CN101905880A - Preparation method of diameter-controllable single-walled carbon nanotubes - Google Patents
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- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 51
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 14
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- 239000010941 cobalt Substances 0.000 claims description 2
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- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
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Abstract
一种纳米材料技术领域的直径可控单壁碳纳米管的制备方法，包括如下步骤：步骤一：以过渡金属为催化剂，将催化剂与99.99％的石墨粉按比例充分混合后制得直径为6mm的阳极棒，阴极采用直径为8mm的纯石墨棒；步骤二：将阳极石墨在充有含一氧化碳的缓冲气体的电弧室内与阴极石墨棒正对，进行电弧放电；通过控制阴阳两极间的放电电流和放电电压和一氧化碳压力，即可制得直径可控的单壁碳纳米管。本发明的方法工艺简单、单壁碳纳米管管径可控、便于大规模制备。
A method for preparing diameter-controllable single-walled carbon nanotubes in the technical field of nanomaterials, comprising the following steps: Step 1: using a transition metal as a catalyst, fully mixing the catalyst with 99.99% graphite powder in proportion to obtain a diameter of 6mm The anode rod, the cathode adopts a pure graphite rod with a diameter of 8 mm; Step 2: The anode graphite is placed in an arc chamber filled with a buffer gas containing carbon monoxide and the cathode graphite rod is facing, and the arc discharge is performed; by controlling the discharge current between the cathode and the cathode And discharge voltage and carbon monoxide pressure, the single-walled carbon nanotubes with controllable diameter can be prepared. The method of the invention has the advantages of simple process, controllable diameter of the single-walled carbon nanotube and convenient large-scale preparation.
Description
技术领域technical field
本发明涉及一种纳米材料技术领域的制备方法，尤其是一种采用电弧放电法的直径可控单壁碳纳米管的制备方法。The invention relates to a preparation method in the technical field of nanometer materials, in particular to a preparation method of a diameter-controllable single-wall carbon nanotube by an arc discharge method.
背景技术Background technique
碳纳米管(Carbon nanotubes；CNT)因具有卓越的机械、热学性能和独特的电学性能，因此在材料科学、化学、物理学、电子学以及其他交叉学科领域中，均具有极其广泛的应用前景，目前将碳纳米管已经被应用于纳电子器件、场发射技术、生物载药、储氢技术等等诸多领域。碳纳米管可分为单璧碳纳米管(SWNT)、双璧碳纳米管(DWNT)和多壁碳纳米管(MWNT)。其中SWNT作为优良的准一维纳米材料，因其具有较高的载流子迁移率而被用作制造场效应晶体管、薄膜晶体管等纳电子器件，有望取代硅材料而成为下一代微电子器件的关键材料。众所周知，单壁碳纳米管的光学、电学性质取决于它们的直径和手性分布，根据直径和手性的不同，SWNT表现为金属性和半导体性。而且半导体性SWNT的带隙也与其直径大小有一定的关系。但是，传统方法制备的SWNT产物中，SWNT具有较宽的直径分布，金属性和半导体性SWNT混合在一起，因而其光学、电学性能变化比较大。因此如何通过各种技术控制SWNT的直径和手性分布，制备直径可控的单壁碳纳米管是解决采用SWNT大规模制造SWNT基纳电子器件的关键技术之一。Carbon nanotubes (Carbon nanotubes; CNT) have extremely broad application prospects in material science, chemistry, physics, electronics and other interdisciplinary fields due to their excellent mechanical, thermal and unique electrical properties. At present, carbon nanotubes have been applied in many fields such as nanoelectronic devices, field emission technology, biological drug loading, hydrogen storage technology and so on. Carbon nanotubes can be classified into single-walled carbon nanotubes (SWNTs), double-walled carbon nanotubes (DWNTs) and multi-walled carbon nanotubes (MWNTs). Among them, SWNT, as an excellent quasi-one-dimensional nanomaterial, is used to manufacture nanoelectronic devices such as field effect transistors and thin film transistors because of its high carrier mobility. It is expected to replace silicon materials and become the next generation of microelectronic devices. key material. It is well known that the optical and electrical properties of single-walled carbon nanotubes depend on their diameter and chirality distribution. According to the difference in diameter and chirality, SWNTs exhibit metallic and semiconducting properties. Moreover, the band gap of semiconducting SWNT also has a certain relationship with its diameter. However, in the SWNT products prepared by traditional methods, SWNTs have a wide diameter distribution, and metallic and semiconducting SWNTs are mixed together, so their optical and electrical properties vary greatly. Therefore, how to control the diameter and chirality distribution of SWNTs through various techniques, and prepare single-walled carbon nanotubes with controllable diameters is one of the key technologies to solve the large-scale manufacture of SWNT-based nanoelectronic devices using SWNTs.
