CN202705048U - Continuous graphene production device - Google Patents
Continuous graphene production device Download PDFInfo
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- CN202705048U CN202705048U CN2012203663135U CN201220366313U CN202705048U CN 202705048 U CN202705048 U CN 202705048U CN 2012203663135 U CN2012203663135 U CN 2012203663135U CN 201220366313 U CN201220366313 U CN 201220366313U CN 202705048 U CN202705048 U CN 202705048U
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- reaction tube
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Abstract
The utility model discloses a continuous graphene production device, which comprises a horizontal reaction chamber, wherein a plurality of quartz reaction tubes are arranged in the horizontal reaction chamber; a heat-resistant steel or heat-resistant alloy pad is arranged at the bottom of each quartz reaction tube and is fixed in the horizontal reaction chamber through a refractory brick rack; a plurality of quartz boats which are arranged along the axial direction and have the smooth inner surface or quartz boats with axial grooves uniformly distributed on the inner surface are arranged in a tube cavity of each quartz reaction tube; a carbon source storage tank, a reducing gas storage tank and an inert gas storage tank are respectively communicated with the quartz reaction tubes through a mass flow controller via a gas mixer; waste gas exhaust ports of the quartz reaction tubes are connected with a waste gas recovery treatment device; and a heating device and a temperature control cabinet are arranged outside the horizontal reaction chamber. The continuous graphene production device is simple in structure and large in reaction area, the graphene yield can be greatly improved, the production cost can be reduced, and the energy consumption is reduced; and moreover, the quartz boats which are arranged along the axial direction sequentially enter a high-temperature region during production, so that the graphene can be continuously produced.
Description
Technical field
The utility model relates to a kind of continuous production device of Graphene, particularly relates to a kind of continuous production device with the standby Graphene of chemical vapor deposition (CVD) legal system.
Background technology
Graphene (Graphene) be a kind of by carbon atom with sp
2Hybridized orbital forms the flat film that hexangle type is the honeycomb lattice, only has the two-dimensional material of a carbon atom thickness.Graphene is considered to hypothetical structure always, independent stable existence, until two the physicist Andre Geim of Univ Manchester UK in 2004 and Konstantin Novoselov success in experiment, from graphite, isolate Graphene, confirmed that it can Individual existence, two people are also therefore common to obtain Nobel Prize in physics in 2010.Why Graphene so attracts people's attention is because it has excellent performance at aspects such as mechanics, calorifics, electricity, optics, is considered to have extremely wide application prospect at numerous areas such as the quantum devices such as single-molecule detection device, unicircuit, field-effect transistor, functional composite material, new forms of energy, support of the catalyst and biomedicines.
At present, the main preparation methods of Graphene has the methods such as mechanical stripping method, oxidation reduction process, chemical vapor deposition (CVD) method.But the mechanical process stripping technology is complicated, and cost length high and consuming time obviously can not satisfy industrial requirement; Although oxidation reduction process can be prepared a large amount of Graphenes, stage product crystallographic characteristics and rule in the Graphene preparation process do not cause scholar's attention, thereby have influence on the scope of its application; It is simple that the CVD method prepares Graphene, have that product quality is high, the growth area is large and can cut out and the advantage such as modification it, so the CVD method becomes the main method of preparation high-quality graphene gradually.
The chemical vapor deposition (CVD) method mainly is to utilize the carbon compound such as hydrocarbon gas as carbon source, under the effect of metal powder grain catalyzer or long strip shape tinsel catalyzer, makes carbon source decompose growing graphenes at the inherent substrate surfaces of 600 ~ 1200 ℃ of temperature ranges.At present, the quartz boat of a single port crystal reaction tube and a smooth inner surface only is set in the reaction chamber of CVD production Graphene equipment usually, the output of Graphene is limited by very large, and a large amount of wastes of heating energy source when having caused pyroreaction have increased the production cost of Graphene.
In addition, the internal surface of quartz boat is level and smooth, because the long-width ratio of tinsel catalyzer is very large, thickness is micro-meter scale, when when the quartz boat of smooth inner surface is placed long strip shape tinsel catalyzer, tinsel is displaced sideways, and causes mutual overlapping, and tinsel is easy to curling under hot conditions, reaction process when these all can cause Graphene to prepare is affected, and reduces the output of Graphene.In addition, crystal reaction tube is directly placed the cavity in horizontal reacting chamber, crystal reaction tube is worked under hot conditions for a long time, thereby be difficult to guarantee high-temperature stability and the work-ing life of crystal reaction tube.
Summary of the invention
The purpose of this utility model provides a kind of Graphene production efficiency that is conducive to improve, the continuous production device of the Graphene that reduces production costs.
