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Theses

In situ diagnostics for the study of carbon nanotube growth mechanism by oating catalyst chemical vapor deposition for advanced composite applications

Abstract : In the vast field of nanoscience and nanotechnology, carbon nanotubes (CNTs) are of particular interest because of their unique structure which provides them outstanding properties. While the number of CNT-based applications as well as the amount of CNTs produced are increasing year by year, it is essential to understand the mechanisms governing the formation of these nanomaterials to control their structure and organization, maximize the yields, reduce the health and environmental risks and improve the performance of the underlying materials and components. Among the listed synthesis techniques, the aerosol-assisted chemical vapor deposition (CVD) process developed in the laboratory MSSMat allows continuous growth of multi-walled CNTs (MWNTs) on various substrates by the simultaneous injection of carbon feedstock(s) (xylene and/or acetylene) and catalytic precursor (ferrocene) in a reactor heated up to a temperature ranging between 400 and 1000°C. The aim of this study was to analyse the different stages of the CNT formation from the first precursor injection until the growth termination. By the mean of a new experimental approach involving several in situ diagnostics coupled with numerical models, we were able to follow the evolution of the different products and reagents during the synthesis under various thermodynamic and chemical conditions. Hence, after investigating the spatial evolution of the droplets formed in the injection, the nanoparticle germination and nucleation in the gas phase has been studied by time resolved laser-induced incandescence (TRL2I) and laser-induced breakdown spectroscopy (LIBS). A relationship between the size of the particles and the CNTs has been highlighted. Moreover, the chemical reactions during the synthesis were analyzed by mass spectrometry (MS) and gas phase chromatography (GPC). Different reaction pathways have thus been identified depending on the carbon source(s) used, while the effect of hydrogen on the CNT growth, either accelerating or inhibiting based on the CVD conditions, was studied. The substrates' roles were then examined by comparing the growth and morphology of the CNTs obtained on various surfaces such as quartz plates, carbon fibers or micro-particles of alumina, silicon carbide, titanium carbide and graphene. The catalytic effect of some substrates or mixtures of substrates on the CNT growth has also been highlighted, as well as the importance of the substrate's surface/volume ratio on the CNT mass yields. Furthermore, the CNT growth kinetics have been studied and different mechanisms inducing catalyst deactivation and subsequently growth termination were identified. Finally, the different as-synthesized nanostructures originated from the hybridization of CNTs with other materials were used to prepare high-performance multi-functional composites. The electrical, thermal and mechanical properties of these materials have been examined.
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Anthony Dichiara. In situ diagnostics for the study of carbon nanotube growth mechanism by oating catalyst chemical vapor deposition for advanced composite applications. Other. Ecole Centrale Paris, 2012. English. ⟨NNT : 2012ECAP0042⟩. ⟨tel-00763604⟩

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