Dissertations / Theses on the topic 'Natural fiber reinforced composites'

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.

Cette thèse présente un aperçu des composites thermodurcissables à base de fibres de lin de deux points de vue : fabrication par moulage par injection de résine et caractérisation mécanique. En particulier, deux matrices thermodurcissables ont été étudiées, à savoir l’époxy classique et la benzoxazine biosourcée. L’influence des propriétés intrinsèques des fibres de lin tels que la variabilité, le gonflement de la fibre et l’absorption de liquide sur la fabrication de pièces composites est étudiée. En considérant le gonflement des fibres et l’absorption des liquides, un modèle mathématique pour l’ascension capillaire des liquides dans les fibres de lin est proposé. Les modèles classiques de perméabilité ne pouvant être adoptés pour les fibres de lin en raison de leurs irrégularités de section et des diamètres de fibres, cette étude a recours à des simulations numériques pour estimer statistiquement la perméabilité. L’influence de la pression d’injection lors du moulage par transfert de résine sur la teneur en vides dans les plaques de lin/époxy est caractérisée et modélisée afin de comprendre les différences entre la formation de vides dans les composites renforcés par fibres de verre et fibres de lin. L’effet du cycle de polymérisation sur les propriétés mécaniques des composites est étudié par des tests de traction de composites de lin unidirectionnels afin de souligner l’évolution d’accroche mécanique à l’interface fibre / matrice provoquée par la pénétration de la résine dans les fibres élémentaires avec l’augmentation de la température de traitement. Enfin, le comportement à long terme des composites est examiné pour les composites lin/époxy et les composites lin/benzoxazine, par test de vieillissement hygrothermique
This dissertation presents insights into flax fiber based thermoset composites from two standpoints; manufacturing the composites by resin transfer molding and their mechanical characterization. In particular, two thermoset matrices have been investigated, i.e. conventional epoxy and bio-based benzoxazine. The influence of the intrinsic properties of flax fibers such as variability, fiber swelling and liquid absorption on the manufacturing of composite parts is investigated. By considering fiber swell and liquid absorption, a mathematical model for the capillary rise of liquid in flax fibers is proposed. As classical tow permeability models cannot be adopted for flax fibers due to their irregularities in cross-section and fiber diameter, this study resorts to numerical simulations to statistically estimate the permeability. The influence of injection pressure during resin transfer molding on void content in flax/epoxy plates is characterized and modeled to understand the differences in void formation from glass fiber composites. The effect of cure cycle on the mechanical properties of composites is investigated by tensile tests of unidirectional flax composites to emphasize the evolution of the mechanical locking at fiber/matrix interface caused by resin penetration into elementary fibers with increase in processing temperature. Finally, the long-term behavior of composites is examined for flax/epoxy composites and flax/benzoxazine composites, by hygrothermal aging test

Bio-based flax fiber polymer composites (FFPC) have the potential to replace metals and synthetic fibers in certain applications due to their unique mechanical properties. However, the long term reliability of FFPC needs to be better understood. In this study, the fatigue limit was evaluated using mathematical, thermographic, and energy-based approaches. Each approach determined fatigue limits around 45% load of ultimate tensile strength at a loading frequency of 5 Hz. Thermographic and energy-based approaches were also implemented at different loading frequencies (5, 7, 10, and 15 Hz) to define the effect of loading frequency on the fatigue life. Fatigue limit was found to decrease slowly with increasing loading frequency. Moreover, two forms of damage energy (thermal and micro-mechanical) during cyclic loading was separated using an experimental approach to pinpoint the main responsible damage energy for decreasing fatigue limit with increasing loading frequency.

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

Thesis (M.S.)--Michigan State University. Dept. of Civil and Environmental Engineering, 2008.
Title from PDF t.p. (viewed on Aug. 3, 2009) Includes bibliographical references (p.129-132). Also issued in print.

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

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.

