CN104495815B - A kind of device and method using carbon dioxide to prepare Graphene - Google Patents
A kind of device and method using carbon dioxide to prepare Graphene Download PDFInfo
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- CN104495815B CN104495815B CN201410767657.0A CN201410767657A CN104495815B CN 104495815 B CN104495815 B CN 104495815B CN 201410767657 A CN201410767657 A CN 201410767657A CN 104495815 B CN104495815 B CN 104495815B
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Abstract
The present invention relates to technical field of graphene preparation, particularly relate to a kind of device and method using carbon dioxide to prepare Graphene.Carbon dioxide is used to prepare the device of Graphene, including heating furnace, growth chamber, air inlet pipe, exhaustor, graphene growth substrate and activated carbon, the middle part of described growth chamber is positioned at described heating furnace, described heating furnace is stretched out at the two ends of described growth chamber respectively, described air inlet pipe all connects and is respectively provided at the two ends of described growth chamber with described growth chamber with described exhaustor, described graphene growth substrate is located at the inside in the middle part of described growth chamber, and described activated carbon is located between the inside in the middle part of growth chamber, described growth substrate and described air inlet pipe.The invention has the beneficial effects as follows: present invention achieves employing carbon dioxide and prepare Graphene as carbon source, it is to avoid use that methane, ethylene, acetylene etc. are inflammable, explosion hazard gases prepares the unsafe factor during Graphene as carbon source.
Description
Technical field
The present invention relates to technical field of graphene preparation, particularly relate to a kind of employing carbon dioxide and prepare graphite
The device and method of alkene.
Background technology
Graphene is the two-dimentional new material of single carbon atom thickness, in mechanics, calorifics, optics, electricity etc.
Aspect is respectively provided with the most excellent character, such as the mechanical strength of superelevation, good heat conductivity, wide spectrum height
Transparency and superpower electric conductivity etc..Before the physical property of Graphene uniqueness determines its wide application
Scape, has caused the research boom of international academic community and industrial quarters.It is applied to flexible transparent electrode, then
The light transmittance of device is higher, electric conductivity more preferable, power consumption is lower, is expected to replace the ITO that existing market is leading
Transparency electrode, is widely used in the optoelectronic device such as Flexible Displays and touch screen.Graphene is used for manufacturing photon
Sensor and photodetector, sensitivity improves several orders of magnitude than similar detector.Graphene also may be used
As the stock of nanoelectronic integrated device of future generation, the device speed of service is made to be up to 500GHz, and
The existing device of observable index significantly reduces.Additionally, Graphene still can play important in other sides such as medical treatment
Effect.
Widely studied through in recent years, chemical vapour deposition technique (CVD) is to prepare graphene film
One of promising method.CVD is the carbon sources such as methane to be heated under specified temp in Dewar vessel
Make it decompose, on the transition metal paper tinsels such as Ni, Cu, then form the technology of graphene film.But, existing
Prepare Graphene commonly using carbon source at CVD is the sources of the gas inflammable, explosive such as methane, ethylene, acetylene, the most right
Bring unsafe factor during commercial production Graphene, and air can be polluted by tail gas, does not reaches
Green, environmental protection Production requirement.
Summary of the invention
The technical problem to be solved is to provide in one the dress using carbon dioxide to prepare Graphene
Put and method, it is to avoid prior art uses the source of the gas conducts inflammable, explosive such as methane, ethylene, acetylene
Carbon source is to bringing unsafe factor in production process.
The technical scheme is that a kind of employing carbon dioxide prepares graphite
The device of alkene, including heating furnace, growth chamber, air inlet pipe, exhaustor, graphene growth substrate and work
Property charcoal, the middle part of described growth chamber is positioned at described heating furnace, and the two ends of described growth chamber are stretched respectively
Going out described heating furnace, described air inlet pipe all connects and is respectively provided at described growth chamber with described exhaustor
The two ends of described growth chamber, described graphene growth substrate is located at the inside in the middle part of described growth chamber,
Described activated carbon be located at the inside in the middle part of described growth chamber, described growth substrate and described air inlet pipe it
Between.
Further, described exhaustor connects exhaust gas processing device away from one end of described growth chamber.
