CN108190868A - A kind of preparation method of grapheme material - Google Patents
A kind of preparation method of grapheme material Download PDFInfo
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- CN108190868A CN108190868A CN201810181284.7A CN201810181284A CN108190868A CN 108190868 A CN108190868 A CN 108190868A CN 201810181284 A CN201810181284 A CN 201810181284A CN 108190868 A CN108190868 A CN 108190868A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention belongs to technical field of graphene, and in particular to step 1 a kind of preparation method of grapheme material, is added graphene oxide into absolute ethyl alcohol, 30 60min of ultrasonic disperse obtains graphite oxide enol liquid；Step 2,60 120min of ultrasonic disperse in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion；Step 3, graphene oxide dispersion is put into pressurization 2 4h of microwave reaction in reaction kettle, constant pressure reacts 1 3h, is quickly cooled down pressure release and obtains graphene oxide prefabricated solution；Step 4, tea polyphenols are added in into graphene oxide prefabricated solution 2 4h of heated sealed reduction reaction, obtains graphene mixed liquor；Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene precipitation obtained after drying.The problem of graphene that the present invention solves prior art preparation is second-rate, and defect is more, improves graphene preparation efficiency, not only improves graphene yield, also improves graphene quality.
Description
Technical field
The invention belongs to technical field of graphene, and in particular to a kind of preparation method of grapheme material.
Background technology
Graphene is a kind of special lamellar structure, it is in 2004 by Univ Manchester UK scientist An Delie
Extra large nurse and Constantine Nuo Woxiao loves are found, and obtain the Nobel prize for physics of 2010.They use mechanical stripping
Method by repeatedly removing, obtains the mono-layer graphite piece being only made of one layer of carbon atom, i.e. graphite from highly oriented pyrolytic graphite
Alkene.Research finds that graphene has the excellent attribute of various remote super current materials, such as：Most thin material (individual layer stone in the world
Black alkene only 0.335nm), be currently known the highest material of intensity, toughness fabulous (elasticity modulus is up to 1.1TPa), be excellent impervious
Property (He atoms can not pass through), at room temperature prominent thermal conductivity, the electron mobility of high speed, high specific surface area (individual layer
The theoretical specific surface area of graphene is up to 2630m2/ g), most light charge carrier etc..Using graphene, a series of tools can be researched and developed
The new material for the matter that has specific characteristics.For example, the transmission speed of grapheme transistor is expected to apply considerably beyond current silicon transistor
In the research and development of completely new supercomputer.Using its excellent electric conductivity and great specific surface area, graphene can be used for manufacturing
Electrode material, sensor material.Compound with other materials, graphene can be additionally used in composite material of the manufacture with property,
So as to make new material thinner, lighter and stretchier, therefore its application prospect is very wide.Graphene not only brings an electricity
Sub- material revolution, but also the development that automobile, aircraft and aerospace industry will be greatly facilitated.
Graphite flake of the number of plies below 10 layers is generally known as " graphene ", one layer is known as " single-layer graphene ", two layers
Above is known as " multi-layer graphene ".They all have physics different with graphite, chemistry and mechanical performance, and the number of plies is higher than
The performance of 10 layers of graphite flake and common graphite-phase are same.Accordingly, for the preparation of graphene and the research mainly research number of plies
Graphite flake below 10 layers.
At present, the preparation method of graphene mainly has：Mechanical stripping method, chemical stripping method, SiC epitaxial growth methods, chemistry
Vapor deposition etc..
Mechanical stripping method：It is that highly oriented pyrolytic graphite is cut into graphite flake, is sticked to thin slice both sides with adhesive tape, then tears
Thin slice is divided into two by the band that comes unglued, and repeats the graphite that above procedure can be obtained by less than 10 layers of graphene, even individual layer
Alkene.The advantages of the method：The graphene film of very high quality can be obtained；Shortcoming：Yield is very low, and cost is very high.
SiC epitaxial growth methods：It is to heat SiC crystal in a vacuum, when temperature reaches 1200 DEG C~1500 DEG C, C-Si keys
It is broken, the Si atoms in the more plane of atom containing C are evaporated out, and remaining carbon atom can be in SiC crystal
(0001) graphene-structured of six sides is arranged on face.The advantages of this method：The graphene and nothing of better quality can be prepared
It must carry out the transfer of substrate；Shortcoming：It is low output, of high cost, and graphene film is in uneven thickness.
