CN105225766A - A kind of preparation method of transparent graphene conductive film - Google Patents
A kind of preparation method of transparent graphene conductive film Download PDFInfo
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- CN105225766A CN105225766A CN201510459265.2A CN201510459265A CN105225766A CN 105225766 A CN105225766 A CN 105225766A CN 201510459265 A CN201510459265 A CN 201510459265A CN 105225766 A CN105225766 A CN 105225766A
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Abstract
The present invention relates to a kind of preparation method of transparent graphene conductive film, described method carries out reduction reaction for being contacted with reductant solution by graphene oxide film, obtains graphene film after clean process.The preparation method of transparent graphene conductive film of the present invention can carry out large area serialization preparation, easy and simple to handle; With metal ion solvent for reductant solution, can stablize and deposit, use safety, there is very high practicality; The transparent graphene conductive film light transmission prepared and electric conductivity excellence.
Description
Technical field
The invention belongs to graphene film preparation field, particularly relate to a kind of preparation method of transparent graphene conductive film.
Background technology
Along with the development of photoelectric device and Display Technique, transparency electrode as this field key element and receive much concern.At present, commercial transparent conductive material is ITO (tin indium oxide), and wherein causes cost higher containing a large amount of rare element indium.Therefore, high-performance transparent conductive material that is cheap, that can prepare in a large number is found very necessary as the substitute of ITO.
Graphene is a kind of monoatomic layer Two-dimensional Carbon nano material, has excellent electron mobility and light transmission, is therefore subject to extensive concern as ideal transparent conductive material.But the large bottleneck that graphene film remains this field is prepared in large area serialization.
Chemical vapour deposition (CVD) (CVD) method can prepare high-quality graphene film, but CVD cost is high, need to carry out under the high temperature conditions, be unsuitable for directly masking on a flexible substrate, preparation and transfer process also very easily introduce defect simultaneously, thus affect the performance of film.Adopt chemical method graphite oxide, then to carry out reducing and obtaining Graphene be a kind of method that cheapness can be prepared in a large number.Although the defect formed in oxidizing process can not be repaired completely, simultaneously because reduction not thoroughly can affect the conductivity of Graphene to a certain extent, graphene film prepared by this method still can be adapted to the application of many transparent conductive films, as touch-screen, electrochromic device etc.
At present, the common reducing agent of redox graphene is the material that the toxicity such as hydroiodic acid, hydrazine hydrate is larger, and reduction process is carried out usually under the gaseous state of reducing agent, to environment and operating personnel's harm comparatively large, be unsuitable for continuous prodution.In the recent period, active metal is also used as the excellent reduction agent (J.Mater.Chem.A of graphene oxide, 2014,2,10969), but realize the even coating of metal in graphene oxide membrane and usually will use the method such as hot evaporation, magnetron sputtering higher to equipment requirement, be still unsuitable for large area and prepare graphene film.Reducing metal ion also has good reproducibility, and can form stable reductant solution, but is not also applied to the work report of redox graphene film at present.Adopt the coating process of liquid phase or graphene oxide membrane directly immersed in reducing solution and can realize reduction process simply, and being easy to adapt to continuous prodution.By regulating reducing condition parameter, the graphene-based transparent conductive film of excellent performance can be obtained, be a kind of cheapness, efficient, serialization can prepare the method for redox graphene film in a large number.
CN102557013A provides a kind of preparation method of redox graphene, and the method comprises and graphene oxide and metal or reducing metal oxide being contacted with acid.The light transmission that transparent conductive film prepared by described method cannot reach simultaneously and conductivity, as when light transmission 91%, sheet resistance at 10k Ω/, and when sheet resistance at 1.2k Ω/ time, light transmission is 86%.
Therefore, a kind of method can preparing high-quality graphene transparent conductive film is urgently developed in this area, and described method is simple, efficient, is easy to operation.
Summary of the invention
An object of the present invention is the preparation method providing a kind of transparent graphene conductive film, and described method carries out reduction reaction for being contacted with reductant solution by graphene oxide film, obtains graphene film after clean process.
Solid-state graphene oxide film fully contacts with reductant solution by the present invention, carry out reduction reaction, graphene oxide film is being kept being reduced to graphene film under the constant state of filminess, afterwards through clean process, go out the impurity such as reducing agent, solvent, after drying, obtain graphene film.
Reductant solution of the present invention is the metal salt solution with reproducibility.
Of the present invention have in the metal salt solution of reproducibility, reducing metal ion plays reduction, graphene oxide is reduced to Graphene, and the solution state of reductant solution can impel reducing metal uniform ion to be distributed in the surface of graphene oxide, and contact with the oxygen atom of graphene oxide under ionization and carry out reduction reaction.
