CN103632771A - Manufacturing process of graphene transparent conductive film - Google Patents
Manufacturing process of graphene transparent conductive film Download PDFInfo
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- CN103632771A CN103632771A CN201310647418.7A CN201310647418A CN103632771A CN 103632771 A CN103632771 A CN 103632771A CN 201310647418 A CN201310647418 A CN 201310647418A CN 103632771 A CN103632771 A CN 103632771A
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Abstract
The invention relates to a manufacturing process of a graphene transparent conductive film. The manufacturing method includes the steps of 1), uncoiling a copper foil in a vacuum chamber, heating a copper-clad chemical deposition reaction zone by using a resistor, feeding in methane gas and hydrogen, subjecting a copper-clad surface to chemical sedimentation to generate a graphene layer, and then adopting plasma to perform etching processing on the graphene layer; 2), adopting a gravure printing process to obtain an oxidize graphene layer; 3), obtaining an oxide graphene film; 4), coating a copper chloride etching solution which is 200g/L in concentration on a copper-clad face of the oxidize graphene film; 5), subjecting the oxidize graphene film to thermal annealing and reduction; 6), coating resin adhesive, sticking the film for packaging, and finally obtaining the patterned graphene transparent conductive film. The manufacturing process is short in film forming time, and low-cost and large-scale mass manufacturing can be realized; the graphene transparent conduction film is high in electric conductivity, good in flexibility, high in pattern definition, higher in acid and alkali resistance of the transparent conductive film and lower in cost.
Description
Technical field
The present invention relates to a kind of manufacture method of graphene conductive film, especially the manufacture craft of transparent graphene conductive film.
Background technology
Along with scientific and technical development, society is also more and more to the demand of new material.Material is the material base of human civilization progress and development in science and technology, and the renewal of material makes people's life that great variety also occur.At present, flourish novel transparent and the thin-film material of conduction are even all widely used in the field such as military project at liquid crystal display, touch-screen, smart window, solar cell, microelectronics, information sensor, and are being penetrated in other sciemtifec and technical sphere.Due to thin film technique and multiple technologies closely related, thereby the interest of the scientists that has excited every field to film preparation and performance thereof.
Conductive film is a kind of film that can conduct electricity, realize some specific electric functions, is widely used in the electronic devices such as display, touch-screen and solar cell.At present, as a kind of transparent and conductive semiconductor material oxidation indium tin (ITO), be widely used in film field always.By adopting magnetron sputtering evaporation ITO to prepare transparent conductive film on transparent base, transparent base comprises as glass and PETG (PET) film etc.Because tin indium oxide has high conductivity, high pass light rate, so become one of main material of preparing by conductive film.But tin indium oxide conductive film in use also exists some shortcomings, comprising: (1) indium resource is less, causes price continuous rise, make ITO become day by day expensive material, as spraying, pulsed laser deposition, plating etc.And indium oxide has certain toxicity, recycle the unreasonable environmental pollution that easily causes.(2) character that ITO is crisp makes it can not meet the performance requirement of some new application (for example flexible flexible display, touch-screen, organic solar batteries), is not suitable for the production of flexible electronic device of future generation.The two dimensional crystal structure of Graphene uniqueness, has given the performance of its uniqueness, and research finds, Graphene has good mechanical performance and excellent electrical properties, and under normal temperature, the electron mobility of Graphene can reach 15000cm
2v
-1s
-1, and resistivity is only 10
-6Ω cm.Graphene has how potential advantage than tin indium oxide in many aspects, such as quality, robustness, pliability, chemical stability, infrared light transmission and price etc.Therefore Graphene is expected to replace tin indium oxide very much, is used for that development is thinner, conduction speed flexible electronic device faster.
The practical application of patterning techniques in large area electron device and flexible circuit must be indispensable.Tradition design technology preparation process is complicated, and the definition of pattern is poor.Printed electronics is a kind of novel pattern electronic manufacturing technology, and by e-inks is transferred on different substrates and can prepares large-sized electronic device, this preparation method's maximum feature is large area, flexibility and low cost.But, the long a kind of development that hampers this technology of the inhomogeneities of ink and film formation time.