Chemical vapour deposition technique：It is using pyrolytic hydrocarbon gas, in very thin Raney nickel or copper catalyst film
In, carbon nickel saturated solid solution is initially formed, then in cooling procedure, carbon atom is gradually precipitated from nickel or copper crystal, and obtains
Obtain graphene sheet layer.The advantages of this method：While high-quality graphene is obtained, moreover it is possible to obtain under rational cost and relatively manage
In addition the yield thought also has certain potentiality in terms of the graphene for preparing large area.Shortcoming：1) graphene prepared is usual
It needs to be transferred in other substrates, increases the difficulty of preparation；2) though the yield of graphene is prepared higher than mechanical stripping method and outer
Epitaxial growth, but far can not also meet people and apply the needs of upper.
Chemical stripping method, also known as " oxidation-reduction method "：Refer to carry out at oxidation common graphite first with strong oxidizer
Reason, makes its interlamellar spacing become larger, be easily isolated；Then using the graphite aoxidized is removed the methods of ultrasound, graphite oxide is obtained
Alkene；Finally, reduction reaction is carried out to graphene oxide in high temperature or in reducing solution, makes the graphite oxide after stripping also
Original obtains graphene.The advantages of this method：Graphite powder raw material are easy to get, preparation process is simple, cost is relatively low, available for big
Amount prepares graphene.Shortcoming：Prepared graphene quality is low, defect is more, and carbon atom arrangement degree of disorder height etc., these features are big
The earth reduces physics, chemistry and mechanical performance of graphene etc., limits the further extensive use of graphene or influences
To application effect.
Graphene is made of the single layer of carbon atom that sp2 hydridization is formed, and belongs to ideal two dimensional crystal, and its perfect hexagonal
Lattice structure and two-dimensional structure impart its high electron mobility, and this mobility causes graphene in the carrier of very little
Also there is excellent electric conductivity under concentration.But research shows that the presence of defect can seriously reduce electron mobility.In graphene
The defects of mainly include：Five-membered ring, heptatomic ring, graphite layers are disorderly arranged and the introducing of foreign atom etc., they are considered as
Caused by sp3 hydridization is introduced on the basis of sp2 hydridization.Judge from Raman spectrum (Raman) characterization：The seldom height of defect
Quality graphene only contains the characteristic peaks such as G peaks and 2D peaks, and the value at D peaks is very low；And the graphene that defect concentration of poor quality is big,
In addition to G peaks, clearly, 2D peaks are weaker at D peaks.It is generally acknowledged that influence graphene quality, that is, structural intergrity it is main because
Element is the type and quantity of " defect " in graphene.
In conclusion from the point of view of the method for graphene is prepared at present, method that high-quality graphene can be obtained, yield
It is very low and of high cost；And can largely prepare graphene and method at low cost, graphene it is second-rate, have it is more
Defect, it is impossible to meet the needs of application.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of grapheme material, solves existing skill
The problem of graphene prepared by art is second-rate, and defect is more, improves graphene preparation efficiency, not only improves graphene production
Rate also improves graphene quality.
For realization more than technical purpose, the technical scheme is that：
A kind of preparation method of grapheme material, the preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 30-60min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 60-120min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide
Dispersion liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 2-4h in reaction kettle, constant pressure reaction 1-3h, soon
But pressure release obtains graphene oxide prefabricated solution to quickly cooling；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 2-4h, obtains graphene
Mixed liquor；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene obtained after drying and is sunk
It forms sediment.
Mass concentration of the graphene oxide in absolute ethyl alcohol in the step 1 is 5-20g/L.
The frequency of ultrasonic disperse in the step 1 is 10-16kHz, and temperature is 40-60 DEG C.
Dispersant addition in the step 2 is the 70-80% of graphene oxide quality, and the dispersant uses poly- second
The mass ratio 3-5 of the mixture of alkene pyrrolidone and o-dichlorohenzene, the polyvinylpyrrolidone and o-dichlorohenzene:2.
The pressure of pressurization microwave reaction in the step 3 is 10-15MPa, and temperature is 100-130 DEG C, and microwave power is
600-1000W, the pressure of the constant pressure reaction is 10-12MPa.
Pressure release is quickly cooled down after first cooling down by the way of pressure release in the step 3, and the cooldown rate of the cooling is
10-15 DEG C/min, the pressure release speed of the pressure release is 1-3MPa/min.
The addition of tea polyphenols in the step 4 is the 30-50% of graphene oxide quality.
The temperature of heated sealed reduction reaction in the step 4 is 90-100 DEG C, pressure 6-9MPa.
Absolute ethyl alcohol washing times in the step 5 are 4-8 times, centrifugal speed 3000-6000r/min.
