CN107445147A - The preparation method and equipment of a kind of graphene - Google Patents
The preparation method and equipment of a kind of graphene Download PDFInfo
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- CN107445147A CN107445147A CN201710810232.7A CN201710810232A CN107445147A CN 107445147 A CN107445147 A CN 107445147A CN 201710810232 A CN201710810232 A CN 201710810232A CN 107445147 A CN107445147 A CN 107445147A
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Abstract
The invention discloses a kind of preparation method of graphene and equipment, belong to technical field of nano material.The equipment includes feed arrangement, high-temperature reaction equipment 3 and drawing mechanism；The preparation method of the graphene is based on equipment of the present invention, metal foil enters the reative cell high-temperature region 39 of high-temperature reaction equipment 3 under the common traction drive of feed arrangement and drawing mechanism, cracked at high temperature using hydrocarbon gas, deposit, assemble, graphene nucleus is formed by reaction and attracted each other, turns into large-area graphene.The preparation method and equipment of a kind of graphene of the present invention, not only production cost is low, and can realize that graphene large area, high quality, scale and serialization prepare production.
Description
Technical field
The present invention relates to technical field of nano material, the preparation method and equipment of a kind of graphene are specifically designed.
Background technology
In recent years, grapheme material is always the Disciplinary Frontiers of scientific and technical innovation.Because of its outstanding electric conductivity, the electricity of superelevation
The advantage such as transport factor and specific surface area, high heat conduction, high printing opacity, high fracture strength and good chemical stability, is described as 21
The magical material in century is extremely wide in the application prospect of numerous technical fields.
At present, the main preparation methods of graphene have：Mechanical stripping method, chemical stripping method, oxidation-reduction method, SiC extensions
Growth method, chemical vapour deposition technique etc..Mechanical stripping method prepares that graphene is simple to operation, and prepared graphene quality is high,
But the usual area of graphene made from the method is smaller and extremely inefficient.Chemical stripping method prepare graphene process exist it is uncontrollable
Property, in preparation process the addition of the material such as strong acid, highly basic can cause graphene sp2Structure is destroyed.Oxidation-reduction method prepares graphite
Alkene cost is low, but the structure of graphene is destroyed in its preparation process, and the graphene defect of preparation is a lot, has a strong impact on its electricity
It is also more difficult for the graphene for preparing large-area high-quality etc. performance.SiC epitaxys can prepare larger area mono-layer graphite
Alkene, but the harsh growth conditions such as HTHP requires very high to graphene production equipment, and expensive monocrystal SiC makes this in addition
Method is difficult to the large-scale production of graphene industrialization.
Relative to other preparation methods, graphene film quality of the chemical vapour deposition technique with preparation is high, the number of plies is controllable,
The advantages that size is big, it can realize prepared by the controllable grapheme of graphene large-area high-quality to a certain extent.Chemical vapor deposition
Area method, which prepares the common equipment of graphene, CVD tube furnaces, microware bursts equipment, magnetron sputtering C VD equipment etc., but by
Protective gas and reacting gas are re-filled with after preparation process usually requires first to vacuumize consersion unit in these equipment, can not
Realize industrialization continuous production, thus vapour deposition process prepares the high cost of graphene and governs the hair of grapheme material always
Exhibition, can not much meet application demand of the Battery Market to grapheme material.
The content of the invention
In order to solve the above problems, the invention provides a kind of preparation method of graphene and equipment, be not only simple in structure,
Production cost is low, and can realize that graphene large area, high quality, scale and serialization prepare production.
In order to achieve the above object, the technical solution adopted by the present invention is as follows：
On the one hand, there is provided a kind of production equipment of graphene, including feed arrangement, high-temperature reaction equipment 3 and drawing mechanism, institute
The both sides that feed arrangement and drawing mechanism are located at the high-temperature reaction equipment 3 respectively are stated, for base material to be drawn through into the height
Warm consersion unit 3；
The high-temperature reaction equipment 3 includes graphite boiler tube 38, induction heating circle 37, reative cell and protection air seal set 31；It is described
Reative cell is located at the inner hub location of high-temperature reaction equipment 3 and extended to the both sides of high-temperature reaction equipment 3, the protection sealing gland
Device 31 is located inside the both ends extension of reative cell；The graphite boiler tube 38 is located at the inside of high-temperature reaction equipment 3 and is distributed on
The periphery of reative cell；The induction heating circle 37 is uniformly looped around the periphery of graphite boiler tube 38, for heating graphite boiler tube 38.
