CN110668426A - Method for preparing aluminum-doped carbon nanotube - Google Patents
Method for preparing aluminum-doped carbon nanotube Download PDFInfo
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- CN110668426A CN110668426A CN201911140780.9A CN201911140780A CN110668426A CN 110668426 A CN110668426 A CN 110668426A CN 201911140780 A CN201911140780 A CN 201911140780A CN 110668426 A CN110668426 A CN 110668426A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
Abstract
The invention discloses a method for preparing an aluminum-doped carbon nanotube, which comprises the following steps: placing a catalyst and an aluminum foil substrate in a heating temperature area of a tubular furnace; sealing the heating temperature area of the tubular furnace, introducing a first mixed gas into the sealed area, and heating the heating temperature area of the tubular furnace to a specified temperature value to perform a reduction reaction; after the reduction reaction is finished, introducing a second mixed gas into the closed area, and growing the carbon nano tube at the specified temperature value; the grown carbon nanotubes were peeled off from the aluminum foil substrate to complete the preparation. According to the method, aluminum metal doping modification treatment is introduced in the preparation process of the carbon nano tube, so that the gas-sensitive property of the carbon nano tube material is improved to a great extent.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a method for preparing an aluminum-doped carbon nanotube.
Background
The unique one-dimensional microscopic morphology of the carbon nano tube nano material enables the carbon nano tube nano material to have rich pore structures, large specific surface area and high surface activity, so that gas components can generate gas-sensitive response characteristics with the surface of the carbon nano tube material through forms of physical or chemical adsorption and the like, and the carbon nano tube nano material becomes an excellent material for detecting the gas components.
Research shows that the intrinsic carbon nanotube gas-sensitive material has good gas-sensitive response characteristic only for part of specific gases due to the limitation of physical and chemical properties; in addition, the gas-sensitive detection sensitivity is low, the gas-sensitive response speed is slow, and the selectivity is poor. Particularly in the field of electrical engineering, partial discharge caused by internal defects of high-voltage insulating equipment decomposes insulating gas SF6 filled in the equipment into a series of characteristic components including SO2F2, SOF2, HF, SOF4 and the like under the condition of micro-water and micro-oxygen, and the sensing capability of intrinsic carbon nanotubes on the gases is very weak, SO that effective high-sensitivity detection cannot be realized.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the present invention provides a method for preparing aluminum-doped carbon nanotubes, which introduces aluminum metal doping modification treatment to improve the gas-sensitive characteristics of carbon nanotube materials.
One of the objects of the present invention is achieved by a method for preparing aluminum-doped carbon nanotubes, comprising the steps of:
placing a catalyst and an aluminum foil substrate in a heating temperature area of a tubular furnace;
sealing the heating temperature area of the tubular furnace, introducing a first mixed gas into the sealed area, and heating the heating temperature area of the tubular furnace to a specified temperature value to perform a reduction reaction;
after the reduction reaction is finished, introducing a second mixed gas into the closed area, and growing the carbon nano tube at the specified temperature value;
the grown carbon nanotubes were peeled off from the aluminum foil substrate to complete the preparation.
Optionally, the catalyst is ferrocene.
Optionally, placing the catalyst and the aluminum foil substrate in a heating temperature zone of a tube furnace, comprising:
ferrocene was placed on top of an aluminum foil substrate and placed in the tube furnace heating temperature zone.
Optionally, before introducing the first mixed gas into the closed area, the method further includes: and introducing protective gas into the closed area until the closed area is filled with the protective gas.
Optionally, the protective gas is argon, and the first mixed gas is a mixed gas of argon and hydrogen;
the step of introducing a first mixed gas into the closed area comprises the following steps:
argon and hydrogen are mixed at different rates and then are introduced into the closed area.
Optionally, the second mixed gas is a mixed gas of acetylene and hydrogen;
and introducing a second mixed gas into the closed area, wherein the second mixed gas comprises:
acetylene and hydrogen are mixed at different rates and then are introduced into the closed area.
Optionally, after the growing of the carbon nanotubes is performed at the specified temperature value, the method further includes:
in the cooling process, introducing the protective gas into the closed area;
stopping introducing the second mixed gas after introducing the protective gas so as to carry out cooling treatment;
and stopping introducing the protective gas after the temperature reduction treatment is finished.
Optionally, before the grown carbon nanotubes are peeled off from the aluminum foil substrate to complete the preparation, the method further includes:
treating tail gas generated in the preparation process.
Due to the adoption of the technical scheme, the invention has the following advantages: according to the method, aluminum metal doping modification treatment is introduced in the preparation process of the carbon nano tube, so that the gas-sensitive property of the carbon nano tube material is improved to a great extent.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
The drawings of the invention are illustrated as follows:
FIG. 1 is a flow chart of an embodiment of the present invention.
Detailed Description
The invention is further illustrated by the following figures and examples.
Examples
The embodiment of the invention provides a method for preparing an aluminum-doped carbon nanotube, which comprises the following steps:
placing a catalyst and an aluminum foil substrate in a heating temperature area of a tubular furnace;
sealing the heating temperature area of the tubular furnace, introducing a first mixed gas into the sealed area, and heating the heating temperature area of the tubular furnace to a specified temperature value to perform a reduction reaction;
after the reduction reaction is finished, introducing a second mixed gas into the closed area, and growing the carbon nano tube at the specified temperature value;
the grown carbon nanotubes were peeled off from the aluminum foil substrate to complete the preparation.
According to the method, aluminum metal doping modification treatment is introduced in the preparation process of the carbon nano tube, so that the gas-sensitive property of the carbon nano tube material is improved to a great extent.
Optionally, the catalyst is ferrocene.
Optionally, placing the catalyst and the aluminum foil substrate in a heating temperature zone of a tube furnace, comprising:
ferrocene was placed on top of an aluminum foil substrate and placed in the tube furnace heating temperature zone.
Specifically, in this embodiment, ferrocene is selected as the catalyst, and the ferrocene is placed in front of the aluminum foil by utilizing the biochemical characteristics of ferrocene, so that the sublimated ferrocene can uniformly fall on the aluminum foil under the action of the air flow.
Optionally, before introducing the first mixed gas into the closed area, the method further includes: and introducing protective gas into the closed area until the closed area is filled with the protective gas.
Optionally, the protective gas is argon, and the first mixed gas is a mixed gas of argon and hydrogen;
the step of introducing a first mixed gas into the closed area comprises the following steps:
argon and hydrogen are mixed at different rates and then are introduced into the closed area.
Specifically, in this embodiment, during the actual operation, a gas mixing system may be used, for example, in an embodiment of the present invention, the shielding gas is introduced into the sealed area until the sealing area is filled with the shielding gas, argon (Ar) may be introduced into the tube furnace at a uniform flow rate of 400sccm (standard per cubic centimeter per minute) by using the gas mixing system, and the time is kept for 10 minutes until the interior of the tube furnace is completely filled with argon (Ar) as the shielding gas.
Further, the first mixed gas may be introduced into the sealed region by mixing Ar (400sccm) + H2(100sccm) in a gas mixing system and then introducing the gas into the tube furnace.
The heating temperature zone of the tube furnace is heated to a specified temperature value to perform a reduction reaction, in this embodiment, the heating temperature zone of the tube furnace is heated to 640 ℃, and the temperature is maintained for 1 hour, so that the precursor is reduced to elemental iron by H2 to perform a catalytic action.
Optionally, the second mixed gas is a mixed gas of acetylene and hydrogen;
and introducing a second mixed gas into the closed area, wherein the second mixed gas comprises:
acetylene and hydrogen are mixed at different rates and then are introduced into the closed area.
After obtaining the elemental iron, in the present embodiment, based on the foregoing example, the type of gas introduced into the tube furnace is further adjusted, acetylene (90sccm) + H2(150sccm) is introduced into the tube furnace, and the growth of the carbon nanotube is performed at the specified temperature value.
The growth of the carbon nanotubes is carried out at a specified temperature, and the growth of the carbon nanotubes can be completed by reacting at 640 ℃ for 1 hour.
Optionally, after the growing of the carbon nanotubes is performed at the specified temperature value, the method further includes:
in the cooling process, introducing the protective gas into the closed area;
stopping introducing the second mixed gas after introducing the protective gas so as to carry out cooling treatment;
and stopping introducing the protective gas after the temperature reduction treatment is finished.
Optionally, before the grown carbon nanotubes are peeled off from the aluminum foil substrate to complete the preparation, the method further includes:
treating tail gas generated in the preparation process.
Specifically, after the growth of the carbon nanotubes is performed, the temperature of the tube furnace needs to be reduced, and in the temperature reduction process, the carrier gas Ar (400sccm) needs to be introduced again to prevent the liquid-sealed water from flowing back to the tube furnace in the temperature reduction process. Then, acetylene and hydrogen were stopped. And then cooling to normal temperature, stopping introducing Ar, opening the flange of the tube furnace, and taking out the carbon nano tube deposited on the substrate. Treating tail gas generated in the process of preparing the carbon nano tube; and stripping the grown carbon nanotubes from the aluminum foil to form modified carbon nanotube powder.
In conclusion, the method of the invention adopts various physical and chemical modes to modify the microstructure of the carbon nanotube sensor, and prepares the carbon nanotube sensor with various specific functions to qualitatively or quantitatively analyze gas components. Through Al metal doping modification treatment, the gas-sensitive property of the carbon nanotube material is improved to a great extent.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as a method, system, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-usable storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and the like) having computer-usable program code embodied therein.
The present application is described with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the application. It will be understood that each flow and/or block of the flow diagrams and/or block diagrams, and combinations of flows and/or blocks in the flow diagrams and/or block diagrams, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, embedded processor, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be stored in a computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner, such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function specified in the flowchart flow or flows and/or block diagram block or blocks.
These computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered thereby.
Claims (8)
1. A method of preparing aluminum-doped carbon nanotubes, comprising the steps of:
placing a catalyst and an aluminum foil substrate in a heating temperature area of a tubular furnace;
sealing the heating temperature area of the tubular furnace, introducing a first mixed gas into the sealed area, and heating the heating temperature area of the tubular furnace to a specified temperature value to perform a reduction reaction;
after the reduction reaction is finished, introducing a second mixed gas into the closed area, and growing the carbon nano tube at the specified temperature value;
the grown carbon nanotubes were peeled off from the aluminum foil substrate to complete the preparation.
2. The method of claim 1, wherein the catalyst is ferrocene.
3. The method of claim 2, wherein placing the catalyst and aluminum foil substrate into a tube furnace heating temperature zone comprises:
ferrocene was placed on top of an aluminum foil substrate and placed in the tube furnace heating temperature zone.
4. The method of claim 1, wherein prior to introducing the first mixed gas into the enclosed area, the method further comprises: and introducing protective gas into the closed area until the closed area is filled with the protective gas.
5. The method of claim 4, wherein the shielding gas is argon and the first mixed gas is a mixed gas of argon and hydrogen;
the step of introducing a first mixed gas into the closed area comprises the following steps:
argon and hydrogen are mixed at different rates and then are introduced into the closed area.
6. The method according to claim 5, wherein the second mixed gas is a mixed gas of acetylene and hydrogen;
and introducing a second mixed gas into the closed area, wherein the second mixed gas comprises:
acetylene and hydrogen are mixed at different rates and then are introduced into the closed area.
7. The method of claim 6, wherein after the growing of the carbon nanotubes is performed at the specified temperature value, the method further comprises:
in the cooling process, introducing the protective gas into the closed area;
stopping introducing the second mixed gas after introducing the protective gas so as to carry out cooling treatment;
and stopping introducing the protective gas after the temperature reduction treatment is finished.
8. The method of claim 1, wherein prior to peeling the grown carbon nanotubes from the aluminum foil substrate to complete the fabrication, the method further comprises:
treating tail gas generated in the preparation process.
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| CN201911140780.9A CN110668426A (en) | 2019-11-20 | 2019-11-20 | Method for preparing aluminum-doped carbon nanotube |
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| CN201911140780.9A CN110668426A (en) | 2019-11-20 | 2019-11-20 | Method for preparing aluminum-doped carbon nanotube |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6811957B1 (en) * | 1999-05-28 | 2004-11-02 | Commonwealth Scientific And Industrial Research Organisation | Patterned carbon nanotube films |
| CN1840471A (en) * | 2005-03-31 | 2006-10-04 | 清华大学 | Carbon nanotube array growing method |
| CN104124122A (en) * | 2014-07-31 | 2014-10-29 | 国家纳米科学中心 | Method for improving carbon nanotube field emitting performance through diamond-like carbon film |
| CN109136986A (en) * | 2018-10-29 | 2019-01-04 | 河南工程学院 | A kind of preparation method of nano nickel/array carbon nano tube composite material |
-
2019
- 2019-11-20 CN CN201911140780.9A patent/CN110668426A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6811957B1 (en) * | 1999-05-28 | 2004-11-02 | Commonwealth Scientific And Industrial Research Organisation | Patterned carbon nanotube films |
| CN1840471A (en) * | 2005-03-31 | 2006-10-04 | 清华大学 | Carbon nanotube array growing method |
| CN104124122A (en) * | 2014-07-31 | 2014-10-29 | 国家纳米科学中心 | Method for improving carbon nanotube field emitting performance through diamond-like carbon film |
| CN109136986A (en) * | 2018-10-29 | 2019-01-04 | 河南工程学院 | A kind of preparation method of nano nickel/array carbon nano tube composite material |
Non-Patent Citations (1)
| Title |
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| 周静等，: "《近代材料科学研究技术进展》", 31 December 2012 * |
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