The continuous production device of Graphene of the present utility model comprises the horizontal reacting chamber, be built-in with some crystal reaction tubes in the horizontal reacting chamber, high temperature steel or refractory alloy liner are arranged at the bottom of every crystal reaction tube, and be fixed in the horizontal reacting chamber by the refractory brick frame, in the tube chamber of every crystal reaction tube, be equipped with a plurality of quartz boats of arranging vertically, said quartz boat is the quartz boat that has the quartz boat of smooth inner surface or be evenly equipped with axial groove for internal surface, the carbon source storage tank, reducing gas storage tank and inertial gas tank are respectively by the carbon source mass flow controller, the reducing gas mass flow controller links to each other with an end of gas mixer with the rare gas element mass flow controller, the other end of gas mixer is communicated with crystal reaction tube, the outlet port of crystal reaction tube links to each other with waste gas recycling device, is provided with heating unit and temperature-controlling cabinet outside the horizontal reacting chamber.
In the utility model, described crystal reaction tube is the single port crystal reaction tube or is the twoport crystal reaction tube.
The heat resisting temperature of described high temperature steel or refractory alloy liner〉1200 ℃.
Be evenly equipped with the quartz boat of axial groove for internal surface, usually, the groove width that makes axial groove is 10 ~ 50mm, and groove depth is 1 ~ 800um, and the distance between two grooves is 0.1 ~ 1.0mm.
The utlity model has following advantage:
1. several crystal reaction tubes are set in the horizontal reacting chamber, therefore, under the constant condition of reaction chamber diameter, by increasing the quantity of silica tube and quartz boat, can increase reaction area, improve Graphene output.
2. when the twoport crystal reaction tube was set in reaction chamber, structure was compacter, can dwindle the volume in horizontal reacting chamber, was conducive to improve the heats of crystal reaction tube.
3. this Graphene production equipment can be evenly equipped with by selection smooth inner surface or internal surface the quartz boat of axial groove, realizes easily the Graphene preparation technology of metal powder grain catalyzer and long strip shape tinsel catalyzer.
4. the quartz boat that adopts internal surface to be evenly equipped with axial groove is placed long strip shape tinsel catalyzer, can prevent that tinsel side direction in quartz boat from sliding out now overlapped, simultaneously can prevent that also tinsel from occurring when pyroreaction curling, reaction process when avoiding Graphene to prepare is affected, and reduces the output of Graphene.
5. in the horizontal reacting chamber, several crystal reaction tubes heat simultaneously, and when significantly reducing energy consumption, Graphene output can improve several times.
6. a plurality of quartz boats of arranging vertically are set in the tube chamber of every crystal reaction tube, and the quartz boat of arranging vertically during production enters the high-temperature zone successively, can realize the continuous production of Graphene, improves Graphene output.
7. the bottom of crystal reaction tube all is provided with high temperature steel or refractory alloy liner, can improve the high-temperature stability of crystal reaction tube and prolong its work-ing life.
Description of drawings
Fig. 1 is Graphene production equipment schematic diagram;
Fig. 2 is the quartz boat schematic diagram of smooth inner surface;
Fig. 3 is the quartz boat schematic diagram that the surface is evenly equipped with axial groove;
Fig. 4 is the cross sectional representation that a twoport crystal reaction tube is set in the horizontal reacting chamber;
Fig. 5 is the cross sectional representation that three single port crystal reaction tubes are set in the horizontal reacting chamber;
Fig. 6 is the cross sectional representation that a twoport crystal reaction tube, a single port crystal reaction tube are set in the horizontal reacting chamber.
Among the figure: 1-crystal reaction tube, 1
/ -single port crystal reaction tube, 2
/ -twoport crystal reaction tube, 3-refractory brick frame, the quartz boat of 4-smooth inner surface, 5-internal surface is evenly equipped with the quartz boat of axial groove, 6-heating unit, 7-temperature-controlling cabinet, 8-carbon source storage tank, 9-reducing gas storage tank, 10-inertial gas tank, 11-carbon source mass flow controller, 12-reducing gas mass flow controller, 13-rare gas element mass flow controller, 14-gas mixer, the recycling of 15-waste gas device, 16-horizontal reacting chamber, 17-high temperature steel or refractory alloy liner.
Embodiment
With reference to Fig. 1, Graphene production equipment of the present utility model comprises horizontal reacting chamber 16, in the legend, be built-in with two crystal reaction tubes 1 in horizontal reacting chamber 16, wherein one is the single port crystal reaction tube, another root is the twoport crystal reaction tube, high temperature steel or refractory alloy liner 17 are arranged in the bottom of every crystal reaction tube, and be fixed in the horizontal reacting chamber 16 by refractory brick frame 3, in the tube chamber of every crystal reaction tube, be equipped with a plurality of quartz boats of arranging vertically, said quartz boat is the quartz boat 4 (shown in Figure 2) with smooth inner surface, or internal surface to be evenly equipped with the quartz boat 5(of axial groove shown in Figure 3), the groove width of quartz boat 5 inner surface axial grooves is 10 ~ 50mm, and groove depth is 1 ~ 800um, and the distance between two grooves is 0.1 ~ 1.0mm.Carbon source storage tank 8, reducing gas storage tank 9 and inertial gas tank 10 link to each other with an end of gas mixer 14 by carbon source mass flow controller 11, reducing gas mass flow controller 12 and rare gas element mass flow controller 13 respectively, the other end of gas mixer 14 is communicated with crystal reaction tube 1, the outlet port of crystal reaction tube 1 links to each other with waste gas recycling device 15, is provided with heating unit 6 and temperature-controlling cabinet 7 outside horizontal reacting chamber 16.
