CN103738943A - Large area transparent conductive graphene film preparation method - Google Patents
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- CN103738943A CN103738943A CN201310563992.4A CN201310563992A CN103738943A CN 103738943 A CN103738943 A CN 103738943A CN 201310563992 A CN201310563992 A CN 201310563992A CN 103738943 A CN103738943 A CN 103738943A
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Abstract
The present invention discloses a large area transparent conductive graphene film preparation method, and belongs to the technical field of carbon nanometer materials. The technical scheme of the present invention comprises: uniformly dispersing graphene oxide in an organic solvent, adding the solution to the surface of ultra pure water in a water tank in a dropwise manner, settling the graphene oxide on the substrate surface through a layer-by-layer settlement manner by controlling outflow of the water in the water tank and moving the substrate, and carrying out drying and reduction to prepare the single-layer or multi-layer large area graphene transparent conductive film. According to the present invention, the preparation method has characteristics of simpleness, green environmental protection, abundant raw materials and high raw material utilization rate, the purpose of application of graphene as the large area conductive transparent film can be achieved, and the prepared large area graphene film has characteristics of high electrical conductivity and high light transmittance, and can be widely used in the fields of OLED, solar batteries, organic memory devices and the like.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of preparation method of large-area transparent conductive graphene membrane, and be superimposed as the technology of preparing of single or multiple lift graphene film.
Background technology
Conductive film can be used as electrode or some semiconductor electrostatic materials, at aspects such as Organic Electricity luminescence display processed (OLED), solar cell, photodiode, photoelectric display and organic memory devices, is with a wide range of applications.Current, conventional electrode in semiconductor device is to utilize the rare earth metal indium and tin oxide film of traditional inorganic materials to prepare, as ITO, IZO etc., but day by day deficient along with rare metal, price is increasingly expensive, the reasons such as conductive electrode fragility deficiency, limit its large-scale application at photoelectric field, particularly aspect flexibility, large-area organic photoelectric functional material electrode device.Therefore, develop a kind of abundant raw materials, the conductive film that cheap, flexible and stability is high has economic benefit and strategic importance to the development of following semicon industry and photoelectric functional device.
At present, there is flexibility simultaneously mainly contain conductive polymers and carbon nanotube with the material of conducting function.Inorganic metal conductive film relatively, conventional conductive polymer materials electroconductibility is poor, and as PANI and PPy, and novel conductive polymer electroconductibility is higher, but price is very high, and as PEDOT and PSS, therefore, conductive polymers is unfavorable for producing in enormous quantities.Carbon nanotube has outstanding chemical property and excellent mechanical property, it is one of ideal material of preparing compliant conductive film, but in the purge process of carbon nanotube, productive rate is lower, separation difficulty and poor efficiency, make the preparation process complexity of film, cost is high and limited its large-area industrial application.
Graphene is as a kind of novel carbon two-dimensional nanostructure material, there is higher mobility, unique quantum hall effect, good conductivity and mechanical property, become study hotspot in recent years, the film of making based on Graphene becomes the desirable conductive film of a new generation.At present, the preparation method of graphene film restores method etc. after mainly containing heating SiC method, epitaxial growth method, chemical Vapor deposition process and oxidation filming.Wherein after graphene oxide film forming, reduction technique has made up graphene oxide film electroconductibility deficiency, and the conductivity of reduction rear film promotes, and has the extremely concern of enterprise and research and development institution of efficiency is high, output is large, cost is low feature.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of large-area transparent conductive graphene membrane, its preparation process comprises:
1. the preparation of graphene oxide (GO)
Using carbon material as raw material, adopt Hummers legal system for graphene oxide.
2. the preparation of graphene oxide film
(1) at one, be with in valvular tank, first close bottom land valve, substrate is put into tank, with the angle of inclination of sink surface be 0 ° ~ 90 °, then add the ultrapure water of cell body long-pending 3/4;
(2) graphene oxide is dispersed in the mixed solution of organic solvent/ultrapure water that volume ratio is 1:10 ~ 1:2, ultrasonic half an hour, drips on the surface of water in groove, then organic solvent volatilization for some time.Wherein, organic solvent is any one or the multiple mixture in methyl alcohol, ethanol, acetone, DMF, methylene dichloride, hexanol, tetrahydrofuran (THF), preferentially selects ethanol;
Etc. (3) after organic solution volatilization, control the outflow of trough inner water, pass through moving substrate, graphene oxide is just attached to substrate surface and forms graphene oxide film, by the slow substrate with graphene oxide out, be placed in the baking oven of 30-100 ℃ and dry, just prepare big area graphene oxide film.If need the graphene oxide film of preparation multilayer, then the graphene oxide film after drying is carried out to secondary or membrane repeatedly, obtain the graphene oxide film of multilayer.
