito ad una rottura in trazione. Parte del progetto seguito è stato direzionato all’ottimizzazione del ciclo produttivo in autoclave. La simulazione del nuovo ciclo di cura industriale, RAPID, è stata eseguita per valutare la variazione della Tg finale e il grado di curing, nonché le proprietà termiche e meccaniche già valutate nel ciclo di cura, STANDARD.

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.

Questa tesi si pone l'obiettivo di studiare e caratterizzare materiali compositi rinforzati con fibra di lino, con particolare attenzione rivolta al confronto tra due diversi tessuti pre-impregnati in resina epossidica. Questi materiali stanno avendo una grande importanza in settori come quello automotive, dove la loro leggerezza e le proprietà meccaniche discrete si stanno facendo spazio tra le ormai usatissime fibre di carbonio e di vetro. Inoltre, il fattore principale per cui molte organizzazioni sportive e produttori di veicoli sono interessati a questi materiali, è sicuramente quello ambientale, vista la sostenibilità della catena di produzione del lino. Approfondita questa tematica, vengono presentate le normative ASTM utilizzate per la caratterizzazione del materiale composito, ovvero test di trazione, taglio in piano, compressione e taglio interlaminare ILSS; queste prove sono essenziali per ottenere informazioni sulle proprietà meccaniche necessarie in fase di progettazione e per determinare, quindi, il campo di applicazione del materiale. Viene, poi, presentato il ciclo di produzione dei provini oggetto dei test, sono esposti i relativi risultati e sono svolte analisi calorimetriche e termogravimetriche, con lo scopo principale di ottenere la temperatura di transizione vetrosa del composito reticolato, in seguito ad un ciclo di cura in autoclave. Infine, viene esposto il confronto tra i risultati ottenuti, in seguito alle prove, dai due materiali presi in esame.

The purpose of this thesis study is to assess the feasibility of using a fiber sorbent module system to remove t-butyl mercaptan (TBM), a common odorant, from pipeline grade natural gas. Odorants such as mercaptans are added to natural gas for safety reasons, but their combustion products are corrosive and decrease the lifetime of the turbines in which they are combusted. Therefore, it is desirable to remove the odorants to extend this lifetime. A TBM removal system attached to a 840 MW natural gas-fueled combined cycle power plant unit such as the one at Plant McDonough-Atkinson (Smyrna, GA) must process gas at a flow rate of approximately 180,000 standard cubic feet per minute. A single 85 MW GE 7EAQ gas turbine has a flow rate of approximately 15,000 standard cubic feet per minute, and will serve as the basis for a system design and process analysis study. The concentration of odorants in natural gas is typically 10 ppm or less. For the purposes of this study, the upper limit of 10 ppm TBM will be used. Zeolite 13X was selected as the model adsorbent for this study due to its high sorption capacity for mercaptans and its ease of incorporation into both fibers and pellets. Design calculations were performed to optimize and determine the feasibility of fiber modules for TBM removal, as well as assess their advantages over conventional pellet packed beds. An understanding of how critical parameters such as heat and mass transfer resistances, pressure drop, and capital and operating costs are affected by design specifications such as sorbent and bed dimensions, allows an optimal design for the needs of the model turbine to be found. Based on these design equations, a fiber sorbent module configuration that selectively and continuously removes TBM from natural gas is developed

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

Human hair and sheep wool are the natural protein fibres of complex structure, composed of Į-keratin chains are analyzed as basic components for the fabrication of nanomaterials. After carrying out some successful experiments in which we demonstrate that silver nanoparticles can be immobilized on the surface and inside hair and wool fibers [1, 2], we attempted to use another type of metal-containing nanoparticles and unite in one composite material such properties as superparamagnetism of iron oxide and nonmagnetism of natural protein fiber. The hair fibers, immersed in a reductant solution in order to break their surface disulfide groups, were placed in a Į-Fe2O3 – nanoparticle suspension while synthesis. After some time, the fiber surface took on a brown tinge. Hematite-containig nanoparti cles were found to penetrate not only into the hair cuticle but also into melanin granules inside the fibre volume. Electron magnetic resonance data (Varian Spectrometer, 9.1 GHz) indicates that the nanoparticles produced in the matrix are upeparamagnetic at room temperature. This interesting finding suggests that such a carrier can be associated with a magnetic bubble. The observed line width and effective g-factor are comparable to those reported for superparamagnetic iron oxide nanoparticles in a nonmagnetic matrix. When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/20653