Preferably, the outside of the high-temperature reaction equipment 3 also includes cooling jacket 4, the both ends of cooling jacket 4 difference
Provided with cooling jacket entrance 41 and cooling jacket outlet 42, wherein cooling jacket entrance 41 is located at the bottom of cooling jacket 4, cooling
Water jacket outlet 42 is located at the top of cooling jacket 4.
Preferably, the bottom of high-temperature reaction equipment 3 is additionally provided with reaction gas inlet 34.
Preferably, the protection air seal set 31 is multiple mutually isolated rectangular channels, and reative cell periphery is with protecting gas
The relative position of seal apparatus 31 is provided with protection gas entrance 33, and the protection gas entrance 33 is the rectangular hollow knot of multiple related insertions
Structure；The reative cell both ends are equipped with sealing gland mouth 32；The reative cell is rectangular cavities.
Preferably, the feed arrangement and drawing mechanism are respectively feed roller 2 and discharge roller 5, the feed roller 2 and discharging
Roller 5 is driven using variable-frequency motor.
Preferably, the induction heating circle 37 is water cooling induction heating circle, is formed using hollow copper pipe coiling, by external
Electric supply installation power supply driving, for heating graphite boiler tube 38；The periphery of the induction heating circle 37 is also sequentially provided with heat preservation carbon felt
36 and quartz sand 35, the corresponding reaction zone of the induction heating circle 37 be reative cell high-temperature region 39.
On the other hand, there is provided the method that graphene is prepared using the said equipment, it is characterised in that：Utilize continous way chemistry
Prepared by vapour deposition process, including following steps：
1）, metal foil high-temperature reaction equipment is entered by sealing gland mouth 32 under the common traction drive of feed arrangement and drawing mechanism
3；
2）, by protecting air seal set 31 be passed through protective gas into high-temperature reaction equipment 3；
3）, high-temperature reaction equipment 3 is heated up in advance, when when reative cell high-temperature region 39, temperature reaches 800 DEG C -1000 DEG C, to reative cell
Hydrocarbon gas are passed through in high-temperature region 39, metal foil pulls out high-temperature reaction equipment 3 through drawing mechanism, and stone is obtained in metal foil surface
Black alkene, form metal foil graphene complex；
4), metal foil graphene complex is corroded with ammonium persulfate aqueous solution or ferric chloride aqueous solutionses, until metal
Paper tinsel corrodes completely, stands, takes remaining membranoid substance；
5）, membranoid substance is cleaned repeatedly, produce graphene.
Preferably, the step 1）Described in metal foil be copper foil；Step 3）In to high-temperature reaction equipment 3 carry out lockup
Wen Shi, programming rate are no more than 20 DEG C per hour.
Preferably, the step 3）Described in protective gas be argon gas or nitrogen；Hydrocarbon gas are methane, ethane, third
One kind in alkane, ethene, propylene, acetylene and propine, its air demand are 0.1m3/h-1m3/h；When reative cell high-temperature region 39 is heated to
At 800 DEG C -1000 DEG C, hydrogen is also passed through while hydrocarbon class gas is passed through into reative cell high-temperature region 39, it is hydrocarbon for being catalyzed
Gas cracks, and promotes the formation of graphene, its air demand is 0.1m3/h-0.5m3/h；Wherein metal foil feeding speed is 0.5-
2mm/s；
Step 4）Described in the mass concentration of ammonium persulfate aqueous solution be 10%-20%, the mass concentration of ferric chloride aqueous solutionses is
10%-50%；Step 5）It is middle that membranoid substance is cleaned repeatedly using acetone and deionized water.
Finally, there is provided a kind of graphene, the graphene are prepared using above-mentioned any one methods described.
Beneficial effect：Compared with prior art, the production equipment and preparation method of a kind of graphene provided by the invention, institute
State equipment has advantages below compared with the equipment of existing preparing graphene through chemical vapor deposition：
1st, it is simple in construction, without forvacuum handle, using the principle of gas expansion under hot conditions realize high temperature reaction zone without
Oxidation completely cuts off, and graphene can be prepared under normal pressure；
2nd, it by adjusting the hauling speed of feed roller and discharge roller, can not only regulate and control the growth result of graphene, ensure graphite
The alkene quality of production, and can realize that the serialization of graphene and large area production, efficiency greatly improve, production cost significantly drops
It is low, mass produced particularly suitable for industrialization.