Substrate described in step (1) is flexible base, board or non-flexible substrate.Flexible base, board is PET(polyethylene terephthalate), PEN(PEN), PC(polycarbonate), PES(polyethersulfone), PI(polyimide), FRP(composite material film) in any one; Non-flexible substrate be in silicon chip, sheet glass, quartz plate, sheet mica any one.
3. the preparation of conductive graphene membrane
By the graphene oxide film of the single or multiple lift obtaining, through high temperature inert gas reduction or reductive agent steam reduction, the graphene film of preparation high conductivity.Wherein, the reaction conditions of high temperature inert gas reduction is that temperature of reaction is 300 ~ 800 ℃, and the reaction times is 20 ~ 200 minutes; Reductive agent is any one or the multiple mixture in hydrazine hydrate, hydroiodic acid HI, phenylhydrazine, anthracene hydrazine, ethylene glycol, and the flow velocity of reductive agent steam is 5 ~ 30 mL/min, and temperature of reaction is 60 ~ 300 ℃, and the reaction times is 5 ~ 90 minutes.
The advantage of transparent conductive graphene membrane prepared by the present invention is:
(1) specific conductivity of graphene film is high;
(2) transmittance of graphene film is high;
(3) preparation method can meet the preparation of large area flexible graphene conductive film;
(4) prepare abundant raw materials and utilization ratio is high;
(5) preparation technology is simple, asepsis environment-protecting and easily realize scale operation;
(6) graphene film of preparing is at high-performance flexible transparent photoelectric device, and semiconductor electrostatic thin-film material field has potential using value.
Accompanying drawing explanation
Fig. 1 is the preparation flow figure of conductive graphene membrane.
Fig. 2 is that graphene oxide is attached to two kinds of mode figure on substrate.
Fig. 3 is the preparation flow figure of compliant conductive graphene film, wherein 1 is Graphene/aqueous dispersions (Modified GF based dispersion tank), 2 is deionization pond (DI-Water tank), 3 is deionized water water reservoir (DI-Water reservoir), 4 for forming graphene film device (M-GF/water LB film forming reservoir), 5 is deionized water recycle pump (DI-water circulation pump system), 6 is PET substrate (PET substrates), 7 is drying oven (Temperature/air flow controlled oven), 8 is large-area transparent conductive graphene membrane volume (Modified GF LB film coated roll).
Fig. 4 is the SEM figure of graphite oxide, graphene conductive film, and in figure, a ~ d is respectively the SEM figure of graphene oxide under different multiples, the fold that in figure, e, f are graphene oxide film and enlarged view.
Fig. 5 is transmittance and the electric conductivity figure of conductive graphene membrane.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be described in detail.
(1) preparation of GO
In beaker, add 2 g natural flake graphites and the dense H of 50 mL
2sO
4, under the condition of ice bath of 0 ℃, with magnetic stirring apparatus, stir 30min, add lentamente 3.54g KMnO
4, mixed solution stirs 2 h at 35 ℃ again after 0 ℃ of stirring 90 min.To reaction solution, add 40 mL deionized waters, after dripping, react half an hour after being warmed up to 90 ℃, add 140mL deionized water dilution mixed solution, when solution temperature is down to 60 ℃, add 15 mL H
2o
2, solution colour immediately becomes transparent faint yellow, washs transparent yellow solution 3 times with the HCl solution centrifugal of 1 M, then uses deionized water centrifuge washing 3 times, and be placed on freeze-drying in refrigerator, is finally placed on the dry graphene oxide that obtains in freeze drier.
