CN103710685A - Spraying method for directly preparing graphene transparent conducting thin film on flexible substrate - Google Patents
Spraying method for directly preparing graphene transparent conducting thin film on flexible substrate Download PDFInfo
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- CN103710685A CN103710685A CN201310723398.7A CN201310723398A CN103710685A CN 103710685 A CN103710685 A CN 103710685A CN 201310723398 A CN201310723398 A CN 201310723398A CN 103710685 A CN103710685 A CN 103710685A
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Abstract
The invention relates to a spraying method for directly preparing a graphene transparent conducting thin film on a flexible substrate. The spraying method comprises the steps of preparing a water-ethanol-graphene oxide dispersion liquid, ultrasonically washing the flexible substrate, drying the flexible substrate in a drying oven, heating the flexible substrate by utilizing a heating plate until reaching a softening temperature of the flexible substrate, adding the water-ethanol-graphene oxide dispersion liquid into an air brush connected with an air pump, spraying the water-ethanol-graphene oxide dispersion liquid to the flexible substrate so as to obtain a graphene oxide thin film, and reducing the graphene oxide thin film to obtain the graphene transparent conducting thin film. Compared with the prior art, the spraying method has the advantages of high efficiency, feasibility, fitness in large-area and large-scale preparation and the like.
Description
Technical field
The invention belongs to function film technical field, especially relate to a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates.
Background technology
Each carbon atom in Graphene is with sp
23 carbon atoms of the mode of hybridized orbital (σ key) and other are connected, and extremely strong C-C key causes graphene sheet layer to have excellent mechanical property.A remaining p electronic orbit is perpendicular to Graphene plane, forms the π key of delocalization with carbon atom around, causes electronics in crystal, to move freely, and given Graphene good electrical property.Because interatomic reactive force is very strong, at normal temperatures, even if around carbon atom telescopes, the interference that the electronics in Graphene is subject to is also very little.When electronics transmits in Graphene, be difficult for scattering occurs, mobility can reach 2 * 10
5cm
2/ (Vs).Its surface resistance is about 31 Ω/sq, and specific conductivity can reach 10
6s/m is the material of electroconductibility the best under room temperature.Compare with traditional ITO, Graphene has the following advantages: (1) has higher conductivity, and (2) have good snappiness, and (3) resource is compared with horn of plenty.Therefore, graphene-based transparent conductive film develops rapidly in recent years, and is applied to the fields such as touch-screen, Organic Light Emitting Diode, organic photovoltaic devices and organic transistor.
The preparation method of graphene-based transparent conductive film is mainly divided into two large classes: Physical and chemical method.Wherein Physical is mainly divided into CVD method and liquid phase physics stripping method.In general, CVD method is than liquid phase physics stripping method and chemical method, and prepared graphene-based transparent conductive film has higher electroconductibility and transmittance.But also have outstanding limitation, be mainly manifested in manufacturing cost higher, preparation technology is comparatively complicated.It is lower that the comparatively outstanding limitation of liquid phase physics stripping method is mainly manifested in production efficiency.And chemical method is than Physical, its advantage is mainly manifested in following method: (1) production cost is lower; (2) preparation technology is comparatively simple; (3) preparation efficiency is higher.Therefore, chemical method prepare graphene-based transparent conductive film and will be after the important directions of research.The method of chemical preparation transparent graphene conductive film mainly contains at present: vacuum filtration, LB method, spin-coating method, self-assembly and spraying method.And spraying method is than the advantage of additive method: (1) spraying can be carried out in curved surface substrate; (2) preparation process is easy, and production efficiency is higher; (3) be applicable to can be used for big area film forming; (4) spray equipment is easy to carry and moves.
Spraying method refers to, with professional airbrush, graphene dispersing solution is sprayed in the substrate of preheating, obtains the process of graphene film after solvent evaporates.The effect of fog gun is atomization dispersion liquid, forms small droplets.Preheating substrate is that solvent can evaporate rapidly, avoids the reunion of graphene film, finally forms graphene-based transparent conductive film in order to guarantee that droplet deposition is to after in substrate.2010, Pham etc. mixed graphene oxide solution and hydrazine hydrate solution, and it is that on the substrate of 240 ℃, to have prepared area be the graphene film of 4 inches that the mode by spraying is ejected into Heating temperature in advance by graphene oxide and hydrazine hydrate mixing solutions.Test shows, when the transmittance of prepared TCFs (λ=550nm) is 84%, square resistance is 2.2k Ω/sq.2013, Iskandar
[deng prepared copper nano-wire net by spraying, utilize spin coating to prepare graphene oxide film, chemical treatment 24h under hydrazine hydrate atmosphere, 400 ℃ of thermal treatment 1h, prepared transparent graphene conductive film, finally by the method shifting, the two is combined, prepared Graphene/copper nano-wire film.Test result shows that gained TCFs is in the wavelength region of λ=550nm, and transmittance is 80%, and square resistance is 34 ± 2.6 Ω/sq.