The main aim of this work id to provide integral methods to predict and characterize the properties of composite structures based on hybrid polymers and reinforcements, that could lead to useful results from an industrial point of view. This is addressed, if possible, by theoretical predictions of the effective properties by using the available experimental data. The first part is focused on the scientific achievements of the author that allowed a quantitative characterization of the main effective properties of several composite architectures from hybrid polymers and reinforcements, based on bio matrices, tailor-made matrices and different theoretical and simulation methods using computer software to allow good comparison. The second part defines the future research lines to continue this initial investigation. The main objectives are clearly defined to give the reader a sound background with the appropriate concepts that are specifically discussed in the following chapters. As a main objective, this research work makes a first attempt to provide a systematic analysis and prediction of composite hybrid structures.
El objetivo general del trabajo es proporcionar medios integrales para predecir y caracterizar las propiedades de las estructuras de compuestos basados en polímeros y refuerzos híbridos, principales que pueden producir resultados de utilidad práctica simultáneamente. Esto se logra comparando, siempre que sea posible, las predicciones teóricas de las propiedades efectivas con los datos experimentales disponibles. Una primera parte se ocupa de los logros científicos del autor que permitieron caracterizar cuantitativamente las principales propiedades efectivas de las arquitecturas de compuestos basados en polímeros y refuerzos híbridos, basados en matrices bio, auto-desarrollados y diferentes métodos teóricos y de simulación por ordenador utilizados para la comparación. La segunda parte identifica las orientaciones futuras para la evolución y desarrollo de la ciencia y la investigación. Los objetivos generales fueron subrayados y concisos para dar al lector una visión previa de los conceptos que serán discutidos específicamente en los siguientes capítulos. Indirectamente, apuntan hacia uno de los objetivos principales de este trabajo, a saber, proporcionar una dirección para el análisis sistemático de materiales compuestos a base de refuerzos híbridos.
L'objectiu general d'aquest treball es proporcionar els mitjos integrals per tal de predir i caracteritzar les propietats d'estructures de compòsits basats en polímers i reforçaments híbrids, que poden produir resultats amb utilitat pràctica simultàniament. Aquest objectiu s'aconsegueix comparant, sempre que és possible, les prediccions teòriques de les propietats efectives amb les dades experimentals disponibles. Una primera part es centra en els temes científics en què ha treballat l'autor que han permès caracteritzar quantitativament les principals propietats efectives de les arquitectures de compòsits basades en polímers i reforçaments híbrids, derivats de matrius bio, auto-desenvolupats i diferents mètodes teòrics i de simulació informàtica per a una correcta comparació. La segona part identifica les orientacions futures per tal d'establir l'evolució i desenvolupament de la ciència i investigació lligada a la temàtica de la tesi. Els objectius generals han sigut clarament definits per tal de donar-li al lector una visió prèvia i sòlida dels conceptes que es discuteixen en capítols venidors. Indirectament, apunten cap a un dels objectius principals d'aquest treball, a saber, proporcionar una direcció per a l'anàlisi sistemàtica de materials compòsits a base de polímers i reforçaments híbrids.
Motoc, D. (2017). Development of green composites based on epoxidized vegetable oils (EVOs) with hybrid reinforcements: natural and inorganic fibers [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/90399
TESIS