(2) configuration of GO dispersion liquid
Sheet glass is placed on to the H that volume ratio is 3:1
2sO
4/ HNO
3in mixing solutions, ultrasonic half an hour at the temperature of 80 ℃, with deionized water, clean surface, dry, obtain clean substrate.Then take the GO solid of 0.08 g, put into beaker, add methyl alcohol/ultrapure water mixing solutions that 25 mL volume ratios are 5:1, ultrasonic 30 minutes, obtain GO dispersion liquid.
(3) preparation of GO film
The sheet glass cleaning up is lain in groove, add the ultrapure water of cell body long-pending 3/4, on trough inner water surface, slowly drip the GO dispersion liquid of (3s/dripping) 7.5 mL, after methyl alcohol volatilization, open bottom land valve, in control flume, water flows out, and is dispersed in the GO thin film deposition of water surface in glass sheet surface, form one deck GO film, then will adhere to the sheet glass of GO film, be placed in the baking oven of 80 ℃ dry 12 hours, obtain transparent GO film.If the GO film of preparation multilayer, then by the sheet glass that adheres to GO film after drying, carry out secondary or membrane repeatedly, obtain the GO film of multi-layer transparent.
(4) preparation of graphene conductive film
By the GO film obtaining in step 3, be placed in tube furnace, pass into pure N
2atmosphere, controls N
2flow velocity be 20 mL/min and react 30 min under 400 ℃ of condition, obtain graphene film.The SEM of conductive graphene membrane under different multiples schemes as shown in Figure 4, and as shown in Figure 5, the number of plies of known conductive graphene membrane is more for the transmittance of different number of plies conductive graphene membranes and electric conductivity, and its transmittance and electric conductivity are lower.
(1) preparation of GO
According to the method in embodiment 1, graphite is replaced with to carbon nanotube, prepare GO.
(2) configuration of GO dispersion liquid
According to the method in embodiment 1, methyl alcohol is replaced with to DMF, add DMF/ultrapure water that 15 mL volume ratios are 1:8, prepare GO dispersion liquid.
(3) preparation of large area flexible GO film
As shown in Figure 3, by the organic solution of filling it up with in 1 containing GO, 2 is the recycle system of ultrapure water, in tank 3, first place the PET substrate of having cleaned, add the ultrapure water of tank volume 3/4, valve-off, then open valve in groove 1 and drip lentamente (3 s/ drip) in 3 grooves on the surface of water by GO dispersion liquid, form film 4, treat N, after dinethylformamide volatilization, open ultrapure water recycle system bottom land valve 5, 6 flexible pet substrate volumes start slowly to roll, the GO film 4 that is dispersed in fluid surface is deposited on flexible pet sheet face, in flexible PET volume rolling process, tank 3 surfaces constantly supplement GO organic solution, then the flexible PET that adheres to GO film is placed in 60 ℃ of baking ovens 7 and is dried 10 hours, then at 8 places, collect the PET film that big area is adhered to GO film, obtain large area flexible graphene oxide film.
(4) preparation of compliant conductive graphene film
By the large area flexible graphene oxide film of preparation in step 3, be placed in tube furnace, the flow velocity of hydroiodic acid HI steam is 15 mL/min, reacts 30 minutes at 180 ℃, cooling, obtains large area flexible graphene film.
(1) preparation of GO
According to the method in embodiment 1, graphite is replaced with to graphene nanobelt, prepare GO.
(2) configuration of GO dispersion liquid
According to the method in embodiment 1, methyl alcohol is replaced with to tetrahydrofuran (THF), add tetrahydrofuran (THF)/ultrapure water that 9.5 mL volume ratios are 1:10, prepare GO dispersion liquid.
(3) preparation of large area flexible GO film
According to the method in embodiment 2, flexible pet substrate is replaced with to FRP(composite material film), prepare large area flexible GO film.
(4) preparation of soft graphite alkene conductive film
According to the method in embodiment 2, hydroiodic acid HI is replaced with to phenylhydrazine, the flow velocity of phenylhydrazine steam is 10 mL/min, prepares the transparent graphene conductive film of large area flexible.
Claims (9)
1. a preparation method for large-area transparent conductive graphene membrane, is characterized in that, concrete preparation process is:
(1), using carbon material as raw material, adopt Hummers legal system for graphene oxide;
(2) graphene oxide is dispersed in organic solvent, and by controlling outflow and the moving substrate of trough inner water, graphene oxide layer by layer deposition, on substrate surface, is prepared into the graphene oxide film of single or multiple lift, then dries at a certain temperature;
(3) by the graphene oxide film after drying, under high temperature inert gas or reductive agent steam condition, reduce, make big area graphene conductive film.
2. the preparation method of large-area transparent conductive graphene membrane according to claim 1, is characterized in that: the carbon material described in step (1) is graphite, band-SO
3any one or multiple mixture in the water-soluble graphene of base, the Graphene of porous, graphene nanobelt, graphene quantum dot, carbon nanotube.
3. the preparation method of large-area transparent conductive graphene membrane according to claim 1, is characterized in that: the detailed process of described step (2) is:
1. at one, be with in valvular tank, bottom land valve closes, puts into groove by substrate, in groove, adds ultrapure water, by being dispersed in graphene oxide in organic solvent, drips in groove on water surface;
2. graphene oxide, under the effect of organic solvent, is uniformly distributed on fluid surface, after organic solvent volatilization, and the outflow of ultrapure water in control flume, by moving substrate, graphene oxide is just attached to substrate surface and forms graphene oxide film;
3. by the graphene oxide film forming on substrate, be placed in the baking oven of 30 ~ 100 ℃ and dry, obtain the graphene oxide film of individual layer, if need the graphene oxide film of preparation multilayer, can again the graphene oxide film after drying be carried out to secondary or Multiple depositions again, obtain the graphene oxide conductive film of multilayer.
4. according to the preparation method of the large-area transparent conductive graphene membrane described in claim 1 or 3, it is characterized in that: described organic solvent is methyl alcohol, ethanol, acetone, N, any one in dinethylformamide, methylene dichloride, hexanol, tetrahydrofuran (THF) or multiple mixture, the volume ratio of organic solvent and ultrapure water is 1:10 ~ 1:2.
5. according to the preparation method of the large-area transparent conductive graphene membrane described in claim 1 or 3, it is characterized in that: described substrate is flexible base, board or non-flexible substrate, flexible base, board is PET(polyethylene terephthalate), PEN(PEN), PC(polycarbonate), PES(polyethersulfone), PI(polyimide), FRP(composite material film) in any one; Non-flexible substrate be in silicon chip, sheet glass, quartz plate, sheet mica any one, the placement location of substrate and the angle of inclination of sink surface are 0 ° ~ 90 °.
6. according to the preparation method of the large-area transparent conductive graphene membrane described in claim 1 or 3, it is characterized in that: the polarity difference of described organic solvent, the graphene film function difference to some extent of preparing at liquid phase surface deposition, also can mix by the organic solvent of multiple different performance, prepare the conductive graphene membrane of multifunction.
7. the preparation method of large-area transparent conductive graphene membrane according to claim 1, is characterized in that: the condition of the high temperature inert gas reduction described in step (3) is: temperature of reaction is at 300 ~ 800 ℃, and the reaction times is 20 ~ 200 minutes; Rare gas element be in nitrogen, helium, neon, argon gas, Krypton, xenon, radon gas any one.
8. the preparation method of large-area transparent conductive graphene membrane according to claim 1, it is characterized in that: the reductive agent described in step (3) is any species or the multiple mixing in hydrazine hydrate, hydroiodic acid HI, phenylhydrazine, anthracene hydrazine, ethylene glycol, the flow velocity of reductive agent steam is 5 ~ 30 mL/min, temperature of reaction is 60 ~ 300 ℃, and the reaction times is 5 ~ 90 minutes.
9. the preparation method of large-area transparent conductive graphene membrane according to claim 1, is characterized in that: described graphene film can be the conductive film of individual layer, bilayer and multilayer.
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Cited By (13)
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| CN104229783A (en) * | 2014-09-10 | 2014-12-24 | 浙江碳谷上希材料科技有限公司 | Preparation method of graphene film with high thermal conductivity |
| CN105217619A (en) * | 2015-10-23 | 2016-01-06 | 南京工业大学 | A kind of preparation method of graphene film |
| CN105600775A (en) * | 2015-11-05 | 2016-05-25 | 北京旭碳新材料科技有限公司 | Graphene film and method and device for continuous production of graphene film |
| WO2016162885A1 (en) * | 2015-04-09 | 2016-10-13 | Indian Institute Of Technology Bombay | Process for transferring graphene oxide monolayer sheets on substrates |
| CN106587016A (en) * | 2016-12-08 | 2017-04-26 | 南京信息职业技术学院 | Oxidized graphene humidity response actuator and preparation method thereof |
| CN107140631A (en) * | 2017-06-09 | 2017-09-08 | 哈尔滨工业大学 | A kind of preparation method of the super-hydrophobic graphene film of bionic intelligence |
| CN107337200A (en) * | 2017-08-03 | 2017-11-10 | 山东金城石墨烯科技有限公司 | A kind of preparation method of toughness thermal conductivity graphene film |
| CN107364844A (en) * | 2017-05-31 | 2017-11-21 | 广东工业大学 | A kind of steam reduction graphene oxide conductive polymer composite film and preparation method and application |
| CN107910129A (en) * | 2017-10-27 | 2018-04-13 | 上海理工大学 | A kind of preparation method of graphene/carbon nano-tube compound transparent electricity conductive film |
| CN108004649A (en) * | 2017-12-28 | 2018-05-08 | 赵文立 | A kind of graphene nanocomposite material and preparation method thereof |
| CN109133039A (en) * | 2017-06-27 | 2019-01-04 | 中国科学院宁波材料技术与工程研究所 | A kind of self assembly graphene nano film and its preparation method and application |
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| CN110127672A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method of redox graphene film |
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Cited By (16)
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| CN104229783A (en) * | 2014-09-10 | 2014-12-24 | 浙江碳谷上希材料科技有限公司 | Preparation method of graphene film with high thermal conductivity |
| CN104229783B (en) * | 2014-09-10 | 2016-04-13 | 浙江碳谷上希材料科技有限公司 | A kind of preparation method of high thermal conductivity graphene film |
| WO2016162885A1 (en) * | 2015-04-09 | 2016-10-13 | Indian Institute Of Technology Bombay | Process for transferring graphene oxide monolayer sheets on substrates |
| CN105217619A (en) * | 2015-10-23 | 2016-01-06 | 南京工业大学 | A kind of preparation method of graphene film |
| CN105600775A (en) * | 2015-11-05 | 2016-05-25 | 北京旭碳新材料科技有限公司 | Graphene film and method and device for continuous production of graphene film |
| CN106587016A (en) * | 2016-12-08 | 2017-04-26 | 南京信息职业技术学院 | Oxidized graphene humidity response actuator and preparation method thereof |
| CN107364844A (en) * | 2017-05-31 | 2017-11-21 | 广东工业大学 | A kind of steam reduction graphene oxide conductive polymer composite film and preparation method and application |
| CN107140631A (en) * | 2017-06-09 | 2017-09-08 | 哈尔滨工业大学 | A kind of preparation method of the super-hydrophobic graphene film of bionic intelligence |
| CN107140631B (en) * | 2017-06-09 | 2019-07-02 | 哈尔滨工业大学 | A kind of preparation method of the super-hydrophobic graphene film of bionic intelligence |
| CN109133039A (en) * | 2017-06-27 | 2019-01-04 | 中国科学院宁波材料技术与工程研究所 | A kind of self assembly graphene nano film and its preparation method and application |
| CN107337200A (en) * | 2017-08-03 | 2017-11-10 | 山东金城石墨烯科技有限公司 | A kind of preparation method of toughness thermal conductivity graphene film |
| CN107910129A (en) * | 2017-10-27 | 2018-04-13 | 上海理工大学 | A kind of preparation method of graphene/carbon nano-tube compound transparent electricity conductive film |
| CN108004649A (en) * | 2017-12-28 | 2018-05-08 | 赵文立 | A kind of graphene nanocomposite material and preparation method thereof |
| CN109449221A (en) * | 2018-12-28 | 2019-03-08 | 苏州腾晖光伏技术有限公司 | A kind of graphene crystal silicon solar battery and its manufacturing method |
| CN109449221B (en) * | 2018-12-28 | 2024-04-09 | 苏州腾晖光伏技术有限公司 | Graphene crystalline silicon solar cell and manufacturing method thereof |
| CN110127672A (en) * | 2019-06-10 | 2019-08-16 | 中国烟草总公司郑州烟草研究院 | A kind of preparation method of redox graphene film |
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Application publication date: 20140423 |