A reactor has been developed at ONERA to investigate the gas phase during carbon nanotube formation by laser-induced fluorescence (LIF), Laser-induced incandescence (LII), coherent anti-Stokes Raman Scattering (CARS), and emission spectroscopy. Continuous vaporization is achieved with a continuous wave CO2 laser. Optimized conditions are used for single-walled nanotube growth, that is, a graphite target doped with 2 atom % Ni and 2 atom % Co, helium as buffer gas at a flow rate of 50 ml/s, and a pressure of 300 hPa. Temperature profiles are measured by CARS on H2, and soot images are obtained by LII in the hot carbonaceous flow. LIF and spontaneous emission of the C2 radical and Ni and Co atoms are presented. Spectral investigations are conducted at 3100 and 3200 K to have an optimized pair of excitation/detection wavelengths. Spatial investigations of the relative concentrations in the hot carbonaceous flow are performed up to 3500 K. The concentrations are measured as a function of target temperature. Two regimes of vaporization are observed. Vaporization is slow up to 3350 K and becomes much faster above this temperature. The fast regime in the 3350-3500 K range corresponds to the observed spatial extent of the metal vapors region. At 3500 K, the C2 profiles obtained with and without catalysts are very different as a result of carbon coalescence as well as carbon dissolution into the metal nanoparticles when these are present in the gas phase. The shape of the C2 profile can be related to nanotube formation and growth at a target temperature of 3500 K.
Laboratory measurements of the recombination of polycyclic aromatic hydrocarbon (PAH) ions with electrons are presented. Experimental data have been obtained at room temperature for azulene (C10H8) and acenaphthene (C12H10) cations by the Flowing Afterglow with PhotoIons method. The results confirm that the recombination of PAH ions is fast although well below the geometrical limit. The set of our recent and present measurements reveal a definite trend of increasing rate with the number of carbon atoms of the PAH. This behaviour that needs further characterization is potentially of great interest for charge state models as recombination is a dominant mechanism of PAH ion destruction in the interstellar medium. The design of experiments to measure the recombination of larger PAHs and their temperature dependence is discussed.
Gas-phase production of carbon nanotubes in presence of a metal catalyst with a continuous wave CO 2 laser is investigated by combining coherent anti-Stokes Raman scattering ͑CARS͒, laser-induced fluorescence ͑LIF͒, and laser-induced incandescence ͑LII͒. These in situ techniques provide a unique investigation of the different transformation processes of the primarily carbon and metal vapors issued from the vaporization of the target by the laser and the temperature at which these processes occur. Continuous-wave laser provides with stable continuous vaporization conditions very well suited for such in situ investigations. Temperature profiles inside the reactor are known from CARS measurements and flow calculations. Carbon soot, density, and size of carbon aggregates are determined by LII measurements. LIF measurements are used to study the gas phases, namely, C 2 and C 3 radicals which are the very first steps of carbon recombination, and metal catalysts gas phase. Spectral investigations allow us to discriminate the signal from each species by selecting the correct pair of excitation/detection wavelengths. Spatial distributions of the different species are measured as a function of target composition and temperature. The comparison of LIF and LII signals allow us to correlate the spatial evolution of gas and soot in the scope of the different steps of the nanotube growth already proposed in the literature and to identify the impact of the chemical nature of the catalyst on carbon condensation and nanotube nucleation. Our study presents the first direct evidence of the nanotube onset and that the nucleation proceeds from a dissolution-segregation process from metal particles as assumed in the well-known vapor-liquid-solid model. Comparison of different catalysts reveals that this process is strongly favored when Ni is present.
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