This thesis explains the manufacturing of recyclable, eco-friendly composites and their fabrication into hollow cores. The composites have been manufactured using compression moulding and extrusion techniques; each representing batch manufacturing and continuous manufacturing respectively. A statistical design of experiments based on Taguchi method has been used to study the multivariable system involved in the process of continuous extrusion. Factorial design of experiments (DoE) has been used to determine the best material formulation to obtain maximum mechanical properties. The composite sheets produced after the DoE were pelletised in a hammer mill and reprocessed by passing them through another cycle of extrusion. The effect of recycling on the mechanical properties, which were determined by performing static tests as per ASTM standards, has been investigated. The extruded composite sheets have been thermoformed into half-hexagonal and sinusoidal profiles using matched-die and roll forming processes. As the process involves bending and stretching the sheet to conform to the geometry of the mould, it is usually accompanied by large strains. These strains have been analysed using grid strain analysis, and the strain path taken during the forming operation has been determined using strain space diagrams. Due to the stretching and bending of the composite sheet during thermoforming process, a stress field is induced in the material, which upon extraction in that state, would result in either spring-forward or spring-back of the material causing dimensional instability, but by holding the part in that deformed state for a period of time will allow the stresses in the materials to relax. This time-stress information (stress relaxation behaviour) has been experimentally investigated and modelled using springs and dashpots arranged in series and parallel. The spring-back and spring-forward phenomena, occurring in the formed part upon de-moulding, have been investigated using single curvature vee-bending experiments. The profiled sheets obtained after forming have been assembled and bonded into honeycomb cores using adhesives and ultrasonic methods. These cores have been sandwiched between two wood veneer facings to form eco-friendly sandwich panels. The compressive and shear properties of these sandwich panels have been modelled and experimentally investigated. The compressive behaviour of the sisal-PP honeycomb cores has been modelled considering the honeycomb cell wall as a linear elastic specially orthotropic plate/lamina under plane stress and as a quasi-isotropic material. A finite element model of the sandwich panel has been developed in ANSYS classic finite element environment, to study the behaviour of the panel and the core, under flexural loading. Some non-structural properties such as, sound absorption, structural damping and energy absorption have been experimentally determined. The sound absorption ability of the honeycomb has been experimentally evaluated using a standing plane wave impedance tube. Three configurations; one with hollow cores, and the other two filled with polyurethane foam and wood fibres, respectively have been tried. The natural frequencies and structural damping have been experimentally determined by subjecting the sandwich beam to harmonic vibrations. The energy absorption characteristic has been experimentally determined by subjecting the honeycomb cores to quasi-static compressive loading.

Natural fibres such as flax, jute and hemp are becoming attractive alternatives to traditional high performance fibres such as glass and carbon fibres for reinforcement in composites. This is because natural fibres are from renewable sources, are biodegradable, and therefore are more environmentally friendly. However, unlike inherently non-flammable glass and carbon fibres, natural fibres thermally degrade and burn readily and their use has been restricted in applications where the fire regulations are stringent. In addition, natural fibres have low compatibility with a polymer matrix, especially hydrophobic polymers such as polypropylene, causing poor fibre/matrix interfacial adhesion in composites. This leads to lower mechanical performance in natural fibre composites. Therefore treatments/modifications of fibre and/or polymer matrix are required to overcome these drawbacks and expand their range of applications. The main aim of this PhD is to develop flame retardant (FR) natural fibre composites for high performance applications by using FR treated fibres and/or polymer matrices with FR treatment. To achieve this, firstly the flammability of different natural fibres and bio/synthetic polymers was studied by using limiting oxygen index (LOI) and cone calorimetry to identify suitable components for producing FR natural fibre composites. Flax was selected as reinforcing component, and three polymers (polypropylene (PP), polylactic acid (PLA) and poly(furfuryl alcohol) (furan resin)) were selected for polymer matrices. Various strategies to develop flame retardant natural fibre composites were adopted. These can be summarised as (1) development of FR composites from FR treated flax/PP and flax/PLA commingled, woven fabrics, (2) surface modification of flax/PP and flax/PLA fabrics for improving fibre-matrix adhesion in FR composites, (3) development of FR bio/synthetic polymer matrix, and (4) Identification of suitable FR strategy involving synergistic combination of different FR components for producing high performance FR natural fibre composites. The fire performance of these natural fibre composites was evaluated by using UL-94 and cone calorimetry, while the mechanical performance was studied by tensile, flexural testing. In order to develop flame retardant flax/PP and flax/PLA composites from commingled flax/PP and flax/PLA woven fabrics, it was established that the best way to render these flame retardant is to apply FR aqueous solutions by using a conventional pad-dry technique, commonly used for textiles. Usually for textile finishes, fabrics are first scoured which helps in improving the pickup of fabrics. As a first step, the effect of fabric pre-treatment (scouring) on fire and mechanical performance of composites was studied. It was concluded that there is no advantage of using an extra process of scouring during FR composite preparation as the improvement in fire and mechanical properties were only marginal. A number of commercially available water soluble flame retardants were used, out of which guanylurea methylphosphonate (GUP), was seen to be the most effective FR to improve fire performance of the composites. However, GUP caused significant reduction in mechanical properties of the composites therefore the effect of flame retardant concentration on fire and mechanical performance of the composites was studied in order to identify an optimised flame retardant formulation that significantly improves fire retardancy (i.e. V-0 rating in UL-94) of each of flax/PP and flax/PLA laminates with minimal effect on their mechanical performances. The optimised GUP content for flax/PP and flax/PLA was identified as those which have respectively 0.9% and 0.6% phosphorus in respective fabric/composite. To improve fibre/matrix interfacial adhesion in these composites, different surface modification treatments of the fabrics were studied including silane! solution application (i.e. triethoxyvinylsilane (VTS) and 3-aminopropyl triethoxysilane (APS) for flax/PP and flax/PLA respectively), exposure to atmospheric argon-plasma and a combination of both. The fibre/matrix interfacial adhesions of these composites were studied by using peeling and flexural tests. The results showed that the combination of plasma and silane treatments was the most effective method to improve the fibre/matrix adhesion for FR treated flax/PP, whereas only plasma treatment was required for FR flax/PLA composites. In order to develop flame retardant polymer matrices, PP and PLA were compounded with different flame retardants and then extruded into fibres. The commercially available organic phosphorus compound (OP) was seen to be the most effective FR to improve flammability of PP and PLA fibres. In furan resin also a number phosphorus based FRs were studied, from which ammonium polyphosphate (APP) and melamine polyphosphate (MPP) were seen to be most effective. These FR components were then used in different combination (i.e. either application of FR on flax, or in polymer matrix, or both) in order to identify the most effective FR strategy to improve fire performance of a composite with minimum effect on mechanical properties. For FR thermoplastic (flax/PP and flax/PLA) composites best results were achieved with the use of FRs in both flax fibre and polymer matrix. On the other hand for FR flax/furan laminates, the addition of FR in the resin provided best results.