Drying temperature in the step 5 is 70-90 DEG C.
Graphene oxide is evenly distributed on by way of ultrasonic disperse in absolute ethyl alcohol by step 1, can form oxidation
Graphite enol liquid.
Step 2 is added a dispersant in graphite oxide enol liquid, under ultrasonication, dispersant stepless action oxidation stone
Black alkene surface, can form relatively stable dispersion；The dispersion mixed using polyvinylpyrrolidone and o-dichlorohenzene
Agent effectively can not only greatly promote graphene oxide using o-dichlorohenzene surface close to the requirement of graphene surface energy
Dispersibility, and polyvinylpyrrolidone has good toughness and stability, can ensure the stabilization point of graphene oxide
Granular media system.
Graphene oxide is carried out pressurization microwave reaction by step 3, is converted into absolute ethyl alcohol by way of integrally heating
Gaseous state, while infiltrate into graphene oxide, uniform pressure system inside and outside formation, ensure structure by way of constant pressure reaction
Stability prevents the aggregation of graphene oxide particle；It is being quickly cooled down and that external and internal pressure can be formed in pressure leak process is unbalance, it is interior
Portion's pressure is big, and external pressure is small, and graphene oxide particle expansion is crushed, and achievees the effect that fragmentation graphene oxide.
Tea polyphenols are put into graphene oxide and prefabricated solution by step 4, by oxygen by way of heated sealed reduction reaction
Graphite alkene restores to form grapheme material；Tea polyphenols can be slowly dissolved in absolute ethyl alcohol by heated sealed process, be formed
Dissolution system can uniformly be dispersed to graphene surface, achieve the effect that quickly to restore, and promote reduction efficiency.
Graphene mixed liquor progress centrifugal filtration can be formed graphene precipitation by step 5, then through multiple absolute ethyl alcohol
Tea polyphenols, polyvinylpyrrolidone and o-dichlorohenzene can be cleaned and removed, obtain the graphene of high quality, high-purity by cleaning
Material.
From the above, it can be seen that the present invention has advantages below：
The problem of 1. graphene that the present invention solves prior art preparation is second-rate, and defect is more, improves graphite
Alkene preparation efficiency, not only improves graphene yield, also improves graphene quality.
2. the present invention can not can be approached using double dispersant systems merely with the surface of o-dichlorohenzene with graphene surface
Characteristic promotes graphene dispersion problem, while the coating function using polyvinylpyrrolidone in itself, ensures graphene oxide
Dispersibility.
3. absolute ethyl alcohol is converted into gaseous state by the present invention using pressurization microwave reaction, ethyl alcohol atmosphere is formed, can not only be carried
For stress reaction, while it can also play good osmosis.
4. the graphene oxide further fragmentation of the invention by the way of pressurization-pressure release, expansionization refinement not only has ring
The characteristics of guarantor, while also have the characteristics that refinement stability is high.
5. the present invention uses heated sealed reduction reaction as the redox reaction system of tea polyphenols, can not only be by tea
Polyphenol uniformly disperses, while ethanol evaporation adherence pressure, tea polyphenols concentration is improved, so as to improve its reduction efficiency.
Specific embodiment
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of grapheme material, the preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 30min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 60min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion
Liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 2h in reaction kettle, constant pressure reaction 1h, fast quickly cooling
But pressure release obtains graphene oxide prefabricated solution；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 2h, obtains graphene and mix
Close liquid；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene obtained after drying and is sunk
It forms sediment.
Mass concentration of the graphene oxide in absolute ethyl alcohol in the step 1 is 5g/L.
The frequency of ultrasonic disperse in the step 1 is 10kHz, and temperature is 40 DEG C.
Dispersant addition in the step 2 is the 70% of graphene oxide quality, and the dispersant uses polyethylene
The mass ratio 3 of the mixture of pyrrolidones and o-dichlorohenzene, the polyvinylpyrrolidone and o-dichlorohenzene:2.
The pressure of pressurization microwave reaction in the step 3 is 10MPa, and temperature is 100 DEG C, microwave power 600W, institute
The pressure for stating constant pressure reaction is 10MPa.
Pressure release is quickly cooled down after first cooling down by the way of pressure release in the step 3, and the cooldown rate of the cooling is
10 DEG C/min, the pressure release speed of the pressure release is 1MPa/min.
The addition of tea polyphenols in the step 4 is the 30% of graphene oxide quality.
The temperature of heated sealed reduction reaction in the step 4 is 90 DEG C, pressure 6MPa.
Absolute ethyl alcohol washing times in the step 5 are 4-8 times, centrifugal speed 3000r/min.
Drying temperature in the step 5 is 70 DEG C.
Embodiment 2
A kind of preparation method of grapheme material, the preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 60min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 120min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion
Liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 4h in reaction kettle, constant pressure reaction 3h, fast quickly cooling
But pressure release obtains graphene oxide prefabricated solution；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 4h, obtains graphene and mix
Close liquid；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene obtained after drying and is sunk
It forms sediment.
Mass concentration of the graphene oxide in absolute ethyl alcohol in the step 1 is 20g/L.
The frequency of ultrasonic disperse in the step 1 is 16kHz, and temperature is 60 DEG C.
Dispersant addition in the step 2 is the 80% of graphene oxide quality, and the dispersant uses polyethylene
The mass ratio 5 of the mixture of pyrrolidones and o-dichlorohenzene, the polyvinylpyrrolidone and o-dichlorohenzene:2.
The pressure of pressurization microwave reaction in the step 3 is 15MPa, and temperature is 130 DEG C, microwave power 1000W, institute
The pressure for stating constant pressure reaction is 12MPa.
Pressure release is quickly cooled down after first cooling down by the way of pressure release in the step 3, and the cooldown rate of the cooling is
15 DEG C/min, the pressure release speed of the pressure release is 3MPa/min.
The addition of tea polyphenols in the step 4 is the 50% of graphene oxide quality.
The temperature of heated sealed reduction reaction in the step 4 is 100 DEG C, pressure 9MPa.
Absolute ethyl alcohol washing times in the step 5 are 8 times, centrifugal speed 6000r/min.
Drying temperature in the step 5 is 90 DEG C.
Embodiment 3
A kind of preparation method of grapheme material, the preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 40min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 80min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion
Liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 3h in reaction kettle, constant pressure reaction 2h, fast quickly cooling
But pressure release obtains graphene oxide prefabricated solution；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 3h, obtains graphene and mix
Close liquid；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene obtained after drying and is sunk
It forms sediment.
Mass concentration of the graphene oxide in absolute ethyl alcohol in the step 1 is 10g/L.
The frequency of ultrasonic disperse in the step 1 is 12kHz, and temperature is 50 DEG C.
Dispersant addition in the step 2 is the 75% of graphene oxide quality, and the dispersant uses polyethylene
The mass ratio 4 of the mixture of pyrrolidones and o-dichlorohenzene, the polyvinylpyrrolidone and o-dichlorohenzene:2.
The pressure of pressurization microwave reaction in the step 3 is 13MPa, and temperature is 110 DEG C, microwave power 800W, institute
The pressure for stating constant pressure reaction is 11MPa.
Pressure release is quickly cooled down after first cooling down by the way of pressure release in the step 3, and the cooldown rate of the cooling is
12 DEG C/min, the pressure release speed of the pressure release is 2MPa/min.
The addition of tea polyphenols in the step 4 is the 40% of graphene oxide quality.
The temperature of heated sealed reduction reaction in the step 4 is 95 DEG C, pressure 7MPa.
Absolute ethyl alcohol washing times in the step 5 are 6 times, centrifugal speed 4000r/min.
Drying temperature in the step 5 is 80 DEG C.
Embodiment 4
A kind of preparation method of grapheme material, the preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 50min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 100min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion
Liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 3h in reaction kettle, constant pressure reaction 2h, fast quickly cooling
But pressure release obtains graphene oxide prefabricated solution；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 3h, obtains graphene and mix
Close liquid；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene obtained after drying and is sunk
It forms sediment.
Mass concentration of the graphene oxide in absolute ethyl alcohol in the step 1 is 15g/L.
The frequency of ultrasonic disperse in the step 1 is 14kHz, and temperature is 50 DEG C.
Dispersant addition in the step 2 is the 75% of graphene oxide quality, and the dispersant uses polyethylene
The mass ratio 4 of the mixture of pyrrolidones and o-dichlorohenzene, the polyvinylpyrrolidone and o-dichlorohenzene:2.
The pressure of pressurization microwave reaction in the step 3 is 12MPa, and temperature is 120 DEG C, microwave power 800W, institute
The pressure for stating constant pressure reaction is 11MPa.
Pressure release is quickly cooled down after first cooling down by the way of pressure release in the step 3, and the cooldown rate of the cooling is
13 DEG C/min, the pressure release speed of the pressure release is 2MPa/min.
The addition of tea polyphenols in the step 4 is the 45% of graphene oxide quality.
