CN101311295B - Device for preparing single wall carbon nanotube film by arc-discharge method - Google Patents
Device for preparing single wall carbon nanotube film by arc-discharge method Download PDFInfo
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- CN101311295B CN101311295B CN2008100595524A CN200810059552A CN101311295B CN 101311295 B CN101311295 B CN 101311295B CN 2008100595524 A CN2008100595524 A CN 2008100595524A CN 200810059552 A CN200810059552 A CN 200810059552A CN 101311295 B CN101311295 B CN 101311295B
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Abstract
The invention discloses a device for preparing single walled carbon nanotube film based on arc discharge. The device comprises an arc discharge vacuum chamber; wherein, the arc discharge vacuum chamber is connected with a vacuum pump and is internally provided with a graphite cathode and a graphite anode which are connected with a DC supply. The device is characterized in that the graphite cathodeand the graphite anode are respectively provided with an upper spherical crown shape graphite plate and a lower spherical crown shape graphite plate which are matched with each other and formed a spherical crown shape capacitor. The device attaches the synthesized single walled carbon nanotube to the inner surface of the spherical crown shape graphite polar plate in the form of large area (100 to200 square centimeters) film. The thickness of the film which can be controlled as needed is a plurality of microns to 1mm. The prepared single walled carbon nanotube film has the conversion above 75percent and the purity above 55 percent.
Description
Technical field
The present invention relates to a kind of device for preparing single wall carbon nano-tube film based on arc discharge method.
Background technology
Single Walled Carbon Nanotube utilizes arc discharge method to prepare at first, from the history that is found to the now existing more than ten years of Single Walled Carbon Nanotube.Utilize the Single Walled Carbon Nanotube (SWCNTs) of arc discharge method preparation to have good crystallinity, characteristics such as preparation time weak point.Along with the continuous development of carbon nanotube research, the research of many application facet is starved of single wall carbon nano-tube film.Utilize the CVD method to make Single Walled Carbon Nanotube, the film forming area is little, and crystallinity is poor, can not satisfy the needs of applied research.And the method for utilizing arc discharge method to prepare the big area single wall carbon nano-tube film yet there are no so far and reports for work.If the utilization arc discharge method promptly enables to make the single wall carbon nanocapsule thin film, also some problems that can exist owing to this method, and influence the quality and the effect of film.Available research achievements shows that when arc discharge method prepared Single Walled Carbon Nanotube, the temperature distribution scope that arc-over produces was big, and anodic graphite spreads naturally because of high temperature makes it when evaporation, thereby makes single wall carbon CNT (carbon nano-tube) output lower, and purity is not high yet.The synthesis temperature that arc process prepares the SWCNTs needs generally is higher than 1000 ℃, how to form a suitable temperature province and has very important significance for synthetic high-quality, high purity single wall carbon nano-tube film.As everyone knows, Single Walled Carbon Nanotube has determined it can become a kind of type material with various performances such as good mechanics, electricity, and very wide application prospect has all been arranged in a lot of fields because of himself having perfect structure.Single Walled Carbon Nanotube is made large area film have vital role for the performance of bringing into play its multiple excellence.Particularly all press for big area, high purity, high-quality single wall carbon nano-tube film at the aspects such as catalysis electrode film of matrix material, field emmision material, fuel cell.
Summary of the invention
The purpose of this invention is to provide a kind of device for preparing single wall carbon nano-tube film based on arc discharge method.
The device for preparing single wall carbon nano-tube film based on arc discharge method comprises the arc-over vacuum chamber, the arc-over vacuum chamber is connected with vacuum pump, be provided with graphite cathode and graphite anode in the arc-over vacuum chamber, graphite cathode is connected with direct supply with graphite anode, it is characterized in that establish respectively on graphite cathode and the graphite anode match on spherical graphite cake and following spherical graphite cake, go up spherical graphite cake and down spherical graphite cake forms the ball crown type electrical condenser.
