CN102009974B - Combined device for preparing single-wall carbon nano tube - Google Patents
Combined device for preparing single-wall carbon nano tube Download PDFInfo
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- CN102009974B CN102009974B CN201010561468A CN201010561468A CN102009974B CN 102009974 B CN102009974 B CN 102009974B CN 201010561468 A CN201010561468 A CN 201010561468A CN 201010561468 A CN201010561468 A CN 201010561468A CN 102009974 B CN102009974 B CN 102009974B
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Abstract
The invention relates to a combined device for preparing a single-wall carbon nano tube. The combine device mainly comprises an arc vacuum discharge device and belongs to the technical field of a nano material manufacturing device. The combined device comprises an arc discharge vacuum furnace, a cage type collecting device, a filtering chamber, a cold trap and auxiliary devices, and is characterized in that the devices are sequentially connected with one another in series by pipelines. The furnace wall of the arc discharge vacuum furnace is a two-layer water-cooling stainless steel cavity wall, and the cavity wall is provided with six windows which are arranged at certain angles and used for accommodating electrodes, so that the relative positions of two electrodes can be distributed and adjusted on the same plane or different planes. By arranging the cage type collecting device in the vacuum cavity and additionally arranging the filtering chamber and the cold trap, most of carbon nano tubes can be collected conveniently, the collection rate of products is improved, the purity of products is increased, and simultaneously nano particle impurities can not enter into air to pollute the atmosphere.
Description
Technical field
The present invention relates to a kind of associated plant for preparing SWCN, mainly include the electric arc vacuum electric-discharge device, metal nanometer material manufacturing installation technical field.
Background technology
After finding multi-walled carbon nano-tubes (MWCNTs) and found SWCN (SWCNTs) in 1993 in 1991, the method for preparing carbon nanotube mainly contains arc discharge method, laser evaporation method and chemical Vapor deposition process (CVD).At present in the report, the laser evaporation method can be prepared high-purity, high crystalline SWCN, but equipment cost is high; CVD method equipment is simple, can prepare carbon nanotube in enormous quantities, but the carbon nanotube crystallinity of preparation is poor, makes the lot of advantages of carbon nanotube to show.At present arc discharge method equipment is simple relatively, and the carbon nanotube of preparing separates with carbon nanometer impurity is difficult, and the dust of Nano grade is easy to get in the atmosphere, thus polluted air.
Chinese patent CN 1463919A discloses the method for preparing carbon nanotube, and wherein negative electrode becomes the angle of 30-80 degree with anode; Chinese patent CN 2475983Y and CN 1712350A have all proposed to carry out the furnace wall heating means of temperature control.These equipment can both be produced carbon nanotube, but not have proposition to carry out separated and collected for carbon nanotube and to the capture of the dust of Nano grade.
Patent of the present invention has proposed to collect through most of SWCN Spider Web thing that sample collection device (cage of rotation) will generate, and small carbon nano-particle impurity is flowed out through the air outlet, reaches to collect and two purposes of raising purity.Simultaneously, through filtration chamber and cold-trap the nearly all carbon nano-particle impurity and the carbon nanotube of escape are captured fully again, avoid it to get into the topsoil air.
Summary of the invention
The purpose of this invention is to provide a kind of collection rate that improves, improve purity and prevent the associated plant of the SWCN of contaminate environment.