The temperature of heated sealed reduction reaction in the step 4 is 95 DEG C, pressure 8MPa.
Absolute ethyl alcohol washing times in the step 5 are 6 times, centrifugal speed 5000r/min.
Drying temperature in the step 5 is 85 DEG C.
Performance test
Performance detection
In conclusion the present invention has the following advantages：
The problem of 1. graphene that the present invention solves prior art preparation is second-rate, and defect is more, improves graphite
Alkene preparation efficiency, not only improves graphene yield, also improves graphene quality.
2. the present invention can not can be approached using double dispersant systems merely with the surface of o-dichlorohenzene with graphene surface
Characteristic promotes graphene dispersion problem, while the coating function using polyvinylpyrrolidone in itself, ensures graphene oxide
Dispersibility.
3. absolute ethyl alcohol is converted into gaseous state by the present invention using pressurization microwave reaction, ethyl alcohol atmosphere is formed, can not only be carried
For stress reaction, while it can also play good osmosis.
4. the graphene oxide further fragmentation of the invention by the way of pressurization-pressure release, expansionization refinement not only has ring
The characteristics of guarantor, while also have the characteristics that refinement stability is high.
5. the present invention uses heated sealed reduction reaction as the redox reaction system of tea polyphenols, can not only be by tea
Polyphenol uniformly disperses, while ethanol evaporation adherence pressure, tea polyphenols concentration is improved, so as to improve its reduction efficiency.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
The described technical solution of inventive embodiments.It will be understood by those of ordinary skill in the art that still the present invention can be carried out
Modification or equivalent replacement, to reach identical technique effect；As long as meeting using needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of grapheme material, it is characterised in that：The preparation method is in accordance with the following steps：
Step 1, it adds graphene oxide into absolute ethyl alcohol, ultrasonic disperse 30-60min, obtains graphite oxide enol liquid；
Step 2, ultrasonic disperse 60-120min in graphite oxide enol liquid is added a dispersant to, obtains graphene oxide dispersion
Liquid；
Step 3, graphene oxide dispersion is put into pressurization microwave reaction 2-4h in reaction kettle, constant pressure reaction 1-3h, fast quickly cooling
But pressure release obtains graphene oxide prefabricated solution；
Step 4, tea polyphenols are added in into graphene oxide prefabricated solution heated sealed reduction reaction 2-4h, obtains graphene mixing
Liquid；
Step 5, it will repeatedly be washed using absolute ethyl alcohol after graphene mixed liquor centrifugal filtration, graphene precipitation obtained after drying.
2. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Oxygen in the step 1
Mass concentration of the graphite alkene in absolute ethyl alcohol is 5-20g/L.
3. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：It is super in the step 1
The frequency of sound dispersion is 10-16kHz, and temperature is 40-60 DEG C.
4. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Point in the step 2
Powder addition is the 70-80% of graphene oxide quality, and the dispersant is using polyvinylpyrrolidone and o-dichlorohenzene
The mass ratio 3-5 of mixture, the polyvinylpyrrolidone and o-dichlorohenzene:2.
5. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Adding in the step 3
The pressure for pressing microwave reaction is 10-15MPa, and temperature is 100-130 DEG C, microwave power 600-1000W, the constant pressure reaction
Pressure is 10-12MPa.
6. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：It is fast in the step 3
But pressure release is after first cooling down by the way of pressure release for quickly cooling, and the cooldown rate of the cooling is 10-15 DEG C/min, and the pressure release is let out
Pressure speed is 1-3MPa/min.
7. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Tea in the step 4
The addition of polyphenol is the 30-50% of graphene oxide quality.
8. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：It is close in the step 4
The temperature of envelope heating reduction reaction is 90-100 DEG C, pressure 6-9MPa.
9. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Nothing in the step 5
Water-ethanol washing times are 4-8 times, centrifugal speed 3000-6000r/min.
10. a kind of preparation method of grapheme material according to claim 1, it is characterised in that：Baking in the step 5
Dry temperature is 70-90 DEG C.
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| CN113912050A (en) * | 2020-07-09 | 2022-01-11 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
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| CN113912050A (en) * | 2020-07-09 | 2022-01-11 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
| CN113912050B (en) * | 2020-07-09 | 2023-11-14 | Tcl科技集团股份有限公司 | Graphene quantum dot and processing method thereof |
| CN113929090A (en) * | 2021-12-03 | 2022-01-14 | 曲靖华金雨林科技有限责任公司 | Preparation method of graphene |
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Application publication date: 20180622 |