CN106365154A - Preparation method of graphene grown by adopting non-high temperature liquid phase method - Google Patents
Preparation method of graphene grown by adopting non-high temperature liquid phase method Download PDFInfo
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- CN106365154A CN106365154A CN201610769878.0A CN201610769878A CN106365154A CN 106365154 A CN106365154 A CN 106365154A CN 201610769878 A CN201610769878 A CN 201610769878A CN 106365154 A CN106365154 A CN 106365154A
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Abstract
The invention relates to a preparation method of graphene grown by adopting a non-high temperature liquid phase method. The preparation method is technically characterized by comprising the following steps: igniting a cold plasma in protective gas, putting a non-high temperature organic solvent in the plasma, then introducing a gaseous or liquid carbon source into the ignited cold plasma, activating and cracking the gaseous carbon source or activating and cracking the evaporated liquid carbon source and fully dissolving cracked carbon in the organic solvent; immersing a super-cooled target film into the organic solvent, so that the carbon dissolved in the organic solvent is subjected to supersaturated precipitation on the super-cooled target film, and a grapheme film is formed on the super-cooled target film. The graphene prepared by the preparation method of the graphene grown by adopting the non-high temperature liquid phase method, provided by the invention, has the advantages of being good in quality, low in cost, high in efficiency and less in pollution and can directly grow on the target film without transfer.
Description
Technical field
The present invention relates to field of new material preparation, specifically a kind of preparation side of non high temperature liquid phase method growth Graphene
Method.
Background technology
Graphene be a kind of by carbon atom with sp2Hydridization and the two dimensional crystal with honeycomb lattice that formed.2004, English
The An Deliehaimu of University of Manchester of state and Constantine's Nuo Woxiao love successfully isolate Graphene from graphite,
And therefore obtain Nobel Prize in physics in 2010.
Graphene has excellent performance.First, the specific surface area of Graphene is very big, up to 2630m2/g.Secondly, stone
Carbon atom in black alkene is with sp2Mode hydridization, it is stable that three carbon atoms that each carbon atom is adjacent pass through σ bond formed
Carbon-carbon bond, thus make Graphene have high mechanical property, its Young's modulus up to 1100gpa, fracture strength up to
130gpa.Again, the pi-electron delocalization in Graphene forms big π key, and pi-electron can move freely, therefore Graphene have excellent
Electric conductivity, its carrier mobility speed may be up to 2 × 105cm2·v-1·s-1, and resistivity only has 10-8ωm.In addition, stone
Black alkene also has good optical property, thermal property and magnetic performance etc..Therefore, Graphene has huge potential application valency
Value is it is considered to be one of contemporary most important new material.
At present, the preparation method of Graphene can be divided into method and from bottom to top method from top to bottom, and wherein, graphite oxide reduces
Method is the main method in method from top to bottom；Chemical vapor deposition (cvd) epitaxial growth method is the main side in method from bottom to top
Method；The method that bed of molten salt prepares Graphene is another kind of method growing Graphene from bottom to top.The subject matter of said method
It is:
1st, graphene oxide go poor performance, defect is many, and pollution is big.Graphene oxide typically adopts improved hummers method, even if
After concentrated sulphuric acid, sodium nitrate and potassium permanganate and graphite vigorous reaction, dilute reduction with hydrogen peroxide, purer through ion exchange
Change, be dried, obtain graphene oxide go.Typically redox graphene rgo can be obtained as reducing agent using hydrazine.So
Preparation product necessarily carry substantial amounts of phenolic group and carboxyl, intrinsic on there is substantial amounts of defect (10～15%), lose excellent
Good electric conductivity.Defect is more and powdered is not so that go mechanical property is also high.Stable processing technique is poor, product structure
There is uncertainty, production process uses strong acid and strong oxidizer, environmental pollution is big, processing cost is high.
2nd, cvd method Graphene performance is good, but cost is very high, and production efficiency is extremely low.The method is to be filled with carbon source at high temperature
Gas (as methane, ethane, acetylene etc.), carbon-source gas decompose and form Graphene on substrate.This method can be in substrate
(such as copper substrate) is upper to form high-quality graphene, but requires strict, response time length, low yield to device and working condition
Under, with high costs.Particularly, it is difficult to from lining in the Graphene of the upper growth of substrate (as copper, nickel, carborundum etc.) by this method
Shift on bottom；Generally require using radical approach such as strong acid burn into high-temperature gasifications during transfer, this has resulted in high cost, environment
Pollution is big, and can damage Graphene finished product.