Not only preparation process is stable, uniformity is good for the preparation method of graphene of the present invention, and the graphene prepared
The number of plies is controllable, finished product crystal mass is higher, continuity is more preferable.
Brief description of the drawings
In order to illustrate more clearly of technical scheme, the required accompanying drawing used in embodiment will be made below
Simply introduce, it should be apparent that, drawings in the following description are only some embodiments of the present invention, general for this area
For logical technical staff, on the premise of not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of structural representation of the production equipment of graphene of the present invention；
Fig. 2 is the left view of high-temperature reaction equipment described in Fig. 1；
Fig. 3 is the partial enlarged drawing in A portions in Fig. 1.
In figure：1- copper foils, 2- feed rollers, 3- high-temperature reaction equipments, 31- protections sealing gland, 32- reative cell sealing glands mouth, 33- are protected
Protect gas entrance, 34- reaction gas inlets, 35- quartz sands, 36- heat preservation carbon felts, 37- induction heating circles, 38- graphite boiler tubes, 39-
Reative cell high-temperature region, 4- cooling jackets, 41- cooling jackets entrance, the outlet of 42- cooling jackets, 5- discharge rollers.
Embodiment
In the description of the invention, it is to be understood that term " " center ", " on ", " under ", "front", "rear", " left side ",
The orientation or position relationship of the instruction such as " right side ", " vertical ", " level ", " top ", " bottom ", " interior ", " outer " are based on shown in the drawings
Orientation or position relationship, be for only for ease of the description present invention and simplify description, rather than instruction or imply signified device or
Element must have specific orientation, with specific azimuth configuration and operation, therefore be not considered as limiting the invention.
Embodiment 1
First, a kind of production equipment of graphene
A kind of production equipment of graphene, including feed arrangement, high-temperature reaction equipment 3 and drawing mechanism, the feed arrangement and
Drawing mechanism is located at the both sides of the high-temperature reaction equipment 3 respectively, for base material to be drawn through into the high-temperature reaction equipment 3,
So that the center of copper foil and high-temperature reaction equipment 3 is maintained at same horizontal line.The feed arrangement and drawing mechanism be respectively into
Expect roller 2 and discharge roller 5, the feed roller 2 and discharge roller 5 are driven using variable-frequency motor.
The high-temperature reaction equipment 3 includes graphite boiler tube 38, induction heating circle 37, reative cell and protection air seal set 31；
The reative cell is located at the inner hub location of high-temperature reaction equipment 3 and extended to the both sides of high-temperature reaction equipment 3, the protection
Air seal set 31 is located inside the both ends extension of reative cell；The graphite boiler tube 38 is located inside high-temperature reaction equipment 3 and equal
Cloth is in the periphery of reative cell；The induction heating circle 37 is uniformly looped around the periphery of graphite boiler tube 38, for heating graphite boiler tube
38。
Preferably, the outside of the high-temperature reaction equipment 3 also includes cooling jacket 4, for ensureing the security of operation.Institute
State the both ends of cooling jacket 4 and be respectively equipped with cooling jacket entrance 41 and cooling jacket outlet 42, wherein cooling jacket entrance 41
In the bottom of cooling jacket 4, cooling jacket outlet 42 is located at the top of cooling jacket 4.The bottom of high-temperature reaction equipment 3 is also set
There is reaction gas inlet 34.
Preferably, the protection air seal set 31 is multiple mutually isolated rectangular channels, and reative cell periphery is with protecting gas
The relative position of seal apparatus 31 is provided with protection gas entrance 33, and the protection gas entrance 33 is the rectangular hollow knot of multiple related insertions
Structure；The reative cell both ends are equipped with sealing gland mouth 32；The reative cell is rectangular cavities.
Preferably, the induction heating circle 37 is water cooling induction heating circle, is formed using hollow copper pipe coiling, by external
Electric supply installation power supply driving, for heating graphite boiler tube 38, simultaneously the logical cooling water in the inside of induction heating circle 37, can be protected
Hinder the long-term use of coil in high temperature environments；The periphery of the induction heating circle 37 is also sequentially provided with heat preservation carbon felt 36 and quartz
Sand 35, has that efficiency of energy utilization is high, high insulating effect, it can be ensured that up to 2500 DEG C of high temperature above conditions it is safe to use.
The corresponding reaction zone of the induction heating circle 37 is reative cell high-temperature region 39.