Described electrode bar is that the diameter that contains metal catalyst is a 6mm Graphite Electrodes rod.The diameter of Graphite Electrodes rod is 8mm.The radius-of-curvature that goes up spherical graphite cake and following spherical graphite cake is 200mm～500mm.The width between centers that goes up between spherical graphite cake and the following spherical graphite cake is 50mm～300mm.The roughness of spherical graphite cake internal surface is 3～3.5 μ m.The thickness of spherical graphite cake is 3mm～6mm.The film forming area of spherical graphite cake is 100～200cm
2The volts DS of direct supply is 20～10000V.The internal surface temperature of spherical graphite cake is 1200K～1600K.
The present invention is made of two pieces large-scale ball crown type graphite pole plates, after two pieces of pole plates are connected direct supply respectively, just becomes the ball crown type electrical condenser that can produce electric field.On this ball crown type electrical condenser, Graphite Electrodes is installed respectively, wherein, the graphite anode rod that contains metal catalyst is installed on the spherical crown graphite pole plate below, the Graphite Electrodes rod is installed on the superincumbent spherical crown graphite cathode plate.When Graphite Electrodes is implemented arc-over, high temperature evaporation graphite-rod anode formation carbon ion because of discharge generation, carbon ion is in the diffusion process of single-wall carbon nanotube synthesizing, because of having negative potential, graphite pole plate above the ball crown type electrical condenser is attracted, simultaneously, utilize the space of the Graphite Electrodes formation of two pieces of ball crown type electrical condensers can change carbon ion diffusion form, thereby make the synthetic Single Walled Carbon Nanotube, can be with big area (100～150cm
2) form of film evenly is attached on the internal surface of negative electrode spherical crown graphite pole plate.The thickness of film can be controlled as required, and thickness is between several microns to 1 millimeter magnitudes, and the transformation efficiency of the single wall carbon nano-tube film of preparing has reached more than 75%, and the purity of Single Walled Carbon Nanotube is more than 55% in the film.
Description of drawings
Fig. 1 prepares the setting drawing of single wall carbon nano-tube film for arc discharge method;
Fig. 2 is for using yttrium oxide and nickel powder binary catalyst, and the field emission scanning electron microscope photo of the single wall carbon nano-tube film of preparation, film surface have a large amount of carbon nanotube bundles, also has some granules of catalyst simultaneously;
Fig. 3 is for using yttrium oxide and nickel powder binary catalyst, the high resolution transmission electron microscopy photo of the single wall carbon nano-tube film of preparation, in carbon nanotube bundles, every Single Walled Carbon Nanotube is high-visible, white short-term institute mark be a Single Walled Carbon Nanotube that diameter is 1.20nm;
Fig. 4 is the Raman spectrogram (at room temperature excitation wavelength is 488nm) of single wall carbon nano-tube film.By 1339cm
-1Decolorizing carbon peak and 1583cm
-1Single Walled Carbon Nanotube characteristic peaks intensity contrast nearby only contains the decolorizing carbon of trace, low frequency range 150～210cm as can be seen in the single wall carbon nano-tube film
-1The peak value of the breathing vibration film mean diameter that can obtain Single Walled Carbon Nanotube be 1.26nm;
Fig. 5 is the thermogravimetric analysis figure of single wall carbon nano-tube film, and the oxidizing temperature of wall carbon nano tube is 460～650 ℃, and the content of single wall carbon nanometer is 55% in hence one can see that the film.
