CN101671001A - Preparation method for semiconductor single wall carbon nano tube - Google Patents
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- CN101671001A CN101671001A CN200910308291A CN200910308291A CN101671001A CN 101671001 A CN101671001 A CN 101671001A CN 200910308291 A CN200910308291 A CN 200910308291A CN 200910308291 A CN200910308291 A CN 200910308291A CN 101671001 A CN101671001 A CN 101671001A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000002109 single walled nanotube Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims description 5
- 239000004065 semiconductor Substances 0.000 title abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 26
- 239000010439 graphite Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 17
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 3
- 150000003624 transition metals Chemical class 0.000 claims abstract description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims 1
- 230000007847 structural defect Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000029058 respiratory gaseous exchange Effects 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 239000002079 double walled nanotube Substances 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021404 metallic carbon Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
本发明公开了一种半导体性单壁碳纳米管的制备方法，以过渡金属为催化剂，将催化剂、硫粉和纯度为99.99％的石墨粉按比例充分混合后制得阳极石墨棒，将制得的阳极石墨棒放在冲有缓冲气体的电弧室内与石墨阴极正对。通过控制阴阳两极间的放电电压和放电电流，使电弧室的阴阳两极发生电弧放电，即可制得半导体性单壁碳纳米管。本发明采用电弧法通过掺杂硫粉直接制备半导体性单壁碳纳米管，工艺简单、产率高，制备的半导体性单壁碳纳米管结构缺陷少，提高了CNT基晶体管的电子迁移率。
The invention discloses a method for preparing semiconducting single-walled carbon nanotubes. Using a transition metal as a catalyst, the catalyst, sulfur powder and graphite powder with a purity of 99.99% are fully mixed in proportion to prepare an anode graphite rod. The anode graphite rod is placed in the arc chamber filled with buffer gas and is facing the graphite cathode. By controlling the discharge voltage and discharge current between the cathode and anode, the cathode and anode of the arc chamber are arc-discharged, and the semiconductor single-walled carbon nanotubes can be prepared. The invention adopts an arc method to directly prepare semiconductive single-wall carbon nanotubes by doping sulfur powder, has simple process and high yield, and the prepared semiconductive single-wall carbon nanotubes have few structural defects, and the electron mobility of CNT-based transistors is improved.
Description
技术领域 technical field
本发明涉及一种材料制备技术领域的方法，具体是一种半导体性单壁碳纳米管的制备方法。The invention relates to a method in the technical field of material preparation, in particular to a method for preparing semiconducting single-walled carbon nanotubes.
背景技术 Background technique
由于碳纳米管(CNT)具有准一维结构和独特的电学性能，所以它自1991年被发现后就引起了科学界的广泛关注，目前广泛开展了将碳纳米管应用于纳电子器件、场发射技术、生物载药、储氢技术等诸多领域的研究工作。碳纳米管可分为单壁碳纳米管(SWNT)、双壁碳纳米管(DWNT)和多壁碳纳米管(MWNT)，其中单壁碳纳米管作为优良的一维纳米材料，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。根据单壁碳纳米管直径和手性不同，SWNT表现为金属性和半导体性，而金属性碳纳米管会严重影响CNT基晶体管的性能，因此制备纯半导体性单壁碳纳米管是解决采用碳纳米管大规模制造CNT基晶体管的关键技术之一。Due to the quasi-one-dimensional structure and unique electrical properties of carbon nanotubes (CNTs), it has attracted widespread attention from the scientific community since its discovery in 1991. Research work in many fields such as launch technology, bio-drug loading, and hydrogen storage technology. Carbon nanotubes can be divided into single-walled carbon nanotubes (SWNT), double-walled carbon nanotubes (DWNT) and multi-walled carbon nanotubes (MWNT), among which single-walled carbon nanotubes are excellent one-dimensional nanomaterials because of their Higher carrier mobility is used to manufacture nanoelectronic devices such as field effect transistors and thin film transistors, and is expected to replace silicon materials and become the key material for next-generation microelectronic devices. Depending on the diameter and chirality of single-walled carbon nanotubes, SWNTs are metallic and semiconducting, and metallic carbon nanotubes will seriously affect the performance of CNT-based transistors. Nanotubes are one of the key technologies for large-scale fabrication of CNT-based transistors.
