CN106829940A - The production equipment and its production technology of a kind of grapheme material - Google Patents
The production equipment and its production technology of a kind of grapheme material Download PDFInfo
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- CN106829940A CN106829940A CN201710208727.2A CN201710208727A CN106829940A CN 106829940 A CN106829940 A CN 106829940A CN 201710208727 A CN201710208727 A CN 201710208727A CN 106829940 A CN106829940 A CN 106829940A
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Abstract
A kind of production technology of grapheme material, comprises the following steps：By in graphite composite powder addition high-pressure bottle；Inert gas is poured in high-pressure bottle, it is 1,000 10000 atmospheric pressure for pressure to control the pressure in high-pressure bottle；Give high-pressure bottle outside uniform heating by heating furnace, control temperature uniformly rises to 1600 DEG C from 200 DEG C；Then so that high-pressure bottle is incubated 30 60 minutes；So that Inert gas molecule is full of in gap of the crystalline flake graphite layer with layer；The pressure of high-pressure bottle is discharged into normal pressure by moment, and Inert gas molecule instantaneous expansion separates graphite linings with layer, forms single-layer graphene material；And the single-layer graphene material of preparation is discharged into cooling device uses Water spray；Suspension in water is collected to dry and can obtain single-layer graphene material.Present invention process is simple, easy to operate, can be quick and inexpensive prepare Graphene, brought great convenience to production.
Description
Technical field
The invention belongs to the preparation of Graphene, the production equipment and its production technology of specially a kind of grapheme material.
Background technology
Graphite is carbonaceous element crystalline mineral, and its crystallization screen work is hexagon layer structure.Distance between each stratum reticulare
It is 3.40, the spacing of carbon atom is 1.42 in same stratum reticulare.Category hexagonal crystal system, has complete stratiform cleavage.Cleavage surface with point
It is weaker to van der Waals' force based on sub-key, therefore its native floatability is fine.Graphite and diamond, carbon 60, CNT etc. are all
The simple substance of carbon, their allotropes each other.In graphite crystal, covalent bond is formed with sp2 hydridization with the carbon atom of layer,
Each carbon atom is connected with three covalent bonds with the other three atom.Six carbon atom forms positive six in approximately the same plane
The ring of shape, is extended into lamellar structure repeatedly, and the bond distance of C-C keys is all 142pm here, and this just belongs to bond distance's model of atomic crystal
Enclose, therefore for same layer, it is atomic crystal.Carbon atom on the same plane is also each to remain next p tracks, their phases
Mutually overlap.Electronics is freer, and equivalent to the free electron in metal, so the heat conduction of graphite energy and conduction, this exactly metal is brilliant
Body characteristicses.Therefore metallic crystal is also ranged.It is separated by 340pm in graphite crystal between layers, it is in larger distance, it is with Van der Waals
What power combined, i.e., belong to molecular crystal between layers.But, due to being combined very between the carbon atom on same plane layer
By force, it is extremely difficult to destroy, so the molten point of graphite is also very high, chemical property is also stablized.In view of its special bonding mode, it is impossible to single
One is considered monocrystal or polycrystal, generally believes that graphite is a kind of mixed crystal now.Graphite is due to its special knot
Structure, and there is following special nature：Heat-resisting quantity：The fusing point of graphite is 3850 ± 50 DEG C, and boiling point is 4250 DEG C, even if through superelevation
Warm electric arc calcination, the loss very little of weight, thermal coefficient of expansion also very little.Graphite intensity is improved and strengthened with temperature, at 2000 DEG C
When, graphite intensity is doubled.Conductive, thermal conductivity：The electric conductivity of graphite is higher than general nonmetallic ore 100 times.Thermal conductivity exceedes
The metal materials such as steel, iron, lead.Thermal conductivity factor is raised and reduced with temperature, or even at very high temperatures, graphite is into heat guard.
Graphite can be conductive because each carbon atom only forms 3 covalent bonds with other carbon atoms in graphite, and each carbon atom is still
Retain 1 free electron to transmit electric charge.Lubricity：The greasy property of graphite depends on the size of graphite flakes, and scale is bigger,
Coefficient of friction is smaller, and greasy property is better.Chemical stability：Graphite has good chemical stability at normal temperatures, can be acidproof, resistance to
The corrosion of alkali and organic solvent-resistant.Plasticity：The good toughness of graphite, can be ground into very thin thin slice.Thermal shock resistance：Graphite is in normal temperature
Lower to be able to take the acute variation of temperature and destroy when using, during temperature jump, the Volume Changes of graphite less, will not be produced
Raw crackle.Graphene is a kind of two dimensional crystal, and the common graphite of people is the planar carbon by being arranged with honeycomb-patterned ordered from level to level
What atom was stacked and formed, the interlaminar action power of graphite is weaker, it is easy to peel off mutually, forms very thin graphite flake.When stone
Ink sheet is shelled into after individual layer, and the individual layer of this only one of which carbon atom thickness is exactly Graphene.The latest find of Graphene is people
In terms of anticorrosion most efficient method.Conventional polymer coating is easy to be scraped off, and reduces protective value；And graphite
Alkene does diaphragm, has significantly delayed corrosion of metal speed, firmer antibody Monoclonal.Graphene is not only the new of electronic industry
Star, the future for being applied to traditional industry is also limitless.Its application direction：The fields such as marine anticorrosion, anti-corrosion of metal, heavy antisepsis.
Graphene has good heat conduction, electric conductivity.Graphene is a kind of two dimensional crystal, is arranged according to hexagon by carbon atom
Cloth, is connected with each other, and forms a carbon molecule, and its structure is highly stable；As the amount of carbon atom for being connected is on the increase, this
The carbon planes of molecules of two dimension constantly expands, and molecule also constantly becomes big.The thickness of single-layer graphene only one of which carbon atom, i.e.,
0.335 nanometer, equivalent to a thickness for 20 a ten thousandths of hair, will nearly there are 1,500,000 layers or so in the graphite of 1 millimeters thick
Graphene.Graphene is a kind of known most thin material, and with high specific surface area, superpower electric conductivity and strong
The advantages of spending.The presence of above-mentioned advantage is that it possesses good market prospects.Graphene（Graphene）Name from English
Graphite (graphite)+- ene (alkenes ending).It is considered as always hypothetical structure, it is impossible to which individually stabilization is deposited
.Common manufacturing method：Tear tape method/slight rubbing manipulation：Most common is micromechanics partition method, directly by graphene platelet from
Cut down on larger crystal.2004, extra large nurse etc. prepared single-layer graphene in this way, it is possible in extraneous ring
Stable existence under border.Exemplary manufacturing process is that the pyrolytic graphite of or introducing defect expanded with another material is rubbed,
The surface of body phase graphite can produce the crystal of flocculus shape, the Graphene containing individual layer in the crystal of these flocculus shapes.But shortcoming
The graphene platelet of to be this method filtered out using the thin slice of the graphite surface acquisition that rubs individual layer, its size is difficult to control, it is impossible to
Reliably factory length foot supply graphite flake sample.Epitaxy method：Epitaxy method is using growth substrate atom
Structure " kind " goes out Graphene, allows carbon atom that ruthenium is penetrated at 1150 DEG C first, then cools down, and after being cooled to 850 DEG C, absorbs before
A large amount of carbon atoms will float to ruthenium surface, the carbon atom of the individual layer of lens shape has been covered with whole stromal surface, it is final they
A complete layer graphene can be grown up to.After ground floor covering 80%, the second layer starts growth.The Graphene of bottom can be produced with ruthenium
Strong interaction, and be just almost kept completely separate with ruthenium after the second layer, only remaining light current coupling, the single-layer graphene for obtaining is thin
Piece performance is satisfactory.But the graphene platelet for producing in this way is often in uneven thickness, and Graphene and matrix it
Between bonding can influence the characteristic of carbon-coating.Silicon carbide epitaxial growth method：The method is to remove silicon by heating monocrystalline silicon carbide
, graphene sheet layer is decomposited on monocrystalline (0001) face.Detailed process is：The sample that will be obtained through oxygen or hydrogen etching processing
Product are heated by electron bombardment under a high vacuum, remove oxide.The oxide quilt completely on surface is determined with Auger electron spectroscopy
After removal, sample heating is allowed to constant temperature 1-20min after temperature is increased to 1250-1450 DEG C, so as to form very thin graphite linings.
