CN108622885A - A kind of preparation method of graphene film - Google Patents
A kind of preparation method of graphene film Download PDFInfo
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- CN108622885A CN108622885A CN201810737911.0A CN201810737911A CN108622885A CN 108622885 A CN108622885 A CN 108622885A CN 201810737911 A CN201810737911 A CN 201810737911A CN 108622885 A CN108622885 A CN 108622885A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The present invention provides a kind of preparation methods of graphene film.Graphene oxide is first prepared in the present invention, the graphene oxide that then will be obtained, and with metal reaction, obtains metal oxide/redox graphene compound；After removing metal oxide, redox graphene solution is obtained；Substrate is placed in beaker, distilled water is added, redox graphene solution is added dropwise, redox graphene film is formed in the water surface, then extra water is slowly sucked out with suction pipe, the graphene film will be obtained after substrate drying.It repeats the above steps, different layers of graphene films can be obtained.Redox graphene is directly self-assembled into film by this method, and method is simple, mild condition, is suitable for the preparation of a variety of substrate graphene films, and preparation method is harmless to substrate.
Description
Technical field
The invention belongs to function nano field of material technology to be more particularly to more particularly to a kind of method of graphene
A kind of preparation method of graphene film.
Background technology
Graphene is possessed unique low with cellular lattice structure made of six-membered cyclic close-packed arrays by monolayer carbon
The skeleton of dimension and sp2 hybrid structures has unique electric property and physicochemical properties.Graphene preparation method is to existing rank
Section has been achieved with huge progress, and main method has redox, mechanical stripping method, chemical vapour deposition technique and organic synthesis method.
With the development of modern science and technology, in order to meet the flexible design and power requirement that can carry electronic device, make it is ultralight,
Flexible, safety energy storage device is just becoming the research hotspot of people.Graphene film is as a kind of new carbon, since it has
The advantages that bigger serface, high-mechanical property, excellent electron transport ability, has in fields such as energy storages and widely answer
With.
Currently, the preparation method of graphene film mainly has suction method, spin-coating method, self-assembly method, electrophoresis and chemical gaseous phase
Sedimentation etc..Suction method prepares film and is controlled by filter paper size.Spin-coating method controls graphene film by dispersion liquid concentration, rotating speed
Thickness and area, the disadvantage is that be easy to causeing wastage of material.Self-assembling method is simple and practicable, and film size size can be controlled arbitrarily
System, preferable uniformity and controllability is presented in film, but using graphene oxide as phragmoplast, subsequent reduction treatment is to stone
Black alkene film and substrate have a great impact.When preparing graphene film using electrophoretic deposition, size is controlled by electrode,
Electrophoretic deposition voltage and sedimentation time are controlled, the graphene film of different-thickness can be prepared, but be not easy to will to obtain
Film is transferred in other substrates.Chemical vapour deposition technique can obtain the single layer graphene film of large-area high-quality, but exist
Of high cost, the problems such as equipment is complicated, technique is unable to continuous production.
Chinese patent 201210034061.0 discloses a kind of graphene oxide membrane, graphene film and preparation method thereof and answers
With.It is described prepare graphene oxide membrane method include：It is using Langmuir-Blodgett methods that the graphene oxide is molten
Drop is added on the water surface, makes to form graphene oxide membrane on water-air interface, the graphene oxide membrane is then transferred to base
On bottom.The preparation method for preparing graphene film is that the graphene oxide being prepared is placed in reducing atmosphere,
15-60min is heated at 800-1000 DEG C, obtains graphene film.
Chinese patent 201310149062.4 discloses a kind of method preparing large-area graphene and its laminated film, tool
Body method includes that graphene oxide water solution is poured over to the film layer that uniform fold is formed it on paper substrates, then executes baking
Dry curing process；The paper substrates for carrying graphene oxide film layer are immersed in hydroiodic acid and carry out reduction reaction, herein mistake
Paper substrates issue unboiled water solution while being reacted with acid in acidic environment in journey generates bubble, thus promotes graphene oxide film layer
Paper substrates are automatically disengaged, and it is thin to obtain required large-area graphene.
