CN104495815A - Device and method for preparing graphene from carbon dioxide - Google Patents

Device and method for preparing graphene from carbon dioxide Download PDF

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CN104495815A
CN104495815A CN201410767657.0A CN201410767657A CN104495815A CN 104495815 A CN104495815 A CN 104495815A CN 201410767657 A CN201410767657 A CN 201410767657A CN 104495815 A CN104495815 A CN 104495815A
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graphene
growth chamber
gas
carbonic acid
acid gas
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CN104495815B (en
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李占成
张永娜
高翾
朱鹏
姜浩
黄德萍
邵丽
史浩飞
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Chongqing Institute of Green and Intelligent Technology of CAS
Chongqing Graphene Technology Co Ltd
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Chongqing Institute of Green and Intelligent Technology of CAS
Chongqing Graphene Technology Co Ltd
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Abstract

The invention relates to the technical field of graphene preparation and in particular relates to a device and a method for preparing graphene from carbon dioxide. The device for preparing the graphene from the carbon dioxide comprises a heating furnace, a growing chamber, an intake pipe, an exhaust pipe, a graphene growing substrate and activated carbon, wherein the middle of the growing chamber is located in the heating furnace; the two ends of the growing chamber extend out of the heating furnace, respectively; the intake pipe and the exhaust pipe both are communicated with the growing chamber and arranged at the two ends of the growing chamber, respectively; the graphene growing substrate is arranged inside the middle of the growing chamber; the activated carbon is arranged inside the middle of the growing chamber and between the growing substrate and the intake pipe. According to the device and the method for preparing the graphene from the carbon dioxide, the carbon dioxide is taken as the carbon source to prepare the graphene, and unsafe factors in the process of preparing the graphene by taking flammable and combustible gases such as methane, ethylene and acetylene as the carbon sources are avoided.

Description

A kind of device and method adopting carbonic acid gas to prepare Graphene
Technical field
The present invention relates to technical field of graphene preparation, particularly relate to a kind of device and method adopting carbonic acid gas to prepare Graphene.
Background technology
Graphene is the two-dimentional novel material of single carbon atom thickness, in mechanics, calorifics, optics, electricity etc., all have very excellent character, as the physical strength of superelevation, good thermal conductivity, wide spectrum high-clarity and superpower electroconductibility etc.The physical properties of Graphene uniqueness determines its wide application prospect, has caused the research boom of international academic community and industry member.Be applied to flexible transparent electrode, then the transmittance of device is stronger, electroconductibility is better, power consumption is lower, is expected to replace the leading ito transparent electrode of existing market, is widely used in the optoelectronic device such as Flexible Displays and touch-screen.Graphene is for the manufacture of photon sensor and photodetector, and the comparable similar detector of sensitivity improves several order of magnitude.Graphene also can be used as the basic material of nanoelectronic integrated device of future generation, makes device travelling speed up to 500GHz, and the existing device of observable index significantly reduces.In addition, Graphene still can play an important role in other sides such as medical treatment.
Through extensive research in recent years, chemical Vapor deposition process (CVD) prepares one of the most promising method of graphene film.CVD makes it decompose under the carbon sources such as methane being heated to specified temp in vacuum vessel, on the transition metal paper tinsels such as Ni, Cu, then form the technology of graphene film.But present CVD prepares Graphene, and to commonly use carbon source be inflammable, the explosive sources of the gas such as methane, ethene, acetylene, and not only to bringing unsafe factor in industrial production Graphene process, and tail gas can pollute air, does not reach green, environmental protection Production requirement.
Summary of the invention
Technical problem to be solved by this invention is to provide in one the apparatus and method adopting carbonic acid gas to prepare Graphene, avoids in prior art inflammable, explosive sources of the gas such as adopting methane, ethene, acetylene and brings unsafe factor as carbon source in production process.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of device adopting carbonic acid gas to prepare Graphene, comprise process furnace, growth chamber, inlet pipe, vapor pipe, graphene growth substrate and gac, the middle part of described growth chamber is positioned at described process furnace, described process furnace is stretched out at the two ends of described growth chamber respectively, described inlet pipe and described vapor pipe are all communicated with described growth chamber and are located at the two ends of described growth chamber respectively, described graphene growth substrate is located at the inside in the middle part of described growth chamber, described gac is located at the inside in the middle part of described growth chamber, between described growth substrate and described inlet pipe.
Further, described vapor pipe connects exhaust gas processing device away from one end of described growth chamber.
Further, described vapor pipe is provided with vacuum pump away from one end of described growth chamber, and the inlet mouth of described vacuum pump connects described vapor pipe, and the air outlet of described vacuum pump connects described exhaust gas processing device by pipeline.
Further, described growth chamber is silica tube or vitrified pipe.
Further, described graphene growth substrate is copper, nickel, iron, cobalt, platinum, the one of ruthenium or its arbitrary combination.
Further, the thickness of described graphene growth substrate is 10-200 micron.
Further, described graphene growth substrate is the Copper Foil of 45 micron thickness.
Adopt carbonic acid gas to prepare a method for Graphene, the method realizes preparing Graphene by using the device as described in any one of claim 1-7, comprises the following steps:
Step one, gac, graphene growth substrate are put into the inside in the middle part of growth chamber, described gac is placed between described inlet pipe and described graphene growth substrate;
Step 2, the foreign gas of draining in growth chamber, is heated the middle part of growth chamber by process furnace, makes growth chamber internal temperature reach 500-1200 DEG C;
Step 3, passes into catalytic gas and carbon dioxide from inlet pipe, growing graphene in graphene growth substrate.
Further, foreign gas, for pass into rare gas element from inlet pipe in growth chamber, is discharged (growth at atmosphere Graphene) from vapor pipe by the method for a kind of foreign gas of draining in described growth chamber of described step.
Further, the method for a kind of foreign gas of draining in described growth chamber of described step is, opens the gas (low-pressure growth Graphene) in vacuum pump extraction growth chamber.
Further, described catalytic gas is hydrogen, and rare gas element is argon gas and/or nitrogen and/or helium.
The invention has the beneficial effects as follows: present invention achieves and adopt carbonic acid gas to prepare Graphene as carbon source, avoid and adopt that methane, ethene, acetylene etc. are inflammable, explosion hazard gases prepares unsafe factor in Graphene process as carbon source, and by exhaust gas processing device, tail gas is processed, avoid the tail gas of discharging in production process to pollute air, reach the demand of green, environmental protection production.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation adopting carbonic acid gas to prepare the device of Graphene of the present invention;
Fig. 2 is a kind of schema adopting carbonic acid gas to prepare Graphene of the present invention;
In accompanying drawing, the list of parts representated by each label is as follows:
1, process furnace, 2, growth chamber, 3, inlet pipe, 4, vapor pipe, 5, graphene growth substrate, 6, gac, 7, exhaust gas processing device, 8, vacuum pump.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
As shown in Figure 1, plant the device adopting carbonic acid gas to prepare Graphene, comprise process furnace 1, growth chamber 2, inlet pipe 3, vapor pipe 4, graphene growth substrate 5 and gac 6, the middle part of described growth chamber 2 is positioned at described process furnace 1, described process furnace 1 is stretched out at the two ends of described growth chamber 2 respectively, described inlet pipe 3 and described vapor pipe 4 are all communicated with described growth chamber 2 and are located at the two ends of described growth chamber 2 respectively, described graphene growth substrate 5 is located at the inside in the middle part of described growth chamber 2, described gac 6 is located at the inside in the middle part of described growth chamber 2, between described graphene growth substrate 5 and described inlet pipe 3.
Described vapor pipe 4 connects exhaust gas processing device 7 away from one end of described growth chamber 2.Described vapor pipe 4 is provided with vacuum pump 8 away from one end of described growth chamber 2, and the inlet mouth of described vacuum pump 8 connects described vapor pipe 4, and the air outlet of described vacuum pump 8 connects described exhaust gas processing device 7 by pipeline.Described growth chamber 2 is silica tube or vitrified pipe.Described graphene growth substrate 5 is copper, nickel, iron, cobalt, platinum, the one of ruthenium or its arbitrary combination.The thickness of described graphene growth substrate 5 is 10-200 micron.
As shown in Figure 2, a kind of method adopting carbonic acid gas to prepare Graphene, specifically comprises following examples:
Embodiment one
Step one, puts into the inside in the middle part of growth chamber 2 by the Copper Foil of gac 6,45 micron thickness, and described gac 6 is placed between described inlet pipe 3 and described Copper Foil;
Step 2, is passed into argon gas from inlet pipe 3 and to drain the foreign gases such as growth chamber 2 inner air, and heated by the middle part of process furnace 1 pair of growth chamber 2, make growth chamber 2 internal temperature reach 500 DEG C;
Step 3, passes into hydrogen and carbon dioxide from inlet pipe 3, growing graphene on Copper Foil.
Embodiment two
Step one, puts into the inside in the middle part of growth chamber 2 by the Copper Foil of gac 6,45 micron thickness, and described gac 6 is placed between described inlet pipe 3 and described Copper Foil;
Step 2, opens vapor pipe 4, after growth chamber to background vacuum 0.1Pa taken out by unlatching vacuum pump 8, is heated, make growth chamber 2 internal temperature reach 1200 DEG C by the middle part of process furnace 1 pair of growth chamber 2;
Step 3, passes into hydrogen and carbon dioxide from inlet pipe 3, growing graphene on Copper Foil.
Embodiment three
Step one, the Copper Foil of gac 6,45 micron thickness is put into growth chamber 2 inner, described gac 6 is placed between described inlet pipe 3 and described Copper Foil;
Step 2, is passed into nitrogen from inlet pipe 3 and to drain the foreign gases such as growth chamber 2 inner air, and heated by the middle part of process furnace 1 pair of growth chamber 2, make growth chamber 2 internal temperature reach 800 DEG C;
Step 3, passes into hydrogen and carbon dioxide from inlet pipe 3, growing graphene on Copper Foil.
Embodiment four
Step one, the Copper Foil of gac 6,45 micron thickness is put into growth chamber 2 inner, described gac 6 is placed between described inlet pipe 3 and described Copper Foil;
Step 2, is passed into helium from inlet pipe 3 and to drain the foreign gases such as growth chamber 2 inner air, and heated by the middle part of process furnace 1 pair of growth chamber 2, make growth chamber 2 internal temperature reach 1000 DEG C;
Step 3, passes into hydrogen and carbon dioxide from inlet pipe 3, growing graphene on Copper Foil.
Principle of work: inlet pipe 3 is communicated with catalytic gas pipeline and carbon dioxide gas line simultaneously, catalytic gas and carbon dioxide is passed in growth chamber 2, heated by process furnace 1 pair of growth chamber 2, growth chamber 2 internal temperature is made to reach 500-1200 DEG C, react with gac 6 under the hot environment of carbon dioxide in growth chamber 2 and generate CO (carbon monoxide converter) gas, CO (carbon monoxide converter) gas is under the effect of catalytic gas, graphene growth substrate 5 grows Graphene, in the process preparing Graphene, the unnecessary gas be passed in growth chamber 2 can be discharged from vapor pipe 4, then enter exhaust gas processing device 7 to process, hydrogen and CO (carbon monoxide converter) gas is avoided to enter polluted air in air.Vacuum pump 8 can be opened in the process preparing Graphene, carbonic acid gas is adopted to prepare uniform graphene film under realizing lower pressure, and improve the air input of carbonic acid gas, increase the speed of carbonic acid gas and gac 6 reaction generation carbon monoxide, improve the sedimentation rate of Graphene.
The invention has the beneficial effects as follows: present invention achieves and adopt carbonic acid gas to prepare Graphene as carbon source, avoid and adopt that methane, ethene, acetylene etc. are inflammable, explosion hazard gases prepares unsafe factor in Graphene process as carbon source, and by exhaust gas processing device, tail gas is processed, avoid the tail gas of discharging in production process to pollute air, reach the demand of green, environmental protection production.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. the device adopting carbonic acid gas to prepare Graphene, it is characterized in that, comprise process furnace (1), growth chamber (2), inlet pipe (3), vapor pipe (4), graphene growth substrate (5) and gac (6), the middle part of described growth chamber (2) is positioned at described process furnace (1), described process furnace (1) is stretched out at the two ends of described growth chamber (2) respectively, described inlet pipe (3) and described vapor pipe (4) are all communicated with described growth chamber (2) and are located at the two ends of described growth chamber (2) respectively, described graphene growth substrate (5) is located at the inside at described growth chamber (2) middle part, described gac (6) is located at the inside at described growth chamber (2) middle part, between described graphene growth substrate (5) and described inlet pipe (3).
2. a kind of device adopting carbonic acid gas to prepare Graphene according to claim 1, is characterized in that, described vapor pipe (4) connects exhaust gas processing device (7) away from one end of described growth chamber (2).
3. a kind of device adopting carbonic acid gas to prepare Graphene according to claim 2, it is characterized in that, described vapor pipe (4) is provided with vacuum pump (8) away from one end of described growth chamber (2), the inlet mouth of described vacuum pump (8) connects described vapor pipe (4), and the air outlet of described vacuum pump (8) connects described exhaust gas processing device (7) by pipeline.
4. a kind of device adopting carbonic acid gas to prepare Graphene according to any one of claims 1 to 3, is characterized in that, described graphene growth substrate (5) is copper, the one of nickel, iron, cobalt, platinum, ruthenium or its arbitrary combination.
5. a kind of device adopting carbonic acid gas to prepare Graphene according to claim 4, is characterized in that, the thickness of described graphene growth substrate (5) is 10-200 micron.
6. a kind of device adopting carbonic acid gas to prepare Graphene according to claim 5, is characterized in that, described graphene growth substrate (5) is the Copper Foil of 45 micron thickness.
7. adopt carbonic acid gas to prepare a method for Graphene, it is characterized in that, the method realizes preparing Graphene by using the device as described in any one of claim 1-6, comprises the following steps:
Step one, gac (6), graphene growth substrate (5) are put into the inside at growth chamber (2) middle part, described gac (6) is placed between described inlet pipe (3) and described graphene growth substrate (5);
Step 2, the foreign gas in growth chamber of draining (2), is heated the middle part of growth chamber (2) by process furnace (1), makes growth chamber (2) internal temperature reach 500-1200 DEG C;
Step 3, passes into catalytic gas and carbon dioxide from inlet pipe (3), growing graphene in graphene growth substrate.
8. a kind of method adopting carbonic acid gas to prepare Graphene according to claim 7, it is characterized in that, described step one drains the method for the foreign gas in described growth chamber (2) for pass into rare gas element by inlet pipe (3) in growth chamber (2), foreign gas is discharged from vapor pipe (4).
9. a kind of method adopting carbonic acid gas to prepare Graphene according to claim 7, it is characterized in that, the method of the foreign gas that described step one is drained in described growth chamber (2) is open the gas in vacuum pump (8) extraction growth chamber (2), and whole process opens vacuum pump (8).
10. a kind of method adopting carbonic acid gas to prepare Graphene according to claim 7 or 8, it is characterized in that, described catalytic gas is hydrogen, and described rare gas element is argon gas and/or nitrogen and/or helium.
CN201410767657.0A 2014-12-12 2014-12-12 A kind of device and method using carbon dioxide to prepare Graphene Active CN104495815B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102092710A (en) * 2010-12-17 2011-06-15 中国科学院化学研究所 Regular graphene and preparation method thereof
WO2012125854A1 (en) * 2011-03-15 2012-09-20 Peerless Worldwide, Llc Facile synthesis of graphene, graphene derivatives and abrasive nanoparticles and their various uses, including as tribologically-beneficial lubricant additives
CN103145117A (en) * 2013-02-28 2013-06-12 中国科学院化学研究所 Method for preparing graphene
CN103303913A (en) * 2013-07-05 2013-09-18 中国科学院宁波材料技术与工程研究所 Porous graphene, preparation method thereof, and supercapacitor
CN103572247A (en) * 2012-07-27 2014-02-12 中国科学院苏州纳米技术与纳米仿生研究所 Method for preparing thin layer graphene on surface of metal catalyst

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102092710A (en) * 2010-12-17 2011-06-15 中国科学院化学研究所 Regular graphene and preparation method thereof
WO2012125854A1 (en) * 2011-03-15 2012-09-20 Peerless Worldwide, Llc Facile synthesis of graphene, graphene derivatives and abrasive nanoparticles and their various uses, including as tribologically-beneficial lubricant additives
CN103572247A (en) * 2012-07-27 2014-02-12 中国科学院苏州纳米技术与纳米仿生研究所 Method for preparing thin layer graphene on surface of metal catalyst
CN103145117A (en) * 2013-02-28 2013-06-12 中国科学院化学研究所 Method for preparing graphene
CN103303913A (en) * 2013-07-05 2013-09-18 中国科学院宁波材料技术与工程研究所 Porous graphene, preparation method thereof, and supercapacitor

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