CN110240151A - A kind of device and preparation method thereof being used to prepare graphene - Google Patents
A kind of device and preparation method thereof being used to prepare graphene Download PDFInfo
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- CN110240151A CN110240151A CN201910459933.XA CN201910459933A CN110240151A CN 110240151 A CN110240151 A CN 110240151A CN 201910459933 A CN201910459933 A CN 201910459933A CN 110240151 A CN110240151 A CN 110240151A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/186—Preparation by chemical vapour deposition [CVD]
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Abstract
A kind of device and preparation method thereof being used to prepare graphene, it is related to technical field of graphene preparation, the present invention in crucible (14) by being arranged molten metal, then gas diverter (17) are set in molten metal, gas into molten metal is drained into molten metal through the venthole (16) on gas diverter and forms multiple bubbles, gas is decomposed into carbon atom in bubble surface, carbon atom is re-assemblied in bubble surface as graphene, further, the continuous production of graphene may be implemented by the respectively arranged powder collector on furnace body (10) and gas blow pipe (4) by the present invention, the present invention has high production efficiency, the advantages that at low cost, it is suitble to large-scale promotion and application.
Description
[technical field]
The present invention relates to technical field of graphene preparation, and in particular to a kind of device for being used to prepare graphene and its preparation
Method.
[background technique]
It is known, graphene be one kind by carbon atom with sp2Hybridized orbit forms the Two-dimensional Carbon that hexangle type is in honeycomb lattice
Nano material.Graphene have excellent optics, electricity, mechanical characteristic, materialogy, micro-nano technology, the energy, biomedicine and
Drug delivery etc. is with important application prospects, it is considered to be a kind of future revolutionary material.Manchester, England is big
Physicist An Deliegaimu and Constantine's Nuo Woxiao love are learned, is isolated from graphite with micromechanics stripping method success
Graphene, therefore Nobel Prize in physics in 2010 is obtained jointly, the method for the common production of graphene is mechanical stripping method, oxygen
Change reduction method, SiC epitaxial growth method and chemical vapour deposition technique (CVD).
Chemical vapour deposition technique is that (CVD) is to carry out the obtained graphene that is vapor-deposited using carbon containing organic gas for raw material
Method.This is current production graphene most efficient method.The graphene of this method preparation has area greatly and quality is high
Feature, but it is primarily present the major drawbacks such as production cost is higher, and production efficiency is low at this stage, and process conditions also need further complete
It is kind, then how to provide a kind of device for being used to prepare graphene and preparation method thereof just at the long-term of those skilled in the art
Technology demand.
[summary of the invention]
In order to realize the goal of the invention, the present invention provides a kind of device for being used to prepare graphene and its preparation sides
Then by the way that molten metal is arranged in crucible gas diverter is arranged, into molten metal in method, the present invention in molten metal
Gas be drained into molten metal through the venthole on gas diverter and form multiple bubbles, gas is decomposed into bubble surface
Carbon atom, carbon atom are re-assemblied in bubble surface as graphene, and the present invention has many advantages, such as high production efficiency, at low cost.
For achieving the above object, the present invention adopts the following technical scheme:
A kind of device being used to prepare graphene, including hollow shaft, bell, gas blow pipe, powder collector, furnace body, crucible
And heater, being equipped with bell in the upper end of the furnace body makes furnace body form a closed cavity, is equipped in the furnace chamber of furnace body
Crucible is equipped with heater in the periphery of crucible, and the heater connection electrode is equipped with crucible cover plate on the top of crucible, in earthenware
It is respectively equipped at least one inflatable mouth and at least one powder outlet on the outer edge surface on crucible top, is respectively equipped in each inflatable mouth
Gas blow pipe, the right end of each gas blow pipe correspond to the graphene powder in crucible, and the left end of each gas blow pipe passes through the outer rim of furnace body
Face connects air blowing source, and each powder outlet is separately connected powder collector by pipeline, gas diverter is equipped in crucible, in gas
The upper surface of body current divider is respectively equipped with a plurality of ventholes and at least one air inlet, and each air inlet, which is separately connected, to be upwardly extended
Hollow shaft, the upper end of the hollow shaft, which sequentially passes through, connects gas source after crucible cover plate and bell, in the upper end connection of hollow shaft
Axis lifting device forms the device for being used to prepare graphene.
