CN102249211A - Method for preparing carbon nanotube by using petroleum ether as raw material - Google Patents
Method for preparing carbon nanotube by using petroleum ether as raw material Download PDFInfo
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- CN102249211A CN102249211A CN2010101767949A CN201010176794A CN102249211A CN 102249211 A CN102249211 A CN 102249211A CN 2010101767949 A CN2010101767949 A CN 2010101767949A CN 201010176794 A CN201010176794 A CN 201010176794A CN 102249211 A CN102249211 A CN 102249211A
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Abstract
The invention discloses a method for preparing a carbon nanotube by using petroleum ether as raw material, comprising the following steps: first, preparing an iron catalytic membrane by using the means of electron-beam evaporation, then preparing the carbon nanotube by using chemical vapor deposition. The method has the advantages of low cost and simple technology, and the prepared carbon nanotube grows orientedly, and can be used in electron devices, field emitters, hydrogen storage material and other high strength conductive composite materials.
Description
Technical field
The present invention relates to a kind of method for preparing carbon nanotube, particularly a kind of is the method for feedstock production carbon nanotube with the sherwood oil.
Background technology
1985, Smalley found soccerballene C
60, particular structure (20 regular hexagons and 12 regular pentagons are formed globosity) makes it become the allotropic substance of another carbon after diamond and graphite.And IIijima in 1991 makes us enter a brand-new stage to the understanding and the research of carbon material to the discovery of carbon nanotube.
Carbon nanotube is a kind of pattern uniqueness, the nano material of electronics and satisfactory mechanical property.Generally speaking, the number of plies according to pipe can be divided into it single wall and multi-walled carbon nano-tubes.In Single Walled Carbon Nanotube, cause the electronics changes of properties according to arranging of carbon atom, it can be divided into two kinds of semi-conductor and conductor carbon nanotubes again; And the electronics performance of multi-walled carbon nano-tubes, because the difference between layer and the layer makes its whole electronics performance complicated more.In addition, carbon nanotube also has the favorable mechanical performance: generally, the physical strength of Single Walled Carbon Nanotube is about 1TPa; And the physical strength of multi-walled carbon nano-tubes is * 10
2In the MPa scope.Therefore, the application of carbon nanotube is more extensive, comprises Nano semiconductor electron device, probe, Field Emission Display, high-strength conductive matrix material and hydrogen storage material or the like.
The preparation method of carbon current nanotube mainly is divided into three kinds: arc discharge method, laser evaporation method and chemical Vapor deposition process.Wherein, chemical Vapor deposition process is a kind of widely used preparation method.Generally, this method is to be raw material with gas, such as methane, acetylene, and synthesizing carbon nanotubes under the condition of certain air pressure, high temperature, catalyst.But because the high-purity gas kind is single, price is higher, makes the preparation of carbon nanotube be subjected to certain restriction.
Summary of the invention
The present invention seeks to be to provide a kind of is the method for feedstock production carbon nanotube with the sherwood oil.
Sherwood oil is a kind of liquid organic mixture, mainly is made up of hydrocarbons, belongs to oils.Generally, the product that is divided into different grades according to the difference of boiling range (30-60 ℃, 60-90 ℃, 90-120 ℃).Boiling range mainly is by pentane at 30-60 ℃ product, and hexane is formed.This product price is cheap, and volatilization can be used as gas after the vaporization easily, is a kind of alternative materials for preparing carbon nanotube preferably.It is worth noting that especially sherwood oil helps depositing as a kind of liquid starting material, be fit to the preparation of varying environment, scale, also help adding the fluid organic material that contains other element (such as, nitrogenous or element silicon) carbon nanotube is mixed.
The present invention at first adopts the method for electron beam evaporation plating to prepare the iron catalytic film on silicon base, adopts chemical Vapor deposition process to prepare carbon nanotube then.
A kind of sherwood oil that adopts is the method for feedstock production carbon nanotube, it is characterized in that this method realizes successively through the following steps:
A adopts the method for electron beam evaporation plating to prepare the iron catalytic film on silicon base:
The vacuum chamber that to put into electron beam coater through the silicon chip and the iron target of acetone ultrasonic cleaning vacuumizes, when air pressure 10
-4Unlocking electronic bundle power supply during Pa, the iron film of evaporation 20-40nm;
B adopts chemical Vapor deposition process to prepare carbon nanotube on the silicon chip that step (1) obtains:
The silicon chip that plated the iron film is put into the cavity of tubular type chemical vapor depsotition equipment, vacuumize, when air pressure reaches 10
-2During Pa, feed argon gas and cavity temperature is elevated to 600-1000 ℃ and keep stable; Then sherwood oil is added with the speed of 10-100 μ l/min in 60 ℃ the vapourizing unit, the vaporization back feeds in the chamber with argon gas, stops behind the reaction 5-10min, and cool to room temperature obtains carbon nanotube under the protection of argon gas.
The boiling point of the sherwood oil that the present invention adopts is 30-60 ℃.
The present invention with iron as catalyzer, thereby it only need be heated to 600-1000 ℃ and just the sherwood oil catalyzed graphitization can be formed carbon nanotube, does not need assisting of other condition, such as magnetic field elements such as (as catalyzer time) nickel.
The present invention is a raw material with the petroleum products sherwood oil of cheapness, has prepared carbon nanotube by chemical vapour deposition technique.We have used liquid starting material, can reduce the use of mass-flow gas meter, directly control what of the required raw material of reaction by the add-on of liquid.Though liquid petroleum ether needs vaporization (60 ℃) as raw material, this raw material relatively and organism such as benzene, toluene as the vaporization temperature low (＞120 ℃) of raw material needs, and less to the toxicity of human body.This liquid starting material required temperature of reaction with respect to other gas, liquid starting material does not almost have any difference.It should be noted that especially sherwood oil is a kind of organic solvent, can be used for dissolved organic matter, therefore this liquid starting material is convenient to mixing of carbon nanotube with respect to gas, thus obtain containing other element (such as: contain C
13, element such as nitrogen, silicon) carbon nanotube, perhaps the heterogeneous of various heterogeneities connects.In addition, this method cost is lower, and technology is simple, and the carbon nanotube oriented growth that obtains also can be widely used in electron device, field emission device, storage hydrogen and the high-strength conductive matrix material.
Description of drawings
The electron scanning micrograph of the oriented growth carbon nanotube that Fig. 1 the present invention is prepared.
The transmission electron microscope photo of the carbon nanotube of the uniform diameter that Fig. 2 the present invention is prepared.
Embodiment
For a better understanding of the present invention, describe by following examples.
Embodiment 1:
Vacuum chamber with the silicon chip and the iron target of acetone ultrasonic cleaning are put into electron beam coater vacuumizes, when air pressure 10
-4Unlocking electronic bundle power supply during Pa, the iron film of evaporation 20-40nm.
The silicon chip that plated the iron film is put into the cavity of tubular type chemical vapor depsotition equipment, vacuumize, when air pressure reaches 10
-2During Pa, feed argon gas and cavity temperature is elevated to 800 ℃ and keep stable; Then sherwood oil (boiling point: 30-60 ℃) is added with the speed of 30 μ l/min in 60 ℃ the vapourizing unit, the vaporization back feeds in the chamber with argon gas, stops behind the reaction 5-10min, and cool to room temperature obtains carbon nanotube under the protection of argon gas.
Scanning electronic microscope result shown in Figure 1 shows, though carbon nanotube has taken place to curl and twine in growth, is epitaxial on the whole.If do not consider to curl, its speed of growth is greatly about 5.4 μ m/min.
Shown in Figure 2, the result of transmission electron microscope shows carbon nanotube caliber homogeneous, is about 10-30nm.
Claims (2)
- One kind to adopt sherwood oil be the method for feedstock production carbon nanotube, it is characterized in that this method realizes successively through the following steps:A adopts the method for electron beam evaporation plating to prepare the iron catalytic film on silicon base:Vacuum chamber with the silicon chip and the iron target of acetone ultrasonic cleaning are put into electron beam coater vacuumizes, when air pressure 10 -4Unlocking electronic bundle power supply during Pa, the iron film of evaporation 20-40nm;B adopts chemical Vapor deposition process to prepare carbon nanotube on the silicon chip that step (1) obtains:The silicon chip that plated the iron film is put into the cavity of tubular type chemical vapor depsotition equipment, vacuumize, when air pressure reaches 10 -2During Pa, feed argon gas and cavity temperature is elevated to 600-1000 ℃ and keep stable; Then sherwood oil is added with the speed of 10-100 μ l/min in 60 ℃ the vapourizing unit, the vaporization back feeds in the chamber with argon gas, stops behind the reaction 5-10min, and cool to room temperature obtains carbon nanotube under the protection of argon gas.
- 2. the method for claim 1, the boiling point that it is characterized in that sherwood oil is 30-60 ℃.
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| CN2010101767949A CN102249211A (en) | 2010-05-18 | 2010-05-18 | Method for preparing carbon nanotube by using petroleum ether as raw material |
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| CN2010101767949A CN102249211A (en) | 2010-05-18 | 2010-05-18 | Method for preparing carbon nanotube by using petroleum ether as raw material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077773A (en) * | 2007-06-15 | 2007-11-28 | 清华大学 | Method for preparing carbon nano-tube array on the basis of chemical vapour deposition |
| CN101365650A (en) * | 2006-01-06 | 2009-02-11 | 独立行政法人产业技术综合研究所 | Bulk assembly of oriented carbon nanotube, method of manufacturing the same and application thereof |
| CN101365651A (en) * | 2006-01-06 | 2009-02-11 | 独立行政法人产业技术综合研究所 | Oriented carbon nanotube/bulk structure having different density portion, its manufacturing method and usage |
| CN101469408A (en) * | 2007-12-25 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for depositing diamond-like carbon film on stainless steel substrate |
-
2010
- 2010-05-18 CN CN2010101767949A patent/CN102249211A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101365650A (en) * | 2006-01-06 | 2009-02-11 | 独立行政法人产业技术综合研究所 | Bulk assembly of oriented carbon nanotube, method of manufacturing the same and application thereof |
| CN101365651A (en) * | 2006-01-06 | 2009-02-11 | 独立行政法人产业技术综合研究所 | Oriented carbon nanotube/bulk structure having different density portion, its manufacturing method and usage |
| CN101077773A (en) * | 2007-06-15 | 2007-11-28 | 清华大学 | Method for preparing carbon nano-tube array on the basis of chemical vapour deposition |
| CN101469408A (en) * | 2007-12-25 | 2009-07-01 | 中国科学院兰州化学物理研究所 | Method for depositing diamond-like carbon film on stainless steel substrate |
Non-Patent Citations (1)
| Title |
|---|
| 颜朝国: "《有机化学》", 31 January 2007, article "第八节 重要的烷烃", pages: 33 * |
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Application publication date: 20111123 |