The production equipment of graphene of the present invention is simple in construction, is handled without forvacuum, passes through high-temperature reaction equipment 3
Using preceding slowly pre- heating, while protective gas is filled with air seal set 31, the principle using gas expansion under hot conditions is true
The isolation of high temperature reaction zone non-oxidation is protected, after reaching graphene growth temperature, reacting gas, normal pressure are passed through toward reative cell high-temperature region 39
Under can prepare graphene, wherein programming rate is no more than 20 DEG C per hour.Run without interruption by equipment, base material is in feed roller
Common traction with discharge roller enters reative cell high-temperature region 39 under driving, can be in substrate surface using reacting gas Pintsch process
Growth in situ goes out continual large scale high quality monolayer or multi-layer graphene.The feed roller 2 and discharge roller 5 use variable-frequency electric
Machine drives, and is easy to adjust time of the base material by high-temperature region, reaches the purpose of control graphene growth time.The graphene
Production equipment is by adjusting the temperature of high-temperature reaction equipment 3, the air demand of reacting gas, feed roller and the rotating speed of discharge roller（
Base material feeding speed can be used to substitute）The extent of reaction can be regulated and controled.Above-mentioned corresponding data needs to regard actual height among practical application
The length experiment of the warm reative cell high-temperature region 39 of consersion unit 3 determines.
2nd, a kind of preparation method of graphene
A kind of preparation method of graphene is based on the said equipment, and the preparation method utilizes continous way chemical vapor deposition（CVD）
Prepared by method, specifically include following steps：
1）, copper foil is smooth under the common traction drive of feed arrangement and drawing mechanism enters pyroreaction by sealing gland mouth 32
Equipment 3；
2）, by protecting air seal set 31 to be passed through protective gas argon gas, air demand 1m into high-temperature reaction equipment 33/h-10m3/
h；
3）, before reaction to the slowly pre- heating of high-temperature reaction equipment 3, it is ensured that device interior high-temperature region be in anaerobic state, and heating is fast
Degree is no more than 20 DEG C per hour；When reative cell high-temperature region 39 is heated to 1000 DEG C, it is passed through into reative cell high-temperature region 39 hydrocarbon
Gases methane, air demand 0.1m3/ h, while hydrogen is passed through again, air demand 0.5m3/ h, for being catalyzed hydrocarbon gas cracking,
Promote the formation of graphene, when copper foil pulls out high-temperature reaction equipment 3 through drawing mechanism, graphene obtained in copper foil surface,
Metal foil graphene complex is formed, wherein copper foil feeding speed is 2mm/s；
4), copper foil graphene complex is corroded with the ammonium persulfate aqueous solution that mass concentration is 10%, until metal foil
Corrosion completely, stand, take remaining membranoid substance；
5）, with acetone and deionized water membranoid substance is cleaned repeatedly, produce graphene.
Among the present embodiment, protective gas can also be nitrogen, and its air demand is identical with argon gas.The hydrocarbon gas
Can be one kind in ethane, propane, ethene, propylene, acetylene and propine, its air demand is identical with methane.The copper foil passes through
Equipment runs without interruption, and copper foil enters reative cell high-temperature region 39 in the case where the common traction of feed roller and discharge roller drives, and utilizes carbon
Hydrogen cracks out carbon atom at high temperature, upper and lower surface deposition of the carbon atom in copper foil, aggregation, passes through sp2Hydridization reacts shape
Into graphene nucleus and attract each other, large stretch of graphene is grown into lower surface on metal foil, then utilizes metal foil and graphite
Alkene dissolution characteristics different among ammonium persulfate aqueous solution or ferric chloride aqueous solutionses, metal foil is corroded, and graphene is then
Depart from from metal foil and form membranoid substance, cleaning repeatedly is carried out to membranoid substance by acetone and deionized water purifies, and has obtained pure
Net graphene, realize graphene large area, prepared by serialization.The growth result of graphene depends on height among the present embodiment
The temperature of warm consersion unit 3, the air demand of reacting gas and assisted Reduction gas hydrogen, the rotating speed of feed roller and discharge roller.This
The length of reative cell high-temperature region 39 is set as 2000mm among embodiment.
3rd, a kind of graphene
The graphene is prepared using the above method.