Preferably, metal ion in described metal salt solution is the combination of any a kind or at least 2 kinds had in the low price ion of multivalent state metal, the combination of any a kind or at least 2 kinds in the lower valency ion of preferred Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Cd, Sn, Pd, Bi, preferred Fe and/or Sn.
The metal ion that the low price ion of multivalent state metal of the present invention refers to have multiple valence state in compound with the metal ion form that lower valence state exists; Such as iron chloride and frerrous chloride, iron is aobvious trivalent in iron chloride compound, and in frerrous chloride, show divalence, so the iron in iron chloride is high-valence state, the iron in frerrous chloride is lower valency.
In metal salt solution of the present invention, the anion contended with metal ion is not particularly limited, and typical but non-limitingly comprises nitrate anion, sulfate radical, halide ion etc.
Preferably, the solvent of described metal salt solution is water-soluble solvent or solution, the mixture of any a kind or at least 2 kinds in preferred water, ethanol, isopropyl alcohol, ammoniacal liquor, sodium hydroxide solution, hydrochloric acid solution.
Preferably, the concentration of described metal salt solution is 0.01 ~ 1mol/L, such as 0.05mol/L, 0.08mol/L, 0.15mol/L, 0.38mol/L, 0.5mol/L, 0.8mol/L, 0.9mol/L etc.
The mode of contact of the present invention is spraying, spin coating, dipping, any a kind or at least 2 kinds dripped in being coated with combination; Preferably graphene oxide film is immersed in reductant solution, or reductant solution is spin-coated on graphene oxide film.
The mode of contact of the present invention is the various modes of carrying out being coated with that those skilled in the art can be known.
Preferably, during described contact, the amount of the metal ion of every square centimeter of graphene oxide film contact is 0.001 ~ 1mmol, such as 0.005mol/L, 0.008mol/L, 0.015mol/L, 0.038mol/L, 0.05mol/L, 0.08mol/L, 0.1mol/L, 0.15mol/L, 0.18mol/L, 0.19mol/L etc.
The temperature of reduction reaction of the present invention is 1 ~ 100 DEG C, such as 3 DEG C, 9 DEG C, 23 DEG C, 35 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 90 DEG C etc., preferably 25 ~ 60 DEG C;
Preferably, the time of described reduction reaction is 1min ~ 24h, such as 0.1h, 0.5h, 3h, 14h, 20h etc., preferably 5 ~ 60min.
The C/O of graphene oxide film of the present invention is than being 1:2 ~ 5:1, preferably 2 ~ 3:1.
Preferably, the build of described graphene oxide film is 2 ~ 1000nm, such as 5nm, 15nm, 50nm, 80nm, 100nm, 110nm, 170nm, 300nm, 500nm, 800nm, 900nm etc., preferably 5 ~ 50nm.
The thickness of graphene oxide film of the present invention, those skilled in the art can require to determine according to the light transmission of graphene film to be prepared, and light transmission requires higher, and usual thickness needs thinner.
The object of cleaning process of the present invention is to remove the such as impurity such as reducing agent, solvent on graphene film, and the process of described cleaning process is: carried out by the graphene film after reduction reaction washing, dry.
Preferably, described washing is for rinsing or the reacted graphene film of soaking and reducing.
Preferably, the solution of described flushing or immersion is the combination of any a kind or at least 2 kinds in water, ethanol or diluted acid.
In order to go out the metal oxide that may occur in preparation process during described diluted acid, the concentration of diluted acid and kind the present invention are not specifically limited, with reactive metal oxide, the diluted acid of it removing all the present invention be can be can be used in principle, typical but non-limitingly the watery hydrochloric acid of 0.01mol/L, the dilute sulfuric acid etc. of 0.01mol/L comprised.
The preparation method of graphene oxide film of the present invention is:
Graphene oxide dispersion is coated on substrate and obtains graphene oxide film.
The present invention does not limit painting method.
Preferably, the method for described coating is the combination of line rod film, spin coating, spraying, Best-Effort request, blade coating, intaglio plate, relief printing plate, any a kind or at least 2 kinds in printing;
Preferably, the decentralized medium of described graphene oxide dispersion is water.
The preparation method of graphene oxide of the present invention is selected from Hummers method, Brodie method, Staudenmaier method, graphite intercalation stripping, the ultrasonic stripping of graphite, graphite shear and peel off in any a kind or any 1 in deriving method.
The method of the invention is that C/O is immersed in concentration than the graphene oxide film being 2.5 ~ 3.5:1 is in the reductant solution of 0.08 ~ 0.12mol/L, at 40 ~ 60 DEG C of temperature, carry out reduction reaction 8 ~ 12min time, after washing, drying, obtain graphene film.
Compared with prior art, the present invention has following beneficial effect:
(1) preparation method of transparent graphene conductive film of the present invention can carry out large area serialization preparation, easy and simple to handle;
(2) reductant solution that the method for the invention uses is metal ion solvent, can stablize and deposit, use safety, have very high practicality;
(3) transparent graphene conductive film that the method for the invention prepares can ensure high light transmittance and high conductivity simultaneously, can when ensureing that light transmission is 90%, and average sheet resistance is lower than 3k Ω/.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) prepare the graphene oxide solution of 1mg/mL, with line rod (linear diameter 20 μm) coating film forming on the pet substrate, obtain graphene oxide membrane in 60 DEG C of dry 2h, C/O is than being 3:1;
(2) hydrochloric acid solution (reductant solution) of the ferrous sulfate containing 0.1mol/L is dropped in graphene oxide membrane, the amount making the metal ion of every square centimeter of graphene oxide film contact is 0.02mmol, be placed on and heat 10min in 60 DEG C of drying boxes and carry out reduction reaction, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Conductivity: test by the conductivity of four-point probe to the graphene film of gained, recording average sheet resistance is 2.1k Ω/;
Light transmission: test by the ultraviolet/light transmission of visible/near infrared spectrophotometer to the graphene film of gained, light transmittance is 91.4% at 550nm wavelength place.
Embodiment 2:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) graphene oxide membrane is immersed in the hydrochloric acid solution of the frerrous chloride of the 0.01mol/L of 20mL, the amount making the metal ion of every square centimeter of graphene oxide film contact is 0.01mmol, be placed in 60 DEG C of drying boxes to heat 10min and carry out reduction reaction, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 1.8k Ω/, 550nm wavelength place light transmittance is 91%.
Embodiment 3:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) graphene oxide membrane is immersed in the hydrochloric acid solution of the ferrous nitrate of the 0.01mol/L of 20mL, carries out reduction reaction 24h under being placed in normal temperature, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 2.2k Ω/, 550nm wavelength place light transmittance is 91.8%.
Embodiment 4
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) in graphene oxide membrane, drip the hydrochloric acid solution of the stannous chloride being coated with 0.1mol/L, be placed in 60 DEG C of drying boxes and heat 10min, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 3.0k Ω/, 550nm wavelength place light transmittance is 90.6%.
Embodiment 5:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) hydrochloric acid solution (reductant solution) of the stannous sulfate containing 0.1mol/L is dropped in graphene oxide membrane, the amount making the metal ion of every square centimeter of graphene oxide film contact is 0.02mmol, be placed on and heat 10min in 60 DEG C of drying boxes and carry out reduction reaction, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 2.3k Ω/, 550nm wavelength place light transmittance is 90.8%.
Embodiment 6:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) containing 0.01mol/L stannous chloride and 1mol/L iron chloride complex reducing agent solution coat on graphene oxide film, then 30min will be heated in 60 DEG C of drying boxes;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 1.7k Ω/, 550nm wavelength place light transmittance is 91.1%.
Embodiment 7:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) identical with the step (1) of embodiment 1;
(2) containing 0.1M stannous chloride and 0.1M stannous sulfate complex reducing agent solution coat on graphene film, then will heat 30 minutes in 70 DEG C of drying boxes;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 1.8k Ω/, 550nm wavelength place light transmittance is 90.9%.
Embodiment 8:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) prepare the graphene oxide solution of 1mg/mL, with line rod (linear diameter 40 μm) coating film forming on the pet substrate, obtain graphene oxide membrane in 60 DEG C of dry 2h, C/O is than being 3:1;
(2) hydrochloric acid solution (reductant solution) of the sub-tin of nitric acid containing 0.05mol/L is dropped in graphene oxide membrane, the amount making the metal ion of every square centimeter of graphene oxide film contact is 0.01mmol, be placed on and heat 10min in 60 DEG C of drying boxes and carry out reduction reaction, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 0.6k Ω/, 550nm wavelength place light transmittance is 86.7%.
Embodiment 9:
A preparation method for transparent graphene conductive film, described method comprises the steps:
(1) prepare the graphene oxide solution of 1mg/mL, with line rod (linear diameter 80 μm) coating film forming on the pet substrate, obtain graphene oxide membrane in 60 DEG C of dry 2h, C/O is than being 3:1;
(2) hydrochloric acid solution (reductant solution) of the stannic bromide containing 1mol/L is dropped in graphene oxide membrane, the amount making the metal ion of every square centimeter of graphene oxide film contact is 0.2mmol, be placed on and heat 10min in 60 DEG C of drying boxes and carry out reduction reaction, obtain graphene film first product;
(3), after taking out graphene film first product, soak with dilute hydrochloric acid solution, wash three times with intermediate water, obtain graphene film in 60 DEG C of dry 2h.