The upper end of the device for being used to prepare graphene, the hollow shaft is equipped with ultrasonic vibration installation.
The air inlet of the device for being used to prepare graphene, the hollow shaft upper end is equipped with Gas mixing valve, the mixed gas
Valve connects gas source.
The device for being used to prepare graphene, the diameter of the venthole are 0.1~1mm.
The device for being used to prepare graphene, the powder outlet connect powder collecting pipe A, the powder collecting pipe A
The powder collecting pipe B being arranged on powder collector is connected, valve is equipped between the powder collecting pipe A and powder collecting pipe B
Door.
The device for being used to prepare graphene, the powder collector include powder collector main body, powder collection
Device cover board, baffle fixed link and umbrella-shaped baffle are equipped with powder collector cover board in the upper end of the powder collector main body, in powder
The lower end of body trap body is exported equipped with powder, the powder outlet connection powder collecting bag, in powder collector main body
Outer edge surface is equipped with the powder collecting pipe B of perforation to powder collector body lumen, on the inner edge surface of powder collector cover board
Equipped with the baffle fixed link extended downwardly, at least one umbrella-shaped baffle is from top to bottom equipped on the outer edge surface of baffle fixed link,
Exhaust outlet is equipped in the upper surface of powder collector cover board.
The device for being used to prepare graphene is equipped with valve between the powder outlet and powder collecting bag.
The inner edge of the device for being used to prepare graphene, the furnace body is equipped with insulating layer, sets in the bottom of furnace body
There is bottom insulating layer.
The device for being used to prepare graphene, the bottom of the crucible are equipped with support base, and the support base setting exists
On the furnace bottom of furnace body.
A method of it being used to prepare graphene, the method specifically comprises the following steps:
The first step, fusing molten metal:
Startup power supply heats crucible by heater, opens after the metal molten in crucible is at molten metal
Gas source, the gas in gas source enter gas diverter by hollow shaft, then start upper axis lifting device, by upper axis lifting device
It drives hollow shaft slowly to decline, gas diverter is submerged into the liquid level of molten metal or less;
Second step is cracked to form graphene:
Take the next step, into molten metal gas through the venthole on gas diverter be drained into molten metal formed it is more
A bubble, gas are decomposed into carbon atom in bubble surface, and carbon atom is re-assemblied in bubble surface as graphene, then with bubble
It reaches molten surface and flocks together;
Third step collects stone graphene powder:
It takes the next step, after the graphene powder on molten metal surface gathers predetermined altitude, starts air blowing source, pass through air blowing
Graphene powder is blown into powder collector by the gas in source.
Due to the adoption of the technical scheme as described above, the invention has the following beneficial effects:
Then by the way that molten metal is arranged in crucible gas diverter is arranged, into gold in the present invention in molten metal
The gas for belonging to melt is drained into molten metal through the venthole on gas diverter forms multiple bubbles, and gas is in bubble surface
It is decomposed into carbon atom, carbon atom is re-assemblied in bubble surface as graphene, and further, the present invention by setting respectively on furnace body
The continuous production of graphene may be implemented in the powder collector and gas blow pipe set, and the present invention has high production efficiency, at low cost etc.
Advantage is suitble to large-scale promotion and application.
