Yes / The clinical application of composites seeks to exploit the mechanical and chemical properties of materials which make up the composite, and in researching polymer composites for biomedical applications the aim is usually to enhance the bioactivity of the polymer, while maintaining the mechanical properties. To that end, in this study medical grade Poly(L-lactic) acid (PLLA) has been reinforced with short phosphate-based glass fibers (PGF). The materials were initially mixed by melting PLLA granules with the short fibers, before being extruded to form a homogenous filament, which was pelletized and used as feedstock for compression moulding. As made the composite materials had a bending strength of 51 MPa ± 5, and over the course of eight weeks in PBS the average strength of the composite material was in the range 20–50 MPa. Human mesenchymal stromal cells were cultured on the surfaces of scaffolds, and the metabolic activity, alkaline phosphatase production and mineralization monitored over a three week period. The short fiber filler made no significant difference to cell proliferation or differentiation, but had a clear and immediate osteoinductive effect, promoting mineralization by cells at the material surface. It is concluded that the PLLA/PGF composite material offers a material with both the mechanical and biological properties for potential application to bone implants and fixation, particularly where an osteoinductive effect would be valuable. / funded in part by the EPSRC Centre for Doctoral Training in Additive Manufacturing and 3D Printing (EP/L01534X/1), the EPSRC Centre for Innovative Manufacture in Medical Devices (EP/K029592/1), and Glass Technology Services Ltd., Sheffield, UK.

Natural fibre composites (NFCs), which are polymers reinforced with cellulosic bast fibres, have the potential to be applied into a range of building products. They are seen as an alternative to glass fibre reinforced plastics (GFRP) in some applications, because of natural fibres (NF) relatively high strength and low density. Moreover, natural fibres have a set of beneficial traits, such as thermal insulation, thermal stability, biodegradability, and are inherently renewable. Those characteristics are of importance when NF are used as reinforcements in polymer composites, but developments in mechanical performance, reliability and economic viability are still required in order to be adopted fully by industry. The goal of this thesis was the development of a processing methodology for NFC laminate and subsequent material characterisation to assess the developed material suitability for building applications. Research objectives included materials selection, processing route development for laminates and tubes, manufacture of NFC laminates and analysis of mechanical properties in order to find an optimal composition. Hemp and flax fibres were selected as the reinforcement, because both have high mechanical properties and are important bast fibre crops in the European region with established cultivation and processing methods. As a matrix, fossil-fuel based and partially bio-derived thermoset resin systems were used. Handling and processing methodologies were developed for laminates and composite tubes based on filament winding and compression moulding techniques. The effects of the selected factors, namely material composition, volume fraction, processing parameters, reinforcement linear density, yarn twist, lamination sequence, yarn waviness and hybrid hemp-wool reinforcement were subsequently described in mechanical properties analysis of laminates. The influence of weathering conditions on the mechanical performance of the NFCs was examined. Furthermore, a study of NFC tubes under compression was performed. Results showed that the developed laminates reinforced with NF yarns have sufficient mechanical properties to be utilised in sandwich panels and/or tubes. However, a low resistance to moisture-related weathering restricts the developed NFCs for indoor applications.

Thesis (M. Tech.) -- Central University of Technology, Free State, 2010 / The aim of this study is to produce more cost effective carbon fibre (CF) parts. To achieve this there must be a saving on materials, labour and time. Thus, a production process to produce cost effective CF moulds while saving time and money is required. This procedure must be suited for the incorporation in the small to medium production ranges. The composite industry is one of the fastest growing industries in the world. Therefore, the faster a mould can be produced, the faster the end product will reach the market. This research project investigates the possibility to sinter CF moulds on the Electro Optical Systems (EOS) Laser Sintering (LS) machine cheaper and faster than the conventional method using computer numerically controlled (CNC) machining. The surface finish produced on the LS machine is not of the same quality as a CNC machined mould, but there are ways to enhance the surface quality of a LS part to the point that it is compatible to the surface quality of a CNC machined mould. The CF moulding process uses many different types of moulding processes. However, it is not possible to use LS parts for all of the available processes to produce CF parts. In this study only one CF moulding process will be investigated, namely compression moulding. The moulds will be designed to be manufactured as cheaply and as quickly as possible. Different methods of mould adapting have been studied to find the cheapest most suitable method of mould design for the LS process.

