CN104681789B - Method for preparing nitrogen-doped graphene membrane and porous carbon integrated material - Google Patents
Method for preparing nitrogen-doped graphene membrane and porous carbon integrated material Download PDFInfo
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- CN104681789B CN104681789B CN201510063898.1A CN201510063898A CN104681789B CN 104681789 B CN104681789 B CN 104681789B CN 201510063898 A CN201510063898 A CN 201510063898A CN 104681789 B CN104681789 B CN 104681789B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for preparing a nitrogen-doped graphene membrane and porous carbon integrated material, relates to a method for preparing a graphene membrane and porous carbon integrated material, and aims to solve the technical problem that a graphite negative electrode of a conventional lithium ion battery is low in power density and energy density. The method comprises the following steps: I, preparing a precursor; II, annealing. The method has the advantages that the nitrogen-doped graphene membrane and porous carbon integrated material can grow on other current collectors (quartz, aluminum oxide or other metals and the like) and has certain universality; the method is simple in overall process, high in operability, good in amplification property, low in cost of used raw materials and free of toxic chemical reagent; the nitrogen-doped graphene membrane and porous carbon integrated material prepared by using the method is high in lithium storage capacity, relatively high in coulombic efficiency, excellent in rate capability, and excellent in circulation stability, can be used as a current collector of a novel lithium ion battery negative electrode, and can be used for preparing high-capacity lithium ion batteries for special demands.
Description
Technical field
The present invention relates to the preparation method of a kind of graphene film and porous carbon integral material.
Technical background
The energy is the basis of world development and progress of human society.As science and technology develops at high speed, oil, coal, day
So the traditional energy such as gas is following has exhausted danger, while including the earth ecology resource severe contamination such as air, soil, subsoil water
The problems such as bring huge challenge to human society, find and develop cleaning new energy and replace traditional energy very urgent, have
The electrochemical cell of removable feature obtains one of as an alternative the extensive concern of academia and industrial quarters.It is secondary with other
Battery is compared, and lithium ion battery has huge advantage, and it mainly shows as follows：(I) output voltage height (3.6V), is advantageously implemented
The integrated of battery, miniaturization, lighting；(II) has extended cycle life (generally up to more than thousand of times), far surpasses other secondary electricity
Pond；(III) specific energy is high, and specific energy has reached at present 100Whkg-1～200Whkg-1, far above other secondary electricity
Pond；(IV) self discharge is little, small volume, lightweight, environmental protection, memory-less effect.Lithium ion battery is in mobile phone, panel computer, number
The various electronic products such as code-phase machine have obtained increasingly being widely applied, in recent years the Devoting Major Efforts To Developing of electric automobile and fast
Speed development, the demand sharp increase of lithium-ion-power cell.Also pollution-free, reproducible energy is being found in the fields such as Aero-Space
Driving source is supported.Lithium ion battery has obtained many battery production enterprises and has recognized with the consistent of Automobile Enterprises under huge applications background
Can so as to become one of focus of current various countries' research and development.But at present the energy density of lithium ion battery is with power density also not
Economy can be met with industry high speed development to high-energy-density and the demand of the battery device of power density, be to solve this to ask
Topic, needs to research and develop energy density and power density that new material further improves lithium ion battery plus-negative plate material.It is with graphite
The carbon negative pole material of representative becomes that lithium ion battery negative material is highly developed, and the theoretical specific capacity of graphite is 372mAh
g-1, well, cycle efficieny is high for electric conductivity, and intercalation potential is low, and aboundresources, relative inexpensiveness, preparation process is fairly simple,
Jing has obtained extensive commercial applications.But graphite cathode capacity is confined to its relatively low theoretical capacity and commercial graphite
Itself microstructure of negative pole, it is also difficult to meet needs of the following high energy density cells to negative material, while power current
It is also that graphite cathode is difficult to what is realized that pond needs the demand of negative material high speed discharge and recharge, develops new with high power density
There is wide following application prospect with the carbonaceous negative material of energy density.
The content of the invention
The present invention is that graphite cathode power density in order to the solve current lithium ion battery technology low with energy density is asked
Topic, and the preparation method of a kind of nitrogen-doped graphene film and porous carbon integral material is provided.
A kind of nitrogen-doped graphene film of the present invention is carried out according to the following steps with the preparation method of porous carbon integral material：
First, presoma is prepared：Business filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes temperature be 60 DEG C
Under conditions of dry 2h, obtain clean filter membrane；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes
Temperature obtains clean Copper Foil to dry 2h under conditions of 60 DEG C；A piece of clean filter membrane is placed in the clean Copper Foil of two panels
Between and clean filter membrane is close to clean Copper Foil, obtain the material of sandwich structure, the material of sandwich structure is placed in into two
In the middle of block quartz wedge fixture and Copper Foil is close to quartz wedge, before obtaining the carbonization of nitrogen-doped graphene film and porous carbon integral material
Drive body；The aperture of described business filter membrane is 0.45 μm～0.8 μm；The thickness of described business Copper Foil is 8 μm；Described quartz
The size of block fixture is long 10cm, width 5cm, thickness 1cm；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
Spend to anneal 2h under conditions of 800 DEG C～1000 DEG C and argon protection, obtain on copper foil of affluxion body nitrogen-doped graphene film with
Porous carbon integral material.
The principle of the invention：Microporous filter membrane in the present invention is at high temperature in annealing process, when organic component is carbonized, part carbon
Atom volatilizees in a gaseous form, these carbon atoms nucleating growth in Copper Foil substrate under the catalytic action of Copper Foil, finally in copper
Large-area Graphene is formed on paper tinsel, this and utilization CH general in the world4For carbon source, using the method synthesizing graphite alkene of CVD
Principle is similar to, will but prepare that Graphene has to parameters such as air-tightness, annealing temperature, the shield gas flow rates of device using CVD
Ask strict；The present invention is to obtain Graphene using the carbon source (business filter membrane) of solid, and simple to operate, annealing temperature requirement is low, and
Except the carbon atom of part volatilization is in addition to copper foil surface obtains Graphene, it is fixed in another part carbon atom carbonisation
Many sky carbon structures are defined, this duct being primarily due in microporous filter membrane is micro- in addition while serve the effect of a template
Itself contain abundant nitrogen in the filter membrane of hole, nitrogen forms hexatomic ring or five-membered ring with carbon and then mixes simultaneously in carbonisation
In product after the miscellaneous carbonization to filter membrane, the present invention produces a pressure to prepare nitrogen-doped graphene film using the deadweight of quartz wedge
With porous charcoal bulk electrode.The present invention by a very simple step annealing can obtain the Graphene of nitrogen-doping with
Many sky carbon complexity integrative-structures.
Advantage of the present invention：
First, the present invention is using the structural advantage and nitrogen-doping of large-area Graphene and the integral material of porous carbon
Strategy, the two forms cooperative effect, prepares high performance novel pure carbon lithium ion cell negative electrode material, and the present invention is except as lithium
Outside ion battery cathode material, the conductive adhesive layer of positive and negative pole material is alternatively arranged as, and in catalysis, lithium-air battery, radiating
The aspects such as coating will all have huge application prospect.
2nd, nitrogen-doped graphene film and porous carbon integral material of the invention can also be grown in (stone on other collectors
English, aluminium oxide or other metals etc.), with certain universality；
3rd, the integrated artistic of the inventive method is very simple, workable, with can amplification, raw materials used cost
It is cheap and without the need for toxic chemical；
4th, the nitrogen-doped graphene film and porous carbon integral material that prepared by the method for the present invention possess high lithium storage content and
Higher coulombic efficiency, excellent high rate performance, remarkable cyclical stability, and can simultaneously serve as new lithium ion battery
Negative current collector, can be according to the lithium ion battery that high power capacity is prepared with extraordinary demand.
Description of the drawings
Fig. 1 is showing for the carbonization presoma of the nitrogen-doped graphene film that step one of the present invention is obtained and porous carbon integral material
It is intended to, wherein 1 is quartz wedge fixture, 2 is clean Copper Foil, and 3 is clean filter membrane；
Fig. 2 is to test the SEM figures for obtaining nitrogen-doped graphene film and porous carbon integral material on copper foil of affluxion body；
Fig. 3 is to test the SEM figures for obtaining nitrogen-doped graphene film and porous carbon integral material on copper foil of affluxion body；
Fig. 4 is to test the SEM figures for obtaining nitrogen-doped graphene film and porous carbon integral material on copper foil of affluxion body；
Fig. 5 is the element image of region A in Fig. 4；
Fig. 6 is XPS spectrum line chart, and curve 1 obtains nitrogen-doped graphene film and porous carbon for test one on copper foil of affluxion body
The XPS spectrum line of integral material, curve 2 is to test the carbon that nitrogen-doped graphene film and porous carbon integral material are obtained in a step one
Change presoma, peak a is the 1s track absworption peaks of C, and peak b is the 1s track absworption peaks of O, and peak c is the 1s track absworption peaks of N；
Fig. 7 is to test the AFM figures that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body；
Fig. 8 is to test the three material object photographs that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body
Piece, 1 is nitrogen-doped graphene film and porous carbon integral material, and 2 is copper foil of affluxion body.
Specific embodiment：
Specific embodiment one：Present embodiment is the preparation side of a kind of nitrogen-doped graphene film and porous carbon integral material
Method, is specifically carried out according to the following steps：
First, presoma is prepared：Business filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes temperature be 60 DEG C
Under conditions of dry 2h, obtain clean filter membrane；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes
Temperature obtains clean Copper Foil to dry 2h under conditions of 60 DEG C；A piece of clean filter membrane is placed in the clean Copper Foil of two panels
Between and clean filter membrane is close to clean Copper Foil, obtain the material of sandwich structure, the material of sandwich structure is placed in into two
In the middle of block quartz wedge fixture and Copper Foil is close to quartz wedge, before obtaining the carbonization of nitrogen-doped graphene film and porous carbon integral material
Drive body；The aperture of described business filter membrane is 0.45 μm～0.8 μm；The thickness of described business Copper Foil is 8 μm；Described quartz
The size of block fixture is long 10cm, width 5cm, thickness 1cm；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
Spend to anneal 2h under conditions of 800 DEG C～1000 DEG C and argon protection, obtain on copper foil of affluxion body nitrogen-doped graphene film with
Porous carbon integral material.
The advantage of present embodiment：
First, present embodiment is mixed using the structural advantage and nitrogen of large-area Graphene and the integral material of porous carbon
Miscellaneous strategy, the two forms cooperative effect, prepares high performance novel pure carbon lithium ion cell negative electrode material, and the present invention is except making
Outside for lithium ion battery negative material, be alternatively arranged as the conductive adhesive layer of positive and negative pole material, and catalysis, lithium-air battery,
The aspects such as thermal dispersant coatings will all have huge application prospect.
2nd, the nitrogen-doped graphene film and porous carbon integral material of present embodiment can also be grown on other collectors
(quartz, aluminium oxide or other metals etc.), with certain universality；
3rd, the integrated artistic of present embodiment method is very simple, workable, with can amplification, it is raw materials used
It is with low cost and without the need for toxic chemical；
4th, the nitrogen-doped graphene film and porous carbon integral material that prepared by the method for present embodiment possesses high storage lithium to be held
Amount and higher coulombic efficiency, excellent high rate performance, remarkable cyclical stability, and can simultaneously serve as new lithium ion
Battery cathode collector, can be according to the lithium ion battery that high power capacity is prepared with extraordinary demand.
Specific embodiment two：Present embodiment from unlike specific embodiment one：Business described in step one
The aperture of filter membrane is 0.45 μm.Other are identical with specific embodiment one.
Specific embodiment three：Unlike one of present embodiment and specific embodiment one to two:Institute in step one
The aperture of the business filter membrane stated is 0.6 μm.Other are identical with one of specific embodiment one to two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Institute in step one
The aperture of the business filter membrane stated is 0.8 μm.Other are identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Will in step 2
The nitrogen-doped graphene film and the carbonization presoma of porous carbon integral material that step one is obtained is that 800 DEG C and argon are protected in temperature
Under conditions of anneal 2h.Other are identical with one of specific embodiment one to four.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Will in step 2
The nitrogen-doped graphene film and the carbonization presoma of porous carbon integral material that step one is obtained is that 900 DEG C and argon are protected in temperature
Under conditions of anneal 2h.Other are identical with one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Will in step 2
The nitrogen-doped graphene film and the carbonization presoma of porous carbon integral material that step one is obtained is that 1000 DEG C and argon are protected in temperature
Anneal 2h under conditions of shield.Other are identical with one of specific embodiment one to six.
Using following verification experimental verifications effect of the present invention：
Test one：This test is the preparation method of a kind of nitrogen-doped graphene film and porous carbon integral material, is specifically pressed
What following steps were carried out：
First, presoma is prepared：Business filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes temperature be 60 DEG C
Under conditions of dry 2h, obtain clean filter membrane；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes
Temperature obtains clean Copper Foil to dry 2h under conditions of 60 DEG C；A piece of clean filter membrane is placed in the clean Copper Foil of two panels
Between and clean filter membrane is close to clean Copper Foil, obtain the material of sandwich structure, the material of sandwich structure is placed in into two
In the middle of block quartz wedge fixture and Copper Foil is close to quartz wedge, before obtaining the carbonization of nitrogen-doped graphene film and porous carbon integral material
Drive body；The aperture of described business filter membrane is 0.45 μm；The thickness of described business Copper Foil is 8 μm；Described quartz wedge fixture
Size be long 10cm, width 5cm, thickness 1cm；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
The 2h that anneals is spent under conditions of protecting with argon for 800 DEG C, nitrogen-doped graphene film and porous carbon one are obtained on copper foil of affluxion body
Body material.
Fig. 2 and Fig. 3 is to obtain nitrogen-doped graphene film in test one on copper foil of affluxion body with porous carbon integral material just
The SEM figures in face (front is nitrogen-doped graphene film and porous carbon integral material and that face of quartz wedge holder contacts), Fig. 4 is examination
Test and obtain nitrogen-doped graphene film on copper foil of affluxion body in one (reverse side is nitrogen-doped graphene with porous carbon integral material reverse side
That face that film is contacted with porous carbon integral material with Copper Foil) SEM figure, as can be seen from the figure this test preparation N doping stone
Black alkene film has excellent integrative-structure with porous carbon integral material, filter membrane is contacted with Copper Foil under the catalytic action of Copper Foil one
Face forms large-area Graphene, and in the part contacted with Copper Foil, porous carbon electrodes are formed.
Fig. 5 is the element image of region A in Fig. 4, it can be seen that N doping is obtained on copper foil of affluxion body in test one
Graphene film is carbon with porous carbon integral material main component, and loose structure is high-visible.
Fig. 6 is XPS spectrum line chart, and curve 1 obtains nitrogen-doped graphene film and porous carbon for test one on copper foil of affluxion body
The XPS spectrum line of integral material, curve 2 is to test the carbon that nitrogen-doped graphene film and porous carbon integral material are obtained in a step one
Change presoma, peak a is the 1s track absworption peaks of C, and peak b is the 1s track absworption peaks of O, and peak c is the 1s track absworption peaks of N, from figure
In it can be seen that this test that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body is first by C, N and O
Element composition, N element has successfully been doped in the material.
Fig. 7 is to test the AFM figures that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body,
Curve 1 obtains altitude information in figure, can draw in figure expression height step figure, and the thickness that can measure Graphene from curve 2 is about
For 4.5nm, nitrogen-doped graphene film is obtained on copper foil of affluxion body with porous carbon integral material in the thickness explanation test one
The thickness of multi-layer graphene is within 10 layers.
Test two：This test is the preparation method of a kind of nitrogen-doped graphene film and porous carbon integral material, is specifically pressed
What following steps were carried out：
First, presoma is prepared：Business filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes temperature be 60 DEG C
Under conditions of dry 2h, obtain clean filter membrane；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes
Temperature obtains clean Copper Foil to dry 2h under conditions of 60 DEG C；A piece of clean filter membrane is placed in the clean Copper Foil of two panels
Between and clean filter membrane is close to clean Copper Foil, obtain the material of sandwich structure, the material of sandwich structure is placed in into two
In the middle of block quartz wedge fixture and Copper Foil is close to quartz wedge, before obtaining the carbonization of nitrogen-doped graphene film and porous carbon integral material
Drive body；The aperture of described business filter membrane is 0.8 μm；The thickness of described business Copper Foil is 8 μm；Described quartz wedge fixture
Size is long 10cm, width 5cm, thickness 1cm；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
The 2h that anneals is spent under conditions of protecting with argon for 1000 DEG C, nitrogen-doped graphene film and porous carbon one are obtained on copper foil of affluxion body
Body material.
Test three：This test is the preparation method of a kind of nitrogen-doped graphene film and porous carbon integral material, is specifically pressed
What following steps were carried out：
First, presoma is prepared：Business filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes temperature be 60 DEG C
Under conditions of dry 2h, obtain clean filter membrane；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes
Temperature obtains clean Copper Foil to dry 2h under conditions of 60 DEG C；A piece of clean filter membrane is placed in the clean Copper Foil of two panels
Between and clean filter membrane is close to clean Copper Foil, obtain the material of sandwich structure, the material of sandwich structure is placed in into two
In the middle of block quartz wedge fixture and Copper Foil is close to quartz wedge, before obtaining the carbonization of nitrogen-doped graphene film and porous carbon integral material
Drive body；The aperture of described business filter membrane is 0.45 μm；The thickness of described business Copper Foil is 8 μm；Described quartz wedge fixture
Size be long 10cm, width 5cm, thickness 1cm；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
Anneal 2h under conditions of 1000 DEG C and argon protection, nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body.
Fig. 8 is to test the three material object photographs that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body
Piece, 1 is nitrogen-doped graphene film and porous carbon integral material, and 2 is copper foil of affluxion body.
Test four：Respectively nitrogen-doped graphene film and porous carbon one are obtained on copper foil of affluxion body to test one, test two
Body material and commercial graphite carry out the capacity section cycle performance test under high low range, it can be seen in table 1 that test one, test two
Capacity, stability and the high rate performance that nitrogen-doped graphene film and porous carbon integral material are obtained on copper foil of affluxion body is far above
Existing commercial graphite electrode, it is seen that the present invention's obtains nitrogen-doped graphene film and porous carbon one material on copper foil of affluxion body
Material effectively improves the storage lithium performance of composite, and the technology is simple, it is easy to amplify, easy industrialized production.
Table 1
Claims (7)
1. the preparation method of a kind of nitrogen-doped graphene film and porous carbon integral material, it is characterised in that nitrogen-doped graphene film with
Porous carbon integral material is carried out according to the following steps：
First, presoma is prepared：Microporous filter membrane is cut into into the rectangle of 4cm × 4cm, with after alcohol washes in the bar that temperature is 60 DEG C
2h is dried under part, clean filter membrane is obtained；Business Copper Foil is cut into into the rectangle of 10cm × 5cm, with after alcohol washes in temperature
To dry 2h under conditions of 60 DEG C, clean Copper Foil is obtained；A piece of clean filter membrane is placed in the middle of the clean Copper Foil of two panels and
Clean filter membrane is close to clean Copper Foil, obtains the material of sandwich structure, and the material of sandwich structure is placed in into two blocks of stones
In the middle of English block fixture and Copper Foil is close to quartz wedge, the carbonization forerunner of nitrogen-doped graphene film and porous carbon integral material is obtained
Body；The aperture of described microporous filter membrane is 0.45 μm～0.8 μm；The thickness of described business Copper Foil is 8 μm；Described micropore filter
Film contains nitrogen；
2nd, anneal：The nitrogen-doped graphene film that step one is obtained and the carbonization presoma of porous carbon integral material are in temperature
Anneal 2h under conditions of 800 DEG C～1000 DEG C and argon protection, nitrogen-doped graphene film and porous are obtained on copper foil of affluxion body
Carbon integral material.
2. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The aperture for being microporous filter membrane described in step one is 0.45 μm.
3. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The aperture for being microporous filter membrane described in step one is 0.6 μm.
4. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The aperture for being microporous filter membrane described in step one is 0.8 μm.
5. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The carbonization presoma for being the nitrogen-doped graphene film and porous carbon integral material for obtaining step one in step 2 is in temperature
Anneal 2h under conditions of 800 DEG C and argon protection.
6. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The carbonization presoma for being the nitrogen-doped graphene film and porous carbon integral material for obtaining step one in step 2 is in temperature
Anneal 2h under conditions of 900 DEG C and argon protection.
7. the preparation method of a kind of nitrogen-doped graphene film according to claim 1 and porous carbon integral material, its feature
The carbonization presoma for being the nitrogen-doped graphene film and porous carbon integral material for obtaining step one in step 2 is in temperature
Anneal 2h under conditions of 1000 DEG C and argon protection.
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| US11618680B2 (en) | 2018-03-23 | 2023-04-04 | Bright Day Graphene Ab | Carbon based composite material |
| CN113422082B (en) * | 2021-07-06 | 2023-04-21 | 中国科学技术大学 | Graphene-like carbon material electrocatalyst containing nitrogen-doped carbon five-membered ring structure, and preparation method and application thereof |
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| CN101760724A (en) * | 2010-01-26 | 2010-06-30 | 电子科技大学 | Method for preparing graphene membrane electrode with overlarge area and high quality |
| CN102616769A (en) * | 2012-03-19 | 2012-08-01 | 浙江大学 | Direct graphene film transfer method |
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| CN103387230A (en) * | 2013-07-23 | 2013-11-13 | 中国科学院微电子研究所 | Preparation method of graphene conductive film |
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| CN101760724A (en) * | 2010-01-26 | 2010-06-30 | 电子科技大学 | Method for preparing graphene membrane electrode with overlarge area and high quality |
| CN102923695A (en) * | 2011-08-09 | 2013-02-13 | 海洋王照明科技股份有限公司 | Graphene preparation method |
| CN102616769A (en) * | 2012-03-19 | 2012-08-01 | 浙江大学 | Direct graphene film transfer method |
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