CN206502603U - A kind of plasma original position etching and the graphene preparation system of assisting growth - Google Patents
A kind of plasma original position etching and the graphene preparation system of assisting growth Download PDFInfo
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- CN206502603U CN206502603U CN201720140485.3U CN201720140485U CN206502603U CN 206502603 U CN206502603 U CN 206502603U CN 201720140485 U CN201720140485 U CN 201720140485U CN 206502603 U CN206502603 U CN 206502603U
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Abstract
The utility model is related to the technical field of graphene preparation system, is related specifically to a kind of plasma original position etching and the graphene preparation system of assisting growth, it is characterised in that：The system is made up of frame, high temperature process furnances, quartz ampoule, microwave plasma generation device, microwave plasma-etching device, magnetic rod.The quartz ampoule is fixed in frame by supporting mechanism；The high temperature process furnances are connected in frame by sliding rail, are moved radially along quartzy pipe outer wall；The system also includes air inlet group, and the air inlet group includes source of the gas and air inlet quartz ampoule, and during one end of the air inlet quartz ampoule extends to quartz ampoule from quartz ampoule sample introduction end, the other end is connected outside quartz ampoule with source of the gas；The microwave plasma generating means is enclosed in outside the air inlet quartz ampoule outside quartz ampoule；The microwave plasma-etching device is enclosed in outside quartz ampoule, is arranged between magnetic rod and high temperature process furnances.By controlling the number of times of growth and etching, the system can controllably prepare graphene layer with the number of plies.
Description
Technical field
The utility model is related to the technical field of graphene preparation system, is related specifically to a kind of plasma original position etching
With the graphene preparation system of assisting growth.
Background technology
Graphene is with sp between carbon atom2The cellular hexaplanar crystal of hydridization bonding formation, graphene is unique
Crystal structure, make it have excellent mechanics, calorifics, electrical and optical properties, graphene per l00nm distances on can bear
Pressure be about 2.9 μ N, thermal conductivity factor is up to 5300W/mK, and single-layer graphene can absorb about 2.3% visible ray, graphite
The resistivity of alkene about 10-8Ω.cm.Therefore graphene has in fields such as electronic device, lithium battery, sensor, transparent conductance electrodes
Huge application prospect.
At present, the preparation method of graphene has mechanical stripping method, oxidation-reduction method, epitaxial growth method and chemical vapor deposition
Method.It is low that mechanical stripping method prepares graphene efficiency；And oxidation-reduction method prepares graphene process and needs to use substantial amounts of strong acid thing
Toxic gas is easily produced in matter, preparation process, and the graphene prepared has larger surface defect；It is prepared by epitaxial growth method
Graphene cost is high, because its sic raw material price is high.By comparing, chemical vapour deposition technique can realize graphene
Extensive, high-quality growth, but the number of plies of chemical vapour deposition technique of the prior art graphene in preparation process is still
So it is difficult to control to.For example, Chinese patent literature CN104498902A discloses a kind of aumospheric pressure cvd graphene film
Preparation method, it controls the number of plies of graphene on copper foil by controlling carbon source amount and growth time, and copper foil is in preparation process
Catalytic action is mainly played, but it is one from limit procedure, after graphene covers with copper foil, copper that graphene grows in copper substrate
Paper tinsel can not play catalytic action again, graphene can not continued growth, therefore this method is only used for single and prepares graphene film,
The number of plies of graphene still can not realize controllable in preparation process.
The content of the invention
To solve not realizing the problem of number of plies is controllable in graphene preparation process in the prior art, and then provide one kind etc.
Gas ions original position etching and the graphene preparation system of assisting growth.
Therefore, the technical scheme that the utility model is taken is：
A kind of plasma original position etching and the graphene preparation system of assisting growth, it is characterised in that：The system by
Frame, high temperature process furnances, quartz ampoule, microwave plasma generation device, microwave plasma-etching device, magnetic rod composition.
The quartz ampoule is fixed in frame by supporting mechanism；The high temperature process furnances are connected in frame by sliding rail, edge
Quartzy pipe outer wall is moved radially；The system also include air inlet group, the air inlet group include source of the gas and air inlet quartz ampoule, it is described enter
During one end of gas quartz ampoule extends to quartz ampoule from quartz ampoule sample introduction end, the other end is connected outside quartz ampoule with source of the gas；It is described micro-
Ripple plasma generator is enclosed in outside the air inlet quartz ampoule outside quartz ampoule；The microwave plasma-etching device is enclosed in
Outside quartz ampoule, it is arranged between magnetic rod and high temperature process furnances.
It is preferred that, the air inlet group also includes gas mass flow controller and valve, the gas mass flow control
Device and valve are arranged between source of the gas and air inlet quartz ampoule, and are connected by airway tube.The air-intake component is two-way, wherein
Entered all the way by microwave plasma generation device in quartz ampoule；Another road is directly entered quartz ampoule.