近几年来，很多研究者致力于直径可控的单壁碳纳米管的制备研究(M.G.Hahm，Y.K.Kwon，E.Lee，C.W.Ahn，Y.J.Jung.Diameter selective growth of vertically aligned singlewalled carbon nanotubes and study on their growth mechanism.J.Phys.Chem.C 2008，112(44)，17143-17147)，其主要手段是通过化学气相沉积法(CVD)控制催化剂大小、碳源或生长条件等来实现单壁碳纳米管的窄直径分布。但由于CVD法所制备的SWNT存在缺陷，对SWNT的电性能有影响。In recent years, many researchers have devoted themselves to the preparation of diameter-controllable single-walled carbon nanotubes (M.G.Hahm, Y.K.Kwon, E.Lee, C.W.Ahn, Y.J.Jung. Diameter selective growth of vertically aligned singlewalled carbon nanotubes and study on their growth mechanism.J.Phys.Chem.C 2008, 112(44), 17143-17147), the main method is to control the catalyst size, carbon source or growth conditions by chemical vapor deposition (CVD) to achieve single-walled carbon Narrow diameter distribution of nanotubes. However, due to defects in SWNTs prepared by CVD, the electrical properties of SWNTs are affected.
发明内容Contents of the invention
本发明的目的在于克服现有技术中的不足，提供了一种直径可控单壁碳纳米管的制备方法。通过向缓冲气体中混合一氧化碳气体来控制单壁碳纳米管直径的分布，所制的单壁碳纳米管产品直径可控，保证了SWNT基晶体管的性能一致性和高电子迁移率。The purpose of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing single-walled carbon nanotubes with controllable diameter. By mixing carbon monoxide gas into the buffer gas to control the distribution of the diameter of the single-walled carbon nanotubes, the diameter of the prepared single-walled carbon nanotubes is controllable, which ensures the performance consistency and high electron mobility of the SWNT-based transistor.
本发明是通过以下技术方案实现，本发明包括以下步骤：The present invention is realized through the following technical solutions, and the present invention comprises the following steps:
步骤一：以过渡金属为催化剂，将催化剂与99.99％的高纯石墨粉按比例充分混合后制得直径为6mm的阳极石墨棒，阴极采用直径为8mm的纯石墨棒。Step 1: using a transition metal as a catalyst, fully mix the catalyst with 99.99% high-purity graphite powder in proportion to prepare an anode graphite rod with a diameter of 6 mm, and a pure graphite rod with a diameter of 8 mm for the cathode.
所述过渡金属催化剂为铁(Fe)、钴(Co)、镍(Ni)、钇(Y)的一种或几种混合物或者化合物。The transition metal catalyst is one or more mixtures or compounds of iron (Fe), cobalt (Co), nickel (Ni), and yttrium (Y).
所述过渡金属催化剂摩尔百分比为1％～6％。The molar percentage of the transition metal catalyst is 1%-6%.
所述阳极棒是将催化剂与99.99％高纯石墨粉按比例充分混合后填棒制得。The anode rod is prepared by fully mixing the catalyst and 99.99% high-purity graphite powder in proportion and then filling the rod.
所述阳极棒是将催化剂与99.99％高纯石墨粉按比例充分混合后加粘结剂挤压成棒并烧结制得。The anode rod is obtained by fully mixing the catalyst and 99.99% high-purity graphite powder in proportion, adding a binder, extruding into a rod and sintering.
步骤二：将步骤一所制备的阳极石墨在充有含一氧化碳的缓冲气体的电弧室内与阴极石墨棒正对，进行电弧放电。通过控制阴阳两极间的放电电流和放电电压和一氧化碳压力，即可制得直径可控的单壁碳纳米管。Step 2: The anode graphite prepared in
所述一氧化碳的压力为8～30kPa。The pressure of the carbon monoxide is 8-30kPa.