经对现有文献检索发现，Z Xu、W Lu和W Wang等人于2008年在Adv.Mater(先进材料)上发表了题为“Converting Metallic Single-Walled Carbon Nanotubes intoSemiconductors by Boron/Nitrogen Co-Doping(通过B/N共掺杂将金属性单壁碳管转变为半导体性单壁碳管)”，该文通过B/N共掺杂的方式采用化学气相沉积法(CVD)制备出了半导体单壁碳纳米管，但是该项技术采用CVD法，工艺复杂、产率低，制备的碳纳米管存在较多的结构缺陷，限制了碳纳米管上高载流子的迁移率的产生。After searching the existing documents, it was found that Z Xu, W Lu and W Wang et al published a paper titled "Converting Metallic Single-Walled Carbon Nanotubes into Semiconductors by Boron/Nitrogen Co-Doping" on Adv.Mater (advanced materials) in 2008. (Converting metallic single-walled carbon tubes into semiconducting single-walled carbon tubes by B/N co-doping)", this paper prepared semiconductor single-walled carbon tubes by chemical vapor deposition (CVD) by B/N co-doping Wall carbon nanotubes, but this technology uses CVD method, the process is complicated, the yield is low, and the prepared carbon nanotubes have many structural defects, which limit the generation of high carrier mobility on the carbon nanotubes.
发明内容 Contents of the invention
本发明的目的在于克服现有技术中存在的不足和缺陷，提供一种半导体性单壁碳纳米管的制备方法。本发明采用电弧放电法(Arc discharging)制备的半导体性单壁碳纳米管具有结构缺陷相对较少的特点，提高了CNT基晶体管的电子迁移率。The purpose of the present invention is to overcome the deficiencies and defects in the prior art, and provide a method for preparing semiconducting single-walled carbon nanotubes. The semiconductor single-walled carbon nanotube prepared by adopting the arc discharge method in the present invention has the characteristics of relatively few structural defects, and improves the electron mobility of the CNT-based transistor.
本发明是通过以下技术方案实现，制备的具体方法为：以过渡金属为催化剂，将催化剂、硫(S)粉和纯度为99.99％的石墨粉按比例充分混合后制得阳极石墨棒，将制得的阳极石墨棒放在冲有缓冲气体的电弧室内与石墨阴极正对。通过控制阴阳两极间的放电电压和放电电流，使电弧室的阴阳两极发生且电弧放电，即可制得半导体性单壁碳纳米管。The present invention is realized through the following technical scheme, and the specific method of preparation is: using transition metal as catalyst, catalyst, sulfur (S) powder and graphite powder with a purity of 99.99% are fully mixed in proportion to obtain an anode graphite rod, and the prepared The obtained anode graphite rod is placed in the arc chamber flushed with buffer gas and faces the graphite cathode. By controlling the discharge voltage and discharge current between the cathode and anode electrodes, the cathode and anode electrodes of the arc chamber are generated and arc discharged, and the semiconducting single-wall carbon nanotubes can be prepared.
所述的催化剂、硫(S)粉和纯度为99.99％的石墨粉按比例混合，其比例是指：催化剂的含量摩尔百分比为：1％～6％，硫粉的含量摩尔百分比为：0.1％～2％，余量为纯度为99.99％的石墨粉。Described catalyst, sulfur (S) powder and the graphite powder that purity is 99.99% are mixed in proportion, and its ratio refers to: the content molar percentage of catalyst is: 1%～6%, the content molar percentage of sulfur powder is: 0.1% ~2%, the balance is graphite powder with a purity of 99.99%.
所述的催化剂是铁(Fe)、钴(Co)、镍(Ni)、钇(Y)中的一种或几种。The catalyst is one or more of iron (Fe), cobalt (Co), nickel (Ni) and yttrium (Y).
所述的阳极石墨棒是将催化剂、硫粉和纯度为99.99％的石墨粉按比例充分混合后填棒制得。The anode graphite rod is prepared by fully mixing catalyst, sulfur powder and graphite powder with a purity of 99.99% in proportion and then filling the rod.
所述的阳极石墨棒是将催化剂、硫粉和纯度为99.99％的石墨粉按比例充分混合后加粘结剂挤压成棒。The anode graphite rod is obtained by fully mixing catalyst, sulfur powder and graphite powder with a purity of 99.99% in proportion, adding a binder and extruding it into a rod.
所述的缓冲气体是惰性气体中的一种或几种。The buffer gas is one or several kinds of inert gases.
所述的缓冲气体的气压范围为20KPa～90KPa。The pressure range of the buffer gas is 20KPa-90KPa.
