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微波場(chǎng)中二茂鐵熱解制備碳納米管實(shí)驗(yàn)研究

發(fā)布時(shí)間:2018-09-12 20:13
【摘要】:碳納米管是一種在機(jī)械、電子、光學(xué)等方面具有優(yōu)異的性能納米碳材料。碳納米管中的碳為sp2雜化碳,可以看成是石墨片層沿某一方向卷曲形成的管狀結(jié)構(gòu)。二茂鐵是一種既可以提供碳納米管生長(zhǎng)所需催化劑(鐵)又可以提供碳源(環(huán)戊二烯基)的金屬有機(jī)物。微波加熱是一種有別于傳統(tǒng)加熱的快速加熱方式,在物質(zhì)合成領(lǐng)域具有廣泛的應(yīng)用。本文綜合二茂鐵、微波加熱的特性,選擇石墨、德固賽炭黑、三菱炭黑、煤熱解半焦四種碳材料作為微波吸收介質(zhì)及催化劑沉積和碳納米管生長(zhǎng)的基體,在微波爐中進(jìn)行二茂鐵裂解制備碳納米管的實(shí)驗(yàn)研究。首先對(duì)作為基體的碳材料(石墨、德固賽炭黑、三菱炭黑)在微波場(chǎng)中多次加熱時(shí)的溫升特性進(jìn)行了研究,總結(jié)討論了多次加熱過程中碳材料所表現(xiàn)出的溫升特性。由于物質(zhì)在微波場(chǎng)中的升溫特性與其微觀結(jié)構(gòu)有密切關(guān)系,本文進(jìn)一步借助X射線衍射技術(shù)和拉曼光譜技術(shù)對(duì)加熱前后的碳基體的微晶結(jié)構(gòu)進(jìn)行了分析,結(jié)果表明碳材料在微波加熱過程中的石墨化程度會(huì)有所改善。隨后進(jìn)行了微波場(chǎng)中不同碳基體(石墨、德固賽炭黑、三菱炭黑、煤熱解半焦)上二茂鐵的裂解沉積實(shí)驗(yàn)。通過對(duì)沉積產(chǎn)物的觀察分析,發(fā)現(xiàn)只有石墨基體上成功沉積了大量的碳納米管。進(jìn)一步的分析得到本文實(shí)驗(yàn)工況下碳納米管生長(zhǎng)的機(jī)理即有頂部生長(zhǎng)機(jī)理,又有底部生長(zhǎng)機(jī)理。借助X射線衍射分析了石墨基體上沉積生長(zhǎng)的碳納米管的特性,碳納米管片層平均間距為0.34nm,平均壁厚為11nm。拉曼光譜分析則表明碳納米管的卷曲方向具有明顯的特征。
[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.
【學(xué)位授予單位】:哈爾濱工業(yè)大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2015
【分類號(hào)】:TQ127.11;TB383.1

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