Natural fibres are increasingly being considered as the reinforcement for polymer matrix composites as they are perceived to be sustainable being a renewable resource. However, they suffer from higher variability in mechanical properties and concerns about their long-term durability in a moist environment. In this study the physical properties of the jute fibres were characterised, the fibre length distribution was determined and the fibre cross-section was analysed using digital images. It was observed that the true fibre area followed a log-normal distribution. The fibre area distribution for different geometrical shapes was estimated and the error in the estimated area of assumed fibre cross-section was also determined to assess the applicability of the assumed cross-section. The mechanical properties of the jute technical fibres from a single batch from South Asia were determined; fibre tensile tests were carried out at ten different gauge lengths between 6 mm and 300 mm and the Young’s modulus, strain to failure and ultimate tensile strengths were determined individually. A strong correlation was observed between the fibre strength/fracture strain and fibre gauge length. It was found as the gauge length increases the fibre strength/fracture strain drops. The fibre failure (Strength/Strain) was modelled using Weibull distribution and three statistical models were developed to relate the fibre strength/fracture strain to the fibre gauge length. Examination of tensile test data reveals that the coefficient of variation (CoV) for failure strain is consistently lower than the CoV for fracture stress (strength), as the failure strain is weakly influenced by the fibre cross-section. Hence, failure strain is the more consistent failure criterion and it is recommended to use failure strain as the key design criterion for natural fibre composites in order to improve reliability in the design of these materials. Different authors have tried to model natural fibre reinforced polymer elastic modulus using micromechanical models and have suggested that further study should include fibre angle and length distribution factors to improve the micromechanical prediction. This thesis further seeks to validate a novel methodology for the prediction of the tensile modulus and strength of natural fibre composites through careful consideration of each of the parameters in the rule of mixtures along with consideration of the statistical variation inherent in reinforcements extracted from plants. The tensile modulus and strength of jute fibre reinforced composites manufactured from well characterised fibres was measured experimentally. Six well established micromechanical models were used to predict the composite elastic modulus. Two micromechanical models were used to predict composite strength. For both mechanical properties, the inclusion of a fibre area correction factor to account for the non-circular cross-section of the fibre resulted in an improved prediction of the respective mechanical properties.

