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Study of the catalyst evolution during annealing preceding the growth of carbon nanotubes by microwave plasma-enhanced chemical vapour deposition

机译：微波等离子体增强化学气相沉积法在碳纳米管生长前退火过程中催化剂演化的研究

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摘要

A two-step catalyst annealing process is developed in order to control the diameter of nickel catalyst particles for the growth of carbon nanotubes (CNTs) by microwave plasma-enhanced chemical vapour deposition (MW PECVD). Thermal annealing of a continuous nickel film in a hydrogen (H_2) environment in a first step is found to be insufficient for the formation of nanometre-size, high-density catalyst particles. In a second step, a H_2 MW plasma treatment decreases the catalyst diameter by a factor of two and increases the particle density by a factor of five. An x-ray photoelectron spectroscopy study of the catalyst after each step in the annealing process is presented. It is found that the catalyst particles interact with the substrate during thermal annealing, thereby forming a silicate, even if a buffer layer in between the catalyst and the substrate is intended to prevent silicate formation. The silicate formation and reduction is shown to be directly related to the CNT growth mechanism, determining whether the catalyst particles reside at the base or the tip of the growing CNTs. The catalyst particles are used for the growth of a high-density CNT coating by MW PECVD. CNTs are analysed with electron microscopy and Raman spectroscopy.
机译：为了控制通过微波等离子体增强化学气相沉积（MW PECVD）来生长碳纳米管（CNT）的镍催化剂颗粒的直径，开发了两步催化剂退火工艺。发现在第一步中在氢（H_2）环境中对连续镍膜进行热退火不足以形成纳米尺寸的高密度催化剂颗粒。在第二步骤中，H_2MW等离子体处理将催化剂直径减小了两倍，并使颗粒密度增加了五倍。提出了退火工艺中每个步骤之后催化剂的X射线光电子能谱研究。发现在热退火期间催化剂颗粒与基底相互作用，从而形成硅酸盐，即使旨在在催化剂和基底之间的缓冲层旨在防止硅酸盐的形成。已显示硅酸盐的形成和还原与CNT的生长机理直接相关，从而确定催化剂颗粒位于生长的CNT的底部还是顶部。催化剂颗粒用于通过MW PECVD生长高密度CNT涂层。碳纳米管用电子显微镜和拉曼光谱分析。

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