Effect of Ferrocene Precursor Mass on Gaseous Detonation Synthesisof Carbon Nanotubes
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摘要: 以甲烷和氧气作为爆源,二茂铁为前驱体,探究了不同前驱体质量对所合成的碳纳米管的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HR-TEM)等手段对碳纳米管的形貌和结构进行表征,结果发现:当二茂铁量较少时,只有碳包覆铁纳米颗粒存在;随着二茂铁质量的增加,逐渐有碳纳米管生成,其管径大多分布在10~50 nm之间,为多壁碳纳米短管。随着前驱体质量的增加, 碳纳米管的石墨化程度提高,结构缺陷也变少。通过对合成产物的热重分析可得,气相爆轰法所制备的碳纳米管具有强烈吸氧性,所得样品中碳纳米管的质量分数为26%左右。Abstract: In the present study we studied the influence of the mass of ferrocene precursors on the synthesis of carbon nanotubes with methane and oxygen as the explosive sources.The morphology and structure of the carbon nanotubes were characterized using X-ray diffraction, transmission electron microscopy and high resolution transmission electron microscopy technologies.The results indicate that when the ferrocene quantity is small only carbon coated iron nanoparticles exist in the products.With the increase of the ferrocene mass, carbon nanotubes are gradually produced with their diameters ranging from 10 to 50 nm, which are multi-walled carbon nanotubes.With the increase of the precursor mass, the degree of the graphitization of the carbon nanotubes is also increased but the structural defects are reduced.In addition, by the thermogravimetric analysis of the synthetic product, it can be concluded that the gaseous detonation synthesis of carbon nanotubes has a great ability of oxygen absorption, and the content of carbon nanotube in the sample is about 26%.
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Key words:
- carbon-encapsulated iron /
- carbon nanotubes /
- ferrocene /
- gaseous detonation method
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表 1 合成条件及配比
Table 1. Synthesis conditions and proportions
Sample Temperature/(℃) Initial pressure/(MPa) Ferrocene mass/(g) n(CH4):n(O2) 1# 110 0.1 0.50 1:1 2# 110 0.1 0.75 1:1 3# 110 0.1 1.00 1:1 4# 110 0.1 1.50 1:1 5# 110 0.1 2.00 1:1 Note:n(CH4):n(O2) is the mole ratio of CH4 to O2. 表 2 前驱体中各元素的摩尔构成以及氧平衡
Table 2. Moles of each element in the precursor composition and the oxygen balance
Sample Mole of each element n(H):n(O) Oxygen balance H O C Fe 1# 0.467 0.220 0.137 0.002 7 2.1:1.0 <0 2# 0.480 0.220 0.150 0.004 0 2.2:1.0 <0 3# 0.494 0.220 0.164 0.005 4 2.3:1.0 <0 4# 0.521 0.220 0.191 0.008 1 2.4:1.0 <0 5# 0.550 0.220 0.220 0.011 0 2.5:1.0 <0 Note:n(H):n(O) is the mole ratio of H to O. -
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