CN103305806B - Device for continuously growing graphene at high temperature - Google Patents
Device for continuously growing graphene at high temperature Download PDFInfo
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- CN103305806B CN103305806B CN201310270021.0A CN201310270021A CN103305806B CN 103305806 B CN103305806 B CN 103305806B CN 201310270021 A CN201310270021 A CN 201310270021A CN 103305806 B CN103305806 B CN 103305806B
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- high temperature
- reaction chamber
- running roller
- substrate
- vertical reaction
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000000758 substrate Substances 0.000 claims description 43
- 238000007664 blowing Methods 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 23
- 238000002156 mixing Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract 2
- 239000012495 reaction gas Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 230000001360 synchronised effect Effects 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a device for continuously growing graphene at high temperature. The device comprises a seal cabinet internally provided with a vacuum chamber, a material discharging roller wheel, a material receiving roller wheel for coiling and receiving a foundation base, a heater, an air inlet mechanism and a vacuum pump set, wherein the foundation base is coiled on the material discharging roller wheel; the end of the foundation base penetrates through a vertical high temperature reaction chamber to be connected to the material receiving roller wheel; the vacuum pump set is used for providing vacuum reaction condition for the vertical reaction chamber; the air inlet mechanism is used for providing graphene growth reaction gas for the vertical reaction chamber; and the heater is used for providing temperature condition for the growth of grapheme. The equipment overcomes the problem that the continuous preparation of graphene growth is incompatible to high temperature, enables the growth foundation base to grow the graphene continuously and stably at high temperature, and realizes large-scale preparation of large-area uniform grapheme.
Description
Technical field
The present invention relates to a kind of device of growing graphene.
Background technology
The two dimensional crystal of the only atomic layers thick that Graphene is made up of carbon atom.But because Graphene has unique optics, electricity, mechanical property, at the extensive concern of the people obtained in recent years.And the discoverer Andre Geim of Graphene and Konstantin Novoselov also obtains Nobel Prize in physics in 2010 because of its initiative work in Graphene.
Graphene is almost completely transparent, and it only absorbs the light of 2.3% at whole wave band.In addition, Graphene also has good thermal conductivity and electroconductibility, and its electronic mobility of normal temperature, more than 15000cm2/Vs, exceedes carbon nanotube and silicon crystal, and resistivity only about 10-6 Ω cm, lower than copper or silver, is the material that resistivity is minimum in the world at present.Because Graphene is the type material integrating the excellent properties such as superelevation physical strength, thermal conductive resin, high optical transparency and superpower electroconductibility, it is with a wide range of applications in fields such as display, the energy, detection and photoelectrons, and the application and development of Graphene also will bring revolutionary transfer to numerous research field.
How extensive, continuous production big area, high-quality Graphene, be the crucial Science and Technology problem faced in Graphene application industry.Through research in a few years, develop several graphene preparation method at present, as mechanically peel method, epitaxial growth method, chemical reduction graphite oxide method, chemical Vapor deposition process (CVD) etc., wherein CVD prepares Graphene is one of promising method of current most, because can prepare the single-layer graphene of Large-Area-Uniform by CVD method.
But due to the restriction of preparation technology, method and apparatus that is extensive, continuous production Large-Area-Uniform single-layer graphene never makes a breakthrough at present, have impact on the popularization of Graphene application industry greatly, hinders further developing of Graphene.Although can realize in experiment the preparation that diagonal lines reaches the individual layer large-area graphene of 30 inches (about 76cm), by the restriction of instrument and supplies, still cannot realize big area, high-quality graphene continuous, prepare fast.
Summary of the invention
The device of object of the present invention continuous growing graphene under being just to provide a kind of high temperature; which overcome graphene growth continuous production and the incompatible problem of high temperature; it can make growth substrate at high temperature continuous, stable growing graphene, realizes the mass-producing preparation of Large-Area-Uniform Graphene.
The object of the invention is by such technical scheme realize, it establishes the sealing cabinet of vacuum chamber in including, volume has the blowing running roller of substrate, for furling the rewinding running roller of substrate and the interior well heater establishing vertical substrate channel, described blowing running roller, rewinding running roller and well heater are installed in vacuum chamber, be provided with for the vertical reaction chamber through substrate in the substrate channel of well heater, rack is provided with the admission gear being communicated to vertical reaction chamber, the cooling body for cooling substrate is also provided with between well heater and rewinding running roller, described device also includes for the vacuum pump group of vacuum chamber.
Further, described admission gear includes three tunnel inlet pipe, a mixing chamber and an escape pipe, and three tunnel inlet pipe are communicated to mixing chamber, and mixing chamber is communicated in vertical reaction chamber by escape pipe, and three tunnel inlet pipe are accurately controlled by proton stream amount controller.
Further, described device also includes the driving guide roller wheels for more than substrate-guided a group, often drive guide roller group corresponding with a blowing running roller and a rewinding running roller respectively, often group drives guide roller wheels to include a blowing and drives a guide roller I and rewinding driving guide roller II, blowing drives guide roller I to be arranged between blowing running roller and well heater, and rewinding drives guide roller II to be arranged between cooling body and rewinding running roller.
Further, described blowing drives guide roller I to include one group and turns to running roller to roller wheel and one.
Further, described cooling system is water-cooling system, air cooling system or liquid nitrogen cooling system.
Further, described device also includes the vacuumometer be arranged on rack.
Further, described rack is provided with pressure release orifice.
Further, described vertical reaction chamber is made up of high-temperature stable tubing, and the length of vertical reaction chamber is 10mm to 5000mm.
Further, described high-temperature stable tubing is silica tube or alundum tube.
Further, described well heater is provided with the temperature regulator of more than a section, every section of all corresponding temperature-measuring heat couple installed on the heaters of temperature regulator.
Owing to have employed technique scheme, the present invention has following advantage:
During work, substrate twists on blowing running roller, the termination of substrate is connected on rewinding running roller through vertical reaction chamber, vacuum pump group provides the reaction conditions of vacuum for vertical reaction chamber, admission gear provides graphene growth reactant gases to vertical reaction chamber, and well heater provides temperature condition for graphene growth.After the growth conditions met, substrate is growing graphene in vertical reaction chamber, after graphene growth, blowing running roller and rewinding running roller synchronous axial system, the substrate that grown Graphene is rolled onto on rewinding running roller, the substrate of non-growing graphene enters vertical reaction chamber, carries out graphene growth cultivation.The invention solves current big area, high-quality graphene preparation need be carried out under the high temperature of growth substrate melting temperature 1000 DEG C; be not suitable for continuously, bottleneck problem prepared by mass-producing; growth substrate after entering vertical reaction chamber except by except gravity; avoid other to pull external force, guarantee growth substrate complete, stable growing graphene at high temperature.
Other advantages of the present invention, target and feature will be set forth to a certain extent in the following description, and to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, or can be instructed from the practice of the present invention.Target of the present invention and other advantages can be realized by specification sheets below and claims and be obtained.
Accompanying drawing explanation
Accompanying drawing of the present invention is described as follows.
Fig. 1 is structural representation of the present invention.
In figure: 1. vacuum chamber; 2. rack; 3. blowing running roller; 4. rewinding running roller; 5. well heater; 6. vertical reaction chamber; 7. cooling body; 8. vacuum pump group; 9. inlet pipe; 10. mixing chamber; 11. escape pipes; 12. blowings drive guide roller I; 13. rewindings drive guide roller II; 14. temperature-measuring heat couples; 15. vacuumometers; 16. pressure release orifices; 17. substrates.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
The device of continuous growing graphene under a kind of high temperature, the sealing cabinet 2 of vacuum chamber 1 is established in including, volume has the blowing running roller 3 of substrate, for furling the rewinding running roller 4 of substrate 17 and the interior well heater 5 establishing vertical substrate channel, described blowing running roller 3, rewinding running roller 4 and well heater 5 are installed in vacuum chamber 1, be provided with for the vertical reaction chamber 6 through substrate in the substrate channel of well heater 5, rack 2 is provided with the admission gear being communicated to vertical reaction chamber 6, the cooling body 7 for cooling substrate 17 is also provided with between well heater 5 and rewinding running roller 4, described device also includes the vacuum pump group 8 for vacuumizing to vacuum chamber 1.Blowing running roller 3 can be arranged to initiatively and passive rotation, and the present embodiment selects the mode of active rotation.
During work, substrate twists on blowing running roller 3, the termination of substrate is connected on rewinding running roller 4 through vertical reaction chamber 6, vacuum pump group 8 provides the reaction conditions of vacuum for vertical reaction chamber 6, admission gear provides graphene growth reactant gases to vertical reaction chamber 6, and well heater 5 provides temperature condition for graphene growth.After the growth conditions met, substrate is 6 growing graphenes in vertical reaction chamber, after graphene growth, blowing running roller 3 and rewinding running roller 4 synchronous axial system, the substrate that grown Graphene be rolled onto on rewinding running roller 4, the substrate of non-growing graphene enters vertical reaction chamber 6, carries out graphene growth cultivation, according to running roller rotating manner, roller uniform rotation mode also can be adopted to grow.The invention solves current big area, high-quality graphene preparation need be carried out under the high temperature of growth substrate melting temperature 1000 DEG C; be not suitable for continuously, bottleneck problem prepared by mass-producing; growth substrate after entering vertical reaction chamber except by except gravity; avoid other to pull external force, guarantee growth substrate complete, stable growing graphene at high temperature.
Described admission gear includes three tunnel inlet pipe, 9, mixing chamber 10 and escape pipe 11, a three tunnel inlet pipe is communicated to mixing chamber 10, and mixing chamber 10 is communicated in vertical reaction chamber 6 by escape pipe 11.As required, the quantity of inlet pipe 9 can also be adjusted, import after multiple gases mixing in vertical reaction chamber 6.Described admission gear accurately controls each road gas flow by proton stream amount controller, all uniform air inlet of inlet pipe 9 and escape pipe 11 and giving vent to anger.Escape pipe stretches in vertical reaction chamber 6, and has little production well at different depths place, ensures gas distribution uniformity in vertical reaction chamber 6.
Described device also includes the driving guide roller wheels of more than a group led for substrate 17, often drive guide roller group corresponding with a blowing running roller 3 and a rewinding running roller 4 respectively, often group drives guide roller wheels to include a blowing and drives a guide roller I12 and rewinding driving guide roller II13, blowing drives guide roller I12 to be arranged between blowing running roller 3 and well heater 5, and rewinding drives guide roller II13 to be arranged between cooling body 7 and rewinding running roller 4.Blowing drives guide roller I12, rewinding drives guide roller II13, blowing running roller 3 and rewinding running roller 4 synchronous axial system, growth substrate 14 can run growth under the high temperature conditions continuously, depend on that blowing running roller 3 and blowing drive guide roller I12 growth substrate 14 to be dominated in vertical reaction chamber 6, guide roller II13 synchronization steering is driven through rewinding after going out vertical reaction chamber 6, again by the synchronous rolling of rewinding running roller 4, avoid substrate 17 except gravity, be subject to other external force under the high temperature conditions to pull and the problem ruptured, achieve the possibility that substrate 17 is at high temperature rotated continuously.Often group drives the corresponding one group of substrate 17 of guide roller wheels, independent growth continuously while simultaneously can realizing 1 group to 100 groups substrate 17 as required, and then improves graphene growth output.Rewinding drives guide roller II13 can be water cooled rolls or non-water cooled rolls, is preferably water cooled rolls.
Described blowing drives guide roller I12 to include one group and turns to running roller to roller wheel and one.
Described cooling system 7 is water-cooling system, air cooling system or liquid nitrogen cooling system.Be preferably water-cooling system.
Described device also includes the vacuumometer 15 be arranged on rack 2.
Described rack 2 is provided with pressure release orifice 16.
Described vertical reaction chamber is made up of high-temperature stable tubing, and the length of vertical reaction chamber is 10mm to 5000mm, and preferred length is 1000mm.
Described high-temperature stable tubing is silica tube or alundum tube.The present embodiment Choice of Quartz Tube Diameters.
Described well heater 5 is provided with the temperature regulator of more than a section, every section of all corresponding temperature-measuring heat couple 14 be arranged on well heater 5 of temperature regulator.The present embodiment selects five sections of temperature regulators and five temperature-measuring heat couples 14.Temperature-measuring heat couple is for monitoring, feeding back the temperature in vertical reaction chamber, and temperature regulator is for realizing the accurate control of vertical reaction chamber.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of the technical program, it all should be encompassed in the middle of right of the present invention.
Claims (8)
1. the device of continuous growing graphene under a high temperature, it is characterized in that: the sealing cabinet establishing vacuum chamber in described device includes, volume has the blowing running roller of substrate, for furling the rewinding running roller of substrate and the interior well heater establishing vertical substrate channel, described blowing running roller, rewinding running roller and well heater are installed in vacuum chamber, be provided with for the vertical reaction chamber through substrate in the substrate channel of well heater, rack is provided with the admission gear being communicated to vertical reaction chamber, the cooling body for cooling substrate is also provided with between well heater and rewinding running roller, described device also includes for the vacuum pump group of vacuum chamber, described admission gear includes three tunnel inlet pipe, a mixing chamber and an escape pipe, and three tunnel inlet pipe are communicated to mixing chamber, and mixing chamber is communicated in vertical reaction chamber by escape pipe, and three tunnel inlet pipe are accurately controlled by proton stream amount controller, described escape pipe stretches in vertical reaction chamber, and has little production well at different depths place, ensures gas distribution uniformity in vertical reaction chamber, described device also includes the driving guide roller wheels for more than substrate-guided a group, often drives guide roller group corresponding with a blowing running roller and a rewinding running roller respectively, and often group drives guide roller wheels to include a blowing and drives guide roller
guide roller is driven with a rewinding
, blowing drives guide roller
be arranged between blowing running roller and well heater, rewinding drives guide roller
be arranged between cooling body and rewinding running roller.
2. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, is characterized in that: described blowing drives guide roller
include one group and running roller is turned to roller wheel and one.
3. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, is characterized in that: described cooling system is water-cooling system, air cooling system or liquid nitrogen cooling system.
4. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, is characterized in that: described device also includes the vacuumometer be arranged on rack.
5. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, is characterized in that: on described rack, be provided with pressure release orifice.
6. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, it is characterized in that: described vertical reaction chamber is made up of high-temperature stable tubing, the length of vertical reaction chamber is 10mm to 5000mm.
7. the device of continuous growing graphene under a kind of high temperature as claimed in claim 6, is characterized in that: described high-temperature stable tubing is silica tube or alundum tube.
8. the device of continuous growing graphene under a kind of high temperature as claimed in claim 1, is characterized in that: the temperature regulator being provided with more than a section on described well heater, every section of all corresponding temperature-measuring heat couple installed on the heaters of temperature regulator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310270021.0A CN103305806B (en) | 2013-06-28 | 2013-06-28 | Device for continuously growing graphene at high temperature |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310270021.0A CN103305806B (en) | 2013-06-28 | 2013-06-28 | Device for continuously growing graphene at high temperature |
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| CN103305806A CN103305806A (en) | 2013-09-18 |
| CN103305806B true CN103305806B (en) | 2015-06-03 |
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| CN201310270021.0A Expired - Fee Related CN103305806B (en) | 2013-06-28 | 2013-06-28 | Device for continuously growing graphene at high temperature |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104152844A (en) * | 2014-08-11 | 2014-11-19 | 江南石墨烯研究院 | Method for carrying substrate in vacuum |
| KR101938874B1 (en) * | 2016-07-20 | 2019-01-15 | 주식회사 참트론 | The heat-treatment device for synthesis of high quality graphene |
| CN106829936B (en) * | 2017-03-27 | 2020-06-19 | 重庆墨希科技有限公司 | Horizontal type graphene roll-to-roll continuous growth equipment |
| CN106756896A (en) * | 2017-03-27 | 2017-05-31 | 重庆墨希科技有限公司 | The continuous growth apparatus of vertical graphite alkene volume to volume |
| CN107217240A (en) * | 2017-07-11 | 2017-09-29 | 江苏星特亮科技有限公司 | Preparation method of graphene film |
| CN107459033A (en) * | 2017-07-11 | 2017-12-12 | 江苏星特亮科技有限公司 | Method for preparing graphene film |
| CN110759648A (en) * | 2018-07-25 | 2020-02-07 | 张文跃 | Graphene wire-plated coiled material preparation device and production process |
| CN109336096B (en) | 2018-10-19 | 2023-09-26 | 深圳市纳设智能装备有限公司 | Equipment for open type continuous growth of carbon nano material and preparation method |
| CN109680259B (en) * | 2019-02-18 | 2023-11-03 | 安徽贝意克设备技术有限公司 | Vertical continuous PE reinforcing roll-to-roll graphene film growth equipment |
| CN112553601A (en) * | 2020-12-04 | 2021-03-26 | 安徽贝意克设备技术有限公司 | Roll-to-roll chemical vapor deposition equipment |
| CN115608292A (en) * | 2022-09-27 | 2023-01-17 | 青岛科技大学 | Internal heat source reactor |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4250148A (en) * | 1978-07-18 | 1981-02-10 | Motorola, Inc. | Apparatus and method for producing polycrystalline ribbon |
| US4900531A (en) * | 1982-06-22 | 1990-02-13 | Harry Levin | Converting a carbon preform object to a silicon carbide object |
| CN101629283B (en) * | 2009-07-16 | 2011-04-27 | 江苏双登集团有限公司 | Roll-to-roll plasma device for enhancing chemical vapor deposition |
| CN102976317B (en) * | 2012-12-21 | 2014-12-24 | 重庆墨希科技有限公司 | Large-scale graphene preparation process |
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2013
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