On flexible base, board, prepare at present graphene film both at home and abroad, mainly contain two kinds of methods, a kind of is that flexible base, board is carried out to hydrophilic treatment, in means such as utilizing spin coating, self-assembly, carries out film forming.The 2nd, by film preparation on hard substrate, by the mode that shifts the most at last graphene oxide film transfer on flexible base, board.This process is very complicated not only, and in transfer process, the integrity of film is damaged.Because flexible base, board is mostly macromolecule material, can not be high temperature resistant, more hydrophobic.As it is, be difficult to directly prepare graphene-based transparent conductive film on flexible base, board.
Summary of the invention
Object of the present invention be exactly in order to overcome the defect that above-mentioned prior art exists, provide a kind of efficient, feasible, be suitable for big area, extensive preparation directly in flexible substrates, prepare the spraying method of transparent graphene conductive film.
Object of the present invention can be achieved through the following technical solutions:
Directly in flexible substrates, prepare a spraying method for transparent graphene conductive film, it is characterized in that, the method adopts following steps:
(1) preparation water-ethanol-graphene oxide dispersion liquid, controls the concentration of graphene oxide at 0.1～2mg/ml, and the volume ratio of water and ethanol is 1: 1～1: 10, and sonic oscillation obtains water-ethanol-graphene oxide dispersion liquid of dispersed and good stability;
(2) flexible base, board is cleaned and dried in baking oven under ultrasonic, guarantee flexible base, board surface clean, dustless;
(3) flexible base, board is heated on hot-plate and approaches flexible base, board softening temperature;
(4) water-ethanol-graphene oxide dispersion liquid is joined in the airbrush that is connected with air pump, be ejected on flexible base, board, obtain graphene oxide film;
(5) graphene oxide film is reduced, prepare transparent graphene conductive film.
Described flexible base, board is that transparent material is made the flexible base, board obtaining.
The preferred PC of described flexible base, board or PET transparent material are made the flexible base, board obtaining.Described flexible base, board softening temperature is 20-200 ℃.
Described flexible base, board softening temperature is preferably 80-120 ℃.
Airbrush, when spraying water-ethanol-graphene oxide dispersion liquid, is 5～20cm apart from the distance of flexible base, board.
Airbrush is when spraying water-ethanol-graphene oxide dispersion liquid, and the injection air pressure of employing is 20～80psi.
Compared with prior art, the invention provides a kind of efficient, feasible, be suitable for big area, prepare on a large scale the method for transparent graphene conductive film, by air pump, provide certain air pressure, graphene oxide solution is sprayed by airbrush.Utilize hot-plate to improve substrate for film deposition surface temperature, be beneficial to solvent flashing better.Spraying ratio juris is graphene dispersing solution to be sprayed in the substrate of preheating with professional airbrush, obtains the process of graphene film after solvent evaporates.The effect of fog gun is atomization dispersion liquid, forms small droplets.Preheating substrate is that solvent can evaporate rapidly, avoids the reunion of graphene film, finally forms graphene-based transparent conductive film in order to guarantee that droplet deposition is to after in substrate.Because the boiling point of ethanol is 78 ℃, lower than the boiling point of water.And the surface tension of ethanol is less, on the material of macromolecule material, wettability is better.Yet graphene oxide, owing to making its surface with carboxyl and hydroxyl in oxidising process, makes it comparatively hydrophilic, and dispersiveness in ethanol is poor.Based on this, in the present invention, we have successfully prepared water-ethanol-graphene oxide dispersion liquid.This dispersion liquid can effectively reduce solvent boiling point, can realize the wettability to some polymer flexible base, boards, and can well disperse graphene oxide simultaneously.Method by spraying is injected in above-mentioned solution on pre-heated substrate, directly on the flexible base, board without any processing, has successfully prepared graphene oxide film, final, through suitable chemical reduction, has prepared transparent graphene conductive film.This patent efficiently, has simply directly been prepared transparent graphene conductive film on flexible base, board, and this technology can be used for extensive, the big area preparation of transparent graphene conductive film, has the following advantages:
(1), by preparing water-ethanol-graphene oxide dispersion liquid, reduced the boiling point of ejection of solvent volatilization.