A kind of associated plant for preparing SWCN of the present invention; Comprise arc-over vacuum oven, cage collection device, filtration chamber, cold-trap and auxiliary equipment; It is characterized in that: electric arc is put purport vacuum oven, cage collection device, filtration chamber, cold-trap, interconnects through before and after the pipeline; The structure and the DeviceMode thereof of each several part device are following:
A. arc-over vacuum oven: the same wall of columnar arc-over vacuum oven is a double-deck water-cooled stainless steel chamber wall; With equidistant 1 the electrode installation of window opening that is provided with 5 electrode installation of window opening and is provided with of wall at electric arc vacuum oven rear wall; Six electrode installation of window opening can satisfy anode and cathode electrode on same plane or Different Plane become different angles to install; Chamber internal upper part at the electric arc vacuum oven is provided with a collection cage; Collecting cage has pipeline to lead to the filtration chamber; Chamber bottom at the electric arc vacuum oven is separately installed with anode and negative electrode through the electrode installation of window opening; Have a gas inlet at the electric arc vacuum oven with the wall bottom; The electric arc vacuum oven is provided with a fire door, and fire door is provided with two view ports up and down, and view port is a bilayer structure, i.e. arc protection window and viewing window; Respectively be provided with the window brush in the view port, with sedimentary particle foreign material on the cleaning viewing window; On the wall of the double-deck water-cooled stainless steel of arc-over vacuum oven chamber, offer a cooling water intake and water outlet, with high-temperature atmosphere in the cooling chamber and cooled furnace wall;
B. cage collection device: the cage collection device is promptly collected cage, and it can be rotated by the hollow cylindrical skeleton that many stainless steels are formed continuously, to capture SWCN;
C. filtration chamber: the filtration chamber has pipeline to link to each other with collecting between the cage, is provided with a netted inner bag in the chamber of filtration chamber, with filtering carbon nanotube;
D. cold-trap: the bottom of cold-trap has pipe to be communicated with the bottom, filtration chamber; Its inside is one to be provided with the inner bag of end socket, and its top is provided with liquid nitrogen feed-pipe and extraction line, is attracted on the inner bladder outer wall to guarantee nano-powder, and wall is exempted to get into air and polluted; The one side mouth of pipe of bleeding on the top of cold-trap, the mouth of pipe of bleeding is connected with vacuum pump, to guarantee the air-flow carriage direction and the vacuum state of this system.
Described negative electrode and anode have the copper anchor clamps in its electrode junction, and it is circle or square aperture; Cathode end is provided with the auxiliary equipment that it is rotated continuously; The welding bellows structure is adopted in the anode end, make before and after the electrode, up and down, about can do to move and fine setting; Anodic-cathodic is long carbon electrode bar, except that circular or square, also can use other shapes.
The rare gas element that the inlet mouth that described electric arc furnace perisporium bottom is offered is sent into is helium or hydrogen-argon-mixed body.
The function situation of associated plant of the present invention is described below: be located at and contain catalyzer anode carbon electrode bar in the arc-over vacuum oven vacuum chamber; And arc between another cathode electrode, anode electrode rod are evaporated the thread SWCN product of generation and in vacuum chamber, are collected by ad hoc cage collection device; The cage collection device is a hollow skeleton, and thread SWCN is hung on the skeleton; Through the pipeline that connects; Sent into the filtration chamber by air-flow; SWCN and nano particle impurity that the filtration chamber not collects major part are collected, and follow the gentle cold-trap that is connected with the filtration chamber that flows into of logistics, and cold-trap captures the stove dirt of Nano grade in inner bladder outer wall wherein; The oil-sealed rotary pump that behind cold-trap, is provided with provides gas flow and vacuum requirement.
Characteristics of the present invention are: when collecting SWCN; No longer as installing, let it be deposited on naturally on the waterway wall in the past, but capture, can improve collection rate like this through the cage collection device; And can SWCN and carbon nano-particle impurity be separated, improved product purity.In addition, adopted the filtration chamber, passed through cold-trap again, can nearly all nano particle impurity have been collected fully, got into the atmospheric pollution atmosphere to avoid it with most of carbon nano-particle and after leaking the SWCN capture of receiving remnants.
Another characteristics of the present invention are: the layout of electrode can realize that not only different angles are discharged on the same plane, and can realize that the Different Plane different angles discharge.
Description of drawings
Fig. 1 is the rear view synoptic diagram of associated plant of the present invention;
The front view of the electric arc vacuum oven when Fig. 2 is the oven door opening state;
Fig. 3 is the run lateral plan of empty stove of electric arc;
Fig. 4 is the opening shape figure of electrode tip copper anchor clamps;
Fig. 5 is provided with synoptic diagram for fire door;
Fig. 6 is the brush schematic perspective view in the fire door viewing window.
Embodiment
Existing specific embodiment further explain with associated plant of the present invention in after.
