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In situ Raman monitoring of the formation and growth of carbon nanotubes via chemical vapor deposition

机译:原位拉曼通过化学气相沉积对碳纳米管的形成和生长进行监测

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An in situ measurement technique based on Raman spectroscopy is established to simultaneously monitor the parameters of interest of the solid and gas phases during the formation and growth of carbon nanotubes (CNT) in a cold wall reactor for catalytic chemical vapor deposition (CCVD). Iron nanoparticles were used as a catalyst and acetylene as a carbon source. This new developed technique makes possible the simultaneous in situ measurement of the gas phase composition, the gas phase temperature and the micro structure of the deposited CNTs, such that finally the decomposition of the carbon source and its effect on the gas temperature and on the CNTs formation and growth can be followed as a function of the reaction time. Comprehensive qualitative and quantitative analyses have been performed to assess the catalyst performance with respect to the growing carbon nanostructures. On the basis of the real-time in situ Raman spectra of the emerging solid phase, the moment of nucleation or first signal detection, the time-range of the CNT growth and the end of the deposition is monitored via the characteristic D and G Raman bands for carbon materials. Information about catalytic activity is qualitatively provided and the estimated in situ D/G ratio reveals the defect and disorder content of the growing nanostructures. The Raman spectroscopy setup for the gas phase analysis exhibits high detection sensitivity as well as high accuracy and precision. Correlation could be found between the catalyst activity, acetylene conversion and micro structure of the resulting CNTs.
机译:建立基于拉曼光谱的原位测量技术,同时监测在冷壁反应器中的碳纳米管(CNT)的形成和生长期间监测固体和气相的兴趣参数,用于催化化学气相沉积(CCVD)。将铁纳米颗粒用作催化剂和乙炔作为碳源。这种新的开发技术使得可以同时以原位测量气相组成,气相温度和沉积的CNT的微结构,使得碳源分解及其对气体温度和CNT的影响可以遵循形成和生长作为反应时间的函数。已经进行了综合定性和定量分析以评估碳纳米结构的催化剂性能。在新出现固相的实时拉曼光谱的基础上,通过特性D和G拉曼监测CNC切割或第一信号检测的时刻,CNT生长的时间范围和沉积的结束碳材料的带。有关催化活性的信息是定性提供的,并且原位D / G的估计揭示了生长纳米结构的缺陷和病症含量。气相分析的拉曼光谱设定具有高检测灵敏度以及高精度和精度。可以在所得CNT的催化剂活性,乙炔转化和微结构之间找到相关性。

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