所述的放电电压范围为40V～80V，放电电流范围是60A～120A。The discharge voltage range is 40V-80V, and the discharge current range is 60A-120A.
与现有技术相比，本发明的有益效果是：采用电弧法通过掺杂硫粉直接制备半导体性单壁碳纳米管，工艺简单、产率高，制备的半导体性单壁碳纳米管结构缺陷少，提高了CNT基晶体管的电子迁移率。Compared with the prior art, the beneficial effect of the present invention is that the semiconductive single-wall carbon nanotubes are directly prepared by doping sulfur powder by the electric arc method, the process is simple, the yield is high, and the prepared semiconductive single-wall carbon nanotubes have structural defects less, improving the electron mobility of CNT-based transistors.
附图说明 Description of drawings
图1是实施例2制备出的半导体性单壁碳纳米管的扫描电镜照片；Fig. 1 is the scanning electron micrograph of the semiconducting single-walled carbon nanotube that embodiment 2 prepares;
图2是实施例2制备出的半导体性单壁碳纳米管的投射电镜照片；Fig. 2 is the transmission electron micrograph of the semiconductive single-walled carbon nanotube prepared in embodiment 2;
图3是实施例2制备出的半导体性单壁碳纳米管的拉曼光谱的径向呼吸模；Fig. 3 is the radial breathing mode of the Raman spectrum of the semiconductive single-walled carbon nanotube prepared in embodiment 2;
其中：(a)为514nm激光下得到的拉曼光谱的径向呼吸模；(b)为633nm激光下得到的拉曼光谱的径向呼吸模。Among them: (a) is the radial breathing mode of the Raman spectrum obtained under the 514nm laser; (b) is the radial breathing mode of the Raman spectrum obtained under the 633nm laser.
具体实施方式 Detailed ways
下面结合附图对本发明的实施例作详细说明，所有实施例都是在以本发明技术方案为前提下进行实施，给出了详细实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. All embodiments are implemented on the premise of the technical solutions of the present invention, and detailed implementation methods and specific operating procedures are provided, but the protection scope of the present invention is not limited to Examples described below.
实施例1Example 1
将纯度为99.99％的石墨粉、Ni粉、氧化钇(Y2O3)粉和硫粉按照摩尔比为94.7％∶4.2％∶1％∶0.1％的比例充分混合均匀后，填充于4mm×4cm×6mm的石墨棒中制得阳极石墨棒。将阳极石墨棒置于通有30KPa氦气的电弧室内与石墨阴极正对，控制阴阳两极间的放电电流为60A～70A，放电电压为40V～50V，放电时间为5分钟，最终得到0.8g的半导体性单壁碳纳米管。Graphite powder with a purity of 99.99%, Ni powder, yttrium oxide (Y 2 O 3 ) powder and sulfur powder are fully mixed according to the molar ratio of 94.7%: 4.2%: 1%: 0.1%, and then filled in a 4mm× Anode graphite rods were prepared from graphite rods of 4cm×6mm. Place the anode graphite rod in an arc chamber filled with 30KPa helium gas to face the graphite cathode, control the discharge current between the cathode and anode to 60A-70A, discharge voltage to 40V-50V, and discharge time for 5 minutes to finally obtain 0.8g of Semiconducting single-walled carbon nanotubes.
实施例2Example 2
将纯度为99.99％的石墨粉、Fe粉和硫粉按照摩尔比为94％∶5％∶1％的比例充分混合均匀后，再加入25wt％煤焦油混合压棒成型，然后将该棒放入氮气保护的高温炉中1000℃处理3小时制得阳极石墨棒。将阳极石墨棒置于通有12KPa氢气、18KPa氩气的电弧室内与石墨阴极正对，控制阴阳两极间的放电电流为90A～100A，放电电压为60V～70V，放电时间为8分钟，最终得1g的半导体性单壁碳纳米管。Graphite powder, Fe powder and sulfur powder with a purity of 99.99% are fully mixed according to the molar ratio of 94%: 5%: 1%, and then 25wt% coal tar is added to press the rod to form it, and then the rod is put into Anode graphite rods were prepared by treating at 1000°C for 3 hours in a nitrogen-protected high-temperature furnace. Place the anode graphite rod in the arc chamber with 12KPa hydrogen and 18KPa argon to face the graphite cathode, control the discharge current between the cathode and anode to 90A-100A, discharge voltage to 60V-70V, and discharge time to 8 minutes. Finally, 1 g of semiconducting single-walled carbon nanotubes.
