CN100467370C - Carbon nanotube preparing apparatus and process - Google Patents
Carbon nanotube preparing apparatus and process Download PDFInfo
- Publication number
- CN100467370C CN100467370C CNB2005100372838A CN200510037283A CN100467370C CN 100467370 C CN100467370 C CN 100467370C CN B2005100372838 A CNB2005100372838 A CN B2005100372838A CN 200510037283 A CN200510037283 A CN 200510037283A CN 100467370 C CN100467370 C CN 100467370C
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- substrate
- reaction chamber
- inlet mouth
- catalyst layer
- carbon nanotube
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/133—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
Abstract
The carbon nanotube preparing apparatus includes one reaction cavity with gas inlet in the bottom and one gas exhaust port in the top and opposite to the gas inlet; one base bearer located inside the reaction cavity and between the gas inlet and the gas exhaust port; and at least one base on the base bearer and with flow guiding holes and one catalyst on its surface. The present invention also provides process of preparing carbon nanotube with the said apparatus.
Description
[technical field]
The invention relates to a kind of device and method of made of carbon nanotubes, especially carry out the device and method of made of carbon nanotubes about chemical Vapor deposition process.
[background technology]
Because of carbon nanotube has excellent performance at aspects such as machinery, electronics, physics, chemistry, as the metal of uniqueness or semi-conductor electroconductibility, high physical strength, high capacity hydrogen storage ability and adsorptive power, electronic emission performance, directed heat conductivility and stronger wideband electromagnetic wave-absorbing property etc., make carbon nanotube be subjected to the very big attention of fields such as physics, chemistry and Materials science and new high-tech industry department, promote the broad research and the practical application of carbon nanotube simultaneously.At present, carbon nanotube is widely used in fields such as strongthener, field electron emission materials, electrode material for super capacitor, gas adsorption material, catalytic material, heat conducting material and sensing material.
At present, comparatively sophisticated preparation method of carbon nano-tube mainly contains three kinds: arc discharge method, laser ablation method and chemical Vapor deposition process.Characteristics such as wherein, chemical Vapor deposition process is easy with its technology, cost is low, can grow in batches and obtain extensive studies and application.
Chemical Vapor deposition process generally is to adopt transition metal or its oxide compound as the catalyzer of carbon nano tube growth, at a certain temperature, makes carbon source gas grow the method for carbon nanotube in catalyst surface generation thermo-cracking.Prior art provides a kind of preparation method of carbon nanotube, it may further comprise the steps: provide a surface to be formed with the substrate of a catalyst layer, it is inserted in the Reaktionsofen, heating reaction furnace, in Reaktionsofen, feed carbon source gas along being basically perpendicular to the carbon nano tube growth direction, carry out carbon nano tube growth, under the katalysis of catalyzer, will upwards grow carbon nanotube in the catalyst layer position.But,,, make that the carbon nanotube collimation that grows is not good because carbon source entraining air stream direction will influence the vertical growth of carbon nanotube to prepare in the process of carbon nanotube in this method.
In view of this, be necessary to provide a kind of carbon nanotube preparing apparatus and method, it can prepare the collimation carbon nanotube.
[summary of the invention]
To a kind of carbon nanotube preparing apparatus and method be described with specific embodiment below, it can prepare the collimation carbon nanotube.
A kind of carbon nanotube preparing apparatus, it comprises:
One reaction chamber;
One is located at the inlet mouth of this reaction chamber bottom;
One is located at the venting port at this reaction chamber top, and this venting port and inlet mouth are oppositely arranged;
One substrate-loading device, it is positioned at reaction chamber, and between described inlet mouth and venting port; And
At least one substrate, it is loaded on the described substrate-loading device, and this substrate comprises a plurality of pod apertures, and is formed at the catalyst layer on the surface thereof, and this catalyst layer is positioned at inlet mouth one side.
And, a kind of preparation method of carbon nano-tube, it comprises step:
One reaction chamber is provided, and it comprises the inlet mouth of being located at this reaction chamber bottom, and one is located at the venting port at this reaction chamber top, and a substrate-loading device of being located at reaction chamber inside;
One substrate is provided, and this substrate comprises a plurality of pod apertures, and is formed on the catalyst layer on the surface thereof, this substrate is loaded on this substrate-loading device, and makes this catalyst layer be positioned at inlet mouth one side;
In this reaction chamber, feed a carbon source gas by inlet mouth, carry out the chemical vapor deposition growth carbon nanotube.
With respect to prior art, carbon nanotube preparing apparatus that the embodiment of the invention provides and method, be located at inlet mouth one side by the catalyst layer that will be loaded into the substrate surface in the reaction chamber, its collocation and carbon nano tube growth direction parallel gas flow direction can realize the preparation of high collimation carbon nanotube down via action of gravity; And can be in reaction chamber with a plurality of substrates with pod apertures of the overlapping loading of predetermined spacing increasing the carbon nano tube growth area, and then can realize the production in enormous quantities of collimation carbon nanotube.
[description of drawings]
Fig. 1 is the carbon nanotube preparing apparatus synoptic diagram that first embodiment of the invention provides.
Fig. 2 is a first embodiment of the invention underlying structure synoptic diagram.
Fig. 3 is the carbon nanotube preparing apparatus synoptic diagram that second embodiment of the invention provides.
Fig. 4 is a second embodiment of the invention underlying structure synoptic diagram.
[embodiment]
Below in conjunction with accompanying drawing the embodiment of the invention is described in further detail.
Referring to Fig. 1, the carbon nanotube preparing apparatus 60 that first embodiment of the invention provides, it comprises: a reaction chamber 61, one heating units 65 and a substrate 10.
Described reaction chamber 61, it also comprises an inlet mouth 62, a venting port 63 and a substrate-loading device 64; Described inlet mouth 62, it is located at reaction chamber 61 bottoms, is used for feeding in reaction chamber 61 a carbon source gas; Described venting port 63, it is located at reaction chamber 61 tops and is oppositely arranged with inlet mouth 62, and it matches with inlet mouth 62, can make carbon source entraining air stream direction parallel with the carbon nano tube growth direction; Described substrate-loading device 64, it is located in the reaction chamber 61, and between inlet mouth 62 and venting port 63.
Described heating unit 65 is arranged at around the reaction chamber 61, is used for reaction chamber 61 heating.
Described substrate 10, it is loaded on the described substrate-loading device 64.Referring to Fig. 2, this substrate 10 comprises a plurality of pod apertures 30, and is formed at the catalyst layer 40 on the surface thereof; Described pod apertures 30 is a through hole, and it can allow the circulation of carbon source gas, and can distribute by any regular, and preferred, pod apertures 30 rules are arranged in the substrate 10.Described catalyst layer 40 can be used as the carbon nano tube growth catalyst.
A kind of method of utilizing this carbon nanotube preparing apparatus 60 to carry out made of carbon nanotubes is provided below, and it comprises step:
(1) substrate 10 that provides a surface to be formed with a catalyst layer 40, this substrate 10 has a plurality of pod apertures 30.Described substrate 10 can be made by following steps (a)～(d):
Step (a): provide a matrix 10 ', matrix 10 ' on form a plurality of pod apertures 30.Described matrix 10 ' material can adopt silicon, quartz or glass, present embodiment adopts silicon.Described pod apertures 30 can form with the method for mechanical workout (as drilling machine boring etc.); Present embodiment adopt drilling machine matrix 10 ' on a plurality of pod apertures 30 of distributing of formation rule.
Step (b): form and pod apertures 30 corresponding mask on described matrix 10 ' surface.Present embodiment adopts the photoresistance processing procedure, and its concrete steps can be: at matrix 10 ' surface applied one photoresist layer; Have with the arrange light shield of corresponding pattern of pod apertures 30 one and to place on the photoresist layer, in UV-light, expose certain hour to the open air; With basic solutions such as potassium hydroxide is photographic developer, adopts the photoresist of wet etching removal through overexposure, can form the mask that cover pod apertures 30 on matrix 10 ' surface.Wherein, photoresist can adopt polymethylmethacrylate, polyvinyl chloride or polycarbonate etc.