Up to 100 layers of multi-layer graphene is become more readily available on C-terminated surfaces.Its thickness is determined by heating-up temperature, prepared
Large area has the Graphene of single thickness relatively difficult；Aoxidize thinning graphite flake method：Graphene can also be by heated oxide
Method graphite flake thinning layer by layer, so as to obtain single, double layer graphene.Hydrazine reducing process：Graphene oxide paper is inserted
Pure hydrazine solution（A kind of compound of hydrogen atom and nitrogen-atoms）, this solution can make graphene oxide paper be reduced to mono-layer graphite
Alkene.Cutting carbon nanotubes method：Cutting carbon nanotubes are also the method just in test for manufacturing graphene ribbon.One of which method
With potassinm permanganate and sulfuric acid incision multilayer wall carbon nano tube in the solution.Another method uses plasma etching one
Divide the nanotube for being embedded in polymer.Current grapheme material volume production is relatively difficult, and reaction condition is complicated, high cost.
The content of the invention
It is an object of the invention to provide a kind of production technology of grapheme material, in solving the problems, such as background technology.
The present invention is realized using following technical scheme：
A kind of production equipment of grapheme material, including band valve inlet, dog-house, high-pressure bottle, band valve discharging tube, band
Filter screen pressure-reducing valve, water inlet pipe, band valve discharging tube, non-pressure vessel and heating furnace, the high-pressure bottle top are provided with dog-house,
The high-pressure bottle middle part is communicated with band valve inlet, and the high-pressure bottle bottom is provided with heating furnace, the high-pressure bottle
Connected by band valve discharging tube between non-pressure vessel, the non-pressure vessel top is provided with band filter screen pressure-reducing valve, described normal
Pressure vessel middle part is provided with water inlet pipe, and the bottom of the non-pressure vessel is provided with band valve discharging tube.The high-pressure bottle is high
Strength seal metal can.
A kind of production technology of grapheme material, comprises the following steps：
S1：By in graphite composite powder addition high-pressure bottle；
S2：Inert gas is poured in high-pressure bottle, it is 1000-10000 air for pressure to control the pressure in high-pressure bottle
Pressure；
S3：Give high-pressure bottle outside uniform heating by heating furnace, control temperature uniformly rises to 1600 DEG C from 200 DEG C；So
Afterwards so that high-pressure bottle is incubated 30-60 minutes；So that inert gas is full of in crystalline flake graphite；Graphite flakes are peeled away, shape
Into single-layer graphene material；
S4：The pressure of high-pressure bottle is discharged into normal pressure by moment；And the single-layer graphene material of preparation is discharged into cooling device
In use Water spray；Suspension in water is collected to dry and can obtain single-layer graphene material.
In the present invention, inert gas is the one or two kinds of in nitrogen or helium.
Beneficial effect：Present invention process is simple, easy to operate, can be quick and inexpensive prepare Graphene, give production band
Very big facility is carried out.
Brief description of the drawings
Fig. 1 is the structural representation of production equipment of the present invention.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Conjunction is specifically illustrating, and the present invention is expanded on further.