[Detailed description of the invention]
Fig. 1 is schematic perspective view of the invention;
Fig. 2 is schematic cross-sectional view of the invention;
In figure: 1, hollow shaft;2, hollow shaft is perforated;3, bell;4, gas blow pipe;5, exhaust outlet;6, powder collecting pipe A;7,
Powder collecting pipe B;8, powder collector main body;9, powder exports;10, furnace body;11, crucible cover plate;12, inflatable mouth;13, graphite
Alkene powder;14, crucible;15, heater;16, venthole;17, gas diverter;18, copper melt;19, insulating layer;20, bottom
Insulating layer;21, electrode;22, powder collector cover board;23, baffle fixed link;24, umbrella-shaped baffle;25, support base.
[specific embodiment]
The present invention can be explained in more detail by the following examples, the open purpose of the present invention is intended to protect the present invention
All changes and improvements in range, the invention is not limited to the following examples;
Firstly the need of explanation, "upper" that the present invention is used in description scheme, "lower", "front", "rear", " left side ",
The orientation or positional relationship of the instructions such as " right side ", "top", "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings,
It is merely for convenience of description and simplification description, rather than the device or element of indication or suggestion meaning there must be specific side
Position is constructed and operated in a specific orientation, therefore is not considered as limiting the invention.
A kind of device for being used to prepare graphene in conjunction with described in attached drawing 1~2, including hollow shaft 1, bell 3, gas blow pipe
4, powder collector, furnace body 10, crucible 14 and heater 15, being equipped with bell 3 in the upper end of the furnace body 10 makes furnace body form one
A closed cavity is equipped with sealing ring, the sealing at this time in order to improve the leakproofness of cavity between furnace body 10 and bell 3
Preferably 0 type ring is enclosed, in the specific implementation, in order to improve the heat insulation effect of cavity, heat preservation is equipped on the inner edge of the furnace body 10
Layer 19 is equipped with bottom insulating layer 20 in the bottom of furnace body 10;
Further, crucible 14 is equipped in the furnace chamber of furnace body 10, the bottom of the crucible 14 is equipped with support base 25, the branch
Support seat 25 be arranged on the furnace bottom of furnace body 10, the periphery of crucible 14 be equipped with heater 15,15 connection electrode 21 of heater,
21 external power supply of electrode;It is equipped with crucible cover plate 11 on the top of crucible 14, is set respectively on the outer edge surface on 14 top of crucible
There are at least one inflatable mouth 12 and at least one powder outlet, in the specific implementation, the setting quantity root of inflatable mouth 12 and powder outlet
It is selected according to the size of crucible 14, is typically chosen and is selected as one;It is respectively equipped with gas blow pipe 4 in each inflatable mouth 12, often
The right end of a gas blow pipe 4 corresponds to the graphene powder 13 in crucible 14, and the left end of each gas blow pipe 4 passes through the outer edge surface of furnace body 10
Connect air blowing source, the preferred nitrogen of gas in the air blowing source;Each powder outlet is separately connected powder collector by pipeline, tool
When body is implemented, powder collector can be set to one, may be set to be multiple, i.e., each powder outlet connects separately through pipeline
A powder collector is connect, a powder collector can also be connected jointly by multiple pipelines;The powder collector includes
Powder collector main body 8, powder collector cover board 22, baffle fixed link 23 and umbrella-shaped baffle 24, in the powder collector master
The upper end of body 8 is equipped with powder collector cover board 22, is equipped with powder outlet 9 in the lower end of powder collector main body 8, the powder goes out
Mouth 9 connects powder collecting bags, and perforation is equipped on the outer edge surface of powder collector main body 8 to 8 inner cavity of powder collector main body
Powder collecting pipe B7 is equipped with the baffle fixed link 23 extended downwardly on the inner edge surface of powder collector cover board 22, solid in baffle
It is from top to bottom equipped at least one umbrella-shaped baffle 24 on the outer edge surface of fixed pole 23, is equipped with row in the upper surface of powder collector cover board 22
Control valve is arranged on exhaust outlet 5 in port 5, when it is implemented, can export between 9 and powder collecting bag in the powder
Equipped with valve, i.e., valve is opened after graphene powder 13 is deposited to a certain amount of and take out graphene powder;It is equipped in crucible 14
Gas diverter 17 is respectively equipped with a plurality of ventholes 16 and at least one air inlet in the upper surface of gas diverter 17, described
The diameter of venthole 16 is 0.1~1mm;Each air inlet is separately connected the hollow shaft 1 upwardly extended, and hollow shaft 1 is specifically set
It sets quantity needs to be determined according to the size of crucible 14, it is generally preferable to which one, the upper end of the hollow shaft 1 sequentially passes through crucible cover
Gas source is connected after plate 11 and bell 3, or Gas mixing valve is arranged in the air inlet in 1 upper end of hollow shaft, the Gas mixing valve connects gas source;Tool
When body is implemented, in order to ensure the airtightness of cavity, hollow shaft perforation 2 is set on bell 3, in hollow shaft 1 and hollow shaft perforation 2
Between sealing ring is set;The upper end of hollow shaft 1 connects upper axis lifting device and forms the device for being used to prepare graphene.