Two approaches for creating a new all-cellulose composite material have been studied: the biosynthesis of compartmentalised bacterial cellulose fibril aggregates and the compression moulding of commercial chemical wood pulps processed with only water. The objective was to study the structural changes during processing and the complexity of relating the mechanical properties of the final biocomposites to the nanoscale structure was highlighted. Solid-state CP/MAS 13C NMR spectroscopy was utilised to determine both the fibril aggregate width and the content of the different crystalline cellulose forms, cellulose I and cellulose II. Using this method, the quantities of hemicellulose present inside the fibre wall and localised at the fibre surfaces could be determined. The formation of cellulose fibrils was affected by the addition of hydroxyethylcellulose (HEC) to a culture medium of Acetobacter aceti, and the fibrils were coated with a thin layer of HEC, which resulted in loose bundles of fibril aggregates. The HEC coating, improved the fibril dispersion in the films and prevented fractures, resulting in a biocomposite with remarkable mechanical properties including improved strength (289 MPa), modulus (12.5 GPa) and toughness (6%). The effect of press temperature was studied during compression moulding of sulphite dissolving-grade pulps at 45 MPa. A higher press temperature yielded increases in the fibril aggregation, water resistance (measured as the water retention value) and Young’s modulus (12 GPa) in the final biocomposite. The high pressure was important for fibril aggregation, possibly including cellulose-cellulose fusion bonds, i.e., fibril aggregation in the fibre-fibre bond region. The optimal press temperature was found to be 170°C because cellulose undergoes thermal degradation at higher temperatures. The effect of hemicellulose was studied by comparing a softwood kraft paper-grade pulp with a softwood sulphite paper and a softwood sulphite dissolving-grade pulp. A significant fibril aggregation of the sulphite pulps suggested that the content and distribution of hemicellulose affected the fibril aggregation. In addition, the hemicellulose structure could influence the ability of the hemicellulose to co-aggregate with cellulose fibrils. Both sulphite pulp biocomposites exhibited Young’s moduli of approximately 12 GPa, whereas that of the kraft pulp was approximately half that value at 6 GPa. This result can be explained by a higher sensitivity to beating in the sulphite pulps. The effect of mercerisation, which introduces disordered cellulose, on the softwood sulphite dissolving-grade pulp was also studied under compression moulding at 170°C and 45 MPa. The mechanisms causing an incomplete transformation of cellulose I to II in a 12 wt% NaOH solution were discussed. The lower modulus of cellulose II and/or the higher quantity of disordered cellulose likely account for the decrease in Young’s modulus in the mercerised biocomposites (6.0 versus 3.9 GPa). / Två metoder för att skapa ett nytt kompositmaterial baserat på enbart cellulosa har studerats, biosyntes av fibrillaggregat bestående av bakteriecellulosa och varmpressning av kommersiella träfiberbaserade massor med vatten som den enda processkemikalien. Målet var att studera de strukturella förändringarna som sker under tillverkningsprocessen. Även komplexiteten i att relatera strukturen på nanonivå till de mekaniska egenskaperna hos de slutliga biokompositerna belystes. Med fastfas CP/MAS 13C NMR-spektroskopi var det möjligt att bestämma både fibrillaggregattjockleken och mängden av cellulosakristallformerna; cellulosa I och cellulosa II. Det var också möjligt att bestämma mängden hemicellulosa dels närvarande inuti fiberväggen och dels mängden lokaliserad på fiberytor. Tillsats av hydroxyetylcellulosa (HEC) i odlingsmediet för Acetobacter aceti påverkade bildandet av cellulosafibriller som blev belagda med ett tunt skikt av HEC, vilket också resulterade i löst bundna fibrillaggregat. HEC-beläggningen förbättrade fibrilldispersionen i filmerna och minskade sprickbildningen, vilket gav en biokomposit med mycket goda mekaniska egenskaper med kombinerad hög styrka (289 MPa), styvhet (12.5 GPa) och seghet (6%). Effekten av presstemperatur vid varmpressning (45 MPa tryck) studerades på sulfit dissolvingmassor. Högre presstemperatur gav ökad fibrillaggregering, ökat vattenmotstånd (mätt som vattenretentionsvärde) och högre styvhet (12 GPa) för biokompositen. Det höga trycket var också viktigt för fibrillaggregeringen, som troligen omfattar cellulosa-cellulosa samkristallisation dvs. fibrillaggregering i fiber-fiber-bindningsregionen. Den optimala presstemperaturen föreslogs vara 170° C pga. termisk nedbrytning av cellulosa vid högre temperaturer. Effekten av hemicellulosa studerades genom att jämföra sulfat pappersmassa med sulfit pappersmassa och sulfit dissolvingmassa. Mängden och fördelningen av hemicellulosa föreslogs ligga till grund för skillnaden i fibrillaggregering, som var mera uttalad i sulfitmassorna. Även hemicellulosans struktur kan påverka förmågan hos hemicellulosa att sam-aggregera med cellulosafibriller. Biokompositerna baserade på sulfitmassorna hade en styvhet på ca. 12 GPa, medan sulfatmassan bara hade hälften av den nivån ca. 6 GPa, vilket förklarades av sulfitmassornas högre känslighet för malning. Även effekten av mercerisering av sulfit dissolvingmassa varmpressad vid 170° C och 45 MPa studerades. Mercerisering introducerar oordnad cellulosa och mekanismerna som endast ger en partiell omvandling av cellulosa I till II i en 12 vikt% NaOH-lösning diskuterades. Den sämre styvheten hos den merceriserade biokompositen (6.0 resp. 3.9 GPa) förklaras troligen genom cellulosa II kristallens lägre styvhet och/eller den högre mängden av oordnad cellulosa. / <p>QC 20121106</p> / Wallenberg Wood Science Center / Biomime

Cellulose-based materials are widely used in a number of important applications (e.g. paper, wood, textiles). Additional developments are suggested by the growing interest for natural fibre-based composite and nanocomposite materials. The motivation is not only in the economic and ecological benefits, but is also related to advantageous properties and characteristics. The objective of this thesis is to provide a better understanding of process-structure-property relationships in some novel cellulose network materials with advanced functionalities, and showing potential large-scale processability. An important result is the favourable combination of mechanical properties observed for network-based cellulose materials. Compression-moulding of cellulose pulp fibres under high pressure (45 MPa) and elevated temperature (120 – 180 oC) provides an environmentally friendly process for preparation of stiff and strong cellulose composite plates. The structure of these materials is characterized at multiple scales (molecular, supra-molecular and microscale). These observations are related to measured reduction in water retention ability and improvement in mechanical properties. In a second part, cellulose nanofibrils (NFC) are functionalized with in-situ precipitated magnetic nanoparticles and formed into dense nanocomposite materials with high inorganic content. The precipitation conditions influence particle size distributions, which in turn affect the magnetic properties of the material. Besides, the decorated NFC network provides high stiffness, strength and toughness to materials with very high nanoparticle loading (up to 50 vol.%). Subsequently, a method for impregnation of wet NFC network templates with a thermosetting epoxy resin is developed, enabling the preparation of well-dispersed epoxy-NFC nanocomposites with high ductility and moisture durable mechanical properties. Furthermore, cellulose fibrils interact positively with the epoxy during curing (covalent bond formation and accelerated curing). Potential large scale development of epoxy-NFC and magnetic nanocomposites is further demonstrated with the manufacturing of 3D shaped compression-moulded objects. Finally, the wet impregnation route developed for epoxy is adapted to prepare UV-curable NFC nanocomposite films with a hyperbranched polymer matrix. Different chemical modifications are applied to the NFC in order to obtain moisture durable oxygen barrier properties. / <p>QC 20131111</p>

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

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L'extraction aqueuse des lipides de la graine de tournesol est étudiée en contacteur agité. La diffusion à l'intérieur des particules est le facteur limitant de l'échange de matière. Les protéines sont impliquées dans l'entraînement et la stabilisation des lipides par l'eau. Le fractionnement de la plante entière est également étudié avec l'eau en extrusion bi-vis. Un extrait et un raffinat sont obtenus séparément et en une seule étape continue. Des rendements d'extraction en huile de 55 % peuvent être obtenus sous forme d'émulsions huile/eau. Leur stabilité est assurée par la présence à l'interface de tensioactifs : les phospholipides et les protéines voire les pectines. Les extraits se composent aussi d'une phase hydrophile. Prépondérante, elle contient des composés hydrosolubles (protéines, pectines…). Riches en fibres, les raffinats présentent une teneur significative en protéines au comportement thermoplastique. Ils peuvent être transformés en agromatériaux par thermomoulage.

This master’s thesis deals with the composite materials and especially aims on the carbon and glass fiber composites. It points out different composition types and manufacturing methods which reflect in the different mechanical properties, final quality of the manufactured part and also in the manufacturing time. The practical part includes two particular manufacturing methods using prepregs, one cured in an autoclave and one by hot compression moulding.