Referring to Fig. 1, a kind of structural representation of the production equipment of grapheme material, a kind of production of grapheme material sets
It is standby, including band valve inlet 1, dog-house 2, high-pressure bottle 3, band valve discharging tube 4, band filter screen pressure-reducing valve 5, water inlet pipe 6, band
Valve discharging tube 7, non-pressure vessel 8 and heating furnace 9, the top of the high-pressure bottle 3 are provided with dog-house 2, in the high-pressure bottle 3
Portion is communicated with band valve inlet 1, and the bottom of the high-pressure bottle 3 is provided with heating furnace 9, the high-pressure bottle 3 and non-pressure vessel 8
Between connected by band valve discharging tube 4, the top of the non-pressure vessel 8 is provided with band filter screen pressure-reducing valve 5, the non-pressure vessel 8
Middle part is provided with water inlet pipe 6, and the bottom of the non-pressure vessel 8 is provided with band valve discharging tube 7.The high-pressure bottle 3 is high-strength
Degree sealing metal tank body.
A kind of production technology of grapheme material, comprises the following steps：
S1：By in graphite composite powder addition high-pressure bottle 3；
S2：Inert gas is poured in high-pressure bottle 3, it is 1000-10000 big for pressure to control the pressure in high-pressure bottle 3
Air pressure；
S3：Give the outside of high-pressure bottle 3 uniform heating by heating furnace 9, control temperature uniformly rises to 1600 DEG C from 200 DEG C；
Then so that high-pressure bottle 3 is incubated 30-60 minutes；So that inert gas is full of in crystalline flake graphite；Graphite flakes are peeled away,
Form single-layer graphene material；
S4：The pressure of high-pressure bottle 3 is discharged into normal pressure by moment；And the single-layer graphene material of preparation is discharged into cooling device
In use Water spray；Suspension in water is collected to dry and can obtain single-layer graphene material.
In the present invention, inert gas is the one or two kinds of in nitrogen or helium.
Embodiment 1
By in graphite composite powder addition high-pressure bottle 3；Inert gas, the pressure in control high-pressure bottle 3 are poured in high-pressure bottle 3
For pressure is 8000 atmospheric pressure；Give the outside of high-pressure bottle 3 uniform heating by heating furnace 9, control temperature is uniform from 200 DEG C
Rise to 1600 DEG C；Then so that high-pressure bottle 3 is incubated 40 minutes；So that inert gas is full of in crystalline flake graphite；By graphite
Scale is peeled away, and forms single-layer graphene material；The pressure of high-pressure bottle 3 is discharged into normal pressure by moment；And the individual layer that will be prepared
Grapheme material uses Water spray in being discharged into cooling device；Suspension in water is collected to dry and can obtain single-layer graphene material
Material.
Embodiment 2
By in graphite composite powder addition high-pressure bottle 3；Inert gas, the pressure in control high-pressure bottle 3 are poured in high-pressure bottle 3
For pressure is 7000 atmospheric pressure；Give the outside of high-pressure bottle 3 uniform heating by heating furnace 9, control temperature is uniform from 200 DEG C
Rise to 1600 DEG C；Then so that high-pressure bottle 3 is incubated 45 minutes；So that inert gas is full of in crystalline flake graphite；By graphite
Scale is peeled away, and forms single-layer graphene material；The pressure of high-pressure bottle 3 is discharged into normal pressure by moment；And the individual layer that will be prepared
Grapheme material uses Water spray in being discharged into cooling device；Suspension in water is collected to dry and can obtain single-layer graphene material
Material.
Embodiment 3
By in graphite composite powder addition high-pressure bottle 3；Inert gas, the pressure in control high-pressure bottle 3 are poured in high-pressure bottle 3
For pressure is 5000 atmospheric pressure；Give the outside of high-pressure bottle 3 uniform heating by heating furnace 9, control temperature is uniform from 200 DEG C
Rise to 1600 DEG C；Then so that high-pressure bottle 3 is incubated 55 minutes；So that inert gas is full of in crystalline flake graphite；By graphite
Scale is peeled away, and forms single-layer graphene material；The pressure of high-pressure bottle 3 is discharged into normal pressure by moment；And the individual layer that will be prepared
Grapheme material uses Water spray in being discharged into cooling device；Suspension in water is collected to dry and can obtain single-layer graphene material
Material.