制备的半导体性单壁纳米管的扫描电镜照片如图1所示；投射电镜照片如图2所示；分别在514nm激光和633nm激光下得到的拉曼光谱的径向呼吸模如图3(a)和图3(b)所示，其中：横坐标为以nm为单位的波长，纵坐标为以arb.unit(任意单位)为单位的光强，M代表金属性，S代表半导体性，由于M的峰值均小于S的峰值，故本实施例所制备的碳纳米管中金属性碳纳米管含量降低。The scanning electron micrograph of the prepared semiconducting single-walled nanotube is shown in Figure 1; the transmission electron micrograph is shown in Figure 2; the radial breathing mode of the Raman spectrum obtained under the 514nm laser and the 633nm laser is shown in Figure 3 (a ) and Fig. 3(b), wherein: the abscissa is the wavelength in nm, the ordinate is the light intensity in arb.unit (arbitrary unit), M represents metallicity, and S represents semiconductivity, because The peak value of M is smaller than the peak value of S, so the content of metallic carbon nanotubes in the carbon nanotubes prepared in this embodiment is reduced.
实施例3Example 3
将纯度为99.99％的石墨粉、Ni粉、Co粉、Fe粉和硫粉按照摩尔比为94.8％∶3％∶0.6％∶0.6％∶1％的比例混合均匀后，再加入25wt％煤焦油混合压棒成型，然后将该棒放入氮气保护的高温炉中在1000℃加热3小时制得阳极石墨棒。将阳极石墨棒置于通有24KPa氢气、36KPa氩气的电弧室内与石墨阴极正对，控制阴阳两极间的放电电流为110A～120A，放电电压为60V～70V，放电时间为10分钟，最终得1.2g的半导体性单壁碳纳米管。After the graphite powder, Ni powder, Co powder, Fe powder and sulfur powder with a purity of 99.99% are mixed uniformly according to the molar ratio of 94.8%: 3%: 0.6%: 0.6%: 1%, then add 25wt% coal tar The mixed press rod is formed, and then the rod is placed in a nitrogen-protected high-temperature furnace and heated at 1000° C. for 3 hours to obtain an anode graphite rod. Place the anode graphite rod in the arc chamber with 24KPa hydrogen and 36KPa argon to face the graphite cathode, control the discharge current between the cathode and anode to be 110A-120A, the discharge voltage to be 60V-70V, and the discharge time to be 10 minutes. Finally, 1.2 g of semiconducting single-walled carbon nanotubes.
实施例4Example 4
将纯度为99.99％的石墨粉、Ni粉、Y2O3粉和硫粉按照摩尔比为92.8％∶4.2％∶1％∶2％的比例混合均匀后，填充于4mm×4cm×6mm的石墨棒中制得阳极石墨棒。将阳极石墨棒置于通有30KPa氦气的电弧室内与石墨阴极正对，控制阴阳两极间的放电电流为80A～90A，放电电压为60V～70V，放电时间为8分钟，最终得到1g的半导体性单壁碳纳米管。Graphite powder, Ni powder, Y 2 O 3 powder and sulfur powder with a purity of 99.99% are mixed uniformly according to the molar ratio of 92.8%: 4.2%: 1%: 2%, and then filled in a 4mm×4cm×6mm graphite Anode graphite rods were made from rods. Place the anode graphite rod in an arc chamber filled with 30KPa helium gas to face the graphite cathode, control the discharge current between the cathode and anode to 80A-90A, discharge voltage to 60V-70V, and discharge time to 8 minutes to finally obtain 1g of semiconductor single-walled carbon nanotubes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101905880A (en) * | 2010-07-23 | 2010-12-08 | 上海交通大学 | Preparation method of diameter-controllable single-walled carbon nanotubes |
| CN102351171A (en) * | 2011-09-15 | 2012-02-15 | 上海交通大学 | Method for selectively preparing single-walled carbon nanotube in magnetic field |
| CN102502571A (en) * | 2011-10-11 | 2012-06-20 | 上海交通大学 | Method for manufacturing single-walled carbon nanotube aligned film by magnetically induced arc discharge |
| CN102602911A (en) * | 2012-03-07 | 2012-07-25 | 上海交通大学 | Method for preparing single-walled carbon nanotube by adopting controllability of low-pressure reactant gas |
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