Although the 3, bed of molten salt is prepared the method for Graphene and can be prepared the Graphene of superior performance at lower cost, made
The Graphene becoming is powder body, coats film forming, need to solve dispersed, bonding, solidification during application after generally requiring to make slurry
Etc. many technological problemses.And, the Graphene number of plies that this method produces, size and quality etc. are all more difficult to be controlled it is impossible to obtain high-quality
The graphene film of amount.
Content of the invention
The purpose of the present invention is aiming at above-mentioned technical problem, proposes that a kind of performance quality is excellent, cost is relatively low, efficiency relatively
Preparation method high, of reduced contamination, that the non high temperature liquid phase method growth Graphene need not shift can be grown directly upon on aimed thin film.
A kind of non high temperature liquid phase method of the present invention grows the preparation method of Graphene, and it is technically characterized in that preparation method bag
Include following steps: the cold plasma being placed in protective gas in reative cell is lighted, be placed with non-in this plasma
The organic solvent of high temperature, then gaseous state or liquid carbon source is introduced in the cold plasma lighted, above-mentioned gaseous carbon source is activated
Cracking or liquid carbon source evaporate postactivated cracking, and the carbon after cracking fully dissolves in above-mentioned organic solvent；By supercool target
Thin film immerses organic solvent so that the supersaturation on supercool aimed thin film of the carbon of dissolving separates out, supercool in organic solvent
Graphene film is formed on aimed thin film.Above-mentioned gaseous state or liquid carbon source at least include aliphatic hydrocarbon, aromatic hydrocarbon, in hydrocarbon derivative
A kind of.
The above-mentioned organic solvent having dissolved carbon also can be by the container of pipeline transportation to another reative cell；Will be supercool
Aimed thin film immerses above-mentioned organic solvent so that the supersaturation on supercool aimed thin film of the carbon of dissolving separates out in organic solvent,
Graphene film is formed on supercool aimed thin film.
Described gaseous state or liquid carbon source at least include one of aliphatic hydrocarbon, aromatic hydrocarbon, hydrocarbon derivative.
Described protective gas is at least one of nitrogen, argon, hydrogen, ammonia.
Described supercool aimed thin film immersion organic solvent can adopt " volume to volume (r2r) " continuous processing mode, supercool
The temperature of aimed thin film is less than the temperature of organic solvent, and aimed thin film puts mode using three stackings, and two outer layers have for macromolecule
Machine thin film, intermediate layer is heat conducting film.
During described carbon dissolution separates out, at least using in copper, copper-bearing alloy, nickel, nickel-containing alloys, platinum, platinum rhodium
Plant as catalyst.
It is higher than the boiling point less than organic solvent for the temperature of organic solvent after described catalyst is heated when using.
Graphene crystal seed is added in the machine solvent of described non high temperature.
A kind of non high temperature liquid phase method of the present invention grows the preparation method of Graphene, is using in solid substrate to existing
The breakthrough of vapour deposition Graphene method, is also the improvement that prepared by bed of molten salt method with Graphene method, has following three big advantages:
1, compared with graphene oxide, the Graphene performance of present invention preparation is good, and low cost pollutes little, efficiency high, ratio of defects ratio
The low several orders of magnitude of graphene oxide, are a kind of cost large-scale production electron level Graphenes that can be less than graphene oxide
Method..
2, compared with cvd method Graphene, low cost of the present invention, efficiency high.Because Graphene is grown directly upon aimed thin film
On need not shift, solve puzzlement scientific research and engineering technological Graphene transport difficulties, cost can be low more several than conventional cvd method
The individual order of magnitude, efficiency then has 100,000 times of raising.In addition, liquid phase is compared with gas phase, crystalline quality is good, and long crystalline substance speed is fast.
3, compared with molten-salt growth method Graphene, performance is excellent, and quality is good, efficiency high, and pollution is little.Product different from molten-salt growth method is
Powder, present invention preparation is high-quality graphene film, and can adopt " volume to volume (r2r) " continuous production processes, raw
Produce in hgher efficiency, eliminate water elution and remove inorganic salt, the processing step such as filter centrifugation separation, pollution is less, and cost is lower.
Therefore, a kind of non high temperature liquid phase method of the present invention grows the preparation method of Graphene, and prepared Graphene is realized
Performance quality is excellent, low cost, efficiency high, pollution less, the purpose need not shift can be grown directly upon on aimed thin film.
Brief description
Fig. 1 is the schematic flow sheet that non high temperature liquid phase method of the present invention grows Graphene embodiment one.
