CN1831212A - A method for synthesizing carbon-coated germanium nanowires - Google Patents

A method for synthesizing carbon-coated germanium nanowires Download PDF

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CN1831212A
CN1831212A CN 200610049547 CN200610049547A CN1831212A CN 1831212 A CN1831212 A CN 1831212A CN 200610049547 CN200610049547 CN 200610049547 CN 200610049547 A CN200610049547 A CN 200610049547A CN 1831212 A CN1831212 A CN 1831212A
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germanium
catalyst
acetylene
carbon
coated
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CN1328417C (en
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陶新永
张孝彬
程继鹏
罗志强
刘芙
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention discloses a method to make compounding carbon covering germanium nm wire. It includes the following steps: using germanium oxide formed by hydrolysis germanium tetrachloride as catalyst, adding the catalyst into fixed bed gas continuously flowing reacting furnace at the temperature of 700-1000 degree centigrade, adding acetylene, argon gas or nitrogen gas that the ratio is 1:5-1:20, taking reaction for 10-60 minutes, collecting the product. The invention has simple method, high yield, low cost, and is benefit for industrial producing.

Description

一种合成碳包覆锗纳米线的方法A method for synthesizing carbon-coated germanium nanowires

技术领域technical field

本发明涉及一种合成碳包覆锗纳米线的方法。The invention relates to a method for synthesizing carbon-coated germanium nanowires.

背景技术Background technique

金属纳米线是近年来发现的一种新型一维纳米材料。碳包覆技术不仅可以有效防止金属纳米线的氧化,而且碳包覆金属纳米线在传感器、电化学储能、纳米器件等方面具有良好的应用前景。化学气相沉积法由于其产量高,操作简单,投资少,因而也已成为当前制备纳米材料的一种流行方法。该方法通常固体催化剂,通过在固定床上裂解有机气体如甲烷、乙炔、乙烯和丙稀,最终得到产物。目前还没有利用化学气相沉积法合成碳包覆锗纳米线的报道。Metal nanowires are a new type of one-dimensional nanomaterials discovered in recent years. Carbon coating technology can not only effectively prevent the oxidation of metal nanowires, but also has good application prospects in sensors, electrochemical energy storage, and nanodevices. Due to its high output, simple operation and low investment, chemical vapor deposition has become a popular method for preparing nanomaterials. The method is usually a solid catalyst, and the final product is obtained by cracking organic gases such as methane, acetylene, ethylene and propylene on a fixed bed. There is no report on the synthesis of carbon-coated germanium nanowires by chemical vapor deposition.

发明内容Contents of the invention

本发明的目的是提供一种低成本,产量高的合成碳包覆锗纳米线的方法。The purpose of the invention is to provide a low-cost, high-yield method for synthesizing carbon-coated germanium nanowires.

本发明的合成碳包覆锗纳米线的方法在固定床气体连续流动反应装置中进行,步骤如下:The method for synthesizing carbon-coated germanium nanowires of the present invention is carried out in a fixed-bed gas continuous flow reaction device, and the steps are as follows:

以水解四氯化锗形成的氧化锗为催化剂,将催化剂放入温度为700~1000℃的固定床气体连续流动反应炉中,通入乙炔、氩气或氮气,乙炔与氩气或氮气的气体流量比为1∶5~1∶20,反应10~60分钟,收集产物。Use germanium oxide formed by hydrolyzing germanium tetrachloride as a catalyst, put the catalyst into a fixed-bed gas continuous flow reaction furnace with a temperature of 700-1000 ° C, and feed acetylene, argon or nitrogen, acetylene and argon or nitrogen gas The flow ratio is 1:5-1:20, react for 10-60 minutes, and collect the product.

上述四氯化锗的水解采用Chinese Journal of Rare Metals,1998,22,345报道的方法进行。The hydrolysis of above-mentioned germanium tetrachloride adopts the method reported in Chinese Journal of Rare Metals, 1998,22,345 to carry out.

本发明提供的方法简单,产量高,成本低,有利于工业化生产。所合成的碳包覆锗纳米线直径分布在30~90nm,长度分布在600nm~2μm。The method provided by the invention is simple, has high output and low cost, and is beneficial to industrialized production. The synthesized carbon-coated germanium nanowires have a diameter distribution of 30-90nm and a length distribution of 600nm-2μm.

附图说明Description of drawings

图1是本发明方法制得的碳包覆锗纳米线的扫描电镜(SEM)照片;Fig. 1 is the scanning electron microscope (SEM) photograph of the carbon-coated germanium nanowire that the inventive method makes;

图2是本发明方法制得的碳包覆锗纳米线的透射电镜(TEM)照片。Fig. 2 is a transmission electron microscope (TEM) photo of carbon-coated germanium nanowires prepared by the method of the present invention.