Chinese patent 201710797478.5 discloses oxidized graphene film, the preparation method of graphene film and described
The application of graphene film, present invention graphene oxide are grafted Tween80 and prepare amphiphilic graphene oxide, be then added
Graphene oxide membrane is formed in DC704 type silicon oil/water diphasic systems, then again spreads over graphene oxide membrane on substrate,
Graphene film is prepared in reduction in aqueous solution added with reducing agent
As described above, the preparation method of graphene film is to form a film first with graphene oxide solution in the prior art, then
Graphene film is prepared being restored to graphene oxide membrane.Surface of graphene oxide current potential is high, can generate sufficiently large
Repulsive force, thus graphene oxide suspension can stable dispersion, but restore after graphene surface current potential reduce, surface row
Repulsion reduces, and is easy to happen reunion, therefore is mostly first to prepare graphene oxide membrane in the prior art, then carries out reduction and is prepared into
To graphene film, but film catalyst is be easy to cause during redox graphene film, and using high temperature, chemistry
It is easy to damage flexible substrates during the restoring method such as agent.Therefore need to design one kind directly by oxygen reduction fossil
The method that black alkene prepares film forming.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of graphene film, the present invention is first
Graphene oxide is restored to obtain redox graphene, reduction-oxidation graphite is directly then self-assembled into film, method letter again
Single, mild condition is suitable for the preparation of a variety of substrate graphene films, and preparation method is harmless to substrate.
It explains：
1, it is the abbreviation of graphene not have special instruction, GO such as.
2, it is the abbreviation of redox graphene not have special instruction, RGO such as.
3, it is the abbreviation of metal oxide not have special instruction, MO such as.
4, it is the aqueous sulfuric acid that mass fraction is 98% not have special instruction, the heretofore described concentrated sulfuric acid such as.
5, it is that the hydrogen peroxide that mass fraction is 30% is water-soluble not have special instruction, heretofore described hydrogen peroxide such as
Liquid.
On the one hand, the present invention provides a kind of preparation method of graphene film, following steps are specifically included：
Step (1)：Mixture A is obtained after 30min is mixed in graphite flake, sodium nitrate and the concentrated sulfuric acid；
Step (2)：Under conditions of ice-water bath, potassium permanganate is added in the mixture A that step (1) obtains and is stirred
Then 12h is added distilled water and stirs 12h, hydrogen peroxide stirring is then added for 24 hours, mixture B is obtained by the reaction；
Step (3)：The mixture that step (2) is obtained, with after distilled water centrifugation washing 5-6 times to get to slurry GO；
Step (4)：Ultrasound 5min in distilled water is put into after sheet metal is polished with sand paper, the sheet metal that obtains that treated；
Step (5)：The graphene oxide for taking step (3) to obtain, is added distilled water thereto, after ultrasonic disperse, is mixed
Close object C；
Step (6)：Step (4) is obtained that treated, and sheet metal is put into the mixture C that step (5) obtains, 25
DEG C oil bath under the conditions of react 12h, the unreacted GO of sheet metal adsorption is washed off with distilled water and absolute ethyl alcohol, then will
Obtained sheet metal is placed in ultrasound in absolute ethyl alcohol and after five minutes takes out sheet metal, obtains MO/RGO complex solutions；
Step (7)：The MO/RGO complex solutions that step (6) obtains are placed in hydrochloric acid solution and stir 2h, use distilled water
After centrifugation washing, it is dispersed in organic solvent, obtains RGO solution；
Step (8)：Substrate is placed in beaker, distilled water is added, the RGO solution that step (7) obtains is added dropwise,
The water surface forms RGO films, and then extra water is slowly sucked out with suction pipe, until liquid level is down to substrate hereinafter, obtaining load has
The substrate of graphene film is placed in baking oven the graphene film described in drying to obtain；
The method for repeating step (8) is multiple, can obtain different layers of graphene films.
The quality of graphite flake in the step (1) is 5.0g, and the volume of the concentrated sulfuric acid is 120mL, and the quality of sodium nitrate is
2g。
The quality of potassium permanganate in the step (2) is 20g, and the volume of deionized water is 200mL, the volume of hydrogen peroxide
For 50mL.
Sheet metal in the step (4) is zinc metal sheet, iron plate or magnesium sheet.
The volume of GO in the step (5) is 10mL, and the volume of distilled water is 90mL.
The volume of absolute ethyl alcohol in the step (6) is 70mL.
The volume of organic solvent in the step (7) is 70mL, and the organic solvent is absolute ethyl alcohol and methanol
Mixture, wherein the volume ratio of absolute ethyl alcohol and methanol is 8-12:1；Preferably, the volume of the absolute ethyl alcohol and methanol
Than being 7:1.
The aqueous hydrochloric acid solution that hydrochloric acid solution in the step (7) is 0.1mol/L.
Preferably, the substrate in the step (8) is sheet glass, silicon chip or polythene strip.
The height distance upper surface of substrate 0.8-1.2cm of the distilled water of addition in the step (8), dry temperature are
50℃。
On the other hand, the present invention provides a kind of graphene films that above-mentioned preparation method obtains.
Beneficial effects of the present invention are：
(1) preparation method of graphene film provided by the invention is that GO is first reduced to RGO, then again RGO self assemblies
Film forming, method is simple, and mild condition does not damage substrate, can be adapted for the preparation of the graphene film of a variety of substrates.
(2) by the circulate operation of step (8), different layers of graphene films can be prepared, are effectively easily adjusted
The thickness of graphene film.
(3) graphene film preparation method provided by the invention is simple, and the uniformity for the graphene film prepared is good, this hair
It is bright to be found surprisingly that through the mixture that the organic solvent in step (7) is ethyl alcohol and methanol, and the volume ratio of ethyl alcohol and methanol
8-12：When 1, the uniformity of graphene film can be improved, and obtained RGO solution is more easy to form a film.
Description of the drawings
Fig. 1 is the transmission electron microscope picture for the graphene film being prepared in embodiment 1.
Fig. 2 is the Raman spectrogram of the GO and RGO that are prepared in embodiment 1
Fig. 3 is the different number of plies graphite being prepared in embodiment 1, embodiment 4, embodiment 5, embodiment 6 and embodiment 7
The transmitted light spectrogram of alkene film.
Specific implementation mode
A kind of preparation method of 1 graphene film of embodiment
Step (1)：Mixture A is obtained after 30min is mixed in 5.0g graphite flakes, 2g sodium nitrate and the 120mL concentrated sulfuric acids；
Step (2)：Under conditions of ice-water bath, 20g potassium permanganate is added in the mixture A that step (1) obtains and is stirred
12h is mixed, 200mL distilled water is then added and stirs 12h, the stirring of 15mL hydrogen peroxide is then added for 24 hours, mixture B is obtained by the reaction；
Step (3)：The mixture that step (2) is obtained, with after distilled water centrifugation washing 5 times to get to slurry GO；
Step (4)：Ultrasound 5min in distilled water is put into after zinc metal sheet is polished with sand paper, the zinc metal sheet that obtains that treated；
Step (5)：The GO 10mL (2mg/mL) that step (3) obtains are taken, 90mL distilled water, ultrasonic disperse are added thereto
Afterwards, mixture C is obtained；
Step (6)：Step (4) is obtained that treated, and 5g zinc metal sheets are put into the mixture C that step (5) obtains, 25
DEG C oil bath under the conditions of react 12h, the unreacted GO of zinc metal sheet adsorption is washed off with distilled water and absolute ethyl alcohol, then will
To zinc metal sheet be placed in ultrasonic disperse in 70mL absolute ethyl alcohols and after five minutes take out zinc metal sheet, obtain ZnO/RGO complex solutions；
Step (7)：The ZnO/RGO complex solutions that step (6) obtains are placed in 20mL 0.1mol/L hydrochloric acid solutions and are stirred
2h is mixed, after distilled water centrifugation washing, is dispersed in the absolute ethyl alcohol of 70mL and the mixture of methanol, wherein anhydrous second
The volume ratio of alcohol and methanol is 10:1, obtain RGO solution；
Step (8)：Sheet glass is placed in beaker, the height distance sheet glass upper surface 0.8cm of the distilled water of addition, it will
The RGO solution that step (7) obtains is added dropwise, and forms RGO films in the water surface, then extra water is slowly sucked out with suction pipe,
Until liquid level is down to substrate hereinafter, obtaining loading the sheet glass for having graphene film, the stone described in drying to obtain is placed in baking oven
Black alkene film.
A kind of preparation method of 2 graphene film of embodiment
Step (1)：Mixture A is obtained after 30min is mixed in 5.0g graphite flakes, 2g sodium nitrate and the 120mL concentrated sulfuric acids；
Step (2)：Under conditions of ice-water bath, 20g potassium permanganate is added in the mixture A that step (1) obtains and is stirred
12h is mixed, 200mL distilled water is then added and stirs 12h, the stirring of 15mL hydrogen peroxide is then added for 24 hours, mixture B is obtained by the reaction；
Step (3)：The mixture that step (2) is obtained, with after distilled water centrifugation washing 5 times to get to slurry GO；
Step (4)：Ultrasound 5min in distilled water is put into after magnesium sheet is polished with sand paper, the iron plate that obtains that treated；
Step (5)：The GO 10mL (2mg/mL) that step (3) obtains are taken, 90mL distilled water, ultrasonic disperse are added thereto
Afterwards, mixture C is obtained；
Step (6)：Step (4) is obtained that treated, and 5g magnesium sheets are put into the mixture C that step (5) obtains, 25
DEG C oil bath under the conditions of react 12h, the unreacted GO of zinc metal sheet adsorption is washed off with distilled water and absolute ethyl alcohol, then will
To magnesium sheet be placed in ultrasonic disperse in 70mL absolute ethyl alcohols and after five minutes take out magnesium sheet, obtain MgO/RGO complex solutions；
Step (7)：The MgO/RGO complex solutions that step (6) obtains are placed in 20mL 0.1mol/L hydrochloric acid solutions and are stirred
2h is mixed, after distilled water centrifugation washing, is dispersed in the absolute ethyl alcohol of 70mL and the mixture of methanol, wherein anhydrous second
The volume ratio of alcohol and methanol is 12:1, obtain RGO solution；
Step (8)：Silicon chip is placed in beaker, the height distance silicon chip upper surface 1.2cm of the distilled water of addition, by step
(7) the RGO solution obtained is added dropwise, and forms RGO films in the water surface, then extra water is slowly sucked out with suction pipe, until
Liquid level is down to substrate hereinafter, obtaining loading the sheet glass for having graphene film, is placed in baking oven the graphene described in drying to obtain
Film.