General principle of the invention and principal character and advantages of the present invention, the technology of the industry has been shown and described above
Personnel it should be appreciated that the present invention is not limited to the above embodiments, simply explanation described in above-described embodiment and specification this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention, the claimed scope of the invention by appending claims and its
Equivalent thereof.
Claims (4)
1. a kind of production equipment of grapheme material, including band valve inlet, dog-house, high-pressure bottle, band valve discharging tube,
Band filter screen pressure-reducing valve, water inlet pipe, band valve discharging tube, non-pressure vessel and heating furnace, it is characterised in that the high-pressure bottle top
Dog-house is provided with, the high-pressure bottle middle part is communicated with band valve inlet, and the high-pressure bottle bottom is provided with heating furnace,
Connected by band valve discharging tube between the high-pressure bottle and non-pressure vessel, the non-pressure vessel top is provided with band filter screen and subtracts
Pressure valve, the non-pressure vessel middle part is provided with water inlet pipe, and the bottom of the non-pressure vessel is provided with band valve discharging tube.
2. the production equipment of a kind of grapheme material according to claim 1, it is characterised in that the high-pressure bottle is high
Strength seal metal can.
3. a kind of production technology of grapheme material, comprises the following steps：
S1：By in graphite composite powder addition high-pressure bottle；
S2：Inert gas is poured in high-pressure bottle, it is 1000-10000 air for pressure to control the pressure in high-pressure bottle
Pressure；
S3：Give high-pressure bottle outside uniform heating by heating furnace, control temperature uniformly rises to 1600 DEG C from 200 DEG C；So
Afterwards so that high-pressure bottle is incubated 30-60 minutes；So that inert gas is full of in crystalline flake graphite；Graphite flakes are peeled away, shape
Into single-layer graphene material；
S4：The pressure of high-pressure bottle is discharged into normal pressure by moment；And the single-layer graphene material of preparation is discharged into cooling device
In use Water spray；Suspension in water is collected to dry and can obtain single-layer graphene material.
4. the production technology of a kind of grapheme material according to claim 1, it is characterised in that inert gas be nitrogen or
One or two kinds of in person's helium.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601478A (en) * | 2017-10-13 | 2018-01-19 | 东北大学 | A kind of preparation method of graphene |
| CN113680299A (en) * | 2021-09-02 | 2021-11-23 | 青岛超晟纳米新材料科技有限公司 | Cold wall reactor |
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| CN102992315A (en) * | 2013-01-17 | 2013-03-27 | 余美群 | Device for preparing graphene |
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| CN104386675A (en) * | 2014-11-03 | 2015-03-04 | 黄德欢 | Method for preparing graphene from solid carbon source |
| CN105417523A (en) * | 2015-07-14 | 2016-03-23 | 张亚妮 | Low-cost and large-scale production process of graphene nano powders and device used for same |
| CN105752972A (en) * | 2016-03-30 | 2016-07-13 | 成都新柯力化工科技有限公司 | Method for preparing graphene material from inorganic laminates through high-pressure draft stripping |
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2017
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| CN102992315A (en) * | 2013-01-17 | 2013-03-27 | 余美群 | Device for preparing graphene |
| CN103935991A (en) * | 2014-04-23 | 2014-07-23 | 中国科学院山西煤炭化学研究所 | Method for large-scale continuous preparation of high-quality graphene |
| CN104386675A (en) * | 2014-11-03 | 2015-03-04 | 黄德欢 | Method for preparing graphene from solid carbon source |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107601478A (en) * | 2017-10-13 | 2018-01-19 | 东北大学 | A kind of preparation method of graphene |
| CN113680299A (en) * | 2021-09-02 | 2021-11-23 | 青岛超晟纳米新材料科技有限公司 | Cold wall reactor |
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Application publication date: 20170613 |