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Growth of carbon nanotubes (CNT) or carbon nano-fibres (CNF) on fibrous substrates is a way to increase the fracture toughness of fibre reinforced composites (FRC), with encouraging results reported in the recent years. The issues for these materials related to manufacturing of these composites are, however, less investigated. Following the study of compressibility of woven carbon fibre preforms with CNT/CNFs grown on the fibres using the CVD method [Compos Sci Technol 2011; 71(3): 315–325], this paper describes compression tests on the carbon tows used in these fabrics. The results of the measurements include pressure vs. thickness diagrams in consecutive compression cycles and hysteresis of the compression. The results confirm a drastic change of compressibility of fibrous assemblies in the presence of CNT/CNF grafting.

This work reports the synthesis of nitrogen-doped carbon nanotubes (N-CNTs) using a Chemical Vapor Deposition (CVD) process at temperature ranging from 600 °C to 850 °C and ethane/ammonia concentration (defined as a volume percentage of C 2 H 6 /(C 2 H 6 + NH 3 )) of 20–100%. Several characterizations, i.e. XPS, SEM and TEM were done on the as-synthesized nitrogen-doped carbon nanotubes in order to get more insight about the influence of the synthesis conditions on the characteristics and properties of these N-CNTs. Depending on the synthesis conditions, the atomic percentage of nitrogen in carbon nanotubes varied from 0 at.% to about 5.5 at.%. The undoped carbon nanotubes (N-free CNTs) and two kinds of N-CNTs with different types of nitrogen incorporated species have been used as the supports for palladium in the liquid-phase hydrogenation of cinnamaldehyde. The introduction of nitrogen atoms into the carbon matrix significantly modified the chemical properties of the support compared to the N-free carbon nanotube resulting in a higher metal dispersion. N-CNTs exhibit much higher activity in the hydrogenation reaction compare to the undoped ones. Nitrogen incorporation also strongly improved the selectivity towards the C C bond hydrogenation. The results show that the type of nitrogen species incorporated in CNTs structure can also influence the catalytic activity. Recycling test confirms the high stability of the catalyst as neither palladium leaching nor deactivation has been observed.

Few-layer graphene (FLG) sheets with sizes exceeding several micrometers have been synthesized by exfoliation of expanded graphite in aqueous solution of ammonia under microwave irradiation, with an overall yield approaching 8 wt.%. Transmission electron microscopy (in bright-field and dark-field modes) together with electron diffraction patterns and atomic force microscopy confirmed that this graphene material consisted mostly of mono-, bi- or few-layer graphene (less than ten layers). The high degree of surface reduction was confirmed by X-ray photoelectron and infrared spectroscopies. In addition, the high stability of the FLG in the liquid medium facilitates the deposition of the graphene material onto several substrates via low-cost solution-phase processing techniques, opening the way to subsequent applications of the material.

The introduction of foreign elements inside the channel of carbon nanotubes could lead to a significant modification of the intrinsic properties of these nanomaterials. Nitrogen atoms entering in the graphene sheets as substitute of carbon could modify in a large extend the acido-basic properties and also adsorption of the nanotube itself. Depending on the synthesis conditions, i.e. nature of the N-source, temperature and C-to-N atomic ratio, various N-doped carbon nanotubes can be synthesized with different surface properties. The aim of the present work is to report the synthesis of N-doped CNTs using a common nitrogen source precursor namely ammonia (NH 3 ) with C 2 H 6 as carbon source. The as-synthesized N-CNTs were subsequently employed as catalyst support in the liquid-phase hydrogenation of cinnamaldehyde using palladium as an active phase.

Multifunctional composites which can fulfil more than one role within a system have attracted considerable interest. This work focusses on structural supercapacitors which simultaneously carry mechanical load whilst storing/delivering electrical energy. Critical mechanical properties (in-plane shear and in-plane compression performance) of two monofunctional and four multifunctional materials were characterised, which gave an insight into the relationships between these properties, the microstructures and fracture processes. The reinforcements included baseline T300 fabric, which was then either grafted or sized with carbon nanotubes, whilst the baseline matrix was MTM57, which was blended with ionic liquid and lithium salt (two concentrations) to imbue multifunctionality. The resulting composites exhibited a high degree of matrix heterogeneity, with the ionic liquid phase preferentially forming at the fibres, resulting in poor matrix-dominated properties. However, fibre-dominated properties were not depressed. Thus, it was demonstrated that these materials can now offer weight savings over conventional monofunctional systems when under modest loading.

This paper addresses the challenge of producing multifunctional composites that can simultaneously carry mechanical loads whilst storing (and delivering) electrical energy. The embodiment is a structural supercapacitor built around laminated structural carbon fibre (CF) fabrics. Each cell consists of two modified structural CF fabric electrodes, separated by a structural glass fibre fabric or polymer membrane, infused with a multifunctional polymeric electrolyte. Rather than using conventional activated carbon fibres, structural carbon fibres were treated to produce a mechanically robust, high surface area material, using a variety of methods, including direct etching, carbon nanotube sizing, and carbon nanotubein situgrowth. One of the most promising approaches is to integrate a porous bicontinuous monolithic carbon aerogel (CAG) throughout the matrix. This nanostructured matrix both provides a dramatic increase in active surface area of the electrodes, and has the potential to address mechanical issues associated with matrix-dominated failures. The effect of the initial reaction mixture composition is assessed for both the CAG modified carbon fibre electrodes and resulting devices. A low temperature CAG modification of carbon fibres was evaluated using poly(3,4-ethylenedioxythiophene) (PEDOT) to enhance the electrochemical performance. For the multifunctional structural electrolyte, simple crosslinked gels have been replaced with bicontinuous structural epoxy–ionic liquid hybrids that offer a much better balance between the conflicting demands of rigidity and molecular motion. The formation of both aerogel precursors and the multifunctional electrolyte are described, including the influence of key components, and the defining characteristics of the products. Working structural supercapacitor composite prototypes have been produced and characterised electrochemically. The effect of introducing the necessary multifunctional resin on the mechanical properties has also been assessed. Larger scale demonstrators have been produced including a full size car boot/trunk lid.

Growth of carbon nanotubes (CNT) or carbon nano-fibres (CNF) on carbon fibrous substrates is a way to increase the fracture toughness of fibre reinforced composites (FRC), with encouraging results reported in the recent years. If these nano-engineered FRC (nFRC) are destined to leave laboratories and enter industrial-scale production, a question of adapting the existing composite manufacturing methods will arise. The paper studies compressibility of woven carbon fibre performs (two types of fabrics) with CNT/CNF grown on the fibres using the CVD method. The results include pressure vs thickness and pressure vs fibre volume fraction diagrams for one and four layers of the fabric. Morphology of the nFRC is studied with SEM. It is shown that the pressure needed to achieve the target fibre volume fraction of the preform increases drastically (for example, from 0.05 MPa to more than 0.5 MPa for a fibre volume fraction of 52%) when CNT/CNF are grown on it. No change in nesting of the fabric plies is noticed. The poor compressibility can lower the achievable fibre volume fraction in composite for economical vacuum assisted light-RTM techniques and increase the pressure requirements in autoclave processing. KU Leuven (GOA/10/004) Technologiestichting STW Netherlands Government University of Twente Stichting voor de Technische Wetenschappen

Des composites à base de carbone présentant une tenue mécanique élevée et de faibles masses volumiques peuvent être élaborés par densification SPS (Spark Plasma Sintering). Ces composites sont réalisés en deux étapes : un précurseur C/C est synthétisé par croissance catalytique CVD de nanofibres de carbone (NFCs) sur une préforme de carbone (feutre ou tissu de graphite), puis le composite obtenu est soumis à un traitement de densification par SPS (frittage à 1750 ◦C sous pression de plusieurs dizaines de kN). La réaction CVD utilise des nanoparticules de métaux de transition comme catalyseurs et de l’éthane (C2H6) comme source de carbone. Cette voie de synthèse permet de conserver la mise en forme macroscopique et de rigidifier la structure du précurseur par le biais des nombreuses jonctions créées pendant la formation des NFCs. Une préforme composite C/C est ainsi obtenue et découpée en pastilles pour subir le traitement SPS. Le frittage peut être précédé d’une étape d’infiltration de résine phénolique afin de réaliser des composites C/C/C : cette étape permet de densifier les composites en adjoignant une matrice de carbone par la décomposition de la résine, ce qui favorise la cohésion de l’ensemble. La présence d’éléments de taille nanoscopique permet d’un côté d’améliorer la résistance mécanique en augmentant le transfert de charge, et d’un autre côté de faciliter le frittage et l’infiltration de la résine dans le composite.