CN109133039A - A kind of self assembly graphene nano film and its preparation method and application - Google Patents
A kind of self assembly graphene nano film and its preparation method and application Download PDFInfo
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- CN109133039A CN109133039A CN201710501009.4A CN201710501009A CN109133039A CN 109133039 A CN109133039 A CN 109133039A CN 201710501009 A CN201710501009 A CN 201710501009A CN 109133039 A CN109133039 A CN 109133039A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 122
- 239000002120 nanofilm Substances 0.000 title claims abstract description 68
- 238000001338 self-assembly Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000006185 dispersion Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- -1 graphite alkenes Chemical class 0.000 claims abstract description 20
- 230000000694 effects Effects 0.000 claims abstract description 11
- 238000012546 transfer Methods 0.000 claims abstract description 9
- 238000002834 transmittance Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000002028 Biomass Substances 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 9
- 239000010409 thin film Substances 0.000 description 8
- 238000002604 ultrasonography Methods 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 4
- 241000446313 Lamella Species 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241001252483 Kalimeris Species 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001652 electrophoretic deposition Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/30—Drying; Impregnating
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The present invention relates to a kind of self assembly graphene nano films and its preparation method and application.Specifically, described method includes following steps: 1) providing the first dispersion liquid, the second solvent and substrate, wherein first dispersion liquid includes the first solvent and the graphite alkenes material being scattered in first solvent；2) first dispersion liquid is added dropwise in second solvent with first rate, is based on marangoni effect, obtains the thin layer of the graphite alkenes material in the liquid level of gained mixed liquor；3) by the thin layer transfer to the substrate of graphite alkenes material obtained by step 2), it is dried products therefrom, obtains self assembly graphene nano film.The invention also discloses self assembly graphene nano film obtained and its applications in this way.The method can rapidly and efficiently, low cost, safety and environmental protection, substrate be without limiting and can be prepared on a large scale graphene nano film.The graphene nano uniformity of film is good, light transmittance is high and electric conductivity is excellent.
Description
Technical field
The present invention relates to Material Fields, more particularly to a kind of self assembly graphene nano film and preparation method thereof and answer
With.
Background technique
Graphene is since discovery in 2004, with performances such as its excellent mechanical property and conductive and heat-conductives, causes extensively
It attractes attention.Graphene has boundless application prospect, and the graphene film based on graphene sheet layer assembling is it applied to macro
The important morphological for seeing occasion, electrically conducting transparent heat conducting film, negative electrode of lithium ion battery, in terms of have and widely answer
With.
Currently, graphene-based method for manufacturing thin film mainly include filtration method, it is electrophoretic deposition, chemical vapour deposition technique, outer
Epitaxial growth, LB are self-assembled into embrane method etc..Processes and apparatus needed for the above method is complex, and film forming speed is slow, limits stone
The prepare with scale of black alkene film.Also, existing method, which exists, is difficult to prepare nanoscale graphite alkene film, at high cost, pollution ring
The limitation of the problems such as border, these methods force researcher to propose new method on preparing graphene film.
Summary of the invention
The purpose of the present invention is to provide one kind can rapidly and efficiently, low cost, safety and environmental protection, substrate without limitation and can advise greatly
The graphene nano film that mould prepares the method for graphene nano film and prepares in this way.The graphene nano is thin
Film uniformity is good, light transmittance is high and electric conductivity is excellent.
The first aspect of the present invention provides a kind of preparation method of self assembly graphene nano film, including walks as follows
It is rapid:
1) the first dispersion liquid, the second solvent and substrate are provided, wherein first dispersion liquid includes the first solvent and dispersion
Graphite alkenes material in first solvent；
2) first dispersion liquid is added dropwise in second solvent with first rate, is based on marangoni effect,
The liquid level of gained mixed liquor obtains the thin layer of the graphite alkenes material；
3) by the thin layer transfer to the substrate of graphite alkenes material obtained by step 2), it is dried products therefrom, is obtained
To self assembly graphene nano film.
In another preferred example, first solvent is different with second solvent, and the surface of second solvent
Ratio >=2 of power and the surface tension of first solvent, preferably >=4, more preferably >=6.
In another preferred example, the surface tension of second solvent and the ratio of the surface tension of first solvent are
2-100, or be 3-50, or be 4-20, or be 5-12.