Further, ultrasonic vibration is equipped in the upper end of hollow shaft 1 with the product quality of graphene in order to improve the production efficiency
Device, the bubble that gas diverter 17 can in this way be discharged are more uniform and tiny.
It should be noted that the upper axis lifting device and ultrasonic vibration installation that are related in the present invention are commonly used in the art
Structure, nor the emphasis that the present invention protects, therefore tired in detail state is not done to its specific structure.
Further, the powder outlet connects powder collecting pipe A6, and the powder collecting pipe A6 connection setting is collected in powder
Powder collecting pipe B7 on device is equipped with valve between the powder collecting pipe A6 and powder collecting pipe B7, the mesh of valve is arranged
Be that cavity and powder collector can be formed to the free switching of two with an airtight cavity when realizing continuous production.
When it is implemented, valve can be selected as electromagnetic valve to improve the degree of automation of equipment.
A method of it being used to prepare graphene, the method specifically comprises the following steps:
The first step, fusing molten metal:
Startup power supply closes the valve for being located at powder collector lower part, and powder collector and airtight cavity form one at this time
Body, is then passed through argon gas in airtight cavity, and pressure 0.1mpa heats crucible 14 by heater 15, to crucible
Metal molten in 14 is at gas source is opened after molten metal, the gas in gas source enters gas diverter 17 by hollow shaft 1, so
Start upper axis lifting device afterwards, drives hollow shaft 1 slowly to decline by upper axis lifting device, gas diverter 17 is submerged into metal
Below the liquid level of melt;Wherein the molten metal is copper melt 18, and the purity of copper preferably 99.9% or more is being embodied
When, the catalyst such as nickel, iron, cobalt can be added in copper melt 18, it is therefore an objective to accelerate reaction rate;
Second step is cracked to form graphene:
It takes the next step, be drained into shape in molten metal through the venthole 16 on gas diverter 17 into the gas of molten metal
At multiple bubbles, gas is decomposed into carbon atom in bubble surface, and carbon atom is re-assemblied in bubble surface as graphene, then with
Bubble reaches molten surface and flocks together;Gas in the gas source is hydrocarbon gas and inert gas or hydrogen or nitrogen
In any one gas mixing after the mixed gas that obtains;Hydrocarbon gas accounts for mixed gas total weight in the mixed gas
2%~5%;The hydrocarbon gas is methane, acetylene, any one in natural gas;The pressure of the gas source be 0.1~
1mpa;
Third step collects stone graphene powder:
It takes the next step, after the graphene powder 13 when molten metal surface gathers predetermined altitude, starts air blowing source, the row of opening
Graphene powder 13 is blown into powder through powder collecting pipe A6, powder collecting pipe B7 through gas blow pipe 4 by port 5, the gas in air blowing source
Body collector, the graphene powder 13 being blown into powder collector deposit downwards under the blocking of umbrella-shaped baffle 24, work as graphene
After powder deposits to constant weight, the valve being first shut off between powder collecting pipe A6 and powder collecting pipe B7 makes powder
Collector forms an individual cavity, guarantees that furnace body is a closed state, does not influence graphene in this way and continues to decompose,
Then the valve for being located at 9 lower section of powder outlet is opened, the graphene powder 13 in powder collector is taken out, when graphene powder 13
After taking-up, close be located at powder outlet 9 lower section valve, powder collector is vacuumized, applying argon gas, when pressure reach with
When furnace body pressure is consistent, the valve between powder collecting pipe A6 and powder collecting pipe B7 is opened, the graphite of a new round is started
Alkene powder is collected.