Further, described exhaustor is provided with vacuum pump, described vacuum pump away from one end of described growth chamber
Air inlet connect described exhaustor, the gas outlet of described vacuum pump connects described vent gas treatment by pipeline
Device.
Further, described growth chamber is quartz ampoule or earthenware.
Further, described graphene growth substrate be copper, nickel, ferrum, cobalt, platinum, the one of ruthenium or its
Meaning combination.
Further, the thickness of described graphene growth substrate is 10-200 micron.
Further, described graphene growth substrate is 45 microns of thick Copper Foils.
A kind of method using carbon dioxide to prepare Graphene, the method is by using such as claim 1-7
Device described in any one realizes preparing Graphene, comprises the following steps:
Step one, puts into the inside in the middle part of growth chamber, described work by activated carbon, graphene growth substrate
Property charcoal is placed between described air inlet pipe and described graphene growth substrate；
Step 2, the foreign gas in growth chamber of draining, by heating furnace, the middle part of growth chamber is added
Heat, makes growth chamber internal temperature reach 500-1200 DEG C；
Step 3, is passed through catalysis gas and carbon dioxide from air inlet pipe, in graphene growth substrate
Growth Graphene.
Further, the method for the foreign gas drained in described growth chamber in described step 2 is for from air inlet
Pipe is passed through noble gas in growth chamber, and from exhaustor, foreign gas is discharged (growth at atmosphere graphite
Alkene).
Further, the method for the foreign gas drained in described growth chamber in described step 2 is, opens
Vacuum pump extracts the gas (low-pressure growth Graphene) in growth chamber out.
Further, described catalysis gas is hydrogen, and noble gas is argon and/or nitrogen and/or helium.
The invention has the beneficial effects as follows: present invention achieves employing carbon dioxide and prepare graphite as carbon source
Alkene, it is to avoid employing methane, ethylene, acetylene etc. are inflammable, explosion hazard gases prepares Graphene mistake as carbon source
Unsafe factor in journey, and tail gas being processed by exhaust gas processing device, it is to avoid production process
Air is polluted by the tail gas of middle discharge, reaches green, the demand of environmental protection production.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of device using carbon dioxide to prepare Graphene of the present invention；
Fig. 2 is a kind of flow chart using carbon dioxide to prepare Graphene of the present invention；
In accompanying drawing, the list of parts representated by each label is as follows:
1, heating furnace, 2, growth chamber, 3, air inlet pipe, 4, exhaustor, 5, graphene growth base
The end, 6, activated carbon, 7, exhaust gas processing device, 8, vacuum pump.
Detailed description of the invention
Being described principle and the feature of the present invention below in conjunction with accompanying drawing, example is served only for explaining this
Invention, is not intended to limit the scope of the present invention.
As it is shown in figure 1, plant the device using carbon dioxide to prepare Graphene, including heating furnace 1, growth
Cavity 2, air inlet pipe 3, exhaustor 4, graphene growth substrate 5 and activated carbon 6, described growth chamber
The middle part of 2 is positioned at described heating furnace 1, and described heating furnace is stretched out at the two ends of described growth chamber 2 respectively
1, described air inlet pipe 3 all connects and is respectively provided at described growth chamber 2 with described exhaustor 4 described
The two ends of growth chamber 2, described graphene growth substrate 5 is located at the inside in the middle part of described growth chamber 2,
Described activated carbon 6 is located at the inside in the middle part of described growth chamber 2, described graphene growth substrate 5 and institute
State between air inlet pipe 3.
Described exhaustor 4 connects exhaust gas processing device 7 away from one end of described growth chamber 2.Described row
Trachea 4 is provided with vacuum pump 8 away from one end of described growth chamber 2, and the air inlet of described vacuum pump 8 is even
Connecing described exhaustor 4, the gas outlet of described vacuum pump 8 connects described exhaust gas processing device 7 by pipeline.
Described growth chamber 2 is quartz ampoule or earthenware.Described graphene growth substrate 5 be copper, nickel, ferrum,
Cobalt, platinum, the one of ruthenium or its combination in any.The thickness of described graphene growth substrate 5 is 10-200
Micron.