Thesis (MEng)--Stellenbosch University, 2015.
ENGLISH ABSTRACT: The building industry is responsible for a substantial contribution to pollution. The production of building materials, as well as the operation and maintenance of structures leads to large amounts of carbon-dioxide (CO2) being release in the atmosphere. The use of renewable resources and construction materials is just one of the ways in which the carbon footprint of the building industry can be reduced. Sisal fibre is one such renewable material. Sisal fibre is a natural fibre from the Agave Sisalana plant. The possibility of incorporating sisal fibre in a cement-based matrix to replace conventional steel and synthetic fibres has been brought to the attention of researchers. Sisal fibre has a high tensile strength in excess of polypropylene fibre and comparable to PVA fibre. Sisal fibre consists mainly of cellulose, hemi-cellulose and lignin. The disadvantage of incorporating sisal fibre in a cement-based matrix is the degradation of the composite. Sisal fibres tend to degrade in an alkaline environment due to changes in the morphology of the fibre. The pore water in a cement base matrix is highly alkaline which leads to the degradation of the fibres and reduced strength of the composite over time. Sisal fibre reinforced cement-based composites (SFRCC) were investigated to evaluate the durability of the composites. Two chemical treatments, alkaline treatment and acetylation, were performed on the fibre at different concentrations to improve the resistance of the fibre to alkaline attack. Alkaline treatment was performed by using sodium hydroxide (NaOH), while acetylation was performed by using acetic acid or acetic anhydride. Single fibre pull-out (SFP) tests were performed to evaluate the influence of chemical treatment on fibre strength, to study the fibre-matrix interaction and to determine a critical fibre length. A matrix consisting of ordinary Portland cement (OPC), sand and water were used for the SFP tests. This matrix, as well as alternative matrices containing fly ash (FA) and condensed silica fume (CSF) as supplementary cementitious material, were reinforced with 1% sisal fibre (by volume) cut to a length of 20 mm. The OPC matrix was reinforced with untreated- and treated fibre while the alternative matrices were reinforced with untreated fibre. Alternative matrices containing varying fibre volumes and lengths were also produced. Three-point bending- (indirect), direct tensile- and compression tests were performed on specimens at an age of 28 days to determine the strength of the matrix. The remainder of the specimens were subjected to ageing by extended curing in water at 24˚C and 70˚C respectively and by alternate cycles of wetting and drying, after which it was tested at an age of 90 days from production to evaluate the durability of the fibre. An increase in fibre volume led to a decrease in compressive strength and peak tensile strength. The optimum fibre length at a volume of 1% was 20 mm for which the highest compression strength was recorded. The combination of alkali treatment and acetylation was the most effective treatment condition, followed by alkali treatment at low concentrations of sodium hydroxide. At higher concentrations of sodium hydroxide, a significant reduction in strength was recorded. The addition of supplementary cementitious materials also proved to be effective in mitigating degradation, especially in the cases where CSF was used. FA proved to be less effective in reducing the alkalinity of the matrix. However, the use of FA as fine filler resulted in higher strengths. Specimens manufactured by extrusion did not have superior mechanical properties to cast specimens. The conclusion was made that the use of sisal fibre in a cement-based matrix is effective in providing ductile failure. Chemical treatment and the addition of supplementary cementitious materials did improve the durability of the specimens, although degradation still took place.
AFRIKAANSE OPSOMMING: Die boubedryf is verantwoordelik vir 'n aansienlike bydrae tot besoedeling. Die produksie van boumateriale, sowel as die bedryf en instandhouding van strukture lei tot groot hoeveelhede koolstof dioksied (CO2) wat in die atmosfeer vrygestel word. Die gebruik van hernubare hulpbronne en boumateriale is maar net een van die maniere waarop die koolstof voetspoor van die boubedryf verminder kan word. Sisal vesels is 'n voorbeeld van 'n hernubare materiaal. Sisal vesel is 'n natuurlike vesel afkomstig vanaf die Agave Sisalana plant. Die moontlikheid om sisal vesels in 'n sement gebasseerde matriks te gebruik om konvensionele staal en sintetiese vesels te vervang, is tot die aandag van navorsers gebring. Sisal vesel het 'n hoër treksterkte as polipropileen vesels en die treksterkte vergelyk goed met die van PVA vesels. Sisal vesel bestaan hoofsaaklik uit sellulose, hemi-sellulose en lignien. Die nadeel verbonde aan die gebruik van sisal vesels in 'n sement gebasseerde matriks is die degradasie van die komposiet. Sisal vesels is geneig om af te breek in 'n alkaliese omgewing as gevolg van veranderinge wat in die morfologie van die vesel plaasvind. Die water in die porieë van 'n sement gebasseerde matriks is hoogs alkalies wat lei daartoe dat die vesel afgebreek word en die sterkte van die komposiet afneem oor tyd. Sisal vesel versterkte sement gebasseerde komposiete is ondersoek om die duursaamheid van die komposiete te evalueer. Twee chemiese behandelings, alkaliese behandeling en asetilering, is uitgevoer op die vesels teen verskillende konsentrasies om die weerstand van die vesels teen alkaliese aanslag te verbeter. Alkaliese behandeling was uitgevoer met natrium-hidroksied (NaOH) terwyl asetilering met asynsuur en asynsuurhidried uitgevoer is. Enkel vesel uittrek toetse is uitgevoer om die invloed van chemiese behandeling op veselsterkte te evalueer, om die vesel/matriks interaksie te bestudeer en om die kritiese vesellengte te bepaal. 'n Matriks wat uit gewone Portland sement (OPC), sand en water bestaan, is gebruik vir die enkel vesel uittrek toetse. Dieselfde matriks, sowel as alternatiewe matrikse wat vliegas (FA) en gekondenseerde silika dampe (CSF) as aanvullende sementagtige materiaal bevat, is versterk met 1% vesel (by volume) wat 20 mm lank gesny is. Die OPC matriks was versterk met onbehandelde- en behandelde vesels, terwyl die alternatiewe matrikse met onbehandelde vesels versterk is. Matrikse wat wisselende vesel volumes en lengtes bevat het is ook vervaardig. Drie-punt buigtoetse (indirek), direkte trek toetse en druktoetse is uitgevoer op proefstukke teen 'n ouderdom van 28 dae om die sterkte van die matriks te bepaal. Die oorblywende proefstukke is onderwerp aan veroudering deur verlengde nabehandeling in water teen 24˚C en 70˚C onderskeidelik en deur afwissilende siklusse van nat- en droogmaak waarna dit op 'n ouderdom van 90 dae vanaf vervaardiging getoets is om die duursaamheid van die matriks te evalueer. 'n Toename in vesel volume het tot 'n afname in druksterkte en piek treksterkte gelei. Die optimum vesel lengte teen 'n volume van 1% was 20 mm, waarvoor die hoogste druksterkte opgeteken is. Die kombinasie van alkaliese behandeling en asetilering was die mees effektiewe behandeling, gevolg deur alkaliese behandeling by lae konsentrasies natrium-hidroksied. Vir hoë konsentrasies natrium-hidroksied is 'n aansienlike afname in sterkte opgeteken. Die toevoeging van aanvullende sementagtige materiale was ook effektief om die degradadering van die vesels te verminder, veral in die gevalle waar CSF gebruik is. FA was minder effektief om die alkaliniteit van die matriks te verminder. Die gebruik van FA as fyn vuller het nietemin hoër sterkte tot gevolg gehad. Proefstukke wat deur ekstrusie vervaardig is, het nie beter meganiese eienskappe gehad as proefstukke wat gegiet is nie. Daar is tot die gevolgtrekking gekom dat sisal vesel in 'n sement gebasseerde matriks wel effektief is om 'n duktiele falingsmode te voorsien. Chemiese behandeling en die toevoeging van aanvullende sementagtige materiale het die duursaamheid van die proefstukke verbeter, alhoewel degradering steeds plaasgevind het.