The present invention can be produced in specific production in furnace body using positive pressure flow regime, can when using flowing production
Air inlet and exhaust outlet is respectively set on furnace body 10.
Not stating part in the above content carefully is the prior art, therefore does not run business into particular one and state.
The embodiment selected herein for the open purpose of the present invention, is presently considered to be suitable, still, Ying Liao
Solution, the present invention is intended to include all changes and improvement that all belong to the embodiment in this design and invention scope.
Claims (10)
1. a kind of device for being used to prepare graphene, including hollow shaft (1), bell (3), gas blow pipe (4), powder collector, furnace
Body (10), crucible (14) and heater (15), it is characterized in that: being equipped with bell (3) in the upper end of the furnace body (10) makes furnace body shape
At a closed cavity, crucible (14) are equipped in the furnace chamber of furnace body (10), are equipped with heater in the periphery of crucible (14)
(15), heater (15) connection electrode (21) is equipped with crucible cover plate (11) on the top of crucible (14), on crucible (14)
At least one inflatable mouth (12) and at least one powder outlet are respectively equipped on the outer edge surface in portion, in each inflatable mouth (12) respectively
Equipped with gas blow pipe (4), the right end of each gas blow pipe (4) corresponds to the graphene powder (13) in crucible (14), each gas blow pipe (4)
Left end pass through the outer edge surface of furnace body (10) and connect air blowing source, each powder outlet is separately connected powder collector by pipeline,
Gas diverter (17) are equipped in crucible (14), the upper surface of gas diverter (17) be respectively equipped with a plurality of ventholes (16) and
At least one air inlet, each air inlet are separately connected the hollow shaft (1) upwardly extended, and the upper end of the hollow shaft (1) is successively
Gas source is connected afterwards across crucible cover plate (11) and bell (3), and the upper axis lifting device of upper end connection of hollow shaft (1) forms described
It is used to prepare the device of graphene.
2. the device according to claim 1 for being used to prepare graphene, it is characterized in that: the upper end of the hollow shaft (1) is set
There is ultrasonic vibration installation.
3. the device according to claim 1 for being used to prepare graphene, it is characterized in that: the hollow shaft (1) upper end into
Port is equipped with Gas mixing valve, and the Gas mixing valve connects gas source.
4. the device according to claim 1 for being used to prepare graphene, it is characterized in that: the diameter of the venthole (16) is
0.1~1mm.
5. the device according to claim 1 for being used to prepare graphene, it is characterized in that: powder outlet connection powder is collected
Pipe A (6), the powder collecting pipe A (6) connect the powder collecting pipe B (7) being arranged on powder collector, receive in the powder
Valve is equipped between collector A (6) and powder collecting pipe B (7).
6. the device according to claim 1 for being used to prepare graphene, it is characterized in that: the powder collector includes powder
Trap body (8), powder collector cover board (22), baffle fixed link (23) and umbrella-shaped baffle (24) are collected in the powder
The upper end of device main body (8) is equipped with powder collector cover board (22), exports in the lower end of powder collector main body (8) equipped with powder
(9), the powder outlet (9) connects powder collecting bag, and perforation is equipped on the outer edge surface of powder collector main body (8) to powder
The powder collecting pipe B (7) of trap body (8) inner cavity is equipped on the inner edge surface of powder collector cover board (22) and extends downwardly
Baffle fixed link (23), on the outer edge surface of baffle fixed link (23) from top to bottom be equipped at least one umbrella-shaped baffle (24),
Exhaust outlet (5) are equipped in the upper surface of powder collector cover board (22).