Embodiment 2
First, a kind of preparation method of graphene
A kind of preparation method of graphene is based on equipment described in embodiment 1, and methods described utilizes continous way chemical vapor deposition
（CVD）Prepared by method, specifically include following steps：
1）, copper foil is smooth under the common traction drive of feed arrangement and drawing mechanism enters pyroreaction by sealing gland mouth 32
Equipment 3；
2）, by protecting air seal set 31 to be passed through protective gas argon gas, air demand 1m into high-temperature reaction equipment 33/h-10m3/
h；；
3）, before reaction to the slowly pre- heating of high-temperature reaction equipment 3, it is ensured that device interior high-temperature region be in anaerobic state, and heating is fast
Degree is no more than 20 DEG C per hour；When reative cell high-temperature region 39 is heated to 800 DEG C, carburetted hydrogen gas is passed through into reative cell high-temperature region 39
Body methane, air demand 1m3/ h, while hydrogen is passed through again, air demand 0.1m3/ h, for being catalyzed hydrocarbon gas cracking, promote
The formation of graphene, when copper foil pulls out high-temperature reaction equipment 3 through drawing mechanism, graphene is obtained in copper foil surface, formed
Metal foil graphene complex, wherein nickel foil feeding speed are 0.5mm/s；
4), copper foil graphene complex is corroded with the ammonium persulfate aqueous solution that mass concentration is 20%, until copper foil is complete
Full corrosion, stands, takes remaining membranoid substance；
5）, with acetone and deionized water membranoid substance is cleaned repeatedly, produce graphene.
2nd, a kind of graphene
The graphene is prepared using the above method.
Embodiment 3
First, a kind of preparation method of graphene
A kind of preparation method of graphene is based on equipment described in embodiment 1, and methods described utilizes continous way chemical vapor deposition
（CVD）Prepared by method, specifically include following steps：
1）, copper foil is smooth under the common traction drive of feed arrangement and drawing mechanism enters pyroreaction by sealing gland mouth 32
Equipment 3；
2）, by protecting air seal set 31 to be passed through protective gas argon gas, air demand 1m into high-temperature reaction equipment 33/h-10m3/
h；
3）, before reaction to the slowly pre- heating of high-temperature reaction equipment 3, it is ensured that device interior high-temperature region be in anaerobic state, and heating is fast
Degree is no more than 20 degree per hour；When reative cell high-temperature region 39 is heated to 900 DEG C, carburetted hydrogen gas is passed through into reative cell high-temperature region 39
Body methane, air demand 0.6m3/ h, while hydrogen is passed through again, air demand 0.3m3/ h, for being catalyzed hydrocarbon gas cracking, promote
Enter the formation of graphene, when copper foil pulls out high-temperature reaction equipment 3 through drawing mechanism, graphene, shape are obtained in copper foil surface
Into metal foil graphene complex, wherein copper foil feeding speed is 1mm/s；
4), copper foil graphene complex is corroded with the ferric chloride aqueous solutionses that mass concentration is 50%, until copper foil is complete
Full corrosion, stands, takes membranoid substance；
5）, with acetone and deionized water membranoid substance is cleaned repeatedly, produce graphene.
The mass concentration of ferric chloride aqueous solutionses is alternatively 10%, 30% or other mass concentration among the present embodiment,
The speed that copper foil corrodes completely is determined for different mass concentrations.
2nd, a kind of graphene
The graphene is prepared using the above method.
It is suitable for other metallic foils for meeting preparation technology temperature requirement prepare graphene as base material, such as
Fe, Ni, Ru, Co, Rh, Ir, Pd, Pt, Au and Cr-Ni, Au-Ni, Ni-Mo, Co-Ni alloy.
Above is the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise without departing from the principles of the invention, some improvements and modifications can also be made, equipment principle prepares phase as described in utilizing
Similar product or method technique, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
- A kind of 1. production equipment of graphene, it is characterised in that：Including feed arrangement, high-temperature reaction equipment (3) and drawing mechanism, The feed arrangement and drawing mechanism are located at the both sides of the high-temperature reaction equipment (3) respectively, for base material to be drawn through into institute State high-temperature reaction equipment (3)；The high-temperature reaction equipment (3) includes graphite boiler tube (38), induction heating circle (37), reative cell and protection air seal set (31)；The reative cell is located at the inner hub location of high-temperature reaction equipment (3) and prolonged to the both sides of high-temperature reaction equipment (3) Stretch, the protection air seal set (31) is located inside the both ends extension of reative cell；It is anti-that the graphite boiler tube (38) is located at high temperature Answer equipment (3) internal and be distributed on the periphery of reative cell；The induction heating circle (37) is uniformly looped around graphite boiler tube (38) Periphery, for heating graphite boiler tube (38).