Performance test:
Method of testing is with embodiment 1, and test result is average sheet resistance be 0.3k Ω/, 550nm wavelength place light transmittance is 82.3%.
Comparative example
The redox graphene transparent conductive film provided with the embodiment 11 of CN102557013A, for comparative example, carries out performance test, and method of testing is identical with embodiment 1, and test result is average sheet resistance be 10k Ω/, 550nm wavelength place light transmittance is 91%.
As can be seen from the experimental data of embodiment and comparative example, graphene film provided by the invention can when ensureing that light transmission is 90%, and average sheet resistance is lower than 3k Ω/.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (9)
1. a preparation method for transparent graphene conductive film, is characterized in that, described method carries out reduction reaction for being contacted with reductant solution by graphene oxide film, obtains graphene film after clean process.
2. preparation method as claimed in claim 1, it is characterized in that, described reductant solution is the metal salt solution with reproducibility;
Preferably, metal ion in described metal salt solution is the combination of any a kind or at least 2 kinds had in the low price ion of multivalent state metal, the combination of any a kind or at least 2 kinds in the lower valency ion of preferred Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Cd, Sn, Pd, Bi, preferred Fe and/or Sn;
Preferably, the solvent of described metal salt solution is water-soluble solvent or solution, the mixture of any a kind or at least 2 kinds in preferred water, ethanol, isopropyl alcohol, ammoniacal liquor, sodium hydroxide solution, hydrochloric acid solution;
Preferably, the concentration of described metal salt solution is 0.01 ~ 1mol/L.
3. preparation method as claimed in claim 1 or 2, is characterized in that, the mode of described contact is spraying, spin coating, dipping, any a kind or at least 2 kinds dripped in painting combination; Preferably graphene oxide film is immersed in reductant solution, or reductant solution is spin-coated on graphene oxide film;
Preferably, during described contact, the amount of the metal ion of every square centimeter of graphene oxide film contact is 0.001 ~ 1mmol.
4. the preparation method as described in one of claims 1 to 3, is characterized in that, the temperature of described reduction reaction is 1 ~ 100 DEG C, preferably 25 ~ 60 DEG C;
Preferably, the time of described reduction reaction is 1min ~ 24h, preferably 5 ~ 60min.
5. the preparation method as described in one of Claims 1 to 4, is characterized in that, the C/O of described graphene oxide film is than being 1:2 ~ 5:1, preferably 2 ~ 3:1;
Preferably, the build of described graphene oxide film is 2 ~ 1000nm, preferably 5 ~ 50nm.
6. the preparation method as described in one of Claims 1 to 5, is characterized in that, described cleaning be treated to the graphene film after by reduction reaction carry out washing, dry;
Preferably, described washing is for rinsing or the reacted graphene film of soaking and reducing;
Preferably, the solution of described flushing or immersion is the combination of any a kind or at least 2 kinds in water, ethanol or diluted acid.
7. the preparation method as described in one of claim 1 ~ 6, is characterized in that, the preparation method of described graphene oxide film is:
Graphene oxide dispersion is coated on substrate and obtains graphene oxide film;
Preferably, the method for described coating is the combination of line rod film, spin coating, spraying, Best-Effort request, blade coating, intaglio plate, relief printing plate, any a kind or at least 2 kinds in printing;
Preferably, the decentralized medium of described graphene oxide dispersion is water.
8. preparation method as claimed in claim 7, it is characterized in that, the preparation method of described graphene oxide is selected from Hummers method, Brodie method, Staudenmaier method, graphite intercalation stripping, the ultrasonic stripping of graphite, graphite shear and peel off in any a kind or any 1 in deriving method.
9. the preparation method as described in one of claim 1 ~ 8, it is characterized in that, described method is that C/O is immersed in concentration than the graphene oxide film being 2.5 ~ 3.5:1 is in the reductant solution of 0.08 ~ 0.12mol/L, at 40 ~ 60 DEG C of temperature, carry out reduction reaction 8 ~ 12min time, after washing, drying, obtain graphene film.
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| CN108314027A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of hydroxyl/epoxy group of high conductivity modifies the preparation method of transparent graphene conductive film outside |
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| CN108314027A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of hydroxyl/epoxy group of high conductivity modifies the preparation method of transparent graphene conductive film outside |
| CN108314024A (en) * | 2018-04-24 | 2018-07-24 | 盐城师范学院 | A kind of plasma preparation method of transparent graphene conductive film |
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| CN108314024B (en) * | 2018-04-24 | 2020-09-01 | 盐城师范学院 | Plasma preparation method of graphene transparent conductive film |
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