(2) by preparing water-ethanol-graphene oxide dispersion liquid, improved the wettability of graphene oxide solution to flexible transparent substrate.
(3) flexible base, board is not carried out to any processing, by the method for spraying, directly on flexible base, board surface, successfully preparing graphene oxide film.
(4) direct spraying water-ethanol-graphene oxide dispersion liquid method is than traditional transfer method, and substrate surface hydrophilic treatment etc. save time, efficiently, succinctly.
(5) the method processing ease, it is mobile that spray equipment is easy to, and than additive method, has outstanding advantage preparing on large area film.
Accompanying drawing explanation
Fig. 1 is that graphene oxide concentration is transparent conductive film AFM picture prepared by 1/8000mg/ml;
Fig. 2 is that graphene oxide concentration is transparent conductive film AFM picture prepared by 1/2000mg/ml;
Fig. 3 is that graphene oxide concentration is transparent conductive film AFM picture prepared by 1/1000mg/ml;
Fig. 4 is that graphene oxide concentration is transparent conductive film AFM picture prepared by 1/400mg/ml;
Fig. 5 is that graphene oxide concentration is transparent conductive film AFM picture prepared by 1/250mg/ml;
Fig. 6 is that graphene oxide consumption is transparent conductive film AFM picture prepared by 1ml;
Fig. 7 is that graphene oxide consumption is transparent conductive film AFM picture prepared by 2ml;
Fig. 8 is that graphene oxide consumption is transparent conductive film AFM picture prepared by 3ml;
Fig. 9 is that graphene oxide consumption is transparent conductive film AFM picture prepared by 4ml.
In Fig. 1-5, graphene oxide solution usage is 1ml, and in Fig. 6-9, the concentration of graphene oxide is 1/1200mg/ml.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
By changing concentration, on sheet mica, prepare the transparent graphene conductive film of different coverages
Get 1mg/ml graphene oxide solution 5ml, add wherein 25ml ethanol.In ultrasonic a moment, get 2ml homogeneous solution and join in airbrush watering can.Clean mica substrate is ultrasonic, with post-drying, put on warm table and be warmed up to 100 ℃.Now utilize the airbrush that is associated with air pump that above-mentioned solution is injected on the flexible mica substrate that area is 1.8 * 1.3cm, jet length is 5cm left and right, and air pump air pressure is 35psi.The consumption of graphene oxide is 1ml, by changing graphene oxide concentration, we have studied graphene oxide concentration to the impact of transparent graphene conductive film microtexture (as Figure 1-5) to be followed successively by 1/8000mg/ml, 1/2000mg/ml, 1/1000mg/ml, 1/400mg/ml, 1/250mg/ml.Result shows, utilize the graphene oxide lamella that this spraying method sprays to be out uniformly dispersed, and fold is less.But along with the increase of concentration, its coverage increases gradually, film fold is also increasing gradually.
On flexible pet substrate, prepare transparent graphene conductive film
Get 1mg/ml graphene oxide solution 1ml, add wherein 5ml ethanol.In ultrasonic a moment, get 2ml homogeneous solution and join in airbrush watering can.Clean pet substrate is ultrasonic, with post-drying, put in heating too and be warmed up to 80 ℃.Now utilize the airbrush that is associated with air pump that above-mentioned solution is injected on the flexible pet substrate that area is 5 * 5cm, jet length is 10cm left and right, and air pump air pressure is 35psi.Final prepared graphene oxide film is immersed in HI acid, and it is reduced, and has finally successfully prepared transparent graphene conductive film.
By changing graphene oxide consumption, on sheet mica, prepare the transparent graphene conductive film of different coverages
Get 1mg/ml graphene oxide solution 5ml, add wherein 25ml ethanol.In ultrasonic a moment, get 2ml homogeneous solution and join in airbrush watering can.Clean mica substrate is ultrasonic, with post-drying, put on warm table and be warmed up to 100 ℃.Now utilize the airbrush that is associated with air pump that above-mentioned solution is injected on the flexible mica substrate that area is 1.8 * 1.3cm, jet length is 5cm left and right, and air pump air pressure is 35psi.Graphene oxide concentration is 1/1200mg/ml, by changing the consumption of graphene oxide, is respectively 1ml, 2ml, 3ml, 4ml, and we have studied graphene oxide consumption to the impact of transparent graphene conductive film microtexture (as Figure 6-9).Result shows, utilize the graphene oxide lamella that this spraying method sprays to be out uniformly dispersed, and fold is less.But along with the increase of consumption, its coverage increases gradually, film fