CN104418318B - CNT continuous growing device - Google Patents
CNT continuous growing device Download PDFInfo
- Publication number
- CN104418318B CN104418318B CN201310398409.9A CN201310398409A CN104418318B CN 104418318 B CN104418318 B CN 104418318B CN 201310398409 A CN201310398409 A CN 201310398409A CN 104418318 B CN104418318 B CN 104418318B
- Authority
- CN
- China
- Prior art keywords
- heating chamber
- substrate
- catalyst film
- cnt
- hole
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
This application discloses a kind of CNT continuous growing device, including: heating chamber, there is a heating chamber, described heating chamber offers the passage being communicated in described heating chamber；Being positioned at the substrate in described heating chamber and be formed at the catalyst film of described substrate surface, described substrate offers the first through hole, and described catalyst film includes the second through hole being communicated in described first through hole；Heater, heats described heating chamber.Owing to the porous of porous substrate connects with the porous of the catalyst film being disposed below, reacting gas is passed through by porous substrate top, can continuously flow into via the porous of substrate in the porous of catalyst film, it is ensured that CNT can grow the most continuously.More preferably, in the device after improvement, the direction of growth of CNT becomes growing vertically downward, under gravity, increases, thus reached the technique effect of continuous fast-growth when the speed of growth grows more vertically upward.
Description
Technical field
The application relates to CNT preparation field, particularly relates to a kind of CNT continuous growing device.
Background technology
At present, CNT preparation technology mainly has arc discharge method, radium-shine ablation and chemical vapour deposition technique.Wherein, chemical vapour deposition technique with its simple process, low cost, nanotube is controlled, length is big, collection rate high is widely studied and applies.The transition metal of chemical vapour deposition technique mainly utilization nanoscale or its oxide, as catalyst, are pyrolyzed the source of the gas of carbon containing at relatively low temperatures to prepare CNT.
Traditional carbon nano-tube growth apparatus, including the quartz ampoule being wrapped resistive heater, cavity it is provided with inside it, substrate is placed in cavity, the catalyst film of about 10nm it is attached with on substrate, by being passed through hydrogen and propane gas in cavity, keep, under uniform temperature effect, catalyst surface growing one layer of CNT.
In traditional carbon nano-tube growth apparatus, substrate is air-locked, when reacting gas is passed through, contact with catalyst film, can be at its superficial growth CNT, along with CNT progressive additive, catalyst film is gradually flooded completely, the catalyst film being submerged can not contact with reacting gas again, does not has the effect of catalyst, causes the CNT cannot continued growth.General when stopping growing, in this case after carbon nano tube growth to about 1-2mm so that CNT can not grow continuously, and growth efficiency is relatively low.
In view of this, it is provided that a kind of CNT that realizes grows and to improve the device of carbon nano tube growth speed the most necessary continuously.
Summary of the invention
It is an object of the invention to provide a kind of CNT continuous growing device, to improve the growth rate of CNT and to realize the continuous growth of CNT.
For achieving the above object, the present invention provides following technical scheme:
Disclosure one CNT continuous growing device, including substrate and the catalyst film that is formed at described substrate surface, wherein, described substrate offers the first through hole, and described catalyst film includes the second through hole being communicated in described first through hole.
Preferably, in above-mentioned CNT continuous growing device, the material of described substrate is silicon, pottery, iron or stainless steel；A diameter of 50 ~ 200nm of the first described through hole.
Preferably, in above-mentioned CNT continuous growing device, the material chosen from Fe of described catalyst film, the oxide of iron, cobalt, the oxide of cobalt, nickel, one or more of oxide of nickel；A diameter of 10 ~ 100nm of the second described through hole；The thickness of described catalyst film is 5 ~ 500nm.
Preferably, in above-mentioned CNT continuous growing device, described catalyst film is formed at the lower surface of described substrate along gravity direction.
Disclosed herein as well is a kind of CNT continuous growing device, including:
Heating chamber, has a heating chamber, and described heating chamber offers the passage being communicated in described heating chamber；
Being positioned at the substrate in described heating chamber and be formed at the catalyst film of described upper surface of base plate, described substrate offers the first through hole, and described catalyst film includes the second through hole being communicated in described first through hole；
Heater, heats described heating chamber.
As a further improvement on the present invention, described heating chamber is quartz ampoule, and described heater is to be wound in the resistance wire outside described quartz ampoule.
As a further improvement on the present invention, the material of described substrate is silicon, pottery, iron or stainless steel；A diameter of 50 ~ 200nm of the first described through hole.
As a further improvement on the present invention, the material chosen from Fe of described catalyst film, the oxide of iron, cobalt, the oxide of cobalt, nickel, one or more of oxide of nickel；A diameter of 10 ~ 100nm of the second described through hole；The thickness of described catalyst film is 5 ~ 500nm.
As a further improvement on the present invention, described catalyst film is formed at the lower surface of described substrate along gravity direction.
Compared with prior art, it is an advantage of the current invention that: owing to substrate and catalyst film are provided with the through hole being connected, therefore can realize the continuous growth of CNT, improve the growth efficiency of CNT.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present application or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in describing below is only some embodiments described in the application, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 show the structural representation of CNT continuous growing device in the specific embodiment of the invention；
Fig. 2 show in the specific embodiment of the invention substrate and is formed at the structural representation of catalyst film layer on substrate.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained on the premise of not making creative work, broadly fall into the scope of protection of the invention.
Shown in ginseng Fig. 1, CNT continuous growing device includes that heating chamber 10, heating chamber 10 are preferably a quartz ampoule, and it has a heating chamber 11.
The top of heating chamber 10 is further opened with being communicated in the passage 12 in heating chamber 11, and passage 12 includes carbon-source gas access apertures 121 and protective gas access apertures 122.Carbon-source gas access apertures 121 is in order to be passed through the carbon-source gas such as ethane, ethene, propane, and protective gas access apertures 122 is in order to be passed through the protective gas such as hydrogen, nitrogen, argon gas.
The outer felt of heating chamber 10 is wound with resistance wire 20, and resistance wire 20 is in order to heat heating chamber 11.
Heating is horizontally installed with substrate 30 in chamber 11, and the lower surface of substrate 30 is formed with catalyst film 40.
The material of substrate 30 is preferably silicon, pottery, iron or stainless steel, and substrate 30 is loose structure, including the first through hole 31, a diameter of 50 ~ 200nm of the first through hole 31.
Catalyst film 40 can by the method such as electron beam evaporation plating, sputtering by catalyst deposit at the lower surface of substrate 30, catalyst thickness is 5-500nm, and its material can be one or more materials of iron, cobalt, nickel and oxide thereof.Catalyst film 40 is loose structure, and including the second through hole 41, the second through hole 41 connects with the first through hole 31, say, that the hole on substrate 30 is at least partly to connect with the hole on catalyst film 40, shown in ginseng Fig. 2.
Hole on substrate 30 is preferably formed by machining, hole on catalyst film 40 can make it directly form loose structure by the condition that control deposits, it is also possible to is that first depositing catalytic agent film is processed into loose structure by machinery means the most again on catalyst film 40.
Catalyst film 40 is positioned at the lower surface of described porous substrate 30, owing to the lower surface of catalyst film 40 exposes and can contact with reacting gas, make the direction of growth of CNT along catalyst lower surface direction, and under gravity, improve the growth rate of CNT.And Automatic-falling under gravity.
Will be readily apparent, in other embodiments, catalyst film 40 can also be formed at the upper surface of substrate 30.
The porous of porous substrate 30 connects with the porous of the described catalyst film 40 being disposed below, reacting gas can continuously via substrate porous flow into catalyst film porous, ensure that reacting gas can continue through catalyst film, cause CNT to grow continuously.
A material taking mouth (not shown) can also be set in the bottom in heating chamber 11, it is also possible to apply suitable collection device (not shown), carry out growth limit, limit and collect, such as spinning etc..Further, owing to CNT 50 comes off continuously, catalyst film 40 is constantly exposed in reacting gas, therefore can realize growing continuously, improve the growth efficiency of CNT.
The method utilizing above-mentioned CNT continuous growing device growth CNT is as follows:
(1) close material taking mouth before reaction, be first passed through hydrogen and air is caught up with to the greatest extent completely；
(2) start Resistant heating to 550 ° C, continue to be passed through hydrogen constant temperature 20 minutes at such a temperature, treat that catalyst fully reduces；
(3) rise high reaction temperature and to 800 ° of C and be passed through hydrogen and propane, after the reaction time of about 10 minutes, grow CNT continuously at catalyst iron film lower surface.
In sum, owing to the porous of porous substrate connects with the porous of the catalyst film being disposed below, reacting gas is passed through by porous substrate top, can continuously flow into via the porous of substrate in the porous of catalyst film, it is ensured that CNT can grow the most continuously.More preferably, in the device after improvement, the direction of growth of CNT becomes growing vertically downward, under gravity, increases, thus reached the technique effect of continuous fast-growth when the speed of growth grows more vertically upward.
It should be noted that, in this article, the relational terms of such as first and second or the like is used merely to separate an entity or operation with another entity or operating space, and not necessarily requires or imply the relation or sequentially that there is any this reality between these entities or operation.And, term " includes ", " comprising " or its any other variant are intended to comprising of nonexcludability, so that include that the process of a series of key element, method, article or equipment not only include those key elements, but also include other key elements being not expressly set out, or also include the key element intrinsic for this process, method, article or equipment.In the case of there is no more restriction, statement " including ... " key element limited, it is not excluded that there is also other identical element in including the process of described key element, method, article or equipment.
The above is only the detailed description of the invention of the application; it should be pointed out that, for those skilled in the art, on the premise of without departing from the application principle; can also make some improvements and modifications, these improvements and modifications also should be regarded as the protection domain of the application.
Claims (5)
1. a CNT continuous growing device, it is characterised in that including:
Heating chamber, has a heating chamber, and described heating chamber offers the passage being communicated in described heating chamber；
Being positioned at the substrate in described heating chamber and be formed at the catalyst film of described substrate surface, described substrate offers the first through hole, and described catalyst film includes the second through hole being communicated in described first through hole；
Heater, heats described heating chamber.
CNT continuous growing device the most according to claim 1, it is characterised in that: described heating chamber is quartz ampoule, and described heater is to be wound in the resistance wire outside described quartz ampoule.
CNT continuous growing device the most according to claim 1, it is characterised in that: the material of described substrate is silicon, pottery, iron or stainless steel；A diameter of 50 ~ 200nm of the first described through hole.
CNT continuous growing device the most according to claim 1, it is characterised in that: the material chosen from Fe of described catalyst film, the oxide of iron, cobalt, the oxide of cobalt, nickel, one or more of oxide of nickel；A diameter of 10 ~ 100nm of the second described through hole；The thickness of described catalyst film is 5 ~ 500nm.
CNT continuous growing device the most according to claim 4, it is characterised in that: described catalyst film is formed at the lower surface of described substrate along gravity direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310398409.9A CN104418318B (en) | 2013-09-05 | 2013-09-05 | CNT continuous growing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310398409.9A CN104418318B (en) | 2013-09-05 | 2013-09-05 | CNT continuous growing device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104418318A CN104418318A (en) | 2015-03-18 |
| CN104418318B true CN104418318B (en) | 2016-09-07 |
Family
ID=52968558
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310398409.9A Active CN104418318B (en) | 2013-09-05 | 2013-09-05 | CNT continuous growing device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104418318B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106379887A (en) * | 2016-08-31 | 2017-02-08 | 无锡东恒新能源科技有限公司 | Carbon nanotube continuous generating device |
| CN106185874A (en) * | 2016-08-31 | 2016-12-07 | 无锡东恒新能源科技有限公司 | CNT continuous preparation device |
| CN108996490A (en) * | 2017-06-07 | 2018-12-14 | 清华大学 | A kind of preparation method of carbon nano pipe array |
| CN114477144B (en) * | 2022-01-21 | 2023-05-30 | 西安电子科技大学 | Preparation method of carbon nanotube array |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043648A (en) * | 2012-12-27 | 2013-04-17 | 青岛艾德森能源科技有限公司 | Preparation method for carbon nanotube |
-
2013
- 2013-09-05 CN CN201310398409.9A patent/CN104418318B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043648A (en) * | 2012-12-27 | 2013-04-17 | 青岛艾德森能源科技有限公司 | Preparation method for carbon nanotube |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104418318A (en) | 2015-03-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1325372C (en) | Production of carbon nanotubes | |
| US9206049B2 (en) | Method for making carbon nanotubes | |
| US10533247B2 (en) | Method for growing carbon nanotubes | |
| CN104418318B (en) | CNT continuous growing device | |
| CN105819710B (en) | A kind of graphene/basalt composite material and preparation method thereof | |
| JP2526782B2 (en) | Carbon fiber and its manufacturing method | |
| CN102092704B (en) | Device and method for preparing carbon nanotube array | |
| US9561962B2 (en) | Reactor and method for growing carbon nanotube using the same | |
| US20090311445A1 (en) | Synthesis of Carbon Nanotubes by Selectively Heating Catalyst | |
| CN103265009B (en) | A kind of preparation method of horizontal array carbon nano tube | |
| CN104005004B (en) | The growth method of a kind of minor diameter, metallic single-wall carbon nano-tube and application | |
| CN104986753B (en) | Overlength carbon nano pipe and preparation method thereof and device | |
| JP2014523385A (en) | Carbon nanotube receptor-catalyst growth process | |
| CN104418317B (en) | A kind of CNT continuous growing device | |
| US20070098623A1 (en) | Method for manufacturing carbon nanotubes | |
| Liu et al. | Highly aligned coiled nitrogen-doped carbon nanotubes synthesized by injection-assisted chemical vapor deposition | |
| CN104310371A (en) | Method for growing carbon nano tube in situ on surface of fiber | |
| CN110429262A (en) | Si-C composite material and preparation method thereof | |
| CN1275851C (en) | Preparation method of carbon nano-pipe | |
| Tian et al. | Potential field emitters: HfC nanorods sheathed with a HfO 2 nanoshell | |
| JP5633841B2 (en) | Metal compound-encapsulated carbon nanotube and method for producing metal compound-encapsulated carbon nanotube | |
| JP2005231952A (en) | Synthesis of carbon nanotube by laser beam | |
| JP2005112659A (en) | Apparatus and method for manufacturing carbon nanotube | |
| JP2011173743A (en) | Method for manufacturing carbon nanotube | |
| CN103668111A (en) | Method and device for depositing diamond film in micropore wire-drawing die inner hole |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |