CN109534327A - A kind of preparation method of graphene - Google Patents
A kind of preparation method of graphene Download PDFInfo
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- CN109534327A CN109534327A CN201910079896.XA CN201910079896A CN109534327A CN 109534327 A CN109534327 A CN 109534327A CN 201910079896 A CN201910079896 A CN 201910079896A CN 109534327 A CN109534327 A CN 109534327A
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Abstract
The present invention proposes a kind of preparation method of graphene, and boiling point is dissolved in including step 1, cupric organic salt higher than in the organic solvent of the organic salt decomposition temperature, is configured to the cupric organic slat solution containing copper concentration for 0.001-0.02mol/L；The cupric organic slat solution prepared is placed in protective atmosphere, normal heating is to 150-300 DEG C, after being heated to preset temperature, carries out the heat preservation of 15-120min；Cupric organic slat solution, which decomposes, generates copper atom and carbon atom, copper and carbon symbiosis, at the liquid-vapor interface between cupric organic slat solution and protective atmosphere, forms area and reaches 0.5cm2Above graphene-the carbon/carbon-copper composite material, the composite material are made of single crystal Cu nanometer sheet and graphene；Step 2, the substrate surface that graphene-carbon/carbon-copper composite material is transferred to selection；Step 3 carries out Chemical Decomposition to the graphene-carbon/carbon-copper composite material for being transferred to substrate surface, obtains the graphene that the carbon atom number of plies is less than 10 layers.The carbon atom number of plies of graphene can be effectively controlled in the above method, has the advantages that at low cost, short preparation period.
Description
Technical field
The present invention relates to the preparation technical field of grapheme material more particularly to a kind of preparations of the graphene of low-temperature atmosphere-pressure
Method.
Background technique
Graphene is a kind of carbon atom with sp2Orbital hybridization bonding forms cellular two-dimensional material, has electron transfer
The features such as rate is high, and thermal conductivity is high, large specific surface area and good mechanical property causes the numerous areas such as physics, chemistry, material science
Family extensive concern.But since graphene generally requires to provide system high temperature, high pressure or high temperature height during the preparation process
Pressure while the reaction condition applied, so that preparation cost is very high.Therefore, seek simple, inexpensive, large-area graphene
Preparation method becomes the difficult point in this field.
CN201510334460 discloses a kind of method that batch prepares graphene and doped graphene, and this method is by applying
It adds high pressure, is in system under the condition of high voltage of 1-5Mpa, realizes the prepare with scale of graphene；CN201680060205 is disclosed
A kind of graphene synthetic method, this method are to be heated at high temperature metal base and carbon source in a sealed meter environment, heating
Minimum 800 DEG C of temperature, so that carbon source is generated carbon vapor and ultimately form deposition graphene after contacting with metal base.As a result table
Bright: when temperature is maintained at 800 DEG C, graphene number of plies is at 1-19 layers, and when temperature is maintained at 900 DEG C, the number of plies is more than 20 layers；
CN201710077369 discloses a kind of method for preparing graphene using compression ignition method, and this method is shelled using Detonation Shock Wave physics
From graphene is obtained, the number of plies is less.Compression ignition reaction temperature is between 500-3200 DEG C, reaction pressure 1.2-8MPa, the system
Standby process is in high-temperature high-pressure state；CN201711173977 discloses a kind of preparation method of graphene, and this method passes through outer
High voltage forms the electric field of high electric-field intensity.By ionizing the methane (purity > 99%) being passed through, the number of plies is finally obtained in 1-
20 layers, the graphene of structural integrity rule；CN201810090218 discloses the preparation method and graphite of a kind of grapheme material
Graphene oxide containing metal impurities or nonmetallic inclusion is placed in carrier by alkene material, this method, and carrier is put into very
It in empty furnace, vacuumizes, heating temperature is 1250-2500 DEG C, finally obtains purity is high, the good graphene of structure；
CN201810670899 discloses a kind of method for preparing graphene, and this method is to apply 115- to graphene oxide solution
125MPa high pressure carries out homogenization, carries out 170-185 DEG C of hydro-thermal reaction again after solution dispersion, final after natural cooling
Obtain graphene, nearly 2 times of electrochemical energy storage performance boost；CN201811134230 discloses a kind of graphene preparation facilities,
The device forms the electric field of high electric-field intensity by applying high voltage, provides energy using the plasma between electrode plate, swashs
The graphite infiltrated is encouraged, and then removes graphite, obtains the graphene of a large amount of single layers；CN201711170496 discloses a kind of graphite
Alkene and preparation method thereof, this method utilize intercalator, carry out intercalation processing at least once to raw material, recycle mechanical refinement
Etc. techniques obtain graphene, obtained graphene number of plies is few, and interlayer spacing is big.It is related to the harm such as strong oxidizer during the preparation process
Property biggish reagent use, therefore there are subsequent steps such as liquid waste processings, technique is relatively more.
In conclusion preparing graphene at present still needs 800 DEG C or more of high temperature, the high pressure of 1Mpa or more or simultaneously
Using the condition of high temperature and pressure, some obtains graphene by multi-step process even with strong oxidizer and high electric field.
Summary of the invention
In order to solve the problems in the existing technology, the invention proposes a kind of preparation method of graphene, so as to
Under low-temperature atmosphere-pressure, it is prepared that the carbon atom number of plies is controllable, graphene of structural integrity, short preparation period.
To achieve the goals above, the invention proposes a kind of preparation methods of graphene, and the method includes following steps
It is rapid:
Step 1 is dissolved in cupric organic salt boiling point higher than in the organic solvent of the organic salt decomposition temperature, is configured to contain
Copper concentration is the cupric organic slat solution of 0.001mol/L-0.02mol/L；Configured cupric organic slat solution is placed in protection
In atmosphere, normal heating is to 150 DEG C -300 DEG C, after being heated to preset temperature, carries out the heat preservation of 15min-120min, described pre-
If temperature is in the range of 150 DEG C -300 DEG C；Cupric organic slat solution, which decomposes, generates copper atom and carbon atom, copper and carbon symbiosis,
At liquid-vapor interface between cupric organic slat solution and protective atmosphere, forms area and reach 0.5cm2Above graphene-the copper is multiple
Condensation material, the composite material are made of single crystal Cu nanometer sheet and graphene；Wherein, the normal pressure refers to that reaction system is in one
Standard atmospheric pressure；
Step 2, the substrate surface that graphene-carbon/carbon-copper composite material is transferred to selection, the selection standard of the substrate are as follows: institute
The surface for stating substrate can be a, and the surface of the graphene-carbon/carbon-copper composite material can be b, the graphene-carbon/carbon-copper composite material attachment
To after the substrate surface, the surface of the entirety can be c, and (a+b) > c, selection meet the substrate of conditions above；It is described
Transfer refers to, by substrate surface slant setting, and from the gas of the liquid-vapor interface formed between cupric organic slat solution and protective atmosphere
Body side moves closer to the graphene-carbon/carbon-copper composite material surface formed at liquid-vapor interface, until contact, graphene-copper are multiple
Condensation material is attached to substrate surface, is completely transferred to substrate surface from liquid-vapor interface.
Step 3, to the single crystal Cu nanometer sheet being transferred in graphene-carbon/carbon-copper composite material of substrate surface and graphene
Chemical Decomposition is carried out, the graphene that the carbon atom number of plies is less than 10 layers is obtained.
Preferably, in the step 1, the cupric organic salt is to contain cupric organic salt；The boiling point is high
In cupric organic salt decomposition temperature organic solvent be hydro carbons, benzene class, ethers, the alcohols of Long carbon chain, ketone, esters, lipoidis
One or more of mixture.
Preferably, in the step 1, the cupric organic salt is copper oleate；The organic solvent is for oleic acid and just
The mixed solvent of octanol.
Preferably, in the step 1, protective gas used by the protective atmosphere is nitrogen, argon gas or both
Mixture, gas flow 60-80mLmin-1。
Preferably, in the step 1, graphene-carbon/carbon-copper composite material of the formation refers to, the direction of growth perpendicular to
The single crystal Cu nanometer sheet of copper (111) crystal face and the graphene symbiosis on copper nanometer sheet surface, graphene-carbon/carbon-copper composite material of formation.
Preferably, in the step 2, the substrate uses silicon or silica.
Preferably, in the step 3, the Chemical Decomposition, which refers to use graphene-carbon/carbon-copper composite material, has oxygen
The dilute acid soln for the property changed is handled, and by copper dissolution, obtains graphene.
Preferably, the dilute acid soln with oxidisability uses the dilute hydrochloric acid solution containing hydrogen peroxide.
Preferably, step 21 is equipped between the step 2 and step 3, the step 21 is to be transferred to base to described
Graphene-carbon/carbon-copper composite material of bottom surface is cleaned, and remaining organic matter, improves the pure of graphene when decomposing to remove
Degree.
The beneficial effect of the program of the present invention is the preparation method of above-mentioned graphene in atmospheric conditions, and cupric is organic
Salting liquid low-temperature decomposition generates copper atom and carbon atom, at the liquid-vapor interface between cupric organic slat solution and protective atmosphere
Interface can be higher, and during the reaction, the copper atom of generation can be preferentially adsorbed at liquid-vapor interface, to reduce liquid-vapor interface
Interface energy.The carbon atom of generation is adsorbed on the copper atom surface at liquid-vapor interface, further decreases maximum system energy.It is adsorbed on gas-
The copper atom of liquid interface carries out self assembly, forms copper nanometer sheet, and carbon atom and the copper atom for being adsorbed on copper atom surface are common
Growth forms graphene on copper nanometer sheet surface, ultimately forms graphene-carbon/carbon-copper composite material, which reaches
0.5cm2More than, maximum area is limited solely by the area of liquid-vapor interface and the dosage of cupric organic slat solution.It is involved in the present invention
Graphene preparation method by change preparation condition, such as the cupric in heating temperature, soaking time, cupric organic slat solution
Concentration etc. is, it can be achieved that effective control to the graphene carbon atom number of plies.Organic solvent selected by this method is nontoxic, Efficient Ring
It protects；Low-temperature atmosphere-pressure prepares graphene, has many advantages, such as at low cost, short preparation period, the prepared graphene carbon atom number of plies is few,
Area is big.
Specific embodiment
A specific embodiment of the invention is further described below with reference to embodiment.
Embodiment 1
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.001mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure into
Row heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the guarantor of 30min when being heated to 250 DEG C
Temperature forms area and reaches 3-4cm2Graphene-carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts the graphite of generation
Alkene-carbon/carbon-copper composite material, specific transfer method are as follows: by silicon chip surface slant setting, and from cupric organic slat solution and protective atmosphere
Between the gas side of liquid-vapor interface that is formed, move closer to the graphene-carbon/carbon-copper composite material surface formed at liquid-vapor interface,
Until contact, graphene-carbon/carbon-copper composite material are attached to silicon chip surface, are completely transferred to silicon chip surface from liquid-vapor interface.
To the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, cleaned using ethyl alcohol and acetone, later to graphite
Single crystal Cu nanometer sheet and graphene in alkene-carbon/carbon-copper composite material carry out Chemical Decomposition, specifically use and contain the dilute of hydrogen peroxide
Hydrochloric acid solution carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is layer 2-4.
Embodiment 2
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.02mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure carries out
Heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the heat preservation of 30min when being heated to 250 DEG C,
It forms area and reaches 3-4cm2Graphene-carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts the graphene-of generation
Carbon/carbon-copper composite material, specific transfer method are as follows: by silicon chip surface slant setting, and from shape between cupric organic slat solution and protective atmosphere
At liquid-vapor interface gas side, move closer at liquid-vapor interface formed graphene-carbon/carbon-copper composite material surface, until
Contact, graphene-carbon/carbon-copper composite material are attached to silicon chip surface, are completely transferred to silicon chip surface from liquid-vapor interface.
It to the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, is cleaned using acetone, later to graphene-copper
Single crystal Cu nanometer sheet and graphene in composite material carry out Chemical Decomposition, specifically molten using the dilute hydrochloric acid containing hydrogen peroxide
Liquid carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 4-6 layers.
Embodiment 3
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.001mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure into
Row heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the guarantor of 30min when being heated to 150 DEG C
Temperature forms area and reaches 0.5-1cm2Graphene-carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts the stone of generation
Black alkene-carbon/carbon-copper composite material, specific transfer method are as follows: by silicon chip surface slant setting, and from cupric organic slat solution and protect gas
The gas side of the liquid-vapor interface formed between atmosphere moves closer to the graphene-carbon/carbon-copper composite material table formed at liquid-vapor interface
Face, until contact, graphene-carbon/carbon-copper composite material are attached to silicon chip surface, silicon wafer table are completely transferred to from liquid-vapor interface
Face.
It to the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, is cleaned using acetone, later to graphene-copper
Single crystal Cu nanometer sheet and graphene in composite material carry out Chemical Decomposition, specifically molten using the dilute hydrochloric acid containing hydrogen peroxide
Liquid carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 2 layers.
Embodiment 4
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.001mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure into
Row heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the guarantor of 30min when being heated to 300 DEG C
Temperature forms area and reaches 4-5cm2Graphene-carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts the graphite of generation
Alkene-carbon/carbon-copper composite material, specific transfer method are as follows: by silicon chip surface slant setting, and from cupric organic slat solution and protective atmosphere
Between the gas side of liquid-vapor interface that is formed, move closer to the graphene-carbon/carbon-copper composite material surface formed at liquid-vapor interface,
Until contact, graphene-carbon/carbon-copper composite material are attached to silicon chip surface, are completely transferred to silicon chip surface from liquid-vapor interface.
It to the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, is cleaned using acetone, later to graphene-copper
Single crystal Cu nanometer sheet and graphene in composite material carry out Chemical Decomposition, specifically molten using the dilute hydrochloric acid containing hydrogen peroxide
Liquid carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 8-10 layers.
Embodiment 5
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.001mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure into
Row heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the guarantor of 15min when being heated to 250 DEG C
Temperature forms area and reaches 0.5cm2Above graphene-the carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts generation
Graphene-carbon/carbon-copper composite material, specific transfer method are as follows: by silicon chip surface slant setting, and from cupric organic slat solution and protect
The gas side of the liquid-vapor interface formed between atmosphere moves closer to the graphene-carbon/carbon-copper composite material formed at liquid-vapor interface
Surface, until contact, graphene-carbon/carbon-copper composite material are attached to silicon chip surface, silicon wafer table are completely transferred to from liquid-vapor interface
Face.
It to the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, is cleaned using acetone, later to graphene-copper
Single crystal Cu nanometer sheet and graphene in composite material carry out Chemical Decomposition, specifically molten using the dilute hydrochloric acid containing hydrogen peroxide
Liquid carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is layer 2-4.
Embodiment 6
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.001mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure into
Row heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the guarantor of 120min when being heated to 250 DEG C
Temperature forms graphene-carbon/carbon-copper composite material.It selects monocrystalline silicon piece as substrate, shifts graphene-carbon/carbon-copper composite material of generation, have
Body transfer method are as follows: by silicon chip surface slant setting, and from the liquid-vapor interface formed between cupric organic slat solution and protective atmosphere
Gas side, move closer at liquid-vapor interface formed graphene-carbon/carbon-copper composite material surface, until contact, graphene-
Carbon/carbon-copper composite material is attached to silicon chip surface, is completely transferred to silicon chip surface from liquid-vapor interface.
It to the graphene-carbon/carbon-copper composite material for being transferred to silicon chip surface, is cleaned using acetone, later to graphene-copper
Single crystal Cu nanometer sheet and graphene in composite material carry out Chemical Decomposition, specifically molten using the dilute hydrochloric acid containing hydrogen peroxide
Liquid carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 8-10 layers.
Embodiment 7
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.02mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure carries out
Heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the heat preservation of 30min when being heated to 250 DEG C,
It forms area and reaches 0.5cm2Above graphene-the carbon/carbon-copper composite material.It selects silica as substrate, shifts the graphite of generation
Alkene-carbon/carbon-copper composite material, specific transfer method are as follows: by silica surface slant setting, and from cupric organic slat solution and protect
The gas side of the liquid-vapor interface formed between atmosphere moves closer to the graphene-carbon/carbon-copper composite material formed at liquid-vapor interface
Surface, until contact, graphene-carbon/carbon-copper composite material are attached to silica surface, are completely transferred to two from liquid-vapor interface
Silicon oxide surface.
To the graphene-carbon/carbon-copper composite material for being transferred to silica surface, cleaned using acetone, later to graphite
Single crystal Cu nanometer sheet and graphene in alkene-carbon/carbon-copper composite material carry out Chemical Decomposition, specifically use and contain the dilute of hydrogen peroxide
Hydrochloric acid solution carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 8-10 layers.
Embodiment 8
At room temperature, it will be dissolved in the in the mixed solvent of oleic acid and n-octyl alcohol containing cupric copper oleate, it is dense that cupric is made
Degree is the cupric organic slat solution of 0.02mol/L；Configured cupric organic slat solution is placed in nitrogen atmosphere, normal pressure carries out
Heating, gas flow 75mLmin-1, heating rate is that 5 DEG C/min carries out the heat preservation of 120min when being heated to 250 DEG C,
It forms area and reaches 0.5cm2Above graphene-the carbon/carbon-copper composite material.It selects silica as substrate, shifts the graphite of generation
Alkene-carbon/carbon-copper composite material, specific transfer method are as follows: by silica surface slant setting, and from cupric organic slat solution and protect
The gas side of the liquid-vapor interface formed between atmosphere moves closer to the graphene-carbon/carbon-copper composite material formed at liquid-vapor interface
Surface, until contact, graphene-carbon/carbon-copper composite material are attached to silica surface, are completely transferred to two from liquid-vapor interface
Silicon oxide surface.
