CN103236324A - Method for preparing reduced graphene oxide-based flexible transparent conductive thin film - Google Patents
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Abstract
The invention relates to a method for preparing a reduced graphene oxide-based flexible transparent conductive thin film. A rod-coating film preparation method can be used for reducing a graphene oxide thin film in a solution processing way by means of a hydroiodic acid under the condition of less than or equal to 100 DEG C, so that a technology for the large-area preparation of the reduced graphene oxide-based flexible transparent conductive thin film is implemented. The prepared flexible transparent conductive thin film can be widely applied to the field of photoelectric display, and has the advantages of high electrical conductivity, high transmittance, high mechanical performance, large-area preparation performance (18*20cm<2>), richness and high utilization rate of raw materials, simplicity and environment friendliness of a preparation process, and the like. According to the flexible transparent conductive thin film obtained by the technology, the shortcoming of qualitative fragile of the conventional indium tin oxide (ITO) can be better overcome; and the flexible transparent conductive thin film is expected to be widely applied to the field of photoelectric functional devices such as an organic electroluminescent display and an organic solar cell as a flexible transparent electrode.
Description
Technical field
The invention belongs to field of nanometer photoelectronic material technology.Specifically refer to a kind ofly can pass through solution processing and utilization bar type coating film-forming method, by hydroiodic acid redox graphene film under smaller or equal to 100 degrees centigrade condition, thereby realize the technology of large-area preparation redox graphene transparent conductive film, this flexible transparent conductive film is at the high-performance transparent conductive film, particularly in the flexible optoelectronic preparation of devices, has potential actual application value.
Background technology
Flexible transparent conductive film has obtained research widely and has used in a lot of fields, and it is mainly used in plastic electronic fields such as flexible touch screen demonstration, flexible transistor, flexible memory, flexible light-emitting diode and flexible solar battery.Current, the most frequently used electrode material has metal oxide (ITO), conducting polymer (PEDOT:PSS) and nano material (carbon nanomaterial and metal nanometer line) etc.Traditional metal oxide is because its natural quality belongs to the pottery material, it is faced with that matter is crisp, resource scarcity, problem that the industrialization cost is high, the conducting polymer that rose in nearly 20 years, has certain mechanical ductility, from having solved the drawback of metal oxide in essence, but very important is the influence that conducting polymer is vulnerable to environment, thereby cause this device to the unsteadiness of environment, in addition, self has color conducting polymer, can present at color to bring interference (presenting blueness as the PEDOT:PSS film).
Now, nano material has been stepped into the field that flexible electronic shows with its unique electricity, optics, mechanical performance, becomes the substitution material that has potential application most.Metal nanometer line, because can't overcome sensitiveness to environment, so, limited its extensive use on large tracts of land film processed; Although carbon nano-tube has good pliability, high conductivity and to the stability of environment, its preparation and purification technique be complexity comparatively, has improved production cost greatly, is not suitable for the extensive use on the large tracts of land film processed equally.Recently, above-mentioned every problem has been alleviated in the appearance of Graphene.Graphene has excellent mechanical ductility, high conductivity (about 10
5S/m), high carrier mobility (2 * 10
5Cm
2V
-1S
-1), many-sided advantage such as strong antiacid corrosivity and abundant raw materials, attracted people's attentiveness, make it obtain broad research, it is expected to become the desirable conductive film of a new generation, especially has huge exploitation and application potential in the flexible optoelectronic devices field.
At present, the manufacture method of Graphene is a lot, mainly contains method such as reduce behind mechanical stripping method, chemical vapour deposition technique, epitaxial growth method, carbon nano-tube patterning method and the oxidation filming.The wherein the most suitable solution processing of the method for oxidation filming reduction has advantages such as low cost, high efficiency, large-scale production, is widely used in the industry research and development and changes into product with industry.Now, being used for the method for redox graphene mainly contains high annealing (more than 1000 ℃), hydrothermal reduction (at least 200 ℃), hydrazine reduction, sodium borohydride reduction etc.The two kinds of method of reducing in front are not suitable for plastic (anti-150 ℃ usually); But classical hydrazine hydrate reduction has significant limitation, and not only being embodied in hydrazine has severe toxicity, and can show obvious defects by the graphene oxide after the hydrazine reduction, greatly reduces the efficiency of transmission of electronics.Sodium borohydride also is so, unavoidably causes huge defective.So, select the suitable original reagent of going back, under prerequisite cheaply, research and development flexible and transparent redox graphene conductive film is a problem demanding prompt solution.