It is preferred that, the source of the gas includes argon gas, methane and hydrogen.
It is preferred that, the equipment also includes vacuum system and overvoltage protector, and the vacuum system and overvoltage protector are logical
Cross flange and be connected to quartz ampoule port input.
It is preferred that, the vacuum system includes vavuum pump and pressure vacuum ga(u)ge, is connected by airway tube with flange.
It is preferred that, one end of the magnetic rod and quartz ampoule is connected by flange.
The purpose of this utility model is that providing a kind of plasma original position etching and the graphene of assisting growth prepares system
System.Copper foil makes envelope shape, and the equipment is first with microwave plasma generation device assisting growth graphene, in this process stone
Black alkene on copper foil substrate by diffusion crystalline growth, be one from limit procedure, when the copper of outer surface all covers with graphite
After alkene, copper foil is not in catalytic cracking methane, and growth stops.The carbon that part high temperature is fused into copper, during cooling, in copper foil
Surface is separated out, in envelope shape copper foil inner surface into raw graphene.Magnetic rod is pulled to grow the copper foil immigration microwave for having graphene
In plasma etching apparatus, etching in situ is carried out to the graphene of envelope shape copper foil outer surface.Because metal has screen to microwave
The effect of covering, the graphene of envelope shape copper foil inner surface still completely retains in etching process, the envelope shape copper foil appearance after etching
The copper in face is exposed, again with catalytic activity.Promote magnetic rod to move into the copper foil after etching again in high temperature process furnances to be added
Hot catalytic growth graphene again, pulls magnetic rod that the copper foil that growth has graphene is moved into microwave etc. again after the completion of growth
Performed etching in ion etching device.And so on growth and etching, realize the controllable growth of the graphene number of plies.
Brief description of the drawings
In order that content of the present utility model is more likely to be clearly understood, below according to specific implementation of the present utility model
Example and with reference to accompanying drawing, the utility model is described in further detail, wherein：
Fig. 1 is the utility model plasma in situ body etching and the structural representation of the graphene preparation system of assisting growth
Figure.
Embodiment
As shown in figure 1, a kind of plasma original position etching and the graphene preparation system of assisting growth, the system is by machine
Frame 1, high temperature process furnances 2, quartz ampoule 3, microwave plasma generation device 4, microwave plasma-etching device 5,6 groups of magnetic rod
Into.The quartz ampoule 3 is fixed on 1 in frame by supporting mechanism 11；The high temperature process furnances 2 are connected to by sliding rail 12
1 in frame, moved radially along the outer wall of quartz ampoule 3；The system also includes air inlet group 7, and the air inlet group 7 includes source of the gas 71 and entered
Gas quartz ampoule 72, one end of the air inlet quartz ampoule 72 is extended in quartz ampoule 3 from quartz ampoule sample introduction end 31, and the other end is in quartz
Pipe 3 is outer to be connected with source of the gas 71；The microwave plasma generating means 4 is enclosed in outside the air inlet quartz ampoule 72 outside quartz ampoule 3；Institute
State microwave plasma-etching device 5 to be enclosed in outside quartz ampoule 3, be arranged between magnetic rod 6 and high temperature process furnances 2.
It is preferred that, the air inlet group 7 also includes gas mass flow controller 73 and valve 74, the gas mass flow
Controller 73 and valve 74 are arranged between source of the gas 71 and air inlet quartz ampoule 72, and are connected by airway tube 75.The air inlet
7 points of group is two-way, wherein 76 tunnels are entered in quartz ampoule 3 by microwave plasma generation device 4；Another 77 tunnel is directly entered
Quartz ampoule 3.
It is preferred that, the source of the gas 71 includes argon gas 711, methane 712 and hydrogen 712.
It is preferred that, the equipment also includes vacuum system 8 and overvoltage protector 9, the vacuum system 8 and overvoltage protector
9 are connected to quartz ampoule port input 32 by flange 13.
It is preferred that, the vacuum system 8 includes vavuum pump 81 and pressure vacuum ga(u)ge 82, passes through airway tube 83 and the phase of flange 13
Connection.
It is preferred that, the magnetic rod 6 is connected with one end of quartz ampoule 3 by flange 13.
Multilayer is grown using the plasma original position etching and the graphene preparation system of assisting growth described in the present embodiment
The key step of graphene includes as follows：
(1) by pretreated copper foil along long side doubling, with tweezers by three rolls it is bent and it is crimped be tamping, make envelope shape,
And during copper foil is put into quartz ampoule from quartz ampoule sample introduction end.
(2) open vavuum pump and the air pressure in quartz ampoule is evacuated to the limit；Using 77 tunnel air inlet groups by the flow set of argon gas
For 100sccm, argon gas is injected into quartz ampoule, argon gas is passed through after 5min, closes the valve of argon gas mass flow controller；Again
Open vavuum pump and the air pressure in quartz ampoule is evacuated to the limit, it is 4~8 × 10 to form air pressure-2Torr vacuum chamber；Repeat above-mentioned step
It is rapid 2~3 times, clean until the oxygen in quartz ampoule and water are removed.
(3) hydrogen is passed through using 77 tunnel air inlet groups, wherein weight flow controller setting 5sccm closes vavuum pump, stopped
Only vacuumize, until the air pressure in quartz ampoule has reached 1 atmospheric pressure, overvoltage protection valve starts external pressure release.
(4) microwave plasma generation device is opened, its power setting is 20~2000W, is passed through using 76 tunnel air inlet groups
Argon gas and hydrogen, make argon gas and hydrogen plasma, and wherein argon gas and hydrogen quality flow controller sets 5sccm.
(5) high temperature process furnances are opened and heat copper foil to 800 DEG C of growth temperature；Methane is passed through, makes methane plasma, wherein
The gas mass flow controller of methane is set as 5sccm, and the time is 10min, grows graphene.
(6) pull magnetic rod that the copper foil that growth has graphene is moved into microwave plasma-etching device, open micro-
Ripple plasma etching apparatus, power setting be 20~2000W, using 77 tunnel air inlet groups, be passed through argon gas and hydrogen, make argon gas and
Hydrogen plasma, wherein argon gas and hydrogen quality flow controller set 5sccm, to the graphene of envelope shape copper foil outer surface
Perform etching.
(7) promote magnetic rod that the copper foil after etching is moved into high temperature process furnances, repeat step (5) is in envelope shape copper foil
Surface regeneration obtains bilayer graphene into a layer graphene.
(8) step (5) and (6) are repeated in and further generate graphene layer in envelope shape copper foil inner surface.
(9) obtained according to step (8) after required multi-layer graphene, remove high temperature process furnances, close microwave device, closed
Source of the gas, is cooled to after room temperature, sampling.
Preferred embodiment of the present utility model is the foregoing is only, it is all at this not to limit the utility model
Any modifications, equivalent substitutions and improvements made within the spirit and principle of utility model etc., should be included in the utility model
Protection domain within.
Claims (6)
1. a kind of plasma original position etching and the graphene preparation system of assisting growth, it is characterised in that：The system is by machine
Frame, high temperature process furnances, quartz ampoule, microwave plasma generation device, microwave plasma-etching device, magnetic rod composition；Institute
Quartz ampoule is stated to be fixed in frame by supporting mechanism；The high temperature process furnances are connected in frame by sliding rail, along stone
English pipe outer wall is moved radially；The system also includes air inlet group, and the air inlet group includes source of the gas and air inlet quartz ampoule, the air inlet
During one end of quartz ampoule extends to quartz ampoule from quartz ampoule sample introduction end, the other end is connected outside quartz ampoule with source of the gas；The microwave
Plasma generator is enclosed in outside the air inlet quartz ampoule outside quartz ampoule；The microwave plasma-etching device is enclosed in stone
Outside English pipe, it is arranged between magnetic rod and high temperature process furnances.
2. a kind of plasma original position etching according to claim 1 and the graphene preparation system of assisting growth, it is special
Levy and be：The air inlet group also includes gas mass flow controller and valve, the gas mass flow controller and valve
It is arranged between source of the gas and air inlet quartz ampoule, and be connected by airway tube；The air-intake component is two-way, wherein passing through all the way
Microwave plasma generation device is entered in quartz ampoule；Another road is directly entered quartz ampoule.
3. a kind of plasma original position etching according to claim 1 and the graphene preparation system of assisting growth, it is special
Levy and be：The source of the gas includes argon gas, methane and hydrogen.
4. a kind of plasma original position etching according to claim 1 and the graphene preparation system of assisting growth, it is special
Levy and be：The equipment also includes vacuum system and overvoltage protector, and the vacuum system and overvoltage protector are connected by flange
It is connected to quartz ampoule port input.
5. a kind of plasma original position etching according to claim 4 and the graphene preparation system of assisting growth, it is special
Levy and be：The vacuum system includes vavuum pump and pressure vacuum ga(u)ge, is connected by airway tube with flange.
6. a kind of plasma original position etching according to claim 1 and the graphene preparation system of assisting growth, it is special
Levy and be：One end of the magnetic rod and quartz ampoule is connected by flange.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112179932A (en) * | 2020-09-18 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Quasi-in-situ normal pressure reaction combination system and imaging method thereof |
-
2017
- 2017-02-16 CN CN201720140485.3U patent/CN206502603U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112179932A (en) * | 2020-09-18 | 2021-01-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Quasi-in-situ normal pressure reaction combination system and imaging method thereof |
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