To the graphene-carbon/carbon-copper composite material for being transferred to silica surface, cleaned using acetone, later to graphite
Single crystal Cu nanometer sheet and graphene in alkene-carbon/carbon-copper composite material carry out Chemical Decomposition, specifically use and contain the dilute of hydrogen peroxide
Hydrochloric acid solution carries out Chemical Decomposition, obtains the graphene that the carbon atom number of plies is 8-10 layers.
Claims (9)
1. a kind of preparation method of graphene, it is characterised in that: the described method comprises the following steps:
Step 1 is dissolved in cupric organic salt boiling point higher than in the organic solvent of the organic salt decomposition temperature, and it is dense to be configured to cupric
Degree is the cupric organic slat solution of 0.001mol/L-0.02mol/L；Configured cupric organic slat solution is placed in protective atmosphere
In, normal heating is to 150 DEG C -300 DEG C, after being heated to preset temperature, carries out the heat preservation of 15min-120min, the default temperature
Degree is in the range of 150 DEG C -300 DEG C；Cupric organic slat solution, which decomposes, generates copper atom and carbon atom, copper and carbon symbiosis, is containing
At liquid-vapor interface between copper organic slat solution and protective atmosphere, forms area and reach 0.5cm2Above graphene-the composite copper material
Material, the composite material are made of single crystal Cu nanometer sheet and graphene；
Step 2, the substrate surface that graphene-carbon/carbon-copper composite material is transferred to selection, the selection standard of the substrate are as follows: the base
The surface at bottom can be a, and the surface of the graphene-carbon/carbon-copper composite material can be b, and the graphene-carbon/carbon-copper composite material is attached to institute
After stating substrate surface, the surface of the entirety can be c, and (a+b) > c, selection meet the substrate of conditions above；
Step 3 carries out the single crystal Cu nanometer sheet being transferred in graphene-carbon/carbon-copper composite material of substrate surface and graphene
Chemical Decomposition obtains the graphene that the carbon atom number of plies is less than 10 layers.
2. the preparation method of graphene according to claim 1, it is characterised in that: in the step 1, the cupric has
Machine salt is to contain cupric organic salt；The boiling point be higher than cupric organic salt decomposition temperature organic solvent be hydro carbons, benzene class,
The mixture of one or more of ethers, the alcohols of Long carbon chain, ketone, esters, lipoidis.
3. the preparation method of graphene according to claim 2, it is characterised in that: in the step 1, the cupric has
Machine salt is copper oleate；The organic solvent is the mixed solvent of oleic acid and n-octyl alcohol.
4. the preparation method of graphene as claimed in any of claims 1 to 3, it is characterised in that: in the step 1
In, protective gas used by the protective atmosphere is the mixture of nitrogen, argon gas or both, gas flow 60-80mL
min-1。
5. the preparation method of graphene according to claim 1, it is characterised in that: in the step 1, the formation
Graphene-carbon/carbon-copper composite material refers to, single crystal Cu nanometer sheet and copper nanometer sheet surface of the direction of growth perpendicular to copper (111) crystal face
Graphene symbiosis, graphene-carbon/carbon-copper composite material of formation.
6. the preparation method of graphene according to claim 1, it is characterised in that: in the step 2, the substrate is adopted
With silicon or silica.
7. the preparation method of graphene according to claim 1, it is characterised in that: in the step 3, the chemistry point
It uses the dilute acid soln with oxidisability to handle graphene-carbon/carbon-copper composite material from referring to, by copper dissolution, obtains graphite
Alkene.
8. the preparation method of graphene according to claim 7, it is characterised in that: the dilute acid soln with oxidisability
Using the dilute hydrochloric acid solution containing hydrogen peroxide.
9. the preparation method of graphene according to claim 1, it is characterised in that: set between the step 2 and step 3
There is step 21, the step 21 is to clean to the graphene-carbon/carbon-copper composite material for being transferred to substrate surface.
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