所述缓冲气体为氦、氩、氢等气体或它们的混合气体，气压为10～30kPa。The buffer gas is gas such as helium, argon, hydrogen or their mixed gas, and the pressure is 10-30kPa.
所述放电电弧的电压为40～80V，电流60～110A。The voltage of the discharge arc is 40-80V, and the current is 60-110A.
与现有技术相比，本发明具有如下的有益效果：本发明通过调节缓冲气体中一氧化碳气体压力，利用电弧放电法可以大量制备直径可控的单壁碳纳米管，从而保证单壁碳纳米管在光学、电学性能的均一性，同时兼具电弧法制备单壁碳纳米管的低缺陷特点，将为制备高性能SWCNT基纳米器件提供更有利的保障。该发明工艺简单、产率高，便于大规模推广与应用。Compared with the prior art, the present invention has the following beneficial effects: the present invention can prepare a large number of single-walled carbon nanotubes with controllable diameters by using the arc discharge method by adjusting the pressure of carbon monoxide gas in the buffer gas, thereby ensuring the single-walled carbon nanotubes The uniformity of optical and electrical properties, as well as the low defect characteristics of single-walled carbon nanotubes prepared by arc method, will provide a more favorable guarantee for the preparation of high-performance SWCNT-based nanodevices. The invention has simple process and high yield, and is convenient for large-scale popularization and application.
附图说明Description of drawings
图1为实施例1所制备的单壁碳纳米管的扫描电镜(SEM)照片；Fig. 1 is the scanning electron microscope (SEM) photo of the single-walled carbon nanotube prepared by
图2为实施例1所制备的单壁碳纳米管的投射电镜(TEM)照片；Fig. 2 is the transmission electron microscope (TEM) photograph of the single-walled carbon nanotube prepared by
图3为对比例所制备的单壁碳纳米管的拉曼光谱图；Fig. 3 is the Raman spectrogram of the single-wall carbon nanotube prepared by comparative example;
图4为实施例1所制备的单壁碳纳米管的拉曼光谱图。FIG. 4 is a Raman spectrum of the single-walled carbon nanotubes prepared in Example 1. FIG.
具体实施方式Detailed ways
以下结合附图对本发明的实施例作详细说明：以下实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和过程，但本发明的保护范围不限于下述的实施例。Embodiments of the present invention are described in detail below in conjunction with the accompanying drawings: the following embodiments are implemented on the premise of the technical solutions of the present invention, and detailed implementation methods and processes are provided, but the protection scope of the present invention is not limited to the following implementations example.
对比例comparative example
步骤一：以高纯石墨粉、Ni粉、Y2O3粉为原料，按照摩尔比(C∶Ni∶Y为94∶4.8∶1.2)，混合均匀后加入25wt％煤焦油混合挤压成直径为6mm的石墨棒，然后放入氮气保护的高温炉中1000℃处理2小时，即制得阳极石墨棒。Step 1: Using high-purity graphite powder, Ni powder, and Y2O3 powder as raw materials, according to the molar ratio (C:Ni:Y is 94:4.8:1.2 ) , mix evenly and add 25wt% coal tar to mix and extrude into a diameter 6mm graphite rod, and then placed in a nitrogen-protected high-temperature furnace for 2 hours at 1000°C to obtain an anode graphite rod.
步骤二：以步骤一所制阳极棒，直径为8mm纯石墨棒作为阴极，电弧放电在通有30kPa氦气的电弧室中进行。放电电流为80～90A，电压为50～60V。放电时间为5分钟，制得约0.6g单壁碳纳米管。所制备产物的拉曼光谱图如3所示，通过计算得出产物中直径为1.71nm、1.49nm、1.35nm和1.28nm。Step 2: The anode rod made in
实施例1Example 1
步骤一：以高纯石墨粉、Ni粉、Y2O3粉为原料，按照摩尔比(C∶Ni∶Y为94∶4.8∶1.2)，混合均匀后加入25wt％煤焦油混合挤压成直径为6mm的石墨棒，然后放入氮气保护的高温炉中1000℃处理2小时，即制得阳极石墨棒。Step 1: Using high-purity graphite powder, Ni powder, and Y2O3 powder as raw materials, according to the molar ratio (C:Ni:Y is 94:4.8:1.2 ) , mix evenly and add 25wt% coal tar to mix and extrude into a diameter 6mm graphite rod, and then placed in a nitrogen-protected high-temperature furnace for 2 hours at 1000°C to obtain an anode graphite rod.