A kind of preparation method of 3 graphene film of embodiment
Step (1)：Mixture A is obtained after 30min is mixed in 5.0g graphite flakes, 2g sodium nitrate and the 120mL concentrated sulfuric acids；
Step (2)：Under conditions of ice-water bath, 20g potassium permanganate is added in the mixture A that step (1) obtains and is stirred
12h is mixed, 200mL distilled water is then added and stirs 12h, the stirring of 15mL hydrogen peroxide is then added for 24 hours, mixture B is obtained by the reaction；
Step (3)：The mixture that step (2) is obtained, with after distilled water centrifugation washing 5 times to get to slurry GO；
Step (4)：Ultrasound 5min in distilled water is put into after iron plate is polished with sand paper, the iron plate that obtains that treated；
Step (5)：The GO 10mL (2mg/mL) that step (3) obtains are taken, 90mL distilled water, ultrasonic disperse are added thereto
Afterwards, mixture C is obtained；
Step (6)：Step (4) is obtained that treated, and 5g iron plates are put into the mixture C that step (5) obtains, 25
DEG C oil bath under the conditions of react 12h, the unreacted GO of iron plate adsorption is washed off with distilled water and absolute ethyl alcohol, then will
To iron plate be placed in ultrasonic disperse in 70mL absolute ethyl alcohols and after five minutes take out iron plate, obtain Fe2O3/ RGO complex solutions；
Step (7)：The Fe that step (6) is obtained2O3/ RGO complex solutions are placed in 20mL 0.1mol/L hydrochloric acid solutions
2h is stirred, after distilled water centrifugation washing, is dispersed in the absolute ethyl alcohol of 70mL and the mixture of methanol, wherein anhydrous
The volume ratio of ethyl alcohol and methanol is 8:1, obtain RGO solution；
Step (8)：Polythene strip is placed in beaker, the height distance silicon chip upper surface 1.0cm of the distilled water of addition, it will
The RGO solution that step (7) obtains is added dropwise, and forms RGO films in the water surface, then extra water is slowly sucked out with suction pipe,
Until liquid level is down to silicon chip hereinafter, obtaining loading the silicon chip for having graphene film, the graphite described in drying to obtain is placed in baking oven
Alkene film.
A kind of preparation method of 4 graphene film of embodiment
Preparation method substantially with embodiment 1, with embodiment 1 the difference is that, repeat step (8) 2 times, obtain 3 layers of graphite
Alkene film.
A kind of preparation method of 5 graphene film of embodiment
Preparation method substantially with embodiment 1, with embodiment 1 the difference is that, repeat step (8) 4 times, obtain 5 layers of graphite
Alkene film.
A kind of preparation method of 6 graphene film of embodiment
Preparation method substantially with embodiment 1, with embodiment 1 the difference is that, repeat step (8) 6 times, obtain 7 layers of graphite
Alkene film.
A kind of preparation method of 7 graphene film of embodiment
Preparation method substantially with embodiment 1, with embodiment 1 the difference is that, repeat step (8) 8 times, obtain 9 layers of graphite
Alkene film.
A kind of preparation method of 1 graphene film of comparative example
Preparation method substantially with embodiment 1, with 1 preparation method of embodiment the difference is that：Solvent in step (7) is second
Alcohol.The graphene film lack of homogeneity being prepared.
A kind of preparation method of 2 graphene film of comparative example
Preparation method substantially with embodiment 1, with 1 preparation method of embodiment the difference is that：Solvent in step (7) is first
Alcohol.The graphene film being prepared is not easy to form a film.
Fig. 1 is the transmission electron microscope picture for the graphene film being prepared in embodiment 1.
Fig. 2 is the Raman spectrogram of the GO and RGO that are prepared in embodiment 1, and wherein GO is to be obtained in step (3)
GO, from the figure, it can be seen that the ratio of the peaks D of GO and G peak intensities is 0.88, and the I of the RGO after restoringD/IGIt is 1.45, from
And can prove that the oxygen-containing group of GO can be removed in Zn reduction processes, to obtain RGO.
Fig. 3 be implement 1, embodiment 4, the different number of plies graphene films that embodiment 5, embodiment 6 and embodiment 7 are prepared
Transmitted light spectrogram.It can be seen that the increase with the RGO numbers of plies, light transmittance are gradually dropped from 90% or more originally from 3
Low, after depositing 9 layers, light transmittance is about 20%.It can be seen that its light transmittance can realize multistage adjusting by the number of plies,
So as to so that it met in the needs of different application.
Only as described above, only the preferred embodiments of the invention, when the model that cannot limit implementation of the invention with this
It encloses, i.e., generally according to simple equivalent changes and modifications made by the content recorded in the claims in the present invention and description of the invention,
All it is still covered by the claims of the invention.It is searched in addition, abstract part and title are intended merely to auxiliary patent document
It seeks and being used, not be used for limiting the interest field of the present invention.
Claims (10)
1. a kind of preparation method of graphene film, which is characterized in that include the following steps：
Step (1)：Mixture A is obtained after 30min is mixed in graphite flake, sodium nitrate and the concentrated sulfuric acid；
Step (2)：Under conditions of ice-water bath, potassium permanganate is added in the mixture A that step (1) obtains and stirs 12h, so
Distilled water is added afterwards and stirs 12h, hydrogen peroxide stirring is then added for 24 hours, mixture B is obtained by the reaction；
Step (3)：The mixture B that step (2) is obtained aoxidizes stone after being washed 5-6 times with distilled water centrifugation to get to slurry
Black alkene；
Step (4)：Ultrasound 5min in distilled water is put into after sheet metal is polished with sand paper, the sheet metal that obtains that treated；
Step (5)：The graphene oxide for taking step (3) to obtain, is added distilled water thereto, after ultrasonic disperse, obtains mixture
C；
Step (6)：Step (4) is obtained that treated, and sheet metal is put into the mixture C that step (5) obtains, at 25 DEG C
12h is reacted under the conditions of oil bath, the unreacted graphene oxide of sheet metal adsorption is washed off with distilled water and absolute ethyl alcohol, so
Obtained sheet metal is placed in ultrasound in absolute ethyl alcohol afterwards after five minutes to take out sheet metal, obtains metal oxide/reduction-oxidation
Graphene complex solution；
Step (7)：Metal oxide/redox graphene complex solution that step (6) obtains is placed in hydrochloric acid solution
2h is stirred, after distilled water centrifugation washing, is dispersed in organic solvent, obtains redox graphene solution；
Step (8)：Substrate is placed in beaker, distilled water is added, the redox graphene solution that step (7) is obtained is dropwise
It is added, forms redox graphene film in the water surface, then extra water is slowly sucked out with suction pipe, until liquid level is down to base
There is the substrate of graphene at bottom hereinafter, obtaining load, is placed in baking oven the graphene film described in drying to obtain.
2. the preparation method of graphene film according to claim 1, which is characterized in that the graphite flake in the step (1)
Quality be 5.0g, the volume of the concentrated sulfuric acid is 120mL, and the quality of sodium nitrate is 2g.
3. the preparation method of graphene film according to claim 1, which is characterized in that the permanganic acid in the step (2)
The quality of potassium is 20g, and the volume of deionized water is 200mL, and the volume of hydrogen peroxide is 50mL.
4. the preparation method of graphene film according to claim 1, which is characterized in that the sheet metal in the step (4)
For zinc metal sheet, iron plate or magnesium sheet.
5. the preparation method of graphene film according to claim 1, which is characterized in that the oxidation stone in the step (5)
The volume of black alkene is 10mL, and the volume of distilled water is 90mL.
6. the preparation method of graphene film according to claim 1, which is characterized in that the anhydrous second in the step (6)
The volume of alcohol is 70mL.
7. the preparation method of graphene film according to claim 1, which is characterized in that organic molten in the step (7)
The volume of agent is 70mL, and the organic solvent is the mixture of absolute ethyl alcohol and methanol, wherein the body of absolute ethyl alcohol and methanol
Product is than being 8-12:1.
8. the preparation method of graphene film according to claim 7, which is characterized in that the organic solvent is anhydrous second
The mixture of alcohol and methanol, wherein the volume ratio of absolute ethyl alcohol and methanol is 10:1.
9. the preparation method of graphene film according to claim 1, which is characterized in that the substrate in the step (8) is
One kind in sheet glass, silicon chip or polythene strip；The preparation method of graphene film according to claim 1, feature exist
In the height distance upper surface of substrate 0.8-1.2cm of the distilled water of the addition in step (8), dry temperature is 50 DEG C.
10. the graphene film being prepared according to the preparation method of graphene film described in any one of claim 1-9.
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| CN112898953A (en) * | 2021-01-14 | 2021-06-04 | 蒋军良 | Preparation method of graphene heat-conducting film |
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