CN107364846A - A kind of device in substrate surface growth graphene film - Google Patents
A kind of device in substrate surface growth graphene film Download PDFInfo
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- CN107364846A CN107364846A CN201710796471.1A CN201710796471A CN107364846A CN 107364846 A CN107364846 A CN 107364846A CN 201710796471 A CN201710796471 A CN 201710796471A CN 107364846 A CN107364846 A CN 107364846A
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- molten bath
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Abstract
The present invention discloses a kind of device in substrate surface growth graphene film, including for providing the atmosphere box of protective gas environment, molten bath is placed with atmosphere box, and molten bath outer wall is provided with heating element heater, substrate elevating frame, batch charger and scummer are provided with above molten bath；Molten bath bottom is provided with the propeller agitator of direction upward, and cooler is provided with above propeller agitator；Batch charger is used to launch carbon into molten bath；Liquid metal is contained with molten bath, and the temperature of liquid metal is controlled by heating element heater；Substrate elevating frame is used for hanging base board, and substrate is immersed in the liquid metal in molten bath；Scummer floats over the undissolved carbon of liquid metal surface for removal；Cooler is used to cool down liquid metal, and propeller agitator makes liquid metal produce convection current from the bottom to top；The graphene film defect prepared using the present apparatus is few, and quality and uniformity are high, and cost it is low, suitable for promoting the use of on a large scale.
Description
Technical field
The present invention relates to technical field of graphene preparation, specifically a kind of dress in substrate surface growth graphene film
Put.
Background technology
Mainly there are two kinds in the method for substrate surface growth graphene film at present：One kind is liquid phase coating method, that is, is utilized
It is raw material that liquid phase, which peels off graphene or redox graphene, and a layer graphene film is coated in substrate surface；Being of another kind
Vapour deposition process is learned, i.e., is deposited on substrate surface using chemical reactant and obtains graphene film.
For liquid phase coating method, mainly there are the modes such as spin coating, roller coat, spraying, the method method can be prepared inexpensively on a large scale
Large-area graphene film, shortcoming is that the continuity, uniformity and quality of the graphene film prepared are all very poor, with theoretical property
There can be very big gap.Reason is：1）It is dense due to graphene dispersing solution when using liquid phase to peel off graphene as raw material
Spend it is extremely low, when coating is too thin, the graphene film skewness of substrate surface, and discontinuously, though translucency is good, electric conductivity
Difference；When coating is too thick, the substrate surface graphene film number of plies is too many, and lamella superposition is serious, though electric conductivity is good, light transmission
It is very poor；2）When using redox graphene as raw material, chemical method reducing process cost is low, but can not recover to aoxidize completely
During caused structure destroy so that the thin film properties of graphite are greatly reduced；Reduction of the high temperature reduction method to graphene oxide
More thoroughly, but the formability of film is difficult to ensure that at high temperature.
For chemical vapour deposition technique, it is typically that graphene film is first grown on tinsel, then again turns film
Moving on in other substrates, graphene film quality made from this method is high, and the number of plies is controllable, and shortcoming is tinsel limited area,
And use high-purity copper, nickel more cost is higher, it is difficult to prepares the high-quality thin film of large-size, it is difficult to pushes away on a large scale for base material
It is wide to use.
The content of the invention
It is an object of the invention to provide a kind of device in substrate surface growth graphene film, prepared by the device
Graphene film defect it is few, quality and uniformity are high, and cost it is low, suitable for promoting the use of on a large scale.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of device in substrate surface growth graphene film, including for providing the atmosphere box of protective gas environment, atmosphere
Molten bath is placed with case, molten bath outer wall is provided with heating element heater, substrate elevating frame, batch charger and scummer are provided with above molten bath；It is molten
Bottom of pond portion is provided with the propeller agitator of direction upward, and cooler is provided with above propeller agitator；
Batch charger is used to launch carbon into molten bath；Liquid metal is contained with molten bath, and liquid metal is controlled by heating element heater
Temperature；
Substrate elevating frame is used for hanging base board, and substrate is immersed in the liquid metal in molten bath；
Scummer floats over the undissolved carbon of liquid metal surface for removal；
Cooler is used to cool down liquid metal, and propeller agitator makes liquid metal produce convection current from the bottom to top.