7. the device according to claim 6 for being used to prepare graphene, it is characterized in that: powder outlet (9) and powder
Valve is equipped between collecting bag.
8. the device according to claim 1 for being used to prepare graphene, it is characterized in that: being set on the inner edge of the furnace body (10)
There are insulating layer (19), is equipped with bottom insulating layer (20) in the bottom of furnace body (10).
9. the device according to claim 1 for being used to prepare graphene, it is characterized in that: the bottom of the crucible (14) is equipped with
Support base (25), the support base (25) are arranged on the furnace bottom of furnace body (10).
10. implementing a kind of one kind for the device for being used to prepare graphene described in claim 1~9 any claim for making
The method of standby graphene, it is characterized in that: the method specifically comprises the following steps:
The first step, fusing molten metal:
Startup power supply heats crucible (14) by heater (15), molten at metal to the metal molten in crucible (14)
Gas source is opened after liquid, the gas in gas source enters gas diverter (17) by hollow shaft (1), then starts upper axis lifting dress
Set, by upper axis lifting device drive hollow shaft (1) slowly decline, by gas diverter (17) submerge the liquid level of molten metal with
Under;
Second step is cracked to form graphene:
It takes the next step, be drained into shape in molten metal through the venthole (16) on gas diverter (17) into the gas of molten metal
At multiple bubbles, gas is decomposed into carbon atom in bubble surface, and carbon atom is re-assemblied in bubble surface as graphene, then with
Bubble reaches molten surface and flocks together;
Third step collects stone graphene powder:
It takes the next step, after the graphene powder (13) when molten metal surface gathers predetermined altitude, starts air blowing source, pass through air blowing
Graphene powder (13) is blown into powder collector by the gas in source.
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CN201910459933.XA CN110240151A (en) | 2019-05-28 | 2019-05-28 | A kind of device and preparation method thereof being used to prepare graphene |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111689489A (en) * | 2020-07-09 | 2020-09-22 | 汤璐 | Preparation device and preparation method for graphene powder production |
CN116177537A (en) * | 2023-04-28 | 2023-05-30 | 厦门凯纳石墨烯技术股份有限公司 | High-quality graphene powder growth and synchronous hydrogen production method and device |
CN116395679A (en) * | 2023-06-08 | 2023-07-07 | 厦门凯纳石墨烯技术股份有限公司 | Graphene growth system with bottom ventilation and graphene preparation method |
CN117945395A (en) * | 2024-03-27 | 2024-04-30 | 东华工程科技股份有限公司 | Reaction device for preparing graphene |
-
2019
- 2019-05-28 CN CN201910459933.XA patent/CN110240151A/en not_active Withdrawn
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111689489A (en) * | 2020-07-09 | 2020-09-22 | 汤璐 | Preparation device and preparation method for graphene powder production |
CN116177537A (en) * | 2023-04-28 | 2023-05-30 | 厦门凯纳石墨烯技术股份有限公司 | High-quality graphene powder growth and synchronous hydrogen production method and device |
CN116395679A (en) * | 2023-06-08 | 2023-07-07 | 厦门凯纳石墨烯技术股份有限公司 | Graphene growth system with bottom ventilation and graphene preparation method |
CN116395679B (en) * | 2023-06-08 | 2023-08-18 | 厦门凯纳石墨烯技术股份有限公司 | Graphene growth system with bottom ventilation and graphene preparation method |
CN117945395A (en) * | 2024-03-27 | 2024-04-30 | 东华工程科技股份有限公司 | Reaction device for preparing graphene |
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Application publication date: 20190917 |