步骤二：以步骤一所制阳极棒，直径为8mm纯石墨棒作为阴极，电弧放电在通有18kPa氦气和12kPa一氧化碳气体的电弧室中进行。放电电流为80～90A，电压为50～60V。放电时间为10分钟，制得约1g窄直径分布的单壁碳纳米管。所制备产物的拉曼光谱图如4所示，与对比例对照可以看出，直径较小的单壁碳纳米管(1.35nm、1.28nm)消失、只剩下直径较大的单壁碳纳米管(1.71nm、1.49nm)。Step 2: The anode rod made in
实施例2Example 2
步骤一：以高纯石墨粉、Fe粉为原料，按照摩尔比(C∶Fe为99∶1)，混合均匀后加入25wt％煤焦油混合挤压成直径为6mm的石墨棒，然后放入氮气保护的高温炉中1000℃处理2小时，即制得阳极石墨棒。Step 1: Using high-purity graphite powder and Fe powder as raw materials, according to the molar ratio (C:Fe is 99:1), mix evenly, add 25wt% coal tar, mix and extrude it into a graphite rod with a diameter of 6mm, and then put in nitrogen Treat in a protected high-temperature furnace at 1000°C for 2 hours to obtain an anode graphite rod.
步骤二：以步骤一所制阳极棒，直径为8mm纯石墨棒作为阴极，电弧放电在通有12kPa氢气、18kPa氩气和8kPa一氧化碳气体的电弧室中进行。放电电流为60～70A，电压为60～70V。放电时间为12分钟，制得约0.8g窄直径分布的单壁碳纳米管。Step 2: Use the anode rod made in
实施例3Example 3
步骤一：以高纯石墨粉、Ni粉、Co粉、Fe粉为原料，按照摩尔比(C∶Ni∶Co∶Fe为95.8∶3∶0.6∶0.6)，混合均匀后填充于内径4mm，深5cm的6mm石墨棒中，即为阳极石墨棒。Step 1: Use high-purity graphite powder, Ni powder, Co powder, and Fe powder as raw materials, according to the molar ratio (C: Ni: Co: Fe is 95.8: 3: 0.6: 0.6), mix evenly and fill in the inner diameter of 4mm, deep Among the 5cm and 6mm graphite rods, it is the anode graphite rod.
步骤二：以步骤一所制阳极棒，直径为8mm纯石墨棒作为阴极，电弧放电在通有8kPa氢气、12kPa氩气和10kPa一氧化碳气体的电弧室中进行。放电电流为100～110A，电压为40～50V。放电时间为5分钟，制得约0.6g窄直径分布的单壁碳纳米管。Step 2: Using the anode rod made in
实施例4Example 4
以高纯石墨粉、Ni粉、Y2O3粉为原料，按照摩尔比(C∶Ni∶Y为94.8∶4.2∶1)，混合均匀后填充于内径4mm，深4cm的6mm石墨棒中，即为阳极石墨棒。Using high-purity graphite powder, Ni powder, and Y2O3 powder as raw materials, according to the molar ratio (C:Ni:Y is 94.8: 4.2 :1), mix them evenly and fill them in a 6mm graphite rod with an inner diameter of 4mm and a depth of 4cm. It is the anode graphite rod.
步骤二：以步骤一所制阳极棒，直径为8mm纯石墨棒作为阴极，电弧放电在通有18kPa氦气和12kPa一氧化碳气体的电弧室中进行。放电电流为100～110A，电压为60～70V。放电时间为4分钟，制得约0.6g窄直径分布的单壁碳纳米管。Step 2: The anode rod made in
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| CN101671001A (en) * | 2009-10-15 | 2010-03-17 | 上海交通大学 | Preparation method for semiconductor single wall carbon nano tube |
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| 《AIP Conference Proceedings》 20011231 Henning Kanzow et al. Macroscopic fibers of carbon nanotubes produced by electric arc discharge 568-571 1-7 , 第591期 2 * |
| 《Nature》 19970821 C.Journet et al. Large-scale production of single-walled carbon nanotubes by the electric-arc technique 756-758 1-7 第388卷, 2 * |
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