Step (c): form a catalyst layer 40 in described matrix 10 ' surperficial non-mask zone.But the material chosen from Fe of described catalyst layer 40, cobalt, nickel or its alloy.The formation method of this catalyst layer 40 can adopt ion plating method, radio frequency magnetron sputter, vacuum vapor deposition method, chemical Vapor deposition process etc.Present embodiment adopts the radio frequency magnetron sputtering method, forms an iron catalyst layer in matrix 10 ' surperficial non-mask zone.
Step (d): the mask of removing described matrix 10 ' surface.Present embodiment with an organic solvent (as acetone etc.) is removed mask, and then can obtain to have a plurality of pod apertures 30, and the surface is formed with the substrate 10 of catalyst layer 40.
(2) substrate 10 is loaded on the substrate-loading device 64 in this reaction chamber 61.The catalyst layer 40 of described substrate 10 is positioned at inlet mouth 62 1 sides, so can make the direction of growth of follow-up carbon nanotube consistent with gravity direction.
(3) in reaction chamber 61, feed carbon source gas from bottom to top by inlet mouth 62, carry out the chemical vapor deposition growth carbon nanotube.Concrete steps can be: by 40 to 500～900 ℃ on heating unit 65 (as High Temperature Furnaces Heating Apparatus, high frequency furnace an etc.) heatable catalyst layer that is surrounded on reaction chamber 61; In reaction chamber 61, feed the mixed gas of carbon source gas (as methane, acetylene, ethene, carbon monoxide or its mixed gas) and shielding gas (as rare gas elementes such as helium, argon gas, hydrogen or ammonia) again by inlet mouth 62; Carbon source gas grows carbon nanotube in catalyst layer 40 position cracking.Because inlet mouth 62 is oppositely arranged with venting port 63, the air flow line that makes feeding reaction chamber 61 interior mixed gass form is parallel with the carbon nano tube growth direction, helps the growth of carbon nanotube collimation.
Referring to Fig. 3, second embodiment of the invention provides another kind of carbon nanotube preparing apparatus, basic identical with first embodiment, its difference is: described substrate-loading device 64 can be used for carrying a plurality of substrates 10, it further comprises a plurality of pads 50 and a pair of bolt pipe 641, described pad 50 is used for a plurality of substrates 10 at interval, and described bolt pipe 641 is used to locate carbon nano tube growth substrate 10.Described substrate 10 also comprises a pair of pilot hole 20 (as shown in Figure 4) that matches with bolt pipe 641, and during use, pilot hole 20 can be arranged on the bolt pipe 641 so that substrate 10 is fixing.
Accordingly, the preparation method of carbon nano-tube of second embodiment of the invention, it comprises step:
(1) substrate 10 that provides a plurality of surface thereof to be formed with a catalyst layer 40, this substrate 10 has a pair of pilot hole 20 and a plurality of pod apertures 30.Described substrate 10 can be made according to the step (a)～(d) of first embodiment.Different is, present embodiment adopt matrix 10 ' on form pilot hole 20 and pod apertures 30, and to its mask, form catalyst layer 40.
(2) a plurality of substrates 10 are loaded on the substrate-loading device 64 in this reaction chamber 61.These a plurality of substrates 10 are serially connected with on the bolt pipe 641 of substrate-loading device by its pilot hole 20, and have predetermined spacing between each substrate 10.The catalyst layer 40 of described a plurality of substrate 10 is positioned at inlet mouth 62 1 sides, and it can make the direction of growth of follow-up carbon nanotube consistent with gravity direction.In the present embodiment, described predetermined spacing can be determined by last required carbon nano tube growth height, generally being good greater than the carbon nano tube growth height; It can be realized by the pad 50 that is serially connected with on the bolt pipe 641 with substrate 10 spaces.
(3) in reaction chamber 61, feed carbon source gas from bottom to top by inlet mouth 62, carry out the chemical vapor deposition growth carbon nanotube.
Carbon nanotube preparing apparatus that the embodiment of the invention provides and method, be located at inlet mouth one side by the catalyst layer that will be loaded into the substrate surface in the reaction chamber, its collocation and carbon nano tube growth direction parallel gas flow direction can realize the preparation of high collimation carbon nanotube down via action of gravity; And can be in reaction chamber with a plurality of substrates with pod apertures of the overlapping loading of predetermined spacing increasing the carbon nano tube growth area, and then can realize the production in enormous quantities of collimation carbon nanotube.