- A kind of 2. production equipment of graphene according to claim 1, it is characterised in that：The high-temperature reaction equipment (3) Outside also include cooling jacket (4), cooling jacket (4) both ends are respectively equipped with cooling jacket entrance (41) and cooling water Set outlet (42), wherein cooling jacket entrance (41) are located at the bottom of cooling jacket (4), and cooling jacket outlet (42) is positioned at cooling The top of water jacket (4).
- A kind of 3. production equipment of graphene according to claim 1, it is characterised in that：The high-temperature reaction equipment (3) Bottom is additionally provided with reaction gas inlet (34).
- A kind of 4. production equipment of graphene according to claim 1, it is characterised in that：The protection air seal set (31) For multiple mutually isolated rectangular channels, and the reative cell periphery position relative with protection air seal set (31) is provided with protection gas entrance (33), the protection gas entrance (33) is multiple related rectangular hollow structures penetrated；The reative cell both ends are equipped with sealing gland Mouth (32)；The reative cell is rectangular cavities.
- A kind of 5. production equipment of graphene according to claim 1, it is characterised in that：The feed arrangement and discharging fill Respectively feed roller (2) and discharge roller (5) are put, the feed roller (2) and discharge roller (5) are driven using variable-frequency motor.
- A kind of 6. production equipment of graphene according to claim 1, it is characterised in that：The induction heating circle (37) is Water cooling induction heating circle, formed using hollow copper pipe coiling, powered and driven by external electric supply installation, for heating graphite boiler tube (38)；The periphery of the induction heating circle (37) is also sequentially provided with heat preservation carbon felt (36) and quartz sand (35), the sensing heating It is reative cell high-temperature region (39) to enclose (37) corresponding reaction zone.
- 7. a kind of method that equipment described in any one prepares graphene in 1-6 using claim, it is characterised in that：Using even Prepared by continuous formula chemical vapour deposition technique, including following steps：1）, metal foil set under the common traction drive of feed arrangement and drawing mechanism by sealing gland mouth (32) into pyroreaction Standby (3)；2）, by protecting air seal set (31) to being passed through protective gas in high-temperature reaction equipment (3)；3）, high-temperature reaction equipment (3) is heated up in advance, when reative cell high-temperature region (39) temperature reaches 800 DEG C -1000 DEG C, to anti- Answer in room high-temperature region (39) and be passed through hydrocarbon gas, metal foil pulls out high-temperature reaction equipment (3) through drawing mechanism, in metal foil table Face obtains graphene, forms metal foil graphene complex；4), metal foil graphene complex is corroded with ammonium persulfate aqueous solution or ferric chloride aqueous solutionses, until metal Paper tinsel corrodes completely, stands, takes remaining membranoid substance；5）, membranoid substance is cleaned repeatedly, produce graphene.
- 8. according to the method for claim 7, it is characterised in that：Step 1）Described in metal foil be copper foil；The step 3）In when being heated up in advance to high-temperature reaction equipment (3), programming rate is no more than 20 DEG C per hour.
- 9. according to the method for claim 7, it is characterised in that：Step 3）Described in protective gas be argon gas or nitrogen； The hydrocarbon gas are one kind in methane, ethane, propane, ethene, propylene, acetylene and propine, and its air demand is 0.1m3/h- 1m3/h；When reative cell high-temperature region (39) are heated to 800 DEG C -1000 DEG C, hydrocarbon class gas is passed through to reative cell high-temperature region (39) are interior Hydrogen is also passed through while body, for being catalyzed hydrocarbon gas cracking, promotes the formation of graphene, its air demand is 0.1m3/h- 0.5m3/h；Wherein metal foil feeding speed is 0.5-2mm/s；Step 4）Described in the mass concentration of ammonium persulfate aqueous solution be 10%-20%, the mass concentration of ferric chloride aqueous solutionses is 10%-50%；Step 5）It is middle that membranoid substance is cleaned repeatedly using acetone and deionized water.
- A kind of 10. graphene, it is characterised in that：The graphene utilizes any one methods described in claim 7-9 to prepare Form.
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| CN112723347A (en) * | 2021-01-28 | 2021-04-30 | 孙华 | Large-scale preparation equipment for CVD deposited graphene |
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| US20140367891A1 (en) * | 2013-06-13 | 2014-12-18 | Donald James Dawson | Method and apparatus for manufacturing graphene |
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Application publication date: 20171208 |