Embodiment 1:Referring to Fig. 1, Fig. 2, Fig. 3.In the present embodiment; The associated plant of preparation SWCN; Comprise arc-over vacuum oven, cage collection device, filtration chamber, cold-trap and auxiliary equipment, it is characterized in that: electric arc is put purport vacuum oven, cage collection device, filtration chamber, cold-trap, interconnects through before and after the pipeline; The structure and the DeviceMode thereof of each several part device are following:
(1), arc-over vacuum oven: the same wall of columnar arc-over vacuum oven is a double-deck water-cooled stainless steel chamber wall; With equidistant 1 the electrode installation of window opening 26 that is provided with 5 electrode installation of window opening 21,22,23,24,25 and is provided with of wall at electric arc vacuum oven rear wall; Six electrode installation of window opening can satisfy anode and cathode electrode on same plane or Different Plane become different angles that (as 45 °, 90 °, 135 °, 180 °) are installed; Chamber internal upper part at the electric arc vacuum oven is provided with a collection cage 1; Collecting cage 1 has pipeline to lead to filtration chamber 5; In the chamber bottom of electric arc vacuum oven, be separately installed with anode 12 and negative electrode 11 through electrode installation of window opening 23,25; Have a rare gas element inlet mouth 2 at the electric arc vacuum oven with the wall bottom; The electric arc vacuum oven is provided with a fire door 13 (referring to Fig. 5), and fire door 13 is provided with two view ports 14,15 up and down, and view port 14,15 is a bilayer structure, i.e. arc protection window 14a, 15a and viewing window 16,19; Respectively be provided with window brush 17,18 in the view port 14,15, with sedimentary particle foreign material on the cleaning viewing window; On the wall of the double-deck water-cooled stainless steel of arc-over vacuum oven chamber, offer a cooling water intake 3 and water outlet 4, with high-temperature atmosphere in the cooling chamber and cooled furnace wall;
(2), cage collection device: the cage collection device is promptly collected cage 1, and it can be rotated by the hollow cylindrical skeleton that many stainless steels are formed continuously, to capture SWCN;
(3), filtration chamber: filtration chamber 5 has pipeline to link to each other with collecting between the cage 1, is provided with a netted inner bag 6 in the chamber of filtration chamber 5, with filtering carbon nanotube;
(4), cold-trap: the bottom of cold-trap 7 has pipe to be communicated with the bottom, filtration chamber; Its inside is one to be provided with the inner bag 8 of end socket, and its top is provided with liquid nitrogen feed-pipe 10 and extraction line 9, is attracted on the inner bladder outer wall to guarantee nano-powder, and wall is exempted to get into air and polluted; The side mouth of pipe 20 of bleeding on the top of cold-trap 7, the mouth of pipe 20 of bleeding is connected with vacuum pump, to guarantee the air-flow carriage direction and the vacuum state of this system.
Described negative electrode 11 and anode 12 have copper anchor clamps (referring to Fig. 4) in its electrode junction, and it is circle or square aperture; Cathode end is provided with the auxiliary equipment that it is rotated continuously; The welding bellows structure is adopted in the anode end, make before and after the electrode, up and down, about can do to move and fine setting; Anodic-cathodic is long carbon electrode bar, except that circular or square, also can use other shapes.
The rare gas element that the inlet mouth 2 that described electric arc furnace perisporium bottom is offered is sent into is helium or hydrogen-argon-mixed body.
In the present embodiment, in the arc-over vacuum oven, arc discharge method can adopt the direct current arc discharge, or adopts the alternating current arc discharge, or adopts the discharge of alternating current-direct current mixed arc.
Claims (3)
1. associated plant for preparing SWCN; Comprise arc-over vacuum oven, cage collection device, filtration chamber, cold-trap and auxiliary equipment; It is characterized in that: arc-over vacuum oven, cage collection device, filtration chamber, cold-trap interconnect through before and after the pipeline;
The structure of described arc-over vacuum oven is: the barrel of columnar arc-over vacuum oven is a double-deck water-cooled stainless steel chamber wall; In equidistant 1 the electrode installation of window opening (26) that is provided with 5 electrode installation of window opening (21,22,23,24,25) and is provided with of barrel at arc-over vacuum oven rear wall; Six electrode installation of window opening can satisfy anode and cathode electrode on same plane or Different Plane become different angles to install; Chamber internal upper part at the arc-over vacuum oven is provided with a collection cage (1); Collecting cage (1) has pipeline to lead to filtration chamber (5); In the chamber interior of arc-over vacuum oven, be separately installed with anode (12) and negative electrode (11) through any two electrode installation of window opening; Have a gas inlet (2) in arc-over vacuum oven barrel bottom; The arc-over vacuum oven is provided with a fire door (13), and fire door (13) is provided with two view ports (14,15) up and down, and view port (14,15) is a bilayer structure, i.e. arc protection window (14a, 15a) and viewing window (16,19); Respectively be provided with window brush (17,18) in the view port (14,15), with sedimentary particle foreign material on the cleaning viewing window; On the wall of the double-deck water-cooled stainless steel of arc-over vacuum oven chamber, offer a cooling water intake (3) and water outlet (4), with high-temperature atmosphere in the cooling chamber and cooled furnace wall;
The structure of described cage collection device is: the cage collection device is promptly collected cage (1), and it can be rotated by the hollow cylindrical skeleton that many stainless steels are formed continuously, to capture SWCN;
The structure of described filtration chamber is: filtration chamber (5) have pipeline to link to each other with collecting between the cage (1), are provided with a netted inner bag (6) in the chamber of filtration chamber (5), with filtering carbon nanotube;
The structure of described cold-trap is: the bottom of cold-trap (7) has pipe to be communicated with the bottom, filtration chamber; Its inside is one to be provided with the inner bag (8) of end socket, and its top is provided with liquid nitrogen feed-pipe (10) and extraction line (9), is attracted on the inner bladder outer wall to guarantee nano-powder, avoids getting into air and pollutes; The side mouth of pipe (20) of bleeding on the top of cold-trap (7), the mouth of pipe of bleeding (20) is connected with vacuum pump, to guarantee the air-flow carriage direction and the vacuum state of this system.