In addition, those skilled in the art also can do other and change in spirit of the present invention, and as the structure of suitable change substrate-loading device, or the quantity of substrate, or pilot hole and bolt pipe quantity, or pod apertures arranges etc., as long as it does not depart from technique effect of the present invention and all can.The variation that these are done according to spirit of the present invention all should be included within the present invention's scope required for protection.
Claims (11)
1. carbon nanotube preparing apparatus, it comprises
One reaction chamber;
One is located at the inlet mouth of this reaction chamber bottom;
One is located at the venting port at this reaction chamber top, and this venting port and inlet mouth are oppositely arranged;
One substrate-loading device, it is positioned at reaction chamber, and between described inlet mouth and venting port; And at least one substrate, it is loaded on the described substrate-loading device, and this substrate comprises a plurality of pod apertures, and is formed at the catalyst layer on the surface thereof, and this catalyst layer is positioned at inlet mouth one side.
2. carbon nanotube preparing apparatus according to claim 1 is characterized in that the material of described substrate is selected from silicon, quartz or glass.
3. carbon nanotube preparing apparatus according to claim 1 is characterized in that described substrate-loading device comprises a pair of bolt pipe, and described substrate comprises a pair of pilot hole that matches with this bolt pipe, is used to locate this substrate.
4. preparation method of carbon nano-tube, it may further comprise the steps:
One reaction chamber is provided, and it comprises the inlet mouth of being located at this reaction chamber bottom, and a substrate-loading device of being located at reaction chamber inside;
One substrate is provided, and this substrate comprises a plurality of pod apertures, and is formed on the catalyst layer on the surface thereof, this substrate is loaded on this substrate-loading device, and makes this catalyst layer be positioned at inlet mouth one side;
In this reaction chamber, feed a carbon source gas by inlet mouth, carry out the chemical vapor deposition growth carbon nanotube.
5. as preparation method of carbon nano-tube as described in the claim 4, it is characterized in that described carbon source gas is selected from methane, acetylene, ethene, carbon monoxide or its mixing.
6. as preparation method of carbon nano-tube as described in the claim 4, it is characterized in that the making method of described substrate may further comprise the steps:
One matrix is provided;
On matrix, form a plurality of pod apertures;
Form and a plurality of pod apertures corresponding mask on matrix one surface;
Form a catalyst layer in this matrix surface non-mask zone;
Remove the mask of matrix surface, to expose a plurality of pod apertures.
7. as preparation method of carbon nano-tube as described in the claim 6, it is characterized in that described a plurality of pod apertures is to form by mechanical workout.
8. as preparation method of carbon nano-tube as described in the claim 6, it is characterized in that described catalyst layer is to form by ion plating method, radio frequency magnetron sputtering method, vacuum vapor deposition method or chemical Vapor deposition process.
9. as preparation method of carbon nano-tube as described in the claim 6, it is characterized in that described catalyst layer material chosen from Fe, cobalt, nickel or its alloy.
10. preparation method of carbon nano-tube, it may further comprise the steps:
One reaction chamber is provided, and it comprises the inlet mouth of being located at this reaction chamber bottom, and a substrate-loading device of being located at reaction chamber inside, and this substrate-loading device comprises a pair of bolt pipe;
A plurality of substrates are provided, described each substrate comprises the pilot hole that a pair of and described bolt pipe matches, a plurality of pod apertures, and be formed on a catalyst layer on the surface thereof, pilot hole by substrate is loaded in this substrate serial connection on the bolt pipe of this substrate-loading device with predetermined spacing, and makes this catalyst layer be positioned at inlet mouth one side;
In this reaction chamber, feed a carbon source gas by inlet mouth, carry out the chemical vapor deposition growth carbon nanotube.
11., it is characterized in that described predetermined spacing is to form by the pad that is serially connected with on the bolt pipe with the substrate space as preparation method of carbon nano-tube as described in the claim 10.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100372838A CN100467370C (en) | 2005-09-12 | 2005-09-12 | Carbon nanotube preparing apparatus and process |
| US11/473,981 US20070116634A1 (en) | 2005-09-12 | 2006-06-23 | Apparatus and method for manufacturing carbon nanotubes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100372838A CN100467370C (en) | 2005-09-12 | 2005-09-12 | Carbon nanotube preparing apparatus and process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1931714A CN1931714A (en) | 2007-03-21 |
| CN100467370C true CN100467370C (en) | 2009-03-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100372838A Expired - Fee Related CN100467370C (en) | 2005-09-12 | 2005-09-12 | Carbon nanotube preparing apparatus and process |
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| Country | Link |
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| US (1) | US20070116634A1 (en) |
| CN (1) | CN100467370C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100851391B1 (en) | 2007-04-27 | 2008-08-08 | 세메스 주식회사 | Carbon nano-tube synthesizing apparatus and method |
| KR100955488B1 (en) * | 2007-10-04 | 2010-04-30 | 세메스 주식회사 | Equipment for producting carbon nano tube and synthesizing substrate used therein |
| CN103896244B (en) | 2012-12-29 | 2016-08-10 | 清华大学 | Reactor and the method for growth CNT |
| CN103896245B (en) | 2012-12-29 | 2016-01-20 | 清华大学 | The method of reactor and carbon nano-tube |
| CN103569998B (en) * | 2013-11-26 | 2016-03-02 | 苏州捷迪纳米科技有限公司 | Carbon nanotube preparing apparatus and method |
| US9896338B1 (en) * | 2015-06-09 | 2018-02-20 | Mainstream Engineering Corporation | Segregated flow reactor and method for growth of ultra-long carbon nanotubes |
| CN106185876A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | The reaction unit of a kind of band heat treatment and the method preparing CNT |
| CN106185872A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | Method prepared by the reaction unit of a kind of band lifting substrate and CNT |
| CN106185871A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | A kind of reaction unit with grid electrode and the preparation method of CNT |
| CN106892422B (en) * | 2017-03-01 | 2018-12-28 | 太原理工大学 | A kind of adding pressure type coal carbon nanotube device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030064169A1 (en) * | 2001-09-28 | 2003-04-03 | Hong Jin Pyo | Plasma enhanced chemical vapor deposition apparatus and method of producing carbon nanotube using the same |
| JP2004323871A (en) * | 2003-04-21 | 2004-11-18 | Hitachi Zosen Corp | Apparatus for manufacturing carbon nanotube |
| JP2005112659A (en) * | 2003-10-07 | 2005-04-28 | Toyota Motor Corp | Apparatus and method for manufacturing carbon nanotube |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3595233B2 (en) * | 2000-02-16 | 2004-12-02 | 株式会社ノリタケカンパニーリミテド | Electron emission source and method of manufacturing the same |
| KR100360470B1 (en) * | 2000-03-15 | 2002-11-09 | 삼성에스디아이 주식회사 | Method for depositing a vertically aligned carbon nanotubes using thermal chemical vapor deposition |
| US6699525B2 (en) * | 2001-04-16 | 2004-03-02 | The Board Of Trustees Of Western Michigan University | Method of forming carbon nanotubes and apparatus therefor |
| US6819561B2 (en) * | 2002-02-22 | 2004-11-16 | Satcon Technology Corporation | Finned-tube heat exchangers and cold plates, self-cooling electronic component systems using same, and methods for cooling electronic components using same |
-
2005
- 2005-09-12 CN CNB2005100372838A patent/CN100467370C/en not_active Expired - Fee Related
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2006
- 2006-06-23 US US11/473,981 patent/US20070116634A1/en not_active Abandoned
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030064169A1 (en) * | 2001-09-28 | 2003-04-03 | Hong Jin Pyo | Plasma enhanced chemical vapor deposition apparatus and method of producing carbon nanotube using the same |
| JP2004323871A (en) * | 2003-04-21 | 2004-11-18 | Hitachi Zosen Corp | Apparatus for manufacturing carbon nanotube |
| JP2005112659A (en) * | 2003-10-07 | 2005-04-28 | Toyota Motor Corp | Apparatus and method for manufacturing carbon nanotube |
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| Publication number | Publication date |
|---|---|
| US20070116634A1 (en) | 2007-05-24 |
| CN1931714A (en) | 2007-03-21 |
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