具体实施方式Detailed ways

实施例1Example 1

利用四氯化锗进行水解得到氧化锗粉末。碳包覆锗纳米线的制备在固定床气体连续流动反应炉上进行。当炉温升至1000℃后,将氧化锗催化剂放入炉中段恒温区,通入乙炔和氮气,流量比为乙炔∶氮气=1∶15,反应20分钟后制得碳包覆锗纳米线。该产品的FESEM照片如图1所示。The germanium oxide powder is obtained by hydrolyzing germanium tetrachloride. The carbon-coated germanium nanowires were prepared in a fixed-bed gas continuous flow reactor. When the temperature of the furnace rose to 1000°C, the germanium oxide catalyst was placed in the constant temperature zone in the middle of the furnace, and acetylene and nitrogen were introduced at a flow ratio of acetylene:nitrogen=1:15. Carbon-coated germanium nanowires were prepared after 20 minutes of reaction. The FESEM photo of the product is shown in Figure 1.

实施例2Example 2

利用四氯化锗进行水解得到氧化锗粉末。碳包覆锗纳米线的制备在固定床气体连续流动反应炉上进行。当炉温升至700℃后,将氧化锗催化剂放入炉中段恒温区,通入乙炔和氩气,流量比为乙炔∶氩气=1∶7,反应30分钟后制得碳包覆锗纳米线。The germanium oxide powder is obtained by hydrolyzing germanium tetrachloride. The carbon-coated germanium nanowires were prepared in a fixed-bed gas continuous flow reactor. When the furnace temperature rises to 700°C, the germanium oxide catalyst is placed in the constant temperature zone in the middle of the furnace, and acetylene and argon are introduced at a flow ratio of acetylene: argon = 1:7. After 30 minutes of reaction, carbon-coated germanium nanoparticles are prepared. Wire.

实施例3Example 3

利用四氯化锗进行水解得到氧化锗粉末。碳包覆锗纳米线的制备在固定床气体连续流动反应炉上进行。当炉温升至850℃后,将氧化锗催化剂放入炉中段恒温区,通入乙炔和氩气,流量比为乙炔∶氮气=1∶10,反应50分钟后制得碳包覆锗纳米线。图2是其TEM照片。The germanium oxide powder is obtained by hydrolyzing germanium tetrachloride. The carbon-coated germanium nanowires were prepared in a fixed-bed gas continuous flow reactor. When the furnace temperature rises to 850°C, put the germanium oxide catalyst into the constant temperature zone in the middle of the furnace, feed acetylene and argon, the flow ratio is acetylene: nitrogen = 1:10, and react for 50 minutes to prepare carbon-coated germanium nanowires . Figure 2 is its TEM photo.

Claims (1)

1.一种合成碳包覆锗纳米线的方法,其步骤如下:以水解四氯化锗形成的氧化锗为催化剂,将催化剂放入温度为700~1000℃的固定床气体连续流动反应炉中,通入乙炔、氩气或氮气,乙炔与氩气或氮气的气体流量比为1∶5~1∶20,反应10~60分钟,收集产物。1. A method for synthesizing carbon-coated germanium nanowires, the steps are as follows: the germanium oxide formed by hydrolysis of germanium tetrachloride is used as a catalyst, and the catalyst is put into a fixed-bed gas continuous flow reaction furnace with a temperature of 700 to 1000°C , feed acetylene, argon or nitrogen, the gas flow ratio of acetylene to argon or nitrogen is 1:5 to 1:20, react for 10 to 60 minutes, and collect the product.
CNB2006100495476A 2006-02-20 2006-02-20 Method for by composition cladding germanium nanometer wire Expired - Fee Related CN1328417C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101176915B (en) * 2006-11-09 2010-05-26 南京大学 A kind of preparation method of carbon-coated nano metal nickel particle material
CN103540995A (en) * 2013-10-15 2014-01-29 东华大学 Method used for liquid phase synthesis of germanium nanowires

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1177351C (en) * 2002-07-17 2004-11-24 浙江大学 Method for growing germanium nanowires using alumina template
CN1315605C (en) * 2005-04-28 2007-05-16 浙江大学 Supersonic liquid phase reduction process for preparing monodisperse nano germanium crystal

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101176915B (en) * 2006-11-09 2010-05-26 南京大学 A kind of preparation method of carbon-coated nano metal nickel particle material
CN103540995A (en) * 2013-10-15 2014-01-29 东华大学 Method used for liquid phase synthesis of germanium nanowires
CN103540995B (en) * 2013-10-15 2016-08-10 东华大学 A method for liquid-phase synthesis of germanium nanowires

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