Local in situ Raman analysis of the gas and solid phase for understanding the catalytic growth process of carbon nanotubes by chemical vapor deposition (CVD)

对气相和固相进行局部原位拉曼分析，以了解化学气相沉积 (CVD) 碳纳米管的催化生长过程

• 批准号: 42164282
• 负责人: Professor Dr.-Ing. Alfred Leipertz
• 金额: --
• 依托单位: Lehrstuhl für Chemische Reaktionstechnik (CRT)
• 依托单位国家: 德国
• 项目类别: Research Grants
• 财政年份: 2007
• 资助国家: 德国
• 起止时间: 2006-12-31 至 2014-12-31
• 项目状态: 已结题
• 来源: https://gepris.dfg.de/gepris/projekt/42164282?language=en
• 关键词: Local; situ; Raman; analysis; gas

In the first project period a strategy was developed and successfully applied to in situ monitor the gas phase composition and the gas phase temperature during the chemical vapor deposition (CVD) of carbon nanotubes (CNTs) on a Si/SiO2-wafer, which was carrying iron nanoparticles to catalyze the CNT formation. This was possible by applying gas phase linear Raman spectroscopy. The resulting CNTs were characterized ex situ via scanning electron microscopy (SEM) and solid phase Raman spectroscopy. The goal of the second project period is to continue the investigations in exploring the influence of different parameters on the decomposition kinetics of the carbon source. In accordance with the results so far achieved, the parameters to be changed comprise the substrate material (Si/SiO2 should be replaced by Al2O3 and MgO), the hydrogen concentration and the carbon source (acetylene and alcohol). The final goal is to combine the measurement technique based on linear Raman spectroscopy for the simultaneous analysis of the gas and the solid phase in situ during the CVD of CNTs. This makes possible the simultaneous in situ measurement of the gas phase composition, the gas phase temperature and the microstructure of the deposited CNTs with high temporal and spatial resolution, such that finally the decomposition of the carbon source and its effect on the gas temperature and on the CNTs growth can be followed as a function of time. Additionally, the characterization of the resulting CNTs via SEM and Raman spectroscopy will be carried out ex situ for validation. These comprehensive investigations into the CNT formation will provide a sustained understanding of the CNTs nucleation and growth mechanism, which for the first time will experimentally consider the intermediate reactions steps taking place inside the CNT reactor.

在第一个项目期间，开发了一种策略，并成功地应用于原位监测碳纳米管（CNTs）化学气相沉积（CVD）在Si/ sio2晶片上的气相组成和气相温度，该晶片携带铁纳米颗粒催化碳纳米管的形成。这可以通过应用气相线性拉曼光谱来实现。通过扫描电子显微镜（SEM）和固相拉曼光谱对所得碳纳米管进行了非原位表征。第二个项目期的目标是继续研究不同参数对碳源分解动力学的影响。根据目前的研究结果，需要改变的参数包括衬底材料（用Al2O3和MgO代替Si/SiO2）、氢浓度和碳源（乙炔和醇）。最终目标是结合基于线性拉曼光谱的测量技术，在cnt CVD过程中同时分析气相和固相。这使得同时在现场测量沉积的CNTs的气相组成、气相温度和微观结构成为可能，具有较高的时间和空间分辨率，从而最终可以跟踪碳源的分解及其对气体温度和CNTs生长的影响。此外，将通过SEM和拉曼光谱对所得碳纳米管进行非原位表征以进行验证。这些对碳纳米管形成的全面研究将提供对碳纳米管成核和生长机制的持续理解，这将首次通过实验考虑碳纳米管反应器内发生的中间反应步骤。

项目成果

Flow field characterization in a vertically oriented cold wall CCVD reactor by particle image velocimetry

• DOI: 10.1016/j.cej.2012.01.062
• 发表时间: 2012-03
• 期刊: Chemical Engineering Journal
• 影响因子: 15.1
• 作者: Karla Reinhold-López;A. Braeuer;A. Schmitt;N. Popovska-Leipertz;A. Leipertz

In Situ Raman Monitoring of the Formation and Growth of Carbon Nanotubes via Chemical Vapor Deposition

• DOI: 10.1016/j.proeng.2015.01.126
• 发表时间: 2015
• 期刊: Procedia Engineering
• 作者: Karla Reinhold-López;A. Braeuer;Bettina Romann;N. Popovska-Leipertz;A. Leipertz