Fig. 2 is the schematic flow sheet that non high temperature liquid phase method of the present invention grows Graphene embodiment two.
Specific embodiment
The invention will be further described to pass through embodiment below in conjunction with the accompanying drawings:
Embodiment one:
As shown in figure 1, a kind of non high temperature liquid phase method of the present invention grows the preparation method of Graphene, it is technically characterized in that preparation
Method comprises the steps: that a kind of non high temperature liquid phase method grows the preparation method of Graphene, and it is technically characterized in that preparation method
Comprise the steps: that the cold plasma 3 being placed in reative cell 2 in protective gas is lighted, place in this plasma 3
There is the container 4 of the organic solvent 5 of non high temperature, then gaseous carbon source 1 is introduced in the cold plasma 3 lighted, above-mentioned gaseous carbon
Source is activated cracking or liquid carbon source evaporates postactivated cracking, and the carbon after cracking fully dissolves in above-mentioned organic solvent 5；Pass through
Supercool aimed thin film 7 is immersed dynamic device 8 organic solvent 5 so that the carbon of dissolving is in supercool target thin in organic solvent 5
On film 7, supersaturation separates out, and forms graphene film on supercool aimed thin film 7.
Specifically, normal pressure microwave (2.5ghz) plasma reactor used as discussed above is as reative cell 2, continue with
Argon, as protective gas, argon plasma 3 is lighted and is kept, and the container 4 filling organic solvent (js-eph) 5 is placed in instead
Answer room 2, not higher than 180 DEG C of the temperature of organic solvent (js-eph) 5；Acetylene gas 1 are injected cold plasma 3 as carbon source
In, acetylene 1 cracks in cold plasma 3；After activation cleavage reaction occurs, the carbon dissolution of cracking is organic in container 4
In solvent (js-eph) 5 and reach saturation；Thin film 7 is closed in three stackings being wound into a roll, and two outer layers are pet thin film, middle
Layer be graphite guide hotting mask, supercool be cooled to 40 DEG C, then by move device 8, unreel, thin film 7 immersed the organic molten of container 4
In agent (js-eph) 5；Local induction heating placed by container 4 and persistently the copper mesh of 200 DEG C of holding and nickel screen 6 are as catalyst, same
When add a small amount of single-layer graphene kind brilliant, the supercooling temperature of thin film 7 makes the carbon dissolving supersaturation on thin film 7 separate out, from
And graphene film is formed on described aimed thin film 7, then moved by dynamic device 8, winding, finally give and be grown in pet
Graphene on film.
The Graphene that said method obtains is the uniformly continuous graphite crystal film of 1～3 atomic layers thick.
Embodiment two
A kind of non high temperature liquid phase method of the present invention grows the preparation method of Graphene, its be technically characterized in that preparation method include as
Lower step: a kind of non high temperature liquid phase method grows the preparation method of Graphene, and it is technically characterized in that preparation method includes walking as follows
Rapid: the cold plasma 3 being placed in protective gas in reative cell 2 is lighted, it is placed with non high temperature in this plasma 3
The container 4 of organic solvent 5, then liquid carbon source 1 is introduced in the cold plasma 3 lighted, above-mentioned gaseous carbon source is activated splitting
Solution or liquid carbon source evaporate postactivated cracking, and the carbon after cracking fully dissolves in above-mentioned organic solvent 5；Above-mentioned dissolve carbon
Organic solvent 5 be transported in the container 11 of another reative cell 10 by pipeline 9；Supercool aimed thin film 7 is immersed organic molten
Agent 5 so that in organic solvent 5 dissolving carbon on supercool aimed thin film 7 supersaturation separate out, on supercool aimed thin film 7
Form graphene film.
Specifically, normal pressure microwave (2.5ghz) plasma reactor used as discussed above is as reative cell 2, with argon
As protective gas, argon plasma 3 is lighted and keeps；The container 4 filling organic solvent (tdph) 5 is placed in reative cell 2,
The container 11 filling organic solvent (tdph) 5 is placed in reative cell 10, reative cell 10 is using argon and hydrogen as shielding gas simultaneously
Body；With pipeline 9 by container 4 and container 11 UNICOM, the temperature of organic solvent (tdph) 5 is not higher than 190 DEG C；Using the second as carbon source
In alcohol 1 injection plasma 3, ethanol 1 drop evaporates in plasma 3 and cracks；After activation cleavage reaction occurs, split
The carbon dissolution of solution and reaches saturation in the organic solvent (tdph) 5 of container 4；The carbon of dissolving is transported to by unicom pipeline 9
Container 11, organic solvent (tdph) 5 temperature in container 4 and container 11 are equal, and the dissolubility of carbon is identical；Three layers being wound into a roll
Overlapping thin film 7, two outer layers are pet thin film, and intermediate layer is graphite guide hotting mask, supercool be cooled to 40 DEG C, then pass through dynamic dress
Put 8, unreel, thin film is immersed in the organic solvent (tdph) 5 of container 11.Place local induction heating in container 11 and persistently protect
Hold 200 DEG C of copper mesh and nickel screen 6 as catalyst, be simultaneously introduced that a small amount of single-layer graphene kind is brilliant, thin film 7 supercooling temperature makes
The supersaturation on thin film 7 of the carbon of dissolving separates out, thus forming graphene film on described aimed thin film 7, then passes through dynamic dress
Put 8, wind, finally give the Graphene being grown on pet film.
The Graphene that said method obtains is the uniformly continuous graphite crystal film of 1～2 atomic layers thick.
Above-mentioned Graphene is easy to, and such as by thermal transfer, transfers in the substrate of needs.
Claims (8)
1. a kind of non high temperature liquid phase method grows the preparation method of Graphene, and it is technically characterized in that preparation method includes walking as follows
Rapid: the cold plasma being placed in protective gas in reative cell is lighted, this plasma is placed with having of non high temperature
Machine solvent, then gaseous state or liquid carbon source is introduced in the cold plasma lighted, and above-mentioned gaseous carbon source is activated cracking or liquid
State carbon source evaporates postactivated cracking, and the carbon after cracking fully dissolves in above-mentioned organic solvent；By supercool aimed thin film immersion
Organic solvent so that in organic solvent dissolving carbon on supercool aimed thin film supersaturation separate out, in supercool aimed thin film
Upper formation graphene film.
2. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that above-mentioned
The organic solvent having dissolved carbon passes through pipeline transportation to the container of another reative cell；Supercool aimed thin film is immersed above-mentioned
Organic solvent so that in organic solvent dissolving carbon on supercool aimed thin film supersaturation separate out, in supercool aimed thin film
Upper formation graphene film.
3. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that described
Gaseous state or liquid carbon source at least include one of aliphatic hydrocarbon, aromatic hydrocarbon, hydrocarbon derivative.
4. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that described
Protective gas is at least one of nitrogen, argon, hydrogen, ammonia.
5. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that described
Supercool aimed thin film immersion organic solvent can adopt " volume to volume (r2r) " continuous processing mode, the temperature of supercool aimed thin film
Degree puts mode less than the temperature of organic solvent, aimed thin film using three stackings, and two outer layers are macromolecule organic film, intermediate layer
For heat conducting film.
6. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that described
During carbon dissolution separates out, copper, copper-bearing alloy, nickel, nickel-containing alloys, platinum, platinum rhodium one of are at least used as catalyst.
7. a kind of non high temperature liquid phase method according to claim 6 grows the preparation method of Graphene it is characterised in that described
It is higher than the boiling point less than organic solvent for the temperature of organic solvent after catalyst is heated when using.
8. a kind of non high temperature liquid phase method according to claim 1 grows the preparation method of Graphene it is characterised in that described
Graphene crystal seed is added in the machine solvent of non high temperature.
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Cited By (4)
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| CN107119316A (en) * | 2017-04-13 | 2017-09-01 | 孙旭阳 | A kind of temperature-varying zone liquid bed Direct precipitation grows the preparation method of graphene |
| CN110983302A (en) * | 2019-12-30 | 2020-04-10 | 宁波柔碳电子科技有限公司 | Roll-to-roll graphene film growth equipment and roll-to-roll graphene film growth method |
| CN112778823A (en) * | 2021-01-27 | 2021-05-11 | 九江纳维新材料科技有限公司 | Ultra-high conductivity electronic grade graphene-silver composite conductive UV curing ink and preparation method and application thereof |
| CN115159510A (en) * | 2022-07-11 | 2022-10-11 | 常州二维碳素科技股份有限公司 | Graphene heat-conducting film and method for efficiently producing graphene heat-conducting film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115159510A (en) * | 2022-07-11 | 2022-10-11 | 常州二维碳素科技股份有限公司 | Graphene heat-conducting film and method for efficiently producing graphene heat-conducting film |
| CN115159510B (en) * | 2022-07-11 | 2023-12-29 | 常州二维碳素科技股份有限公司 | Graphene heat conduction film and method for efficiently producing graphene heat conduction film |
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