The effect of different fibre volume fractions of hemp and nanoclay reinforcement on the mechanical, thermal and environmental properties of unsaturated polyester composites has been investigated experimentally. Due to the incorporation of different fibre volume fractions of hemp into polyester resin an improvement in tensile strength and tangent modulus was realised. Likewise, the flexural strength and modulus of unsaturated polyester (UPE) matrix increased with the introduction of hemp fibre. The mechanical tests results suggest that the tensile and flexural properties of composites are related to the fibre volume fractions and interfacial bond strengths between the fibre and matrix. Flexural properties of the composites were found to be comparable to those of chopped strand mat (CSM) glass fibre reinforced UPE composites. Low velocity instrumented falling weight impact tests were conducted to evaluate impact and damage characteristics of hemp and nanoclay reinforced composites. A significant improvement in load bearing capability and impact energy absorption was found by introducing hemp fibre and nanoclay as reinforcement. The impact test results in this study show that the total energy absorbed by the 0.21 fibre volume fraction of hemp reinforced specimen is comparable to the energy absorbed by the composites specimen equivalent in fibre weight percentage of CSM E-glass fibre. All nanoclay reinforced nanocomposite specimens have shown a significant improvement in their impact strength and energy absorption properties compared to unreinforced UPE matrix. The effects of various loading levels of nanoclay reinforcement on the nanomechanical properties of UPE/layered silicate nanocomposites were investigated by a nanoindentation test method. It has shown that the nanoindentation behaviour is strongly influenced by nanoclay reinforcement and the extent of clay dispersion in the polymer matrix. The creep behaviour of hemp fibre reinforced unsaturated polyester (LIFRUPE) composites was investigated using a three-point bending clamp system. Creep strain decreased as the hemp fibre reinforcement increased. The creep deflection value was significantly higher for unreinforced samples compared to hemp fibre reinforced samples. Thermal properties were evaluated using Thermogravimetric Analysis (TGA), Thermo Mechanical Analyser (TMA), Differential Scanning Calorimetry (DSC) and thermal conductivity analysis. TGA results suggest that various concentrations of nanoclay and hemp reinforcement increases the thermal stability of UPE/layered silicate nanocomposites and IIFRUPE composites. Glass transition temperatures (Tg) were also increased with the introduction of clay and hemp fibre reinforcement. Hemp reinforced specimens also showed increased thermal stability indicated by an increased Tg value and decreased decomposition rate. Thermal conductivity values were found to be higher for both clay and hemp reinforced specimens compared to unreinforced polyester. Different fibre volume fraction of HFRUPE composites were subjected to water immersion tests in order to study the effects of water absorption on a range of properties. Water absorption tests were conducted by immersing specimens in a de-ionised water bath at room temperature and 100 °C for different time durations. The tensile, flexural and nanohardness properties of water immersed specimens subjected to both aging conditions were evaluated and compared alongside dry composite specimens. The percentage of moisture uptake increased as the fibre volume fraction increased. The tensile, flexural and nanohardness properties of HFRUPE specimens were found to decrease with increase in percentage moisture uptake. However, the impact properties of HFRUPE composites were found increased after water immersion. Moisture induced degradation of composite samples was significant at elevated temperature. The water absorption pattern of these composites at room temperature was found to follow Fickian behaviour, whereas at elevated temperatures it exhibited non- Fickian. Keywords: Polymer matrix composites (PMCs); Layered silicate nanocomposites; Natural fibre reinforced composites (NFRC); Mechanical properties; Mechanical testing; Moisture absorption; Thermal stability

Includes abstract.
Includes bibliographical references (leaves 83-85).
A multi-scale methodology for small strain linear elasticity is presented in this thesis. The homogenisation process is discussed in general, with particular attention to the required boundary constraints on the micro-domain and the extraction of an effective elastic modulus. For the case of a non-linear problem the enforcement of the required boundary constraints becomes non-trivial and thus implementation via the penalty method and lagrange multipliers is investigated.

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.

Commonly encountered accidental impact, e.g. due to roadway stone hitting, is detrimental not only because it can produce apparent surface defects, but also because barely visible impact damage (BVID) can be induced inside the material, which is not easy to detect by routine inspection. Reliable prediction of the amount of damage of this type induced under known service conditions is particularly important. Therefore, this type of impact was chosen as the focus of the present investigation. A combination of experimental techniques and finite element modelling was used to explore the behaviour of a fibre reinforced natural gas powered vehicle (NGV) pressure cylinder subjected to a low energy impact. In order to identify the modes of failure and understand the structural response, quasi-static indentation tests were carried out on sections of composite pipes and of a composite pressure cylinder. Delamination and matrix cracking were established to be the two major failure modes induced by indentation. Experimental findings were used as a basis for assessing the validity of the modelling approach. Thick shell and three dimensional finite element models were developed using PAFEC, a general purpose finite element code for dynamic and static analysis. It established that the composite pressure cylinder under this type of impact behaves quasi-statically, i.e. the impact phenomenon predominately excites low frequency response. Repeated impact was considered in order to extend the study to include the impact behaviour of a cylinder with pre-existing damage. It was found that a bulging effect was produced in the pressure cylinder at the impact site, where a weak spot was created due to fibre breakage. A fully three dimensional finite element model with static analysis was developed to investigate the damage and material degradation during the BVID phenomenon. The contact pressure distribution based on the Hertzian contact' relationship was applied. Failure mode identification criteria proposed by Hashin (1980) and Chang and Springer (1986) were used to establish the mode and extent of damage in the composite cylinder under quasi-static loading. The predicted failure modes agreed well with the experimental results. Finally, the present study sets out the methodology allowing systematic design of structures having optimal impact tolerance. Based on the findings of this project, suggestions for the improvement of impact resistance of NGV cylinders were given in Chapters ix.

PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO
CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO
O presente trabalho tem como objetivo estudar o comportamento e a durabilidade de solos reforçados com fibras de vegetais (sisal e curauá) aleatoriamente distribuídas, submetidos ao envelhecimento natural por exposição às condições ambientais diversas, visando mostrar o seu potencial de utilização em obras de terra. O programa experimental consistiu na realização de ensaios triaxiais convencionais em amostras de areia e areia-fibras no tempo zero (de controle) e em compósitos expostos aos agentes do ambiente externo por até 8 meses. Visando melhorar a durabilidade desses compósitos, foi avaliado também o comportamento mecânico destes com as fibras vegetais tratadas por impermeabilização superficial, com sílica coloidal e com polímero estireno butadieno. Para buscar explicar a variação nos resultados obtidos, ensaios de tração direta, microscopia eletrônica de varredura, espectroscopia na região do infravermelho e análise de perda de massa foram realizados nas fibras após cada período de exposição (0, 60, 120 e 240 dias). A análise global dos resultados permitiu identificar que os efeitos do envelhecimento natural afetaram consideravelmente o comportamento mecânico das fibras vegetais, o que consequentemente vieram a afetar o comportamento mecânico dos compósitos areia-fibra vegetal. As perdas de resistência ao cisalhamento foram mais relevantes e acentuadas nos compósitos com fibras de curauá, indicando que estas fibras, mesmo apresentando maior resistência à tração sem exposição, são mais susceptíveis à degradação em ambientes naturais do que as fibras de sisal. O tratamento superficial das fibras por impregnação com sílica coloidal resultou em melhorias no comportamento mecânico deste compósito, proporcionando também uma maior vida útil das fibras com relação à degradação. Mesmo com a perda do comportamento mecânico das fibras, após 8 meses de exposição aos agentes climáticos, estas continuaram contribuindo como elemento de reforço na matriz arenosa, visto que um dos parâmetros de resistência permaneceu maior quando comparado ao solo arenoso sem reforço.
The objective of this work is to study the behavior and durability of soils reinforced with randomly distributed vegetal fibers (sisal and curauá) submitted to natural aging by their exposure to diverse environmental conditions, aiming to boost its use in earthworks. The experimental program consisted of conventional triaxial tests on sand and sand-fibers samples at zero time (sample control) and on composites exposed to agents from the external environment for up to 8 months. In order to improve the durability of these composites, it was also evaluated the mechanical behavior of these with vegetal fibers treated by surface waterproofing, with colloidal silica and styrene butadiene polymer. In order to explain the variation in the obtained results, direct tensile tests, scanning electron microscopy, infrared spectroscopy and mass loss analysis were performed on the fibers after each exposure period (0, 60, 120 and 240 days). The overall analysis of the results allowed to identify that the effects of natural aging had a significant effect on the mechanical behavior of the vegetable fibers, which consequently affected the mechanical behavior of the sand-fiber composites. Shear strength losses were more relevant and accentuated in composites with curauá fibers, indicating that these fibers, even with higher tensile strength without exposure, are more susceptible to degradation in natural environments than sisal fibers. Surface treatment of the fibers by impregnation with colloidal silica resulted in improvements in the mechanical behavior of this composite, also providing a longer fiber life with respect to degradation. Even with the loss of mechanical behavior of the fibers, after 8 months of exposure to the climatic agents, they continued to contribute as a reinforcing element in the sandy matrix, since one of the resistance parameters remained higher when compared to the sandy soil without reinforcement.

Biobased thermoset resins were synthesized by functionalizing the tall oil fatty acid with hydrogen peroxide and then methacrylic anhydride. The obtained resins were characterized by FTIR to confirm the conversions. The cross-linking ability of the resins were checked by curing experiments and followed by DSC analysis regarding the extent of cross linking. TGA analysis was conducted to identify the thermal degradation patterns of cured resins. The obtained resins (blended with or without 33wt% styrene) were used as matrix and knitted viscose fibers were used as reinforcements to make bio-based composites. Ten layers of knitted viscose fibers were stacked crosswise (0/90⁰С) and hand lay-up impregnation was performed. The fiber ratio of all composites was around 63-66%. The composites were characterized by flexural testing, dynamic mechanical thermal analysis and charpy testing. This work demonstrates that manufacture of composites with both matrix and reinforcement fiber coming from renewable resources is feasible, and the resulted composites have satisfied mechanical performance.
Program: MSc in Resource Recovery - Sustainable Engineering

Currently, the production of most non-asbestos organic (NAO) friction materials depends on a long and energy intensive manufacturing process and an unsustainable supply of synthetic resins and fibres; it is both expensive and bad for the environment. In this research, a new, more energy efficient, manufacturing process was developed which makes use of a naturally derived resin and natural plant fibres. The new process is known as 'cold moulding' and is fundamentally different from the conventional method. It was used to develop a new brake pad for use in low temperature (<400 °C) applications, such as rapid urban rail transit (RURT) trains. A commercially available resin based upon cashew nut shell liquid (CNSL) was analysed and found to have properties suitable for cold moulding. In addition, hemp fibre was identified as a suitable composite reinforcement. This was processed to improve its morphology and blended with aramid to improve its thermal stability. Each stage of cold mould manufacture was thoroughly investigated and the critical process parameters were identified. The entire procedure was successfully scaled up to produce an industrially sized 250 kg batch of material and the resultant composites were found to have appropriate thermal and mechanical properties for use in a rail brake pad. The tribological performance of these composites was iteratively developed through a rigorous testing and evaluation procedure. This was performed on both sub- and full-scale dynamometers. By adding various abrasives, lubricants, and fillers to the formulation it was possible to produce a brake pad with similar friction characteristics to the current market material, but with a 60% lower wear rate. In addition, this brake pad caused 15% less wear to the brake disc. A detailed examination of both halves of the friction couple found that cold moulded composites exhibit a different wear mechanism from the current market material, which was suggested to be the reason for their superior properties. Cold moulding is 3.5x faster and uses 400% less energy than the conventional method.

Nowadays, exceptional advantages of silk fibroin over synthetic and natural polymers have impelled the scientists to application of this biomaterial for tissue engineering purposes. Recently, we showed that embedding natural degummed silk fibers in regenerated Bombyx mori silk-based scaffold significantly increases the mechanical stiffness, while the porosity of the scaffolds remains the same. In the present study, we evaluated degradation rate, biocompatibility and regenerative properties of the regenerated 2% and 4% wt silk-based composite scaffolds with or without embedded natural degummed silk fibers within 90 days in both athymic nude and wild-type C57BL/6 mice through subcutaneous implantation. In all scaffolds, a suitable interconnected porous structure for cell penetration was seen under scanning electron microscopy. Compressive tests revealed a functional relationship between fiber reinforcement and compressive modulus. In addition, the fiber/fibroin composite scaffolds support cell attachment and proliferation. On days 30 to 90 after subcutaneous implantation, the retrieved tissues were examined via gross morphology, histopathology, immunofluorescence staining and reverse transcription-polymerase chain reaction as shown in Figure 1. Results showed that embedding the silk fibers within the matrix enhances the biodegradability of the matrix resulting in replacement of the composite scaffolds with the fresh connective tissue. Fortification of the composites with degummed fibers not only regulates the degradation profile but also increases the mechanical performance of the scaffolds. This report also confirmed that pore size and structure play an important role in the degradation rate. In conclusion, the findings of the present study narrate key role of additional surface area in improving in vitro and in vivo biological properties of the scaffolds and suggest the potential ability of these fabricated composite scaffolds for connective tissue regeneration.

Les composites renforcés à fibres de carbone (CRFC) sont des matériaux de haute technicité appliqués à de nombreux domaines, du sport à l’aéronautique. Cette dernière décennie a vu leur demande croitre continuellement, générant en conséquence une augmentation du volume de déchets. Incités par les directives Européennes sur la gestion des déchets, des traitements thermiques de recyclage industriel ont été développés afin de récupérer les fibres de carbone issues des CFRC, principalement à matrice thermodurcissable. Actuellement, les CRFC en développement et/ou de dernières générations, utilisent des matrices thermostables telles que le Poly Ether Ether Cétone (PEEK). Une partie des travaux de thèse consiste à étudier la faisabilité de recyclage de ce composite thermostable, seul et en mélange avec d’autres types de composites à matrice thermodurcissable et thermoplastique. Un pilote semi-industriel a été employé sous atmosphères inerte (pyrolyse) et réactives (vapo-thermolyse et air). Les premiers résultats sur des mélanges ont montré que sous atmosphère inerte la récupération des fibres de carbone issues des matrices thermostables est quasi impossible. A l’inverse, les essais sur les composites PEEK en atmosphères oxydantes permettent l’extraction de la fibre mais induisent des modifications morphologiques et chimiques de la surface ainsi qu’une réduction de la résistance en traction. Les travaux de thèse se focalisent également sur des solutions alternatives de valorisation des fibres de carbone recyclées. Ces fibres ont été recouvertes de nanocellulose en tant qu’agent d’ensimage, en vue de leur réutilisation dans de nouvelles formulations. La perte de propriétés mécaniques induite par le recyclage a été partiellement compensée par ce traitement de surface. Des fibres recyclées ont également été incorporées dans un composite à renfort naturel de jute et matrice PA6 dans le but de créer un composite hybride offrant des propriétés équilibrées en termes de résistance, prix et impact écologique
Carbon Fiber Reinforced Composites (CFRC) are high technical materials applied in various fields from sports to aeronautics. During the last decade, the demand of CFRC has extended significantly resulting in increasing the volume of composite waste generated each year. Incited by European directives, thermal recycling treatments have been developed at industrial scale to recover carbon fibers, mostly from thermosetting composites. Nowadays CFRP in development used thermoresistant resins such as Poly Ether Ether Ketone (PEEK). Part of this work is to study the recycling feasibility of this type of CFRP alone and mixed with thermosetting and thermoplastics matrix based composites. Semi-industrial pilot was used in inert (pyrolysis) and reactive (steam-thermolysis, oxydation) atmosphere conditions. First results of mixture perform in nitrogen have revealed that inert atmosphere cannot allow the recovery of carbon fibers from thermoresistant resins. On the contrary trials on PEEK in oxydative atmospheres enable the extraction of fiber, but induce morphological and chemical modifications and tensile strength reduction. New approach on the recycled carbon fiber valorization have also been studied. These fibers have been coated by nanocellulose as sizing agent for their reuse in new composite formulations. Mechanical properties loss induce by recycling have been offset thank to this surface treatment. Recycled fibers was also incorporate in jute/PA6 composite to create a hybrid composite with balance properties in terms of strength, price and environmental impact

In this study, several types of modified methods were tried for improving natural fiber reinforced composites and also three kind of natural fibers were used for reinforced composite. Plasma polymerization increased fiber tensile and composites mechanical properties. It is higher effect than alkali treatment. Resin impregnation was expected cheaper method than plasma polymerization. Polyvinyl Alcohol resin impregnation method can increase fiber tensile strength, interfacial shear strength between fiber and composites mechanical properties. And with Bamboo/polypropylene/maleic anhydride polypropylene water absorption ratio also can decrease.
博士(工学)
Doctor of Philosophy in Engineering
同志社大学
Doshisha University

The aim of this research was to analyze the mechanical and thermal properties of composites andhybrid composites prepared with four types of jute fibers and two different resins; biobased thermosetresins acrylated epoxidized soybean oil (AESO) and mathacrylated anhydride modified soybean oil(MMSO). The processing technique used was vacuum injection molding (VIM). Tensile and, flexuraltestings and dynamic mechanical and thermal analysis (DMTA) were used to characterize thecomposites’ properties. The results showed that the AESO composites have better tensile and flexuralproperties. This may be due to the fact that the curing conditions were quite the same for both AESOand MMSO composites but MMSO composites showed different behavior during curing step. Theywere completely cured in a shorter time compared to AESO composites. Having equal curing time forboth resins’ composites can damage the structure of MMSO composites and hybrids. Tan delta peak forthe MMSO reinforced composites occurs at higher temperatures, compared to AESO reinforcedcomposites, which means better thermal properties for MMSO reinforced composites.

A utilização de fibras vegetais como reforço constitui um grande interesse na obtenção de novos materiais para a construção civil produto de seu baixo custo, alta disponibilidade e reduzido consumo de energia para sua produção. Este trabalho avalia a incorporação de fibras de sisal, de comprimento 20 e 40 mm, e fração volumétrica de 0,5 e 1%, em concretos para a alvenaria de blocos estruturais e determina o uso destas unidades na execução de prismas e mini-paredes. Foram realizados os testes de caracterização da fibra, blocos e argamassa de assentamento e os ensaios de resistência à compressão axial das unidades, prismas e mini-paredes. O sisal apresentou baixa massa específica aparente e elevada absorção de água, constituindo uma característica comum desse tipo de material pela grande incidência de poros permeáveis. As propriedades físicas dos blocos com e sem adição cumpriram com os requisitos das normas estabelecidas validando sua utilização. Os resultados do ensaio à compressão mostraram que as mini-paredes reforçadas com fibras obtiveram valores muito próximos ou mesmo superiores aos obtidos para as mini-paredes sem fibras, apresentando melhor desempenho que os blocos e prismas. Todos os elementos com adição mostraram um ganho da capacidade de deformação e ductilidade conferida pelas fibras, observado nas curvas tensão x deformação. O modo de ruptura dos blocos, prismas e mini-paredes de referência foi caracterizado por uma fratura brusca e catastrófica e os reforçados mantiveram suas partes unidas pelas fibras, não perdendo sua continuidade e tornando a ruptura um processo progressivo.
The use of natural fibers as reinforcement is a great interest in obtaining new materials for construction, owing of its low cost, high availability and reduced energy consumption for its production. This paper evaluates the incorporation of sisal fibers of 20 mm and 40 mm length and volume fraction of 0.5 and 1%, for concrete for masonry structural blocks, and determines the use of these units in making of prisms and mini-walls. The laboratory tests were carried to characterize physical properties the fiber, blocks and mortar, and besides axial compression tests of the units, prisms, and mini-walls. The sisal had low apparent density and high water absorption, constituting a common feature of such material by the high incidence of permeable pores. The physical properties of the blocks with and without addition complied with the requirements of standards established by validating their use. The axial compression test results showed that mini-walls reinforced with fibers obtained values very close to or even superior to those obtained for the mini-walls without fibers, showing better performance than the blocks and prisms. All elements with the addition had increased the deformation capacity and ductility afforded by the fibers, observed in the curves stress/strain. The rupture mode of blocks, prisms and mini-walls reference was characterized by an abrupt and catastrophic fracture, and elements reinforced maintained their shares together by the fibers, without losing its continuity and becoming a progressive rupture.

This thesis investigates the utilization of mineral wool (glasswool and rockwool) as precursor with metakaolin in geopolymerization. In 2015, mineral wool waste in Europe is estimated to be 2.4 metric tonnes, and it is currently landfilled. The utilization of this waste in geopolymer composites is one of the motivation towards this study. Indeed, addition of these mineral wools to metakaolin-based geopolymers matrices showed significant improvement in the mechanical properties. The literature section of this thesis describes the previous knowledge on geopolymerization, the materials used in geopolymer and the factors affecting the mechanical strength. In the experimental part, the first goal was to achieve mix composition with highest mechanical strength and also a workable paste of geopolymers. This was done with the following factors held constant: SiO₂/Al₂O₃ = 3.8 and Na₂O/Al₂O₃ = 1, and varying the following: H₂O/Na₂O from 10 to 13, SiO₂/Na₂O from 3.21 to 4.02, mineral wool/metakaolin mass ratio from 0–1, and water/binder (w/b) mass ratio from 0.42 to 0.55. The different mix compositions was calculated at varying substitution (10%, 20%, 30%, 40% and 50%) of metakaolin with mineral wool using both glasswool and rockwool in different matrices to determine the effect of mineral wool substitution on the properties of the geopolymer. Mechanical strength tests were done to determine the effects of mineral wool addition in the geopolymer. Results from the test shows maximum compressive strength of 33 MPa when 20% of the metakaolin was substituted with mineral wool. Further substitution was observed to reduce the mechanical properties of the geopolymer. Also, optimization of glasswool and rockwool in different compositional mixes was done to select a particular mineral wool to be used further in the course of the study. Glasswool precursor with metakaolin showed better compressive strength using the chosen SiO₂/Al₂O₃ and Na₂O/Al₂O₃-ratios, compared to rockwool and was continued as the co-binder with metakaolin during reinforcement with fibres. Additionally, during the investigation the matrices were cured at various temperatures (50, 60, 80 and 100 °C). Results showed best mechanical strength was achieved when the geopolymer matrices were cured at 50 °C. XRD and TGA where used to characterize the behaviour of the raw materials and geopolymer samples and to verify geopolymer formations and its thermal stability respectively. Geopolymers in general during testing experiences brittle failure, this limitation can be corrected using fibre reinforcement. Geopolymer composites with glass, carbon and cotton/polyester fibres were investigated using a simple layering method. Data from these preliminary tests showed that cotton/polyester blend fibre exhibited better ductility and flexural strength than glass and carbon fibre.

In the field of renewable materials, natural fiber composites demonstrate the capacity to be a viable structural material. When normalized by density, flax fiber mechanical properties are competitive with E-glass fibers. However, the hydrophilic nature of flax fibers reduces the interfacial bond strength with polymer thermosets, limiting composite mechanical properties. Corn zein protein was selected as a natural bio-based coupling agent because of its combination of hydrophobic and hydrophilic properties. Zein was deposited on the surface of flax, which was then processed into unidirectional composite. The mechanical properties of zein treated samples where measured and compared against commonly utilized synthetic treatments sodium hydroxide and silane which incorporate harsh chemicals. Fourier transform infrared spectroscopy, chemical analysis, and scanning electron microscopy were also used to determine analyze zein treatments. Results demonstrate the environmentally friendly zein treatment successfully increased tensile strength 8%, flexural strength 17%, and shear strength 30% compared to untreated samples.

Das Forschungsvorhaben liefert einen Beitrag zum Schweißen von Gleich- und Mischmaterialverbindungen aus Naturfaserverstärkten Kunststoffen (NFK) sowie deren Verarbeitung im Compoundieren und Spritzguss. Es wurde holzfasergefülltes (WPC) und flachsfasergefülltes (FFC) Polypropylen (PP) mit unterschiedlichen Füllgraden verwendet. Der Einsatz synthetisch-organsicher Fasern (PET-Fasern) im Compound zielte darauf ab, besonders die Schlagzähigkeit zu verbessern. Im Bereich des Urformens wurden Aussagen zur Verarbeitbarkeit, zu rezepturabhängigen Kurz- und Langzeiteigenschaften sowie Aussagen zur Dauergebrauchsfähigkeit erarbeitet. Die Anwendbarkeit der Fügeverfahren Heizelement- (HE-Schweißen) und Vibrationsschweißen (VIB-Schweißen) konnte für Gleich- und Mischmaterialverbindungen sowohl ohne als auch mit angepasster Energieeinbringung nachgewiesen werden. In diesem Zusammenhang können Aussagen zur Rezepturabhängigkeit, Verfahrensführung, Parameterauswahl, Prüfkriterien sowie den technischen Grenzen der Schweißverbindung unter kurzzeitmechanischer Beanspruchung getroffen werden. Weiterhin wird ein Beitrag zur Dauergebrauchsfähigkeit unter UV-Globalbewitterung und thermischer Alterung sowie zu langzeitmechanischen Eigenschaften von NFK-Schweißverbindungen geliefert.

Thesis (Honors)--Ohio State University, 2007.
Title from first page of PDF file. Document formatted into pages: contains 67 p.; also includes graphics. Includes bibliographical references (p. 60-62). Available online via Ohio State University's Knowledge Bank.

PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO
COORDENAÇÃO DE APERFEIÇOAMENTO DO PESSOAL DE ENSINO SUPERIOR
CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO
PROGRAMA DE SUPORTE À PÓS-GRADUAÇÃO DE INSTS. DE ENSINO
Compósitos são materiais tipicamente não homogêneos e anisotrópicos,tanto do ponto de vista microestrutural quanto de suas propriedadesmecânicas. Os mecanismos de falha são afetados pela distribuição espacial e pela qualidade da adesão na interface reforço-matriz. As técnicas tradicionais de caracterização microscópica são bastante limitadas para caracterizar este tipo de material, já que seções ou projeções bidimensionais podem não revelar completamente a microestrutura anisotrópica. Quando se busca entender a origem de mecanismos de falha, estas limitações são ainda mais importantes. Nesta dissertação foi desenvolvida uma metodologia de caracterização tridimensional baseada em microtomografia de raios-x. O material avaliado foi um compósito de matriz epóxi reforçado com fibras de vidro alinhadas unidirecionalmente. Corpos de prova (CP) foram tomografados antes e depois de ensaios de flexão em diferentes níveis de tensão. As imagens 3D foram analisadas para visualizar e quantificar vazios e trincas, tanto originados no processo de fabricação como gerados durante o ensaio mecânico. Para visualizar a evolução de defeitos com a tensão/deformação, foi estabelecido um procedimento de registro 3D entre as imagens dos CP´s como recebidos, após ensaio no regime elástico e após a falha. Uma avaliação da incerteza do procedimento foi realizada tomografando mais do que uma vez o CP, registrando e comparando as imagens 3D. Os resultados indicaram um crescimento do volume de defeitos após a falha do material. A visualização 3D de regiões específicas das tomografias permitiram identificar a formação e o crescimento de defeitos gerados pelo esforço mecânico.
Composites are typically no homogeneous and anisotropic materials, both from the point of microstructural view as well mechanical properties. The failure mechanisms are affected by the spatial distribution and quality of the adhesion the interface matrix-reinforcement. The traditional techniques of microscopic characterization are enough limited to characterize this type of material since sections or two-dimensional projections may not fully reveal the anisotropic microstructure. When search to understand the origin of failure mechanisms, these limitations are even more important. In the present work, a three-dimensional characterization methodology based on X-ray microtomography was developed. The material evaluated was an epoxy matrix composite reinforced with glass fibers unidirectionally aligned. The samples (CP) were tomographed before and after the bending tests at different loads. The 3D images were analyzed to identify and quantify voids and cracks, both defects were originated in the process of manufacturing as were generated during the mechanical tests. A 3D registration procedure was developed between the sample images obtained before and after the bending tests, in the elastic range and after the failure. An assessment of the uncertainty of the procedure was performed doing more than one tomography of the samples as received, registering and comparing the resulting 3D images. The results showed a clear increase in the volume of the defects after material failure. The 3D visualization of specific regions of the tomographies allowed the identification of the formation and the growth of these defects generated by the mechanical stress.

PONTIFÍCIA UNIVERSIDADE CATÓLICA DO RIO DE JANEIRO
CONSELHO NACIONAL DE DESENVOLVIMENTO CIENTÍFICO E TECNOLÓGICO
O objetivo deste trabalho foi produzir, caracterizar e avaliar o comportamento mecânico de um compósito de matriz termoplástica (ABS) reforçado por fibras de carbono para uso futuro em manufatura aditiva. Misturas foram produzidas contendo diferentes quantidades (0 por cento, 5 por cento e 16,7 por cento) e comprimentos (3 mm e 6 mm) de fibras. Cada mistura foi processada através de uma extrusora dupla rosca para a produção de pellets. Os pellets de cada mistura (incluindo pellets de ABS puro) foram analisados para a caracterização do material processado. Posteriormente, corpos de prova foram extrusados para a determinação das propriedades mecânicas e análise da superfície de fratura. As técnicas utilizadas para a caracterização do material foram: espectroscopia no infravermelho (FTIR), análise termogravimétrica (TGA), reometria capilar e microscopia eletrônica de varredura (MEV). Para a avaliação do comportamento mecânico, os corpos de prova extrusados foram ensaiados para a determinação da resistência à tração, módulo de elasticidade e ductilidade. Em seguida, as superfícies de fratura dos corpos de prova foram analisadas no MEV. Foi verificada a possibilidade de degradação da matriz polimérica e formação de vazios durante o processamento inicial do material, que foram eliminados após a segunda extrusão. As fibras de carbono causaram aumento no módulo de elasticidade e diminuição da ductilidade do compósito, apesar de pouco influenciarem as propriedades reológicas. Além disto, pequenas variações na estabilidade térmica foram observadas. Ao final, em anexo, foi elaborado um panorama sobre a Manufatura Aditiva (MA) e a oportunidade de utilização de compósitos em técnicas de impressão 3D.
The goal of this work was to produce, characterize and analyze the mechanical behavior of a carbon fiber reinforced thermoplastic composite with future applications in additive manufacturing. Mixtures were produced with varying carbon fiber content (0 per cent, 5 per cent, and 16,7 per cent) and initial length (3 mm and 6 mm). Each mixture was processed via a twin-screw extruder to produce pellets. Pellets from each mixture (including pure ABS) were analyzed to investigate the processed material properties. Afterwards, test specimens were extruded from each mixture s pellets for mechanical testing and fracture surface analysis. The following techniques were used for material characterization: Fourrier-Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA), capillary rheology and Scanning Electron Microscopy (SEM). For the evaluation of mechanical properties, the extruded test specimens yield strength, Young s modulus and ductility were determined. Also, the fracture surfaces were observed using SEM. The effects of processing parameters and of the introduction of carbon fibers in the ABS polymer were determined. Results pointed out the possibility of degradation during initial processing and the formation of voids in the pellets structure, which were eliminated during the second extrusion. Results also showed an increase in modulus and a decrease in ductility of the composite, whereas rheological properties seemed largely unaffected. Additionally, small variations in thermal stability were observed with varying carbon fiber content and length. Finally, as an annex, a brief overview of Additive Manufacturing and the opportunities for using carbon fiber reinforced thermoplastics in 3D printing techniques is presented.