In another preferred example, the surface tension of first solvent is 10-30Nm-1, preferably 10-25Nm-1, more preferably 15-25Nm-1。
In another preferred example, the surface tension of second solvent is 40-100Nm-1, preferably 40-80Nm-1, more preferably 60-80Nm-1。
In another preferred example, first solvent is selected from the group: methanol, ethyl alcohol, ethylene glycol, 1,3-PD, second two
Amine, acetone, the deionized water containing surfactant；And/or
Second solvent is selected from the group: water, sodium chloride solution, dimethyl sulfoxide, or combinations thereof.
In another preferred example, the surfactant is selected from the group: NaTDC, lauryl sodium sulfate or its
Combination.
In another preferred example, the graphite alkenes material is selected from the group: electrochemical stripping graphene, graphene oxide,
Redox graphene, mechanical stripping graphene, fluorinated graphene, biomass graphene, or combinations thereof.
In another preferred example, the graphite alkenes material with a thickness of 1-30nm, preferably 1-10nm, more preferably
1-5nm.
In another preferred example, in first dispersion liquid, the dispersion concentration of the graphite alkenes material is 0.01-
20mg/mL, preferably 0.03-10mg/mL, more preferably 0.05-5mg/mL.
In another preferred example, the substrate is selected from the group: metal and its oxide material, nonmetallic and its oxide material
Material, high molecular material.
In another preferred example, the metal and its oxide material are selected from the group: stainless steel base, aluminum alloy substrate,
Copper-based bottom.
In another preferred example, described nonmetallic and its oxide material is selected from the group: quartz substrate, substrate of glass, silicon
Substrate, diamond substrate, mica substrate.
In another preferred example, the high molecular material is selected from the group: PET substrate, polytetrafluoro
Vinyl bottom, polyvinyl chloride substrate.
In another preferred example, the first rate is 0.01-1000mL/min, preferably 0.1-500mL/min, more
Good ground 10-100mL/min.
In another preferred example, before step 2), the method also optionally includes step: ultrasonic treatment described first
Dispersion liquid.
In another preferred example, the time of the ultrasonic treatment is 10-300min, preferably 30-100min.
In another preferred example, in step 2), the mixed volume ratio of first dispersion liquid and second solvent is 1-
30:80-120, preferably 2-25:90-110.
In another preferred example, in step 2), the thin layer of the graphite alkenes material with a thickness of 1-100nm, preferably
3-80nm, more preferably 5-50nm.
In another preferred example, in step 3), the treatment temperature of the drying process is 40-120 DEG C, preferably 50-100
℃；And/or
The processing time under the treatment temperature is 10-120min, preferably 30-100min, more preferably 50-80min.
The second aspect of the present invention, provides a kind of self assembly graphene nano film, and the graphene nano film is
Using the preparation of method described in first aspect present invention.
In another preferred example, the graphene nano film has one or more features selected from the group below:
1) the graphene nano film with a thickness of 1-100nm, preferably 3-80nm, more preferably 5-50nm；
2) light transmittance of the graphene nano film is 50%-90%；
3) electric conductivity of the graphene nano film be 1000-1000000 Ω/sq, preferably 2000-300000 Ω/
Sq, more preferably 5000-100000 Ω/sq.
The third aspect of the present invention, provides a kind of product, and the product includes graphite described in second aspect of the present invention
Alkene nano thin-film or the graphene nano film described in second aspect of the present invention are made.
In another preferred example, the product is selected from the group: conductive film, thermally conductive film, electro-magnetic screen layer, choke block water
Layer.
It should be understood that above-mentioned each technical characteristic of the invention and having in below (eg embodiment) within the scope of the present invention
It can be combined with each other between each technical characteristic of body description, to form a new or preferred technical solution.As space is limited, exist
This no longer tires out one by one states.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained self assembly graphene nano film 1 of embodiment.
Fig. 2 is the Raman figure of 1 gained self assembly graphene nano film 1 of embodiment.
Fig. 3 is the light transmittance analysis test chart of 1 gained self assembly graphene nano film 1 of embodiment.
The SEM that Fig. 4 is 1 gained graphene film C1 of comparative example schemes.
The SEM that Fig. 5 is 2 gained graphene film C2 of comparative example schemes.
The SEM that Fig. 6 is 3 gained graphene film C3 of comparative example schemes.
Specific embodiment
The present inventor's in-depth study by long-term, unexpectedly obtain one kind can rapidly and efficiently, low cost, safety collar
It protects, substrate is without the method for limiting and can be prepared on a large scale graphene nano film.On this basis, inventor completes this hair
It is bright.
Preparation method
It is to realize the feasible way that largely prepares of graphene that solwution method, which prepares graphene film, preparation process also more at
It is ripe, graphene solution well dispersed in solvent is obtained, has laid good basis for next step self assembly.Marangoni effect is
Refer to that there are surface tension gradients for two kinds of different liquid surfaces of surface tension, the big liquid of surface tension is to its circumferential surface tension
The pulling force of small liquid is strong, flows liquid from the small direction big to surface tension of surface tension.It, can using marangoni effect
So that graphene forms self-assembled nanometer grade film on liquid-gas interface.
Specifically, the present invention utilizes marangoni effect, and graphene nano lamella is made to be self-assembly of ultra-thin receive in the water surface
Rice thin layer, resulting nano thin-film are transferred to any substrate surface.Method of the invention is simple and easy, and raw material is easy to get, to ring
Border is pollution-free, and gained nano thin-film has high transparency and certain electric conductivity, there is good application prospect.
More specifically, including the following steps: the present invention provides a kind of preparation method of self assembly graphene nano film
1) the first dispersion liquid, the second solvent and substrate are provided, wherein first dispersion liquid includes the first solvent and dispersion
Graphite alkenes material in first solvent；
2) first dispersion liquid is added dropwise in second solvent with first rate, is based on marangoni effect,
The liquid level of gained mixed liquor obtains the thin layer of the graphite alkenes material；
3) by the thin layer transfer to the substrate of graphite alkenes material obtained by step 2), it is dried products therefrom, is obtained
To self assembly graphene nano film.
In the present invention, the mixed volume ratio of first dispersion liquid and second solvent is 1:200~1:5.
It should be understood that in the present invention, the ratio of the surface tension of the surface tension of second solvent and first solvent
Value answers >=2, and as ratio < 2, the surface tension of the surface tension of the first solution and the second solution is got too close to, kalimeris dagger-axe Buddhist nun
Effect is not significant, and graphene is difficult to that self assembly behavior occurs in solution surface.
It should be understood that in the present invention, first solvent includes (but being not limited to) the following group: methanol, ethyl alcohol, ethylene glycol,
1,3- propylene glycol, ethylenediamine, acetone, the deionized water containing surfactant；And/or
Second solvent include (but being not limited to) the following group: water, sodium chloride solution, dimethyl sulfoxide, or combinations thereof.
It should be understood that in the present invention, the first rate answers≤1000mL/min, as rate > 1000mL/min,
When relative motion occurs for the surface of the second solution, excessively violent to liquid surface fluctuation, graphene is difficult to steadily lead to first solution
It crosses marangoni effect and self assembly behavior occurs in solution surface.
Furthermore, it is to be understood that the film of the method for the invention preparation is after reduction, effect is more excellent.
Graphene nano film and its application
The present invention also provides a kind of self assembly graphene nano film, the graphene nano film is using described
Method preparation.
In the present invention, the graphene nano film has one or more features selected from the group below:
1) the graphene nano film with a thickness of 1-100nm, preferably 3-80nm, more preferably 5-50nm；
2) light transmittance of the graphene nano film is 50%-90%；
3) electric conductivity of the graphene nano film be 1000-1000000 Ω/sq, preferably 2000-300000 Ω/
Sq, more preferably 5000-100000 Ω/sq.
The present invention also provides a kind of product, the product is comprising the graphene nano film or by the graphite
Alkene nano thin-film is made.
In another preferred example, the product includes (but being not limited to) the following group: conductive film, thermally conductive film, electromagnetic screen
Cover layer, choke water blocking layer.
Compared with prior art, the present invention has following major advantage:
(1) the method have rapidly and efficiently, low cost, simple process, safety and environmental protection, substrate without limit and can be extensive
The characteristics of preparing graphene nano film can substitute process for preparing graphenes by chemical vapour deposition film；
(2) the method with chemical reagent without being restored, without high temperature and special atmosphere, no pollution to the environment；
(3) the graphene nano uniformity of film is good, light transmittance is high and electric conductivity is excellent.
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip
Part or according to the normal condition proposed by manufacturer.Unless otherwise stated, otherwise percentage and number are calculated by weight.
Unless otherwise defined, it anticipates known to all professional and scientific terms as used herein and one skilled in the art
Justice is identical.In addition, any method similar to or equal to what is recorded and material can be applied to the method for the present invention.Wen Zhong
The preferred implement methods and materials are for illustrative purposes only.
1 graphene nano film 1 of embodiment
Electrochemical stripping graphene is mixed with ethyl alcohol, the dispersion liquid that concentration is 0.5mg/mL is configured to, is placed in ultrasonic machine
Middle ultrasound 60min.Dispersion liquid after taking 20mL ultrasound, is slowly added dropwise into 200mL water, is self-assembly of in the water surface uniformly thin
Layer.By on the thin layer transfer to quartz substrate of formation, 60min is dried at 60 DEG C, removes remaining water and dispersing agent, is obtained from group
Fill graphene nano film 1.
Fig. 1 is the scanning electron microscope (SEM) photograph of 1 gained self assembly graphene nano film 1 of embodiment.
As can be seen from Figure 1: graphene is spliced into comparatively dense nano-level thin-membrane by self assembly, and coverage rate is more than
99%.
Fig. 2 is the Raman figure of 1 gained self assembly graphene nano film 1 of embodiment.
As can be seen from Figure 2: wave number 1350cm-1The peak at place is the peak D of graphene, wave number 1600cm-1The peak at place is
The peak G of graphene, wave number 2700cm-1The peak at place is the peak 2D of graphene, and this kind of graphene yield is at low cost greatly.
Fig. 3 is the light transmittance analysis test chart of 1 gained self assembly graphene nano film 1 of embodiment.
As can be seen from Figure 3: graphene nano film in 300 to 800nm wave-length coverage without characteristic absorption, light
For transmissivity 80% or more, transparency is good.
Further, after tested, the electric conductivity of the graphene nano film 1 is 20000 Ω/sq.
2 graphene nano film 2 of embodiment
Electrochemical stripping graphene is mixed with methanol, the dispersion liquid that concentration is 1mg/mL is configured to, is placed in ultrasonic machine
Ultrasonic 60min.Dispersion liquid after taking 10mL ultrasound, is slowly added dropwise (such as with the rate of 20mL/min) into 200mL water, in the water surface
It is self-assembly of thin uniform layer.By on the thin layer transfer to substrate of glass of formation, 60min is dried at 60 DEG C, removes remaining water
And dispersing agent, obtain self assembly graphene nano film 2.
The performance of 2 gained graphene nano film 2 of embodiment and the performance class of 1 gained graphene nano film 1 of embodiment
Seemingly.
3 graphene nano film 3 of embodiment
Graphene oxide is mixed with ethyl alcohol, is configured to the dispersion liquid that concentration is 0.05mg/mL, is placed in ultrasonic machine ultrasonic
120min.Take 20mL ultrasound after dispersion liquid, be slowly added dropwise (such as with the rate of 20mL/min) into 100mL water, the water surface oneself
Assembling forms thin uniform layer.By on the thin layer transfer of formation to stainless steel base, 60min is dried at 80 DEG C, removes remaining water
And dispersing agent, obtain self assembly graphene nano film 3.
The performance of 3 gained graphene nano film 3 of embodiment and the performance class of 1 gained graphene nano film 1 of embodiment
Seemingly.
4 graphene nano film 4 of embodiment
Graphene oxide is mixed with ethylene glycol, the dispersion liquid that concentration is 0.1mg/mL is configured to, is placed in ultrasonic machine and surpasses
Sound 120min.Dispersion liquid after taking 10mL ultrasound, is slowly added dropwise (such as with the rate of 20mL/min) into 100mL water, in the water surface
It is self-assembly of thin uniform layer.By on the thin layer transfer to PET substrate of formation, dried at 80 DEG C
60min removes remaining water and dispersing agent, obtains self assembly graphene nano film 4.
The performance of 4 gained graphene nano film 4 of embodiment and the performance class of 1 gained graphene nano film 1 of embodiment
Seemingly.
5 graphene nano film 5 of embodiment
Redox graphene is mixed with acetone, the dispersion liquid that concentration is 2mg/mL is configured to, is placed in ultrasonic machine and surpasses
Sound 120min.Take 5mL ultrasound after dispersion liquid, be slowly added dropwise (such as with the rate of 20mL/min) into 200mL water, the water surface oneself
Assembling forms thin uniform layer.By on the thin layer transfer to silicon base of formation, 60min is dried at 60 DEG C, remove remaining water and is divided
Powder obtains self assembly graphene nano film 5.
The performance of 5 gained graphene nano film 5 of embodiment and the performance class of 1 gained graphene nano film 1 of embodiment
Seemingly.
1 graphene film C1 of comparative example
With embodiment 1, difference is: self-assembling method is not used, directly by graphene dispersion drop on substrate.
The SEM that Fig. 4 is 1 gained graphene film C1 of comparative example schemes.
As can be seen from Figure 4: graphene film C1 cannot form the film of even compact, and surface is very coarse.
2 graphene film C2 of comparative example
With embodiment 1, difference is: the concentration of graphene is 0.005mg/mL in graphene dispersing solution, and concentration is insufficient.
The SEM that Fig. 5 is 2 gained graphene film C2 of comparative example schemes.
As can be seen from Figure 5: since graphene concentration is insufficient, substrate surface cannot be completely covered in gained graphene film C2, no
It can be at continuous film.
3 graphene film C3 of comparative example
With embodiment 1, difference is: graphene used with a thickness of 200nm.
The SEM that Fig. 6 is 3 gained graphene film C3 of comparative example schemes.
As can be seen from Figure 6: in graphene film C3, graphene is reunited seriously, cannot form uniform film.
To sum up, the method that the present invention provides one kind rapidly and efficiently, can be prepared on a large scale graphene nano film.The present invention
Using marangoni effect, graphene nano lamella is made to be self-assembly of ultrathin nanometer thin layer, resulting nano thin-film in the water surface
It is transferred to any substrate surface.Method of the invention is simple and easy, and raw material is easy to get, no pollution to the environment, gained nano thin-film
With high transparency and certain electric conductivity, there is good application prospect.
All references mentioned in the present invention is incorporated herein by reference, independent just as each document
It is incorporated as with reference to such.In addition, it should also be understood that, after reading the above teachings of the present invention, those skilled in the art can
To make various changes or modifications to the present invention, such equivalent forms equally fall within model defined by the application the appended claims
It encloses.
Claims (10)
1. a kind of preparation method of self assembly graphene nano film, which comprises the steps of:
1) the first dispersion liquid, the second solvent and substrate are provided, wherein first dispersion liquid includes the first solvent and is scattered in institute
State the graphite alkenes material in the first solvent；
2) first dispersion liquid is added dropwise in second solvent with first rate, marangoni effect is based on, in gained
The liquid level of mixed liquor obtains the thin layer of the graphite alkenes material；
3) by the thin layer transfer to the substrate of graphite alkenes material obtained by step 2), it is dried products therefrom, is obtained certainly
Assemble graphene nano film.
2. the method as described in claim 1, which is characterized in that first solvent is different with second solvent, and described
Ratio >=2 of the surface tension of second solvent and the surface tension of first solvent.
3. the method as described in claim 1, which is characterized in that first solvent is selected from the group: methanol, ethyl alcohol, ethylene glycol,
1,3- propylene glycol, ethylenediamine, acetone, the deionized water containing surfactant；And/or
Second solvent is selected from the group: water, sodium chloride solution, dimethyl sulfoxide, or combinations thereof.
4. the method as described in claim 1, which is characterized in that the graphite alkenes material is selected from the group: electrochemical stripping stone
Black alkene, graphene oxide, redox graphene, mechanical stripping graphene, fluorinated graphene, biomass graphene or its group
It closes.
5. the method as described in claim 1, which is characterized in that in first dispersion liquid, point of the graphite alkenes material
Dissipating concentration is 0.01-20mg/mL.
6. the method as described in claim 1, which is characterized in that the first rate is 0.01-1000mL/min.
7. the method as described in claim 1, which is characterized in that in step 2), first dispersion liquid and second solvent
Mixed volume ratio be 1-30:80-120.
8. a kind of self assembly graphene nano film, which is characterized in that the graphene nano film is using claim 1 institute
The method preparation stated.
9. graphene nano film as claimed in claim 8, which is characterized in that the graphene nano film, which has, to be selected from down
The one or more features of group:
1) the graphene nano film with a thickness of 1-100nm；
2) light transmittance of the graphene nano film is 50%-90%；
3) electric conductivity of the graphene nano film is 1000-1000000 Ω/sq.
10. a kind of product, which is characterized in that the product is comprising graphene nano film according to any one of claims 8 or by right
It is required that graphene nano film described in 8 is made.
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| CN112126095A (en) * | 2020-09-30 | 2020-12-25 | 华中科技大学 | PEDOT (Polytetrafluoroethylene-PSS) film as well as preparation method and application thereof |
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|---|---|---|---|---|
| CN103738943A (en) * | 2013-11-14 | 2014-04-23 | 南京新月材料科技有限公司 | Large area transparent conductive graphene film preparation method |
| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738943A (en) * | 2013-11-14 | 2014-04-23 | 南京新月材料科技有限公司 | Large area transparent conductive graphene film preparation method |
| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112126095A (en) * | 2020-09-30 | 2020-12-25 | 华中科技大学 | PEDOT (Polytetrafluoroethylene-PSS) film as well as preparation method and application thereof |
| CN112126095B (en) * | 2020-09-30 | 2021-12-03 | 华中科技大学 | PEDOT (Polytetrafluoroethylene-PSS) film as well as preparation method and application thereof |
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