Further, the substrate elevating frame is to tilt down to the clamping face of substrate.
Further, the molten bath outer wall is covered with heat-insulation layer, and heating element heater is between molten bath outer wall and heat-insulation layer.
Further, the heating element heater, propeller agitator and cooler pass through computer system control, cooler
Top is with being respectively arranged below with the temp probe for detecting liquid metal temperature, temp probe and computer system input interface
It is connected.
The beneficial effects of the invention are as follows：
The lower surface of substrate pastes some separate graphene films in advance, then tilts substrate by substrate elevating frame and immerse
In liquid metal, the carbon saturation that batch charger is launched into molten bath is dissolved in liquid metal；Cooler carries out cold to liquid metal
But, separate out carbon；Propeller agitator makes the carbon of precipitation float, the nuclei of crystallization of the graphene film as graphene growth, floating
Carbon is combined as carbon source with the nuclei of crystallization, the nuclei of crystallization is constantly increased on lateral dimension, these final independent graphene films by
Gradually it is stitched together, forms complete graphene film.
Cooling rate can be controlled using cooler, carbon atom is separated out with extremely slow speed, makes carbon source concentration very low,
It is adapted to the growth of high-quality thin film.Propeller agitator promotes carbon to float, and improves the transporting velocity of carbon source, is advantageous to improve thin
Layer-growth rate；And the mobility of liquid metal, carbon source can be promoted in the migration velocity of base lower surface, along with substrate tilts
Guide functions, carbon source is fully contacted with base lower surface, be advantageous to the combination of carbon source and nucleus and the growth of film.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples：
Fig. 1 is the structural representation of the present invention.
Embodiment
As shown in figure 1, the present invention provides a kind of device in substrate surface growth graphene film, including for providing guarantor
The atmosphere box 1 of gaseous environment is protected, the top of atmosphere box 1 is provided with air inlet 1a, bottom is provided with gas outlet 1b, air inlet 1a connective protections
Gas source 2.
Molten bath 3 is placed with atmosphere box 1, molten bath outer wall is sequentially provided with heating element heater 4 and heat-insulation layer 5, and heating element heater 4 is located at
Between the outer wall of molten bath 3 and heat-insulation layer 5.
The top of molten bath 3 is provided with substrate elevating frame 6, batch charger 7 and scummer 8, substrate elevating frame 6, batch charger 7 and scummer
8 are both secured to the top of atmosphere box 1.The bottom of molten bath 3 is provided with the propeller agitator 9 of direction upward, and the top of propeller agitator 9 is set
There is cooler 10.
Batch charger 7 is used to launch carbon into molten bath 3；Liquid metal 11 is contained with molten bath 3, and is controlled by heating element heater 4
The temperature of liquid metal processed；Substrate elevating frame 6 is used for hanging base board 12, and the liquid metal for enabling substrate 12 to immerse in molten bath
In, substrate elevating frame 6 is to tilt down to the clamping face of substrate；It is undissolved that scummer 8 for removal floats over liquid metal surface
Carbon；Cooler 10 is used to cool down liquid metal, and propeller agitator 9 makes liquid metal produce convection current from the bottom to top.
The heating element heater 4, propeller agitator 9 are controlled with cooler 10 by computer system 13, cooler 10
Top and be respectively arranged below with for the upper temp probe 14 that detects liquid metal temperature and lower temp probe 15, temp probe with
Computer system input interface is connected.
When in use, can be operated according to following steps：
S1, adhere to some graphene films in advance in the lower surface of substrate 12 first, it is spaced between graphene film, formed mutually only
Vertical graphene island, each graphene island can exist a large amount of as the nuclei of crystallization of graphene growth, around each nuclei of crystallization
Dangling bond, being advantageous to be combined with carbon atom expands crystal size.