Shown in Figure 4, placing the crystal reaction tube in the horizontal reacting chamber 16 is a twoport crystal reaction tube 2
/ A tube chamber of twoport crystal reaction tube is built-in with for the smooth inner surface quartz boat 4 of placing the metal powder grain catalyzer, another tube chamber is built-in with the quartz boat 5 that is evenly equipped with axial groove for the internal surface of placing long strip shape tinsel catalyzer, in the bottom of crystal reaction tube high temperature steel liner 17 is arranged, and be fixed on the horizontal reacting chamber 16 by refractory brick frame 3.
Shown in Figure 5, be built-in with 3 single port crystal reaction tubes 1 in horizontal reacting chamber 16
/ , be useful on the quartz boat 4 of the smooth inner surface of placing the metal powder grain catalyzer in every single port crystal reaction tube, in the bottom of crystal reaction tube high temperature steel liner 17 is arranged, and be fixed on the horizontal reacting chamber 16 by refractory brick frame 3.
Shown in Figure 6, be built-in with a single port crystal reaction tube 1 in horizontal reacting chamber 16
/ With a twoport crystal reaction tube 2
/ Be built-in with the quartz boat 5 that internal surface is evenly equipped with axial groove at the single port crystal reaction tube, a tube chamber at the twoport crystal reaction tube is built-in with smooth inner surface quartz boat 4, another tube chamber is built-in with the quartz boat 5 that internal surface is evenly equipped with axial groove, in the bottom of crystal reaction tube high temperature steel liner 17 is arranged, and be fixed on the horizontal reacting chamber 16 by refractory brick frame 3.
Claims (4)
1. the continuous production device of a Graphene, it is characterized in that comprising horizontal reacting chamber (16), be built-in with some crystal reaction tubes (1) in horizontal reacting chamber (16), high temperature steel or refractory alloy liner (17) are arranged at the bottom of every crystal reaction tube, and be fixed in the horizontal reacting chamber (16) by refractory brick frame (3), in the tube chamber of every crystal reaction tube, be equipped with a plurality of quartz boats of arranging vertically, said quartz boat is the quartz boat (4) with smooth inner surface or the quartz boat (5) that is evenly equipped with axial groove for internal surface, carbon source storage tank (8), reducing gas storage tank (9) and inertial gas tank (10) are respectively by carbon source mass flow controller (11), reducing gas mass flow controller (12) links to each other with the end of rare gas element mass flow controller (13) with gas mixer (14), the other end of gas mixer (14) is communicated with crystal reaction tube, the outlet port of crystal reaction tube links to each other with waste gas recycling device (15), is provided with heating unit (6) and temperature-controlling cabinet (7) outside horizontal reacting chamber (16).
2. the continuous production device of Graphene according to claim 1 is characterized in that said crystal reaction tube (1) is the single port crystal reaction tube or is the twoport crystal reaction tube.
3. the continuous production device of Graphene according to claim 1 is characterized in that the heat resisting temperature of high temperature steel or refractory alloy liner〉1200 ℃.
4. the continuous production device of Graphene according to claim 1 is characterized in that the groove width of quartz boat (5) inner surface axial groove is 10 ~ 50mm, and groove depth is 1 ~ 800um, and the distance between two grooves is 0.1 ~ 1.0mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012203663135U CN202705048U (en) | 2012-07-27 | 2012-07-27 | Continuous graphene production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012203663135U CN202705048U (en) | 2012-07-27 | 2012-07-27 | Continuous graphene production device |
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| Publication Number | Publication Date |
|---|---|
| CN202705048U true CN202705048U (en) | 2013-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012203663135U Expired - Fee Related CN202705048U (en) | 2012-07-27 | 2012-07-27 | Continuous graphene production device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529099A (en) * | 2013-09-23 | 2014-01-22 | 西南交通大学 | Method for preparing graphene chemically modified electrode through in-situ growth |
| CN104528702A (en) * | 2014-12-22 | 2015-04-22 | 青岛麦特瑞欧新材料技术有限公司 | Electric heating furnace for preparing graphene |
-
2012
- 2012-07-27 CN CN2012203663135U patent/CN202705048U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103529099A (en) * | 2013-09-23 | 2014-01-22 | 西南交通大学 | Method for preparing graphene chemically modified electrode through in-situ growth |
| CN103529099B (en) * | 2013-09-23 | 2016-06-29 | 西南交通大学 | A kind of growth in situ prepares the method for Graphene chemically modified electrode |
| CN104528702A (en) * | 2014-12-22 | 2015-04-22 | 青岛麦特瑞欧新材料技术有限公司 | Electric heating furnace for preparing graphene |
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| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130130 Termination date: 20160727 |