Summary of the invention
Technical problem:The objective of the invention is to propose a kind of by solution processing and utilization bar type coating film-forming method, reduction under smaller or equal to 100 degrees centigrade condition prepares the method for redox graphene conductive film based on graphene oxide film by hydroiodic acid.The film of this method preparation has that pliability is good, light transmission is high, excellent conductivity, large-area preparation, preparation technology is simple, cost is low and be beneficial to advantage such as suitability for industrialized production.This flexible transparent conductive film has potential actual application value in high-performance flexible transparent photoelectric function element field.
Technical scheme:The present invention prepares graphene oxide film at the PET substrate a kind of comprising by solution (bar type coating) technology of processing by solution processing film processed and the method that prepare the redox graphene conductive film under the reducing condition of gentleness, passes through the preparation process smaller or equal to 100 degrees centigrade reducing condition redox graphene film then;
The preparation method of the flexible transparent conductive film based on redox graphene of the present invention utilizes the bar type coating technology to prepare graphene oxide film, utilizes the hydroiodic acid reduction to obtain the redox graphene film then, and its concrete preparation process is as follows:
Step 1: by plasma treatment polyethylene terephtalate substrate, make it be with hydrophilic radical;
Step 2: by the graphene oxide film of bar type coating technology in the dispersion of hydrophilic PET substrate preparation water;
Step 3: under smaller or equal to 100 degrees centigrade condition, the graphite oxide film that obtains is dipped in the hydroiodic acid solution reduces the graphene oxide conductive film that obtains reducing;
Step 4: with the surface of alcohol flushing, soaking and reducing graphene oxide film, remove residual hydroiodic acid, improve the light transmittance of film, finally obtain the redox graphene film of high light transmittance, high conductivity.
Described graphene oxide is greater than 1000 μ m
2Graphene oxide, its dispersant is water; The used substrate of film of preparation graphene oxide is hydrophilic PET substrate, wherein the method for hydrophilic treated is to utilize plasma to make PET be with hydrophilic group, the condition of plasma is power 200 W, its volume of mixing atmosphere of oxygen atmosphere or oxygen and argon gas is respectively 70% and 20%, and the processing time is 90-180 s.
The described bar type coating technology of utilizing prepares in the graphene oxide film, and the graphene oxide area equates with the area of PET substrate.
The number of plies of the concentration of the thickness of the graphene oxide film of preparation by regulator solution, coating, the dragging speed of changing different-diameter coating rod and adjusting the coating rod are controlled effectively.
The preparation method of described graphene oxide film is the graphene oxide film that obtains homogeneous with oven for drying, and its temperature range is 50-120 ℃.
The reduction of graphene oxide film is to realize under smaller or equal to 100 degrees centigrade condition, is to reduce in the 55% hydroiodic acid solution by graphene oxide film being immersed in mass fraction namely, and reduction temperature is no more than 100 ℃, and the recovery time is the shortest to be 30s.
Described method of removing hydroiodic acid residual on the film be the redox graphene film will through ethanol greater than 5 times flushing, immersion, in order to improve the light transmittance of film.
Beneficial effect:Among the present invention by on the PET substrate by bar type coating technology preparation, smaller or equal to the flexible and transparent redox graphene conductive film of 100 degrees centigrade conditions reduction, its area is 18 * 20 cm
2, be that film side resistance under 90.5% and 61.8% the condition is respectively 17.2 and 1.53 k Ω/sq at printing opacity under the 550 nm wavelength, be the optimal value of preparation redox graphene under the equal conditions.In addition, the raw material of this big conductive film are natural graphite, and its aboundresources, cost are low; Simple, the environmental protection of the preparation technology of this film simultaneously and utilance height.So this flexible transparent conductive film has potential actual application value in high-performance flexible transparent photoelectric function element field.
Major advantage of the present invention is:
1. conductivity height;
2. light transmission is good;
3. mechanical performance is excellent;
4. large-area preparation;
5. reducing condition gentleness;
6. abundant raw material and utilance height;
7. the simple and environmental protection of preparation technology.
Description of drawings
Fig. 1. the x-ray photoelectron energy spectrogram of graphene oxide;
Fig. 2. the x-ray photoelectron energy spectrogram of redox graphene;
Fig. 3. be 1000-1200 μ m based on area
2The light transmittance of flexible and transparent redox graphene conductive film of the graphite oxide preparation relation between hindering with the side;
Fig. 4. be 100-200 μ m based on area
2The light transmittance of flexible and transparent redox graphene conductive film of the graphite oxide preparation relation between hindering with the side;
Fig. 5. be 10-20 μ m based on area
2The light transmittance of flexible and transparent redox graphene conductive film of the graphite oxide preparation relation between hindering with the side.
Embodiment
The preparation method of flexible and transparent redox graphene conductive film of the present invention comprises by solution processing (bar type coating) technology and prepares graphene oxide film at the PET substrate, then by obtain the technology of redox graphene flexible transparent conductive film smaller or equal to 100 degrees centigrade reducing condition.
(area is 1000-1200 μ m to the graphene oxide that the present invention uses as the graphene oxide of sheet
2), its dispersant is water; The used substrate of film of preparation graphene oxide is hydrophilic PET substrate, and wherein hydrophilic processing method is to be respectively 70% and 20% by plasma at its volume of mixing atmosphere of oxygen atmosphere or oxygen and argon gas, and the processing time is 90-180 s.
Graphene oxide film prepares by the bar type coating technology; The graphene oxide area equates with the area of PET substrate, and the concentration that the thickness of graphene oxide film can be by regulator solution, the number of plies of coating, the dragging speed of changing different-diameter (thickness) coating rod and adjusting the coating rod are controlled effectively.
The method that obtains the graphene oxide film of homogeneous is to use oven for drying, and its temperature range is 50-120 ℃.
The reduction of graphene oxide film is to realize in the 55% hydroiodic acid solution by being immersed in mass fraction, and this reduction temperature is no more than 100 ℃, and the recovery time is the shortest to be 30 s.
The method of removing hydroiodic acid residual on the film effectively be the redox graphene film will through ethanol greater than 5 times flushing, immersion, in order to improve the light transmittance of film.
In order to understand the content of patent of the present invention better, be described further below by instantiation.But these examples do not limit the present invention, and those skilled in the art make some nonessential improvement and adjust according to the foregoing invention content and all belong to protection scope of the present invention.
Concrete experimental procedure is as follows:
1) hydrophilic treated of PET substrate surface;
2) the bar type coating process prepares graphene oxide film;
3) hydroiodic acid redox graphene film;
4) further optimize the light transmission of flexible and transparent redox graphene conductive film with ethanol.
Example: the preparation method of flexible and transparent redox graphene conductive film.
The preparation of graphene oxide film and reduction: at first, the suspension liquid of aqueous phase (3 mg/mL) of large stretch of graphene oxide obtains the solution of stably dispersing by ultrasonic 20 min of brute force concussion ultrasonic machine.For the influence of size in conductivity of outstanding graphene oxide size, prepared the graphite oxide aqueous solution of different size respectively: this solution is divided into three parts, and (the graphene oxide area is 1000-1200 μ m to keep a copy of it
2), get two parts of remaining solution and use ultrasonic 10 min of probe ultrasonic machine and 20 min respectively, (the ultrasonic 10 min graphene oxide areas of probe are 100-200 μ m to be intended to obtain the solution of different size graphene oxide
2The ultrasonic 20 min graphene oxide areas of probe are 10-20 μ m
2).Secondly, by plasma oxygen be 70% and argon gas be to handle the PET substrate under 20% the condition, the processing time is 90 s, the power of selecting for use is 200 W.Again, use bar type coating masking technique, at the film of hydrophilic PET substrate preparation graphene oxide, after obtaining moistening graphene oxide film and in 80 ℃ baking oven, curing 3 min, obtain the film of solid graphene oxide.At last, it is 55% hydroiodic acid solution reduction, 30 s that this film is placed 100 ℃ mass fraction, obtains the redox graphene conductive film.
The optimization of flexible and transparent redox graphene conductive film: because after the hydroiodic acid processing, a large amount of hydroiodic acids is still adsorbed on the surface of film, have a strong impact on the light transmission of film, so will use alcohol flushing (greater than 5 times), the most hydroiodic acid of flush away this moment; And then the film that obtains is immersed in the ethanol bath, remove hydroiodic acid residual in the film as much as possible, to improve the light transmission of film.
Claims (7)
1. preparation method based on the flexible transparent conductive film of redox graphene, it is characterized in that this method utilizes the bar type coating technology to prepare graphene oxide film in plastic, utilize the hydroiodic acid reduction to obtain the redox graphene conductive film then, its concrete preparation process is as follows:
Step 1: by plasma treatment polyethylene terephtalate substrate, make it be with hydrophilic radical;
Step 2: by the graphene oxide film of bar type coating technology in the dispersion of hydrophilic PET substrate preparation water;
Step 3: under smaller or equal to 100 degrees centigrade condition, the graphite oxide film that obtains is dipped in the hydroiodic acid solution reduces, obtain the redox graphene conductive film;
Step 4: with the surface of alcohol flushing, soaking and reducing graphene oxide film, remove residual hydroiodic acid, improve the light transmittance of film, finally obtain the redox graphene film of high light transmittance, high conductivity.
2. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 1 is characterized in that described graphene oxide is for greater than 1000 μ m
2Graphene oxide, its dispersant is water; The used substrate of film of preparation graphene oxide is hydrophilic PET substrate, wherein the method for hydrophilic treated is to utilize plasma to make PET be with hydrophilic group, the condition of plasma is power 200 W, its volume of mixing atmosphere of oxygen atmosphere or oxygen and argon gas is respectively 70% and 20%, and the processing time is 90-180 s.
3. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 1 is characterized in that the described bar type coating technology of utilizing prepares in the graphene oxide film, and the graphene oxide area equates with the area of PET substrate.
4. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 3 is characterized in that the number of plies of the concentration of the thickness of the graphene oxide film for preparing by regulator solution, coating, the dragging speed of changing different-diameter coating rod and adjusting the coating rod control effectively.
5. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 1, the preparation method who it is characterized in that described graphene oxide film, be the graphene oxide film that obtains homogeneous with oven for drying, its temperature range is 50-120 ℃.
6. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 1, the reduction that it is characterized in that graphene oxide film is to realize under smaller or equal to 100 degrees centigrade condition, be to reduce in the 55% hydroiodic acid solution by graphene oxide film being immersed in mass fraction namely, reduction temperature is no more than 100 ℃, and the recovery time is the shortest to be 30s.
7. the preparation method of the flexible transparent conductive film based on redox graphene according to claim 1, it is characterized in that described method of removing hydroiodic acid residual on the film be the redox graphene film will through ethanol greater than 5 times flushing, immersion, in order to improve the light transmittance of film.
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| CN103545121A (en) * | 2013-10-23 | 2014-01-29 | 南京大学 | Supercapacitor electrode material preparation method based on three-dimensional graphene |
| CN103545053A (en) * | 2013-10-25 | 2014-01-29 | 深圳市华星光电技术有限公司 | Preparation method of transparent conducting thin film and preparation method of CF substrate with conducting thin film |
| CN104030275A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Preparation method of reduction graphene oxide heat-conducting film |
| CN104319012A (en) * | 2014-10-17 | 2015-01-28 | 南京皓轩新材料科技有限公司 | Preparation method of flexible electrode based on graphene |
| CN105000552A (en) * | 2015-07-24 | 2015-10-28 | 浙江大学 | Preparation method for graphene oxide |
| CN105225766A (en) * | 2015-07-30 | 2016-01-06 | 国家纳米科学中心 | A kind of preparation method of transparent graphene conductive film |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
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| CN103545121A (en) * | 2013-10-23 | 2014-01-29 | 南京大学 | Supercapacitor electrode material preparation method based on three-dimensional graphene |
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| CN105225766A (en) * | 2015-07-30 | 2016-01-06 | 国家纳米科学中心 | A kind of preparation method of transparent graphene conductive film |
| CN105225766B (en) * | 2015-07-30 | 2017-10-20 | 国家纳米科学中心 | A kind of preparation method of transparent graphene conductive film |
| JP2018523169A (en) * | 2015-12-04 | 2018-08-16 | ダブリュージーテック（ジアンシー） カンパニー リミテッド | Embedded touch panel and display device having high resistivity film |
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| US10429685B2 (en) | 2015-12-04 | 2019-10-01 | Wgtech (Jiangxi) Co., Ltd. | Embedded touch panel having high resistance film and display device |
| CN105732038A (en) * | 2016-01-15 | 2016-07-06 | 东南大学 | Highly conductive flexible self-supported graphene film and preparation method thereof |
| CN112376266A (en) * | 2020-09-24 | 2021-02-19 | 浙江理工大学 | Composite fiber with shape memory performance and strain sensing performance and preparation method thereof |
| CN112376266B (en) * | 2020-09-24 | 2023-04-28 | 浙江理工大学 | Composite fiber with shape memory performance and strain sensing performance and preparation method thereof |
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Application publication date: 20130807 |