S2, liquid metal 11 is loaded to molten bath 3, graphite powder loads batch charger 7, and substrate 12 adheres to is clamped in substrate downwards
On crane 6, the top of molten bath 3 is suspended from, is then shut off atmosphere cover.
S3, protective gas source of the gas 2 is opened, protective gas enters atmosphere box 1 by air inlet 1a, discharges, makes from gas outlet 1b
Molten bath 3 is under protective gas environment all the time.
S4, start heating element heater 4, be kept molten by the liquid metal in molten bath 3, heat-insulation layer 5 is that molten bath 3 provides guarantor
Temperature；Graphite powder is put into liquid metal 11 by batch charger 7, according to the difference of selected metal and selected substrate material
Difference, it is determined that corresponding holding temperature point, after this temperature spot constant temperature 1~2 hour, the basic convergence of carbon content in liquid metal
Saturation, then removed with scummer 8 and float over the undissolved graphite powder of liquid metal surface.
S5, operation substrate crane 6 decline, and make in the liquid metal that substrate 12 is completely immersed in molten bath 3.
S6, heating element heater 4 is closed, start cooler 10 and propeller agitator 9, propeller agitator 9 promotes liquid gold
Category flows through cooler 10, and liquid metal is cooled, and separates out carbon；Meanwhile propeller agitator 9 promotes liquid metal to upstream
Dynamic, the carbon of precipitation rises therewith.The temperature of liquid metal is uploaded to computer system 13, computer system by two temp probes
13 control to adjust the temperature of cooling medium, flow in cooler 10, and adjust the rotating speed of propeller agitator 9, so as to control liquid
The cooling rate of state metal, carbon atom is set to be separated out with extremely slow speed.
S7, the carbon separated out rise with flow of liquid metal, reach the bottom surface of substrate 12, encounter graphene film edge, tie therewith
Symphysis is grown, and independent graphene film incrementally increases, and over time, each independent graphene film gradually splices one
Rise, form complete graphene film.
S8, by substrate elevating frame 6 substrate 12 is taken out from liquid metal 11, after annealing, that is, obtaining surface attachment has
The substrate of graphene film.
It should be noted that note also in operation it is following some：
First, selected liquid metal must be inert to carbon, it is impossible to form carbide；The solubility very little of carbon wherein,
It can be deposited in the form of atom solution；The solubility of carbon wherein has preferable linear relationship with temperature, raises and increases with temperature.
2nd, selected substrate material must be inert to the liquid metal of selection, to carbon and inert.
3rd, in order to obtain the graphene film of high quality, to liquid metal cooling outlet temperature should >=1000 DEG C, because
The defects of can effectively reducing substrate surface graphene for high temperature, the favourable quality and uniformity for improving graphene film.
The above described is only a preferred embodiment of the present invention, any formal limitation not is made to the present invention；Appoint
What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above
Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations
Apply example.Therefore, every content without departing from technical solution of the present invention, the technical spirit according to the present invention are done to above example
Any simple modification, equivalent substitution, equivalence changes and modification, still fall within the range of technical solution of the present invention protects.
Claims (4)
1. a kind of device in substrate surface growth graphene film, it is characterised in that including for providing protective gas environment
Atmosphere box, molten bath is placed with atmosphere box, molten bath outer wall is provided with heating element heater, and substrate elevating frame is provided with above molten bath, is fed intake
Machine and scummer；Molten bath bottom is provided with the propeller agitator of direction upward, and cooler is provided with above propeller agitator；
Batch charger is used to launch carbon into molten bath；Liquid metal is contained with molten bath, and liquid metal is controlled by heating element heater
Temperature；
Substrate elevating frame is used for hanging base board, and substrate is immersed in the liquid metal in molten bath；Scummer is used to remove
Float over the undissolved carbon of liquid metal surface；Cooler is used to cool down liquid metal, and propeller agitator makes liquid golden
Category produces convection current from the bottom to top.