As in figure 2 it is shown, a kind of method using carbon dioxide to prepare Graphene, specifically include following enforcement
Example:
Embodiment one
6,45 microns of thick Copper Foils of activated carbon are put into the inside in the middle part of growth chamber 2, institute by step one
State activated carbon 6 to be placed between described air inlet pipe 3 and described Copper Foil；
Step 2, is passed through argon from air inlet pipe 3 and drains the foreign gases such as growth chamber 2 inner air, and
By heating furnace 1, the middle part of growth chamber 2 is heated, make growth chamber 2 internal temperature reach 500 DEG C；
Step 3, is passed through hydrogen and carbon dioxide from air inlet pipe 3, grows Graphene on Copper Foil.
Embodiment two
6,45 microns of thick Copper Foils of activated carbon are put into the inside in the middle part of growth chamber 2, institute by step one
State activated carbon 6 to be placed between described air inlet pipe 3 and described Copper Foil；
Step 2, opens exhaustor 4, opens vacuum pump 8 and takes out growth chamber to background vacuum 0.1Pa
After, by heating furnace 1, the middle part of growth chamber 2 is heated, make growth chamber 2 internal temperature reach 1200
℃；
Step 3, is passed through hydrogen and carbon dioxide from air inlet pipe 3, grows Graphene on Copper Foil.
Embodiment three
6,45 microns of thick Copper Foils of activated carbon are put into growth chamber 2 internal, described activity by step one
Charcoal 6 is placed between described air inlet pipe 3 and described Copper Foil；
Step 2, is passed through nitrogen from air inlet pipe 3 and drains the foreign gases such as growth chamber 2 inner air, and
By heating furnace 1, the middle part of growth chamber 2 is heated, make growth chamber 2 internal temperature reach 800 DEG C；
Step 3, is passed through hydrogen and carbon dioxide from air inlet pipe 3, grows Graphene on Copper Foil.
Embodiment four
6,45 microns of thick Copper Foils of activated carbon are put into growth chamber 2 internal, described activity by step one
Charcoal 6 is placed between described air inlet pipe 3 and described Copper Foil；
Step 2, is passed through helium from air inlet pipe 3 and drains the foreign gases such as growth chamber 2 inner air, and
By heating furnace 1, the middle part of growth chamber 2 is heated, make growth chamber 2 internal temperature reach 1000
℃；
Step 3, is passed through hydrogen and carbon dioxide from air inlet pipe 3, grows Graphene on Copper Foil.
Operation principle: air inlet pipe 3 is connected simultaneously catalysis gas pipeline and carbon dioxide gas line, to
It is passed through catalysis gas and carbon dioxide in growth chamber 2, by heating furnace 1, growth chamber 2 is added
Heat, makes growth chamber 2 internal temperature reach 500-1200 DEG C, and carbon dioxide is in growth chamber 2
Generating CO (carbon monoxide converter) gas with activated carbon 6 reaction under interior hot environment, CO (carbon monoxide converter) gas is at catalysis gas
Under the effect of body, graphene growth substrate 5 grows Graphene, during preparing Graphene,
The unnecessary gas being passed in growth chamber 2 can be discharged from exhaustor 4, fills subsequently into vent gas treatment
Put 7 to process, it is to avoid hydrogen and CO (carbon monoxide converter) gas enter contaminated air in air.Preparing graphite
Vacuum pump 8 can be opened, it is achieved under lower pressure, use carbon dioxide to prepare uniform graphite during alkene
Alkene thin film, and improve the air inflow of carbon dioxide, increase carbon dioxide and activated carbon 6 reaction generates an oxygen
Change the speed of carbon, improve the sedimentation rate of Graphene.
The invention has the beneficial effects as follows: present invention achieves employing carbon dioxide and prepare graphite as carbon source
Alkene, it is to avoid employing methane, ethylene, acetylene etc. are inflammable, explosion hazard gases prepares Graphene mistake as carbon source
Unsafe factor in journey, and tail gas being processed by exhaust gas processing device, it is to avoid production process
Air is polluted by the tail gas of middle discharge, reaches green, the demand of environmental protection production.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention
Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this
Within bright protection domain.
Claims (10)
1. one kind uses the device that carbon dioxide prepares Graphene, it is characterised in that include heating furnace (1),
Growth chamber (2), air inlet pipe (3), exhaustor (4), graphene growth substrate (5) and activity
Charcoal (6), the middle part of described growth chamber (2) is positioned at described heating furnace (1), described growth chamber
The two ends of body (2) stretch out described heating furnace (1), described air inlet pipe (3) and described exhaustor respectively
(4) all connect and be respectively provided at the two ends of described growth chamber (2) with described growth chamber (2),
Described graphene growth substrate (5) is located at the inside at described growth chamber (2) middle part, described activated carbon
(6) inside, described graphene growth substrate (5) and the institute at described growth chamber (2) middle part it are located at
State between air inlet pipe (3).
A kind of device using carbon dioxide to prepare Graphene the most according to claim 1, it is special
Levying and be, described exhaustor (4) connects exhaust gas processing device away from one end of described growth chamber (2)
(7)。
A kind of device using carbon dioxide to prepare Graphene the most according to claim 2, it is special
Levying and be, described exhaustor (4) is provided with vacuum pump (8) away from one end of described growth chamber (2),
The air inlet of described vacuum pump (8) connects described exhaustor (4), giving vent to anger of described vacuum pump (8)
Mouth connects described exhaust gas processing device (7) by pipeline.
4. use carbon dioxide to prepare Graphene according to a kind of described in any one of claims 1 to 3
Device, it is characterised in that described graphene growth substrate (5) is copper, nickel, ferrum, cobalt, platinum, ruthenium
One or its combination in any.
A kind of device using carbon dioxide to prepare Graphene the most according to claim 4, it is special
Levying and be, the thickness of described graphene growth substrate (5) is 10-200 micron.
A kind of device using carbon dioxide to prepare Graphene the most according to claim 5, it is special
Levying and be, described graphene growth substrate (5) is 45 microns of thick Copper Foils.
7. one kind uses the method that carbon dioxide prepares Graphene, it is characterised in that the method is by making
Realize preparing Graphene with the device as described in any one of claim 1-6, comprise the following steps:
Step one, puts into activated carbon (6), graphene growth substrate (5) in growth chamber (2)
The inside in portion, described activated carbon (6) is placed on described air inlet pipe (3) and described graphene growth substrate
(5) between；
Step 2, the foreign gas in growth chamber of draining (2), by heating furnace (1) to growth chamber
The middle part heating of body (2), makes growth chamber (2) internal temperature reach 500-1200 DEG C；
Step 3, is passed through catalysis gas and carbon dioxide from air inlet pipe (3), in graphene growth
Graphene is grown in substrate.
A kind of method using carbon dioxide to prepare Graphene the most according to claim 7, it is special
Levying and be, the method for the foreign gas in described growth chamber of draining in described step 2 (2) is for passing through
Air inlet pipe (3) is passed through noble gas in growth chamber (2), by foreign gas from exhaustor (4)
Discharge.
A kind of method using carbon dioxide to prepare Graphene the most according to claim 7, it is special
Levying and be, the method for the foreign gas in described growth chamber of draining in described step 2 (2) is for opening
Vacuum pump (8) extracts the gas in growth chamber (2) out, and whole process opens vacuum pump (8).
A kind of method using carbon dioxide to prepare Graphene the most according to claim 8, it is special
Levying and be, described catalysis gas is hydrogen, and described noble gas is argon and/or helium.
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| CN104495815B true CN104495815B (en) | 2016-09-21 |
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| CN102092710B (en) * | 2010-12-17 | 2013-01-23 | 中国科学院化学研究所 | Regular graphene and preparation method thereof |
| US8865113B2 (en) * | 2011-03-15 | 2014-10-21 | 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 |
| CN103145117B (en) * | 2013-02-28 | 2015-06-10 | 中国科学院化学研究所 | Method for preparing graphene |
| CN103303913B (en) * | 2013-07-05 | 2015-10-07 | 中国科学院宁波材料技术与工程研究所 | A kind of porous graphene and preparation method thereof, ultracapacitor |
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