The aim of this work was to establish a range of suitable process parameters which can be utilized to produce needlepunched nonwoven fabrics for geotextile applications. Nonwoven fabrics were produced from 100% PP, a blend of 50/50% PP/kenaf and 100% kenaf fibres. The depths of needle penetration of 4, 7 and 10 mm, stroke frequencies of 250, 350 and 450 strokes/min and mass per unit area of 300, 600 and 900 g/m2 were utilized for producing the fabrics, on a Dilo loom. The effect of depth of needle penetration, stroke frequency and mass per unit area on the fabric properties, namely, tensile strength, puncture resistance, pore size, water permeability and transmissivity were analysed. In addition, the effect of chemicals, namely, 10% ammonium hydroxide (NH4OH), 10% sodium chloride (NaCl) and 3% sulphuric acid (H2SO4) solutions on degradation of the fabric was also studied. The results have shown that density, thickness and nominal weight of the needlepunched nonwoven fabrics were related to each other and they were influenced by stroke frequency, depth of needle penetration and feed rate of the needlepunching process. The increase in nominal weight of the fabrics also increases thickness and density of the fabrics. The tensile strength and puncture resistance of the fabrics increased with the increases in stroke frequency, depth of needle penetration and fabric mass per unit area. However, lower tensile strength and puncture resistance were achieved in the fabrics produced at lower stroke frequency, lower depth of needle penetration and lower mass per unit area. Bigger pores were resulted in the fabrics produced at lower stroke frequency, lower depth of needle penetration and lower mass per unit area, however, pore size decreased with increases in stroke frequency, depth of needle penetration and mass per unit area. Water permeability depends on the pore size, properties of the fibres, stroke frequency, depth of needle penetration and mass per unit area. Higher tensile strength and higher puncture resistance were achieved in the needlepunched nonwoven fabrics produced from 100% PP fibres, therefore, they are suitable for some load-bearing geotextile applications, such as reinforcement and separation. However, higher water permeability was achieved in the fabrics produced from 100% kenaf fibres, therefore, they are ideal for geotextile applications where good water permeability is required. Higher values for transmissivity were obtained in the fabrics produced from a blend of 50/50% PP/kenaf fibres, therefore they are suitable for drainage applications. The fabrics produced from a blend of 50/50% PP/kenaf fibres achieved better values of tensile strength, puncture resistance, pore size and water permeability in comparison to that produced from 100% PP and 100% kenaf fibres. However, better tensile strength and puncture resistance were achieved in the fabrics produced from 100% PP fibres and bigger pore size and higher water permeability were achieved in the fabrics produced from 100% kenaf fibres. Therefore, it can be suggested that the nonwoven fabrics produced from a blend of 50/50% PP/kenaf fibres can fulfil almost all requirements of geotextile applications, such as, filtration, separation, reinforcement and drainage. The fabrics produced from 100% PP fibres were not damaged or deteriorated when treated with all the three chemicals due to chemical inertness of polypropylene. However, the fabrics produced from a blend of 50/50% PP/kenaf and 100% kenaf fibres were damaged and deteriorated when treated with H2SO4.

碩士
亞東技術學院
纖維與材料應用產業研發碩士專班
100
This study used the same twists of warp yarns and different twists of weft yarns，which were woven into greige ( 96×80/50×50/62”)，then did the shrinkage test in hot water and mercerization process with different concentration and temperature of sodium hydroxide，as to confirm the nature shrinkage and stretch in weft yarn of fabrics.According to previous tests，to change the densities of warp and weft yarns base on empirical value，also passed by pretreatment and mercerization process which got their stretch qualities，and found the better (greige) grey specefication by Grosberg’s fractional cover and correlation and regression equations.The results indicated that the (greige) grey fabric(92×84/50×50/62”)，the twist multiplier is 4.0 and 5.5 in warp and weft yarns respectively，and passed by pretreatment and mercerization process with concentration 26 Be’ and temperature 20℃ of sodium hydroxide，endued with super natural stretch in 20～25％ of pure cotton fabrics which is familiar with Lycra stretch ones.Besides,qualities of stretch、growth and washing shrinkage are also match the market requirement.