2. a kind of associated plant for preparing SWCN according to claim 1 is characterized in that described negative electrode (11) and anode (12), in its electrode junction the copper anchor clamps is arranged, and the copper anchor clamps are circle or square aperture; Cathode end is provided with the auxiliary equipment that it is rotated continuously; The welding bellows structure is adopted in the anode end, make before and after the electrode, up and down, about do to move and fine setting; Anodic-cathodic is long carbon electrode bar, and its cross section is circular or square.
3. a kind of associated plant for preparing SWCN according to claim 1 is characterized in that the gas that inlet mouth (2) that described arc-over vacuum oven barrel bottom is offered is sent into is helium or hydrogen-argon-mixed body.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010561468A CN102009974B (en) | 2010-11-28 | 2010-11-28 | Combined device for preparing single-wall carbon nano tube |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010561468A CN102009974B (en) | 2010-11-28 | 2010-11-28 | Combined device for preparing single-wall carbon nano tube |
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| CN102009974A CN102009974A (en) | 2011-04-13 |
| CN102009974B true CN102009974B (en) | 2012-08-29 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110182787B (en) * | 2019-06-19 | 2022-11-01 | 江西铜业技术研究院有限公司 | Device and method for continuously growing carbon nano tube |
| CN112798884B (en) * | 2020-12-15 | 2021-11-30 | 珠海格力电器股份有限公司 | Convenient arc burning device, control method, arc generator and application |
| CN115215327B (en) * | 2022-02-23 | 2023-10-03 | 无锡东恒新能源科技有限公司 | Device and method for purifying carbon nano tube |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3423639B2 (en) * | 1999-04-27 | 2003-07-07 | キヤノン株式会社 | Method and apparatus for producing carbon nanotube |
| CN1463919A (en) * | 2002-06-10 | 2003-12-31 | 中国科学院化学研究所 | A carbon nano tube derivative and method for preparing same |
| CN1608979A (en) * | 2003-10-18 | 2005-04-27 | 鸿富锦精密工业（深圳）有限公司 | Equipment and prepn process of embedding carbon nanotube into metal |
| CN1712350A (en) * | 2004-06-15 | 2005-12-28 | 南开大学 | Arc synthesizer of sing-wall carbon nanometer tubes |
| KR20090000669U (en) * | 2007-07-19 | 2009-01-22 | 조영상 | Automatic control of electrode space for arc discharge carbon nanotube synthesis |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0202397D0 (en) * | 2002-02-01 | 2002-03-20 | Nanofilm Technologies Int | Production of nanotubes |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3423639B2 (en) * | 1999-04-27 | 2003-07-07 | キヤノン株式会社 | Method and apparatus for producing carbon nanotube |
| CN1463919A (en) * | 2002-06-10 | 2003-12-31 | 中国科学院化学研究所 | A carbon nano tube derivative and method for preparing same |
| CN1608979A (en) * | 2003-10-18 | 2005-04-27 | 鸿富锦精密工业（深圳）有限公司 | Equipment and prepn process of embedding carbon nanotube into metal |
| CN1712350A (en) * | 2004-06-15 | 2005-12-28 | 南开大学 | Arc synthesizer of sing-wall carbon nanometer tubes |
| KR20090000669U (en) * | 2007-07-19 | 2009-01-22 | 조영상 | Automatic control of electrode space for arc discharge carbon nanotube synthesis |
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