Intaglio printing is a kind of ink contained in intaglio plate pit to be imprinted directly into the technology of preparing on stock.Because it possesses the advantages such as the high and printing quality of output is good, now become a kind of effective process means of preparing flexible pattern electronic device.It is high that intaglio printing requires ink to have concentration, the feature such as be uniformly dispersed and viscosity is little, Graphene is a kind of high hydrophobicity material, in solution, solubility is low, easy coagulation, in order to access, concentration is high, the Graphene ink of stable dispersion, and a lot of research groups join surface dispersant in graphene solution.But, surface dispersant add the conductivity that membership directly has influence on Graphene, thereby cause the conductance of the conductive film prepared greatly to decline, and graphene oxide is a kind of hydroaropic substance, in the aqueous solution, solubility is more much larger than Graphene.
At present, the preparation method of Graphene mainly contains: micromechanics stripping method, oxidation-reduction method, chemical vapour deposition technique, organic molecule graft process etc.From 2006, by employing chemical vapour deposition techniques such as Somani, the camphanone (camphor) of take was presoma, obtains graphene film on nickel foil, and scientists has obtained and much in different matrix, obtained the progress of the controlled graphene sheet layer of thickness.By carry out chemical etching on metallic matrix, graphene sheet layer is separated and is transferred on another matrix, and this obtains high-quality graphene sheet layer with regard to having removed complicated machinery or chemical treatment method from.The states such as Korea S and Japan adopt one after another and have prepared in this way big size graphene transparent conductive film, and the main application fields of expectation is in flat-panel screens, serves as anode.The for example exploitation in new organic light emitting display (OLED), OLED has the features such as cost is low, all solid state, active illuminating, brightness is high, contrast is high, visual angle is wide, fast response time, thin thickness, low-voltage direct-current driving, low in energy consumption, operating temperature range is wide, can realize that soft screen display is shown, becomes the developing direction of following display technology.
Summary of the invention
For overcoming the deficiency in prior art, the manufacture craft that the object of this invention is to provide a kind of black alkene transparent conductive film, this preparation method's film formation time is short, can realize low cost, batch production on a large scale, and the conductance of the graphene conductive film of preparing is high, pliability good, clear patterns degree is high, improve the resistance to acids and bases of transparent conductive film, and reduce costs.
Object of the present invention is achieved through the following technical solutions:
A preparation method for patterned Graphene conductive film, is characterized in that, described graphene conductive film comprises that graphene layer and film are as base material, the thickness of described film is 150 ~ 200 μ m, be less than ± 2 μ m of thickness deviation, light transmittance is greater than 93%, and mist degree is less than 1%; Described film surface also has hardened layer more than one deck hardness 3H;
Its method step comprises:
(1) in vacuum chamber, Copper Foil is wound off to volume, make to be heated by resistive the chemical deposition reaction zone of Copper Foil, pass into methane gas and hydrogen, the throughput ratio of described methane gas and hydrogen is 12:1, under catalytic condition, copper foil surface chemical deposition generates graphene layer, then graphene layer is cleaned, dried up, with plasma, graphene layer is processed, the throughput while graphene layer being carried out to etching processing with plasma is 5-200sccm, and power is 5-120W, etch period is rolling after 5-600s, and vacuum chamber carries out exhaust simultaneously; The pressure of described vacuum chamber is 1000 ~ 1500Pa;
800 ~ 850 ℃ of the heating-up temperatures of the chemical deposition reaction zone of described Copper Foil, by resistance heating Copper Foil, control current strength 800A;
(2) adopt gravure printing technique, the concentration that Hummers method is made is on 13mg/mL graphene oxide ink printing graphene layer, places it in baking oven and is dried, and obtains graphene oxide layer;
(3) in step (1) film decoiling, with woodburytype at film surface coated with resins adhesive, then the uncoiling of graphene oxide layer, graphene oxide aspect is fitted on the film substrate that is coated with resin binder, finally by crossing ultraviolet ray irradiation graphene oxide film, resin bed is solidified, by graphene oxide film rolling;
(4) graphene oxide film uncoiling, at the copper-clad surface of graphene oxide film, applying concentration is 200g/L copper chloride etching solution, and water rinses removes Copper Foil, dry after by graphene oxide film rolling;
(5) graphene oxide film is carried out to thermal annealing reduction, the step of described thermal annealing reduction is graphene oxide film to be placed in to vacuum inert environments, annealing in process 2-10 hour at 600-610 ℃ of temperature;
(6), after reduction is processed, coated with resins adhesive, pastes thin-film package, finally makes patterned Graphene transparent conductive film, finished product rolling;
Further, the plasma in described step (1) is oxygen plasma, argon plasma or nitrogen plasma.
Further, in described step (2), baking temperature is 110 ℃, and be 5 minutes drying time.
Further, in described step (1), the thickness of described Copper Foil is 20 ~ 50 μ m, and purity reaches more than 99.9%.
Further, the rolling speed in described step (1)-(3) is 0.01 ~ 0.1m/min.
Further, described film is PETG (PET), Merlon (PC) or polymethyl methacrylate (PMMA).
Further, described resin binder is photo-curing epoxy resin, and its light transmittance is greater than 95%, and mist degree is less than 1%, and UV resistant irradiates, free of birefringence, and coating thickness scope is 5 ~ 10 μ m.
Further, described photo-curing epoxy resin is transparent bisphenol-A type epoxy resin or aliphatic epoxy resin, and contains aromatic sulfonium salts or salt compounded of iodine initator.
Compared with prior art, beneficial effect of the present invention is:
(1) the inventive method is bonded together Graphene and the transparent substrates of transiting metal surface growth by binding agent, by mechanical external force, transition metal is separated with Graphene, Graphene after separation is transferred to transparent substrates surface, transparent graphene conductive film prepared by the method, size is large, conductivity is high, visible light transmittance rate is high, surface no-pollution; And pliability is good, conductance is high, and pattern is very clear.
(2) mode that the present invention adopts graphene oxide ink to combine with intaglio printing technology is prepared patterned Graphene conductive film, so this preparation method's film formation time is short, productive rate is high, can realize large-scale batch production.
(3) this preparation method's the cost of raw material is low and be easy to get, and preparation technology is simple.
(4) method of this employing high temperature reduction or electronation is prepared transparent graphene conductive film, there is light penetrability good, conductivity is good, prepare area large, preparation method is simple, the advantage that cost is low, is expected to replace traditional inorganic oxide electrode material ITO, for the development of transparent conductive film and association area provides immensity.
Embodiment
For technological means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
The preparation method of a kind of patterned Graphene conductive film of this enforcement, described graphene conductive film comprises that graphene layer and film are as base material, the thickness of described Copper Foil is 20 ~ 50 μ m, purity reaches more than 99.9%, and described film is PETG (PET), Merlon (PC) or polymethyl methacrylate (PMMA); Its thickness is 150 ~ 200 μ m, be less than ± 2 μ m of thickness deviation, and light transmittance is greater than 93%, and mist degree is less than 1%; The employing of the present embodiment Copper Foil be that thickness is 30 μ m, purity reaches 99.99%, the thickness of film is 180 μ m, be less than ± 1 μ m of thickness deviation, light transmittance 96% also has hardened layer more than one deck hardness 3H on described film surface; Its method step comprises:
(1) in vacuum chamber, Copper Foil is wound off to volume, make to be heated by resistive the chemical deposition reaction zone of Copper Foil, pass into methane gas and hydrogen, the throughput ratio of described methane gas and hydrogen is 12:1, under catalytic condition, copper foil surface chemical deposition generates graphene layer, then graphene layer is cleaned, dried up, with plasma, graphene layer is processed, the throughput while graphene layer being carried out to etching processing with plasma is 5-200sccm, and power is 5-120W, after etch period is 5-600s, then carry out rolling with 0.01 ~ 0.1m/min speed.Vacuum chamber carries out exhaust simultaneously; The pressure of described vacuum chamber is 1000 ~ 1500Pa; Wherein, the plasma in step (1) is oxygen plasma, argon plasma or nitrogen plasma.