Embodiment
The present invention comprises vacuum chamber by a covering device, vacuum chamber is connected with vacuum pump, be provided with graphite cathode and graphite anode in the vacuum chamber, graphite cathode is connected with direct supply with graphite anode, it is characterized in that establish respectively on graphite cathode and the graphite anode match on spherical graphite cake and following spherical graphite cake, constitute the device of ball crown type electrical condenser (comprising the flat capacitor device), realize the target of preparation big area, high-quality single wall carbon nano-tube film.The feature of present method is that the arc-over of negative electrode graphite rod and the graphite anode rod that contains metal catalyst is carried out in the space that two pieces of ball crown type graphite pole plates form.In the discharge process,, therefore, be in the ball crown type graphite cathode plate of negative potential, have the character that attracts carbon ion owing to have electric field all the time between two pieces of ball crown type graphite pole plates.On the other hand, because the spaces that two pieces of ball crown type graphite pole plates form, change the diffusion form of carbon ion etc., increased the synthetic probability of Single Walled Carbon Nanotube.Simultaneously, charge under atmosphere of inert gases and the certain pressure at vacuum chamber, the high temperature evaporation that arc-over produces contain the graphite anode rod of metal catalyst, at this moment, carbon ion is because of effect of electric field and specific gaseous diffusion form, the synthetic Single Walled Carbon Nanotube is just with uniform form of film, almost all on the internal surface attached to last spherical graphite cathode plate.This single wall carbon nano-tube film has big area (100～200cm
2), high purity (55%), high-quality characteristics, and the thickness of single wall carbon nano-tube film also can be controlled as required, thickness is between several microns to 1 millimeter magnitudes.To the observation of synthetic single wall carbon nano-tube film sample among the embodiment through field emission scanning electron microscope (FSEM) and high resolution transmission electron microscopy (HRTEM), the research and the test shows of Raman (Raman) spectral characterization and thermogravimetric analysis (TGA), the transformation efficiency of the Single Walled Carbon Nanotube of preparing has reached more than 75%, purity is more than 55%, mean diameter is 1.27nm, and length is the number micron dimension.Its equipment drawing, electromicroscopic photograph and test curve are seen accompanying drawing 1～5.
As shown in Figure 1, the device for preparing single wall carbon nano-tube film based on arc discharge method comprises arc-over vacuum chamber 3, the arc-over vacuum chamber is connected with vacuum pump 6, be provided with graphite cathode 5 and graphite anode 4 in the arc-over vacuum chamber, graphite cathode is connected with direct supply 7 with graphite anode, it is characterized in that establish respectively on graphite cathode 5 and the graphite anode 4 match on spherical graphite cake 1 and spherical graphite cake 2 down, go up spherical graphite cake 1 and down spherical graphite cake 2 forms the ball crown type electrical condensers.
Described electrode bar 4 is a 6mm Graphite Electrodes rod for the diameter that contains metal catalyst.The diameter of Graphite Electrodes rod 5 is 8mm.The radius-of-curvature that goes up spherical graphite cake 1 and following spherical graphite cake 2 is 200mm～500mm.The width between centers that goes up between spherical graphite cake 1 and the following spherical graphite cake 2 is 50mm～300mm.The roughness of spherical graphite cake internal surface is 3～3.5 μ m.The thickness of spherical graphite cake is 3mm～6mm.The film forming area of spherical graphite cake is 100～200cm
2The volts DS of direct supply 5 is 20～10000V.The internal surface temperature of spherical graphite cake is 1200K～1600K.
The experiment condition of preparation single wall carbon nanocapsule thin film is to become uniform powder with one or more combined hybrid among Fe, Co, Ni, Y, the Mo, mix with Graphite Powder 99 with certain proportion, be filled in the graphite rod that diameter is 6mm and be prepared into the composite graphite anode, negative electrode uses the graphite rod of diameter as 8mm, also can directly use circular arc graphite cake negative electrode.Atmosphere gas is high-purity He gas or Ar gas, pressure between 50～600Torr, by the anodic electric current between 50～100A.The graphite anodic-cathodic has formed single wall carbon nano-tube film implement arc-over in the space that spherical electrical condenser forms after on the internal surface of last spherical negative electrode graphite pole plate.
Embodiment 1:
Use yttrium oxide (Y
2O
3) and nickel (Ni) powder binary catalyst, with the mass ratio Y of Graphite Powder 99
2O
3: Ni: C=5: 2: 5, charge in the graphite rod of Φ 6 * 50mm, be the composite graphite anode, discharging current is 70A, pressure is to implement arc-over 2min under the condition of 600Torr, and can collect quality on circular arc graphite cake negative electrode is that 110mg, area reach 200cm
2Single wall carbon nano-tube film (the about 0.3mm of thickness).
Embodiment 2: use yttrium oxide (Y
2O
3) and nickel (Ni) binary catalyst, with the mass ratio Y of Graphite Powder 99
2O
3: Ni: C=5: 2: 5, the graphite rod of Φ 6 * 50mm, be the composite graphite anode, discharging current is 60A, pressure is to implement arc-over 2min under the condition of 400Torr, collecting quality on circular arc graphite cake negative electrode is 40mg, area reaches 80cm
2Single wall carbon nano-tube film (the about 0.3mm of thickness).
Claims (4)
1. device for preparing single wall carbon nano-tube film based on arc discharge method, comprise arc-over vacuum chamber (3), the arc-over vacuum chamber is connected with vacuum pump (6), be provided with graphite cathode (5) and graphite anode (4) in the arc-over vacuum chamber, graphite cathode is connected with direct supply (7) with graphite anode, it is characterized in that on graphite cathode (5) and graphite anode (4), establishing respectively the last spherical graphite cake (1) and the following spherical graphite cake (2) that match, go up spherical graphite cake (1) and following spherical graphite cake (2) formation ball crown type electrical condenser; The radius-of-curvature that goes up spherical graphite cake (1) and following spherical graphite cake (2) is 200mm～500mm, and the width between centers that goes up between spherical graphite cake (1) and the following spherical graphite cake (2) is 50mm～300mm.
2. according to claim 1ly a kind ofly prepare the device of single wall carbon nano-tube film, it is characterized in that described graphite anode (4) is a 6mm Graphite Electrodes rod for the diameter that contains metal catalyst based on arc discharge method.
3. according to claim 1ly a kind ofly prepare the device of single wall carbon nano-tube film based on arc discharge method, the diameter that it is characterized in that described graphite cathode (5) is 8mm.
4. according to claim 1ly a kind ofly prepare the device of single wall carbon nano-tube film based on arc discharge method, the volts DS that it is characterized in that described direct supply (7) is 20～10000V.
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| CN102092707B (en) * | 2010-12-16 | 2013-02-13 | 中国科学院高能物理研究所 | Carbon rod activator |
| CN107083556B (en) * | 2017-04-22 | 2019-01-01 | 富吉一纯 | The electrolysis electrode of water and the manufacturing method of the electrode |
| CN108220997B (en) * | 2018-01-31 | 2019-06-18 | 中国科学院福建物质结构研究所 | A kind of carbon containing nickel coat single-walled carbon nanotube composite material and preparation method and purposes |
| CN110721699B (en) * | 2018-07-16 | 2023-01-13 | 中国石油化工股份有限公司 | Gasoline hydrodesulfurization catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004189573A (en) * | 2002-12-13 | 2004-07-08 | Jfe Engineering Kk | Carbon nanotube aggregate, and carbon nanotube setting device with the same set therein |
| JP2004323292A (en) * | 2003-04-24 | 2004-11-18 | Hiroshi Takigawa | Method and apparatus for carbon nanoparticle |
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1765735A (en) * | 2004-10-28 | 2006-05-03 | 鸿富锦精密工业（深圳）有限公司 | Preparation method of carbon nano-tube and its equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004189573A (en) * | 2002-12-13 | 2004-07-08 | Jfe Engineering Kk | Carbon nanotube aggregate, and carbon nanotube setting device with the same set therein |
| JP2004323292A (en) * | 2003-04-24 | 2004-11-18 | Hiroshi Takigawa | Method and apparatus for carbon nanoparticle |
| CN1579931A (en) * | 2004-05-17 | 2005-02-16 | 西安交通大学 | Method for batch type production of single-wall nano carbon tube suing temperature-controlled electric arc furnace |
| CN1765735A (en) * | 2004-10-28 | 2006-05-03 | 鸿富锦精密工业（深圳）有限公司 | Preparation method of carbon nano-tube and its equipment |
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