A kind of 2. device in substrate surface growth graphene film according to claim 1, it is characterised in that the base
Plate crane is to tilt down to the clamping face of substrate.
A kind of 3. device in substrate surface growth graphene film according to claim 1 or 2, it is characterised in that institute
State molten bath outer wall and be covered with heat-insulation layer, heating element heater is between molten bath outer wall and heat-insulation layer.
A kind of 4. device in substrate surface growth graphene film according to claim 1 or 2, it is characterised in that institute
Heating element heater, propeller agitator and cooler are stated by computer system control, cooler top is with being respectively arranged below with
For detecting the temp probe of liquid metal temperature, temp probe is connected with computer system input interface.
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| CN201710796471.1A CN107364846A (en) | 2017-09-06 | 2017-09-06 | A kind of device in substrate surface growth graphene film |
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| CN201710796471.1A CN107364846A (en) | 2017-09-06 | 2017-09-06 | A kind of device in substrate surface growth graphene film |
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| CN201710796471.1A Withdrawn CN107364846A (en) | 2017-09-06 | 2017-09-06 | A kind of device in substrate surface growth graphene film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594168A (en) * | 2022-10-29 | 2023-01-13 | 胡飞飞（Cn） | Device for preparing graphene |
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| JP2009091222A (en) * | 2007-10-11 | 2009-04-30 | Sumitomo Metal Ind Ltd | PRODUCTION METHOD FOR SiC SINGLE CRYSTAL, SiC SINGLE CRYSTAL WAFER AND SiC SEMICONDUCTOR DEVICE |
| JP2012006824A (en) * | 2010-05-28 | 2012-01-12 | Nippon Telegr & Teleph Corp <Ntt> | Method for synthesizing graphene and carbon molecule thin film |
| CN102373433A (en) * | 2011-11-21 | 2012-03-14 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN105399089A (en) * | 2015-12-15 | 2016-03-16 | 深圳市国创新能源研究院 | Graphene generation method, device and equipment based on arbitrary substrate |
| CN105624778A (en) * | 2016-03-30 | 2016-06-01 | 北京大学 | Method for quickly and continuously preparing large-crystal-domain graphene film |
| CN207142834U (en) * | 2017-09-06 | 2018-03-27 | 蚌埠玻璃工业设计研究院 | A kind of device in substrate surface growth graphene film |
-
2017
- 2017-09-06 CN CN201710796471.1A patent/CN107364846A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009091222A (en) * | 2007-10-11 | 2009-04-30 | Sumitomo Metal Ind Ltd | PRODUCTION METHOD FOR SiC SINGLE CRYSTAL, SiC SINGLE CRYSTAL WAFER AND SiC SEMICONDUCTOR DEVICE |
| JP2012006824A (en) * | 2010-05-28 | 2012-01-12 | Nippon Telegr & Teleph Corp <Ntt> | Method for synthesizing graphene and carbon molecule thin film |
| CN102373433A (en) * | 2011-11-21 | 2012-03-14 | 武汉大学 | Method for preparing ultrathin carbon film by using carbon cluster ion beam |
| CN102627275A (en) * | 2012-04-28 | 2012-08-08 | 郑州大学 | Method for preparing graphene by melting carbon-containing alloy to separate out carbon in solidification process |
| CN105399089A (en) * | 2015-12-15 | 2016-03-16 | 深圳市国创新能源研究院 | Graphene generation method, device and equipment based on arbitrary substrate |
| CN105624778A (en) * | 2016-03-30 | 2016-06-01 | 北京大学 | Method for quickly and continuously preparing large-crystal-domain graphene film |
| CN207142834U (en) * | 2017-09-06 | 2018-03-27 | 蚌埠玻璃工业设计研究院 | A kind of device in substrate surface growth graphene film |
Non-Patent Citations (1)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115594168A (en) * | 2022-10-29 | 2023-01-13 | 胡飞飞（Cn） | Device for preparing graphene |
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Application publication date: 20171121 |
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