800 ~ 850 ℃ of the heating-up temperatures of the chemical deposition reaction zone of described Copper Foil, by resistance heating Copper Foil, control current strength 800A;
(2) adopt gravure printing technique, the concentration that Hummers method is made is on 13mg/mL graphene oxide ink printing graphene layer, places it in baking oven and is dried, and baking temperature is 110 ℃, and be 5 minutes drying time, obtains graphene oxide layer;
(3) in step (1) film decoiling, with woodburytype at film surface coated with resins adhesive, then the uncoiling of graphene oxide layer, graphene oxide aspect is fitted on the film substrate that is coated with resin binder, finally by crossing ultraviolet ray irradiation graphene oxide film, resin bed is solidified, by graphene oxide film rolling, rolling speed is 0.01 ~ 0.1m/min; Resin binder is photo-curing epoxy resin, and its light transmittance is greater than 95%, and mist degree is less than 1%, and UV resistant irradiates, free of birefringence, and coating thickness scope is 5 ~ 10 μ m.
Further, described photo-curing epoxy resin is transparent bisphenol-A type epoxy resin or aliphatic epoxy resin, and contains aromatic sulfonium salts or salt compounded of iodine initator.
(4) graphene oxide film uncoiling, at the copper-clad surface of graphene oxide film, applying concentration is 200g/L copper chloride etching solution, and water rinses removes Copper Foil, dry after by graphene oxide film rolling;
(5) graphene oxide film is carried out to thermal annealing reduction, the step of described thermal annealing reduction is graphene oxide film to be placed in to vacuum inert environments, annealing in process 2-10 hour at 600-610 ℃ of temperature;
(6), after reduction is processed, coated with resins adhesive, pastes thin-film package, finally makes patterned Graphene transparent conductive film, finished product rolling; Resin binder is photo-curing epoxy resin, and its light transmittance is greater than 95%, and mist degree is less than 1%, and UV resistant irradiates, free of birefringence, and coating thickness scope is 5 ~ 10 μ m.
By above-mentioned character express, can find out, adopt after the present invention, by binding agent, Graphene and the transparent substrates of transiting metal surface growth are bonded together, by mechanical external force, transition metal is separated with Graphene, Graphene after separation is transferred to transparent substrates surface, transparent graphene conductive film prepared by the method, size is large, conductivity is high, visible light transmittance rate is high, surface no-pollution; And pliability is good, conductance is high, and pattern is very clear.
In addition, the mode that adopts graphene oxide ink to combine with intaglio printing technology is prepared patterned Graphene conductive film, so this preparation method's film formation time is short, productive rate is high, can realize large-scale batch production; And the cost of raw material is low and be easy to get, preparation technology is simple.
And, the employing high temperature reduction of the present embodiment or the method for electronation are prepared transparent graphene conductive film, there is light penetrability good, conductivity is good, prepare area large, preparation method is simple, the advantage that cost is low, be expected to replace traditional inorganic oxide electrode material ITO, for the development of transparent conductive film and association area provides immensity.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (7)
1. the manufacture craft of transparent graphene conductive film, is characterized in that, described graphene conductive film comprises that graphene layer and film are as base material, the thickness of described film is 150 ~ 200 μ m, be less than ± 2 μ m of thickness deviation, light transmittance is greater than 93%, and mist degree is less than 1%; Described film surface also has hardened layer more than one deck hardness 3H;
Its method step comprises:
(1) in vacuum chamber, Copper Foil is wound off to volume, make to be heated by resistive the chemical deposition reaction zone of Copper Foil, pass into methane gas and hydrogen, the throughput ratio of described methane gas and hydrogen is 12:1, under catalytic condition, copper foil surface chemical deposition generates graphene layer, then graphene layer is cleaned, dried up, with plasma, graphene layer is processed, the throughput while graphene layer being carried out to etching processing with plasma is 5-200sccm, and power is 5-120W, etch period is rolling after 5-600s, and vacuum chamber carries out exhaust simultaneously; The pressure of described vacuum chamber is 1000 ~ 1500Pa;
800 ~ 850 ℃ of the heating-up temperatures of the chemical deposition reaction zone of described Copper Foil, by resistance heating Copper Foil, control current strength 800A;
(2) adopt gravure printing technique, the concentration that Hummers method is made is on 13mg/mL graphene oxide ink printing graphene layer, places it in baking oven and is dried, and obtains graphene oxide layer;
(3) in step (1) film decoiling, with woodburytype at film surface coated with resins adhesive, then the uncoiling of graphene oxide layer, graphene oxide aspect is fitted on the film substrate that is coated with resin binder, finally by crossing ultraviolet ray irradiation graphene oxide film, resin bed is solidified, by graphene oxide film rolling;
(4) graphene oxide film uncoiling, at the copper-clad surface of graphene oxide film, applying concentration is 200g/L copper chloride etching solution, and water rinses removes Copper Foil, dry after by graphene oxide film rolling;
(5) graphene oxide film is carried out to thermal annealing reduction, the step of described thermal annealing reduction is graphene oxide film to be placed in to vacuum inert environments, annealing in process 2-10 hour at 600-610 ℃ of temperature;
(6), after reduction is processed, coated with resins adhesive, pastes thin-film package, finally makes patterned Graphene transparent conductive film, finished product rolling;
Manufacture craft according to the transparent graphene conductive film described in claim 1, is characterized in that: the plasma in described step (1) is oxygen plasma, argon plasma or nitrogen plasma.
2. according to the manufacture craft of the transparent graphene conductive film described in claim 1, it is characterized in that: in described step (2), baking temperature is 110 ℃, and be 5 minutes drying time.
3. according to the manufacture craft of the transparent graphene conductive film described in claim 1, it is characterized in that: in described step (1), the thickness of described Copper Foil is 20 ~ 50 μ m, and purity reaches more than 99.9%.
4. according to the manufacture craft of the transparent graphene conductive film described in claim 1, it is characterized in that: the rolling speed in described step (1)-(3) is 0.01 ~ 0.1m/min.
5. according to the manufacture craft of transparent graphene conductive film described in claim 1, it is characterized in that: described film is PETG (PET), Merlon (PC) or polymethyl methacrylate (PMMA).
6. according to the manufacture craft of the transparent graphene conductive film described in claim 1, it is characterized in that: described resin binder is photo-curing epoxy resin, and its light transmittance is greater than 95%, mist degree is less than 1%, UV resistant irradiates, free of birefringence, and coating thickness scope is 5 ~ 10 μ m.
7. according to the manufacture craft of the transparent graphene conductive film described in claim 6, it is characterized in that: described photo-curing epoxy resin is transparent bisphenol-A type epoxy resin or aliphatic epoxy resin, and contain aromatic sulfonium salts or salt compounded of iodine initator.
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| CN105152165A (en) * | 2015-09-01 | 2015-12-16 | 复旦大学 | Method of directly synthesizing large-area graphene oxide based on plasma-enhanced chemical vapor deposition |
| WO2016011987A1 (en) * | 2014-07-21 | 2016-01-28 | 中国科学院深圳先进技术研究院 | Graphene thin film and preparation method therefor |
| CN107634328A (en) * | 2017-09-01 | 2018-01-26 | 中国科学院重庆绿色智能技术研究院 | A kind of graphene transparent antenna and preparation method thereof |
| CN109817828A (en) * | 2019-01-25 | 2019-05-28 | 重庆石墨烯研究院有限公司 | A kind of graphene transparent electrode and its work function regulate and control method |
| CN110078057A (en) * | 2019-04-02 | 2019-08-02 | 华东师范大学 | A kind of the redox graphene and preparation method of low-resistivity |
| CN113260241A (en) * | 2021-04-13 | 2021-08-13 | 浙江大学 | High-temperature-resistant high-conductivity graphene material and preparation method thereof |
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Application publication date: 20140312 |