微波场中二茂铁热解制备碳纳米管实验研究
发布时间：2018-09-12 20:13
【摘要】：碳纳米管是一种在机械、电子、光学等方面具有优异的性能纳米碳材料。碳纳米管中的碳为sp2杂化碳,可以看成是石墨片层沿某一方向卷曲形成的管状结构。二茂铁是一种既可以提供碳纳米管生长所需催化剂(铁)又可以提供碳源(环戊二烯基)的金属有机物。微波加热是一种有别于传统加热的快速加热方式,在物质合成领域具有广泛的应用。本文综合二茂铁、微波加热的特性,选择石墨、德固赛炭黑、三菱炭黑、煤热解半焦四种碳材料作为微波吸收介质及催化剂沉积和碳纳米管生长的基体,在微波炉中进行二茂铁裂解制备碳纳米管的实验研究。首先对作为基体的碳材料(石墨、德固赛炭黑、三菱炭黑)在微波场中多次加热时的温升特性进行了研究,总结讨论了多次加热过程中碳材料所表现出的温升特性。由于物质在微波场中的升温特性与其微观结构有密切关系,本文进一步借助X射线衍射技术和拉曼光谱技术对加热前后的碳基体的微晶结构进行了分析,结果表明碳材料在微波加热过程中的石墨化程度会有所改善。随后进行了微波场中不同碳基体(石墨、德固赛炭黑、三菱炭黑、煤热解半焦)上二茂铁的裂解沉积实验。通过对沉积产物的观察分析,发现只有石墨基体上成功沉积了大量的碳纳米管。进一步的分析得到本文实验工况下碳纳米管生长的机理即有顶部生长机理,又有底部生长机理。借助X射线衍射分析了石墨基体上沉积生长的碳纳米管的特性,碳纳米管片层平均间距为0.34nm,平均壁厚为11nm。拉曼光谱分析则表明碳纳米管的卷曲方向具有明显的特征。
[Abstract]:Carbon nanotubes (CNTs) have excellent mechanical, electronic and optical properties. The carbon in carbon nanotubes is sp2 hybrid carbon, which can be regarded as the tubular structure of graphite lamellar curling along a certain direction. Ferrocene is a metal organic substance which can provide both catalyst (iron) and carbon source (cyclopentadienyl) for carbon nanotube growth. Microwave heating is a kind of rapid heating method, which is different from the traditional heating. It is widely used in the field of material synthesis. Based on the characteristics of ferrocene and microwave heating, four kinds of carbon materials, graphite, Degusai carbon black, Mitsubishi carbon black and coal pyrolysis semi-coke, were selected as microwave absorbing medium, catalyst deposition and carbon nanotube growth matrix. Carbon nanotubes were prepared by ferrocene pyrolysis in microwave oven. Firstly, the temperature rise characteristics of carbon materials (graphite, Degusai carbon black, Mitsubishi carbon black) in microwave field were studied, and the temperature rise characteristics of carbon materials during multiple heating were summarized and discussed. Because the heating characteristics of matter in microwave field are closely related to its microstructure, the microcrystalline structure of carbon matrix before and after heating is further analyzed by means of X-ray diffraction and Raman spectroscopy. The results show that the graphitization degree of carbon materials will be improved during microwave heating. Then the pyrolysis and deposition experiments of ferrocene on different carbon matrix (graphite, Degusai carbon black, Mitsubishi carbon black, coal pyrolysis semi-coke) in microwave field were carried out. Through the observation and analysis of the deposited products, it was found that only a large number of carbon nanotubes were deposited successfully on the graphite matrix. Further analysis shows that the growth mechanism of carbon nanotubes under experimental conditions is either the top growth mechanism or the bottom growth mechanism. The characteristics of carbon nanotubes deposited on graphite substrate were analyzed by X-ray diffraction. The average spacing and wall thickness of carbon nanotubes were 0.34 nm and 11 nm respectively. Raman spectroscopy analysis shows that the curling direction of CNTs has obvious characteristics.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.11;TB383.1
本文编号：2240104
[Abstract]:Carbon nanotubes (CNTs) have excellent mechanical, electronic and optical properties. The carbon in carbon nanotubes is sp2 hybrid carbon, which can be regarded as the tubular structure of graphite lamellar curling along a certain direction. Ferrocene is a metal organic substance which can provide both catalyst (iron) and carbon source (cyclopentadienyl) for carbon nanotube growth. Microwave heating is a kind of rapid heating method, which is different from the traditional heating. It is widely used in the field of material synthesis. Based on the characteristics of ferrocene and microwave heating, four kinds of carbon materials, graphite, Degusai carbon black, Mitsubishi carbon black and coal pyrolysis semi-coke, were selected as microwave absorbing medium, catalyst deposition and carbon nanotube growth matrix. Carbon nanotubes were prepared by ferrocene pyrolysis in microwave oven. Firstly, the temperature rise characteristics of carbon materials (graphite, Degusai carbon black, Mitsubishi carbon black) in microwave field were studied, and the temperature rise characteristics of carbon materials during multiple heating were summarized and discussed. Because the heating characteristics of matter in microwave field are closely related to its microstructure, the microcrystalline structure of carbon matrix before and after heating is further analyzed by means of X-ray diffraction and Raman spectroscopy. The results show that the graphitization degree of carbon materials will be improved during microwave heating. Then the pyrolysis and deposition experiments of ferrocene on different carbon matrix (graphite, Degusai carbon black, Mitsubishi carbon black, coal pyrolysis semi-coke) in microwave field were carried out. Through the observation and analysis of the deposited products, it was found that only a large number of carbon nanotubes were deposited successfully on the graphite matrix. Further analysis shows that the growth mechanism of carbon nanotubes under experimental conditions is either the top growth mechanism or the bottom growth mechanism. The characteristics of carbon nanotubes deposited on graphite substrate were analyzed by X-ray diffraction. The average spacing and wall thickness of carbon nanotubes were 0.34 nm and 11 nm respectively. Raman spectroscopy analysis shows that the curling direction of CNTs has obvious characteristics.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.11;TB383.1
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