In the present thesis, the sources of linear/non-linear viscoelastic and viscoplastic behaviour in polymer composite materials are under study. The significance of this work is related to the nature of all composite materials. All polymer composites tend to indicate a time-dependent behaviour. This behaviour can be either linear or nonlinear. No matter what it is, is very important to be taken into account in the analysis, since it is related to strain rate effects, microdamage induced to the structure of the composite and/or irreversible plastic strains.This microdamage is usually caused due to the application of high stresses or high strain. For that reason additional stiffness degradation experiments were performed. In these tests, samples were subjected to high stress levels. Such high stress levels are also responsible for irreversible phenomena that were mentioned before. Then, a material model was used to study the viscoelastic and viscoplastic behaviour. This model assumes that the viscoelastic and viscoplastic responses may be decoupled; the micro-damage influenced viscoelastic strain response can be separated from viscoplastic response which is also affected by damage. In this thesis, three materials were studied, each one corresponding to a submitted/published scientific article. The first paper entitled "Time dependent nonlinear behaviour of recycled PolyPropylene (rPP) in high tensile stress loading" studied the behaviour of recycled polypropylene and recycled polypropylene with the addition of Maleic Anhydride grafted PolyPropylene (MAPP). The time dependent response was decomposed into nonlinear viscoelastic and viscoplastic parts and each of them was quantified. It was found that the elastic properties did not degrade due to high loading. The addition of MAPP did not change the mechanical properties of the rPP. Then the material model was applied and the involved parameters were identified.In the second article, entitled "Mechanical properties of a recycled carbon fibre reinforced MAPP modified polypropylene composite", the previously studied rPP/MAPP matrix was used to form a composite by using recycled carbon fibres. It was found that in creep tests, the time and stress dependence of viscoplastic strains follows a power law, which makes the determination of the parameters in the viscoplasticity model relatively simple. What is more, the viscoelastic response of the composite was found to be linear in the investigated stress domain. The material model was validated in constant stress rate tensile tests. Finally, in the third article, entitled "The sources of inelastic behaviour of GF/VE NCF [45/-45]s laminates" a glass fibre non-crimp fabric laminate was studied. The viscoelastic and viscoplastic material model parameters were calculated and it was found that the material indicates no linear region. This fact was also attributed to the fibre orientation. Loading the fibres in an off-axis direction caused shear stresses, which are responsible for microdamage (related to the fibre-matrix interface and intralaminal cracks) which is considered to be an important source of non-linearity.
Godkänd; 2010; 20101020 (kongia); LICENTIATSEMINARIUM Ämnesområde: Polymera konstruktionsmaterial/Polymeric Composite Materials Examinator: Professor Janis Varna, Luleå tekniska universitet Diskutant: PhD, Research Engineer Lars-Olof Nordin, Material LKAB MetLab, Luleå Tid: Onsdag den 8 december 2010 kl 10.00 Plats: E1624, Luleå tekniska universitet

Porous ceramics and porous ceramic composites are emerging functional materials that have found numerous industrial applications, especially in energy conversion processes. They are characterized by random microstructure and high porosity. Examples are ceramic candle filters used in coal-fired power plants, gas-fired infrared burners, anode and cathode materials of solid oxide fuel cells, etc. In this research, both experimental and theoretical work have been conducted to characterize and to model the mechanical behavior and durability of this novel class of functional material. Extensive experiments were performed on a hot gas candle filter material provided by the McDermott Technologies Inc (MTI). Models at micro-/meso-/macro- geometric scales were established to model the porous ceramic material and fiber reinforced porous ceramic material. The effective mechanical properties are of great technical interest in many applications. Based on the average field formalism, a computational micromechanics approach was developed to estimate the effective elastic properties of a highly porous material with random microstructure. A meso-level analytical model based on the energy principles was developed to estimate the global elastic properties of the MTI filament-wound ceramic composite tube. To deal with complex geometry, a finite element scheme was developed for porous material with strong fiber reinforcements. Some of the model-predicted elastic properties were compared with experimental values. The long-term performance of ceramic composite hot gas candle filter materials was discussed. Built upon the stress analysis models, a coupled damage mechanics and finite element approach was presented to assess the durability and to predict the service life of the porous ceramic composite candle filter material.
Ph. D.

Steam exploded fibers from Yellow Poplar (Liriodendron tulipifera) wood were assessed in terms of (a) their impact on torque during melt processing of a thermoplastic cellulose ester (plasticized CAB); (b) their fiber incorporation and dispersion characteristics in a CAB-based composite by SEM and image analysis, respectively; and (c) their impact on the mechanical properties (under tension) of CAB-based composites having fiber contents of between 10 and 40% by weight. The fibers included water-washed steam exploded fibers (WEF), alkali-extracted fibers (AEF), acetylated fibers (AAEF), all from Yellow poplar (log Ro = 4.23), and oat fillers (COF) as control. The stepwise increase in cellulose content by extraction, and especially the (surface) modification by acetylation, contributed to increased torque during melt processing, and to improved interfacial adhesion as well as fiber dispersion. As compared to pure CAB, AAEF generated the highest increase in torque (+ 421%) followed by AEF (+ 260%) and WEF (+ 190%) at 40% fiber content by weight. AAEF was also found to enhance the tensile properties of the resulting composites. SEM studies of the tensile fracture surfaces indicated significant interfacial delamination and also pull - out of fibers when WEF, AEF, and COF were used to reinforce the CAB matrix. Composites with AAEF, by contrast, revealed fracture surfaces with reduced interfacial delamination and with significant fiber fracturing during failure. Image analysis was used to determine fiber dispersion within the resulting composites quantitatively. Significant improvement in fiber dispersion was achieved when the matrix was reinforced with acetylated fibers (AAEF). Fiber addition to the matrix resulted in loss of strain at break (- 80 to - 93%) and slight or significant increases in modulus (+ 47 to + 103%) depending on fiber type at 40% fiber content. Maximum stress declined for all fibers except AAEF at all fiber contents. AAEF-based composites revealed a decline in maximum stress when fiber content rose to 10%, and this reversed when fiber content increased beyond 10%. This increase in strength is consistent with the rule of mixtures that stipulates reinforcement of the matrix by fibers that are capable of transferring stresses across the fiber-matrix interface. All fibers suffered length decreases during melt processing.
Master of Science