本文選題：碳納米管薄膜 + 二茂鐵��； 參考：《江西理工大學(xué)》2015年碩士論文

【摘要】：傳統(tǒng)金屬電磁屏蔽材料由于其自身密度高的特點(diǎn),限制了其發(fā)展。當(dāng)前,電磁屏蔽材料研究最為熱點(diǎn)的是以碳納米管(CNTs)填充輕質(zhì)高分子材料的導(dǎo)電復(fù)合材料,但其性能在目前階段還難以得到很大提高,維持在20 d B左右。究其原因在于CNTs的分散性能差,導(dǎo)致復(fù)合材料中的CNTs含量低、分布不均勻,導(dǎo)電率差。而CNTs因其管長(zhǎng),相互纏繞和成束,使得其均勻分散難以解決。解決含碳類(lèi)屏蔽材料的關(guān)鍵在于增加基體中碳的含量�；谝陨显�,本文開(kāi)展了CNTs電磁屏蔽薄膜的研究,制備超輕、高效的CNTs屏蔽薄膜,具體包括以下內(nèi)容:采用浮動(dòng)催化的化學(xué)氣相沉積法(CVD),以正己烷為碳源,二茂鐵為金屬催化劑,噻吩為催化劑,甲醇為生長(zhǎng)調(diào)節(jié)劑,生長(zhǎng)出雙壁碳納米管(DWCNTs)和少量多壁碳納米管(MWCNTs),通過(guò)自沉積技術(shù)得到低密度,較好柔韌性和易操作的薄膜。通過(guò)在導(dǎo)磁填充法和電鍍法在CNTs中填充磁性材料,微觀上可觀察到管壁上附著有大量的Fe顆粒。通過(guò)導(dǎo)磁填充法在CNTs薄膜中填充二茂鐵/乙醇溶液,制備出中間體二茂鐵/CNTs復(fù)合材料。通過(guò)熱分解法,二茂鐵受熱分解出Fe顆粒,則制備出具有磁性能的Fe/CNTs屏蔽薄膜。通過(guò)差熱/熱重分析,導(dǎo)磁填充相比原始薄膜,Fe含量從之前的21%增加到了35%。磁滯回線中飽和磁化強(qiáng)度由35.43 emu g-1提升到47.35 emu g-1,屏蔽效能在6-9和12-15 GHz的范圍內(nèi)有了很大的提高。通過(guò)導(dǎo)磁填充法在CNTs薄膜中填充二茂鐵/甲醇制備CNTs薄膜屏蔽材料。甲醇既可以降低碳源的濃度,從而控制反應(yīng)過(guò)程中碳原子的供應(yīng)量與碳源的分解速度;另一方面,還可以增加了金屬催化劑二茂鐵的溶解量,使生成的CNTs管壁表面附著更多的Fe原子,提升薄膜的屏蔽效能。本實(shí)驗(yàn)通過(guò)增加一根石英毛細(xì)管通入二茂鐵/甲醇溶液,直接制備出高性能的屏蔽薄膜。通過(guò)差熱/熱重分析,填充二茂鐵/甲醇溶液相比原始樣品,Fe含量從21%增加到了31.5%。磁滯回線中的飽和磁化強(qiáng)度也由原始的35.43 emu g-1增加到了57.3 emu g-1,屏蔽效能得到很大的提升,在5和19 GHz附近屏蔽效能達(dá)到了60-65 d B。探索研究了電鍍制備CNTs薄膜屏蔽材料。以硫酸亞鐵為渡液的主鹽,硫酸為渡液緩蝕劑。調(diào)節(jié)渡液的PH值為2-3,電流為0.1-0.2A。采用純鐵作為陽(yáng)極材料,CNTs薄膜作為陰極材料,在薄膜表面覆蓋一層納米鐵。通過(guò)差熱/熱重分析,電鍍法相比原始薄膜,Fe含量從21%增加到了22.4%。由于Fe顆粒長(zhǎng)時(shí)間處于濕潤(rùn)環(huán)境中,磁滯回線中的飽和磁化強(qiáng)度由原始的35.45 emu g-1增加到了38.35 emu g-1,屏蔽效能在小頻段內(nèi)有提升。導(dǎo)磁填充法在常溫下填充二茂鐵/乙醇溶液,在高溫下填充二茂鐵/甲醇溶液,屏蔽薄膜中Fe含量、鐵磁性以及薄膜的屏蔽效能都有了很大的提升。電鍍作為本實(shí)驗(yàn)探索制備高屏蔽薄膜的一種新方法,屏蔽性也有一定的提升。
[Abstract]:The development of traditional metal electromagnetic shielding materials is limited because of their high density. At present, conductive composites filled with carbon nanotubes (CNTs) are the most popular electromagnetic shielding materials. However, the properties of the composites are difficult to be improved at present and maintained at about 20 dB. The reason lies in the poor dispersion property of CNTs, which leads to low CNTs content, uneven distribution and poor conductivity. Because of its tube length, intertwining and bunching, it is difficult to solve the problem of uniform dispersion of CNTs. The key to solve the problem of carbon-containing shielding materials is to increase the content of carbon in the matrix. For the above reasons, the study of CNTs electromagnetic shielding thin films was carried out, and the ultra-light and high efficiency CNTs shielding films were prepared, including the following contents: using floating catalytic chemical vapor deposition method, using n-hexane as carbon source, Ferrocene was used as metal catalyst, thiophene as catalyst and methanol as growth regulator. DWCNTsand a few multi-walled carbon nanotubes (MWCNTs) were grown. Low density, good flexibility and easy to operate thin films were obtained by self-deposition. By filling magnetic materials in CNTs by magnetic-conductive filling and electroplating, a large number of Fe particles can be observed on the tube wall microscopically. The intermediate ferrocene / CNTs composite was prepared by magnetic conductivity filling method in ferrocene / ethanol solution. Fe particles were decomposed by thermal decomposition of ferrocene, and Fe/CNTs shielding films with magnetic properties were prepared. By differential thermal / thermogravimetric analysis (DTA), the Fe content of the original film was increased from 21% to 35%. The saturation magnetization in the hysteresis loop is increased from 35.43 emu g ~ (-1) to 47.35 emu g ~ (-1), and the shielding efficiency is greatly improved in the range of 6-9 and 12-15 GHz. Ferrocene / methanol was filled into CNTs thin film by magnetic conductivity filling method. The shielding material of CNTs thin film was prepared. Methanol can not only reduce the concentration of carbon source, so as to control the supply of carbon atoms and the decomposition rate of carbon source during the reaction, on the other hand, it can also increase the dissolution of ferrocene in the metal catalyst. More Fe atoms are attached to the surface of the CNTs tube wall, and the shielding efficiency of the film is improved. In this experiment, high performance shielding films were prepared by adding a quartz capillary through ferrocene / methanol solution. By differential thermogravimetric analysis, the Fe content of ferrocene / methanol solution was increased from 21% to 31.5% compared with the original sample. The saturation magnetization in hysteresis loop also increased from 35.43 emu g ~ (-1) to 57.3 emu g ~ (-1), and the shielding efficiency increased greatly, and the shielding efficiency reached 60-65 dB near 5 and 19 GHz. The shielding material of CNTs thin film prepared by electroplating was studied. Ferrous sulfate was used as the main salt and sulfuric acid as corrosion inhibitor. The pH value of the regulating solution is 2-3 and the current is 0. 1-0. 2 A. Pure iron was used as anode material and CNTs film was used as cathode material, and a layer of nanometer iron was coated on the surface of the film. By differential thermal / thermogravimetric analysis (DTA), the Fe content increased from 21% to 22.4% by electroplating compared with the original film. The saturation magnetization of Fe particles in hysteresis loop increases from 35.45 emu g ~ (-1) to 38.35 emu g ~ (-1) for a long time in wet environment, and the shielding efficiency is improved in small frequency range. The magnetic conductivity filling method filled ferrocene / ethanol solution at room temperature and ferrocene / methanol solution at high temperature. The Fe content, ferromagnetism and shielding efficiency of the film were greatly improved. Electroplating is a new method to fabricate high shielding films in this experiment.
【學(xué)位授予單位】：江西理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類(lèi)號(hào)】：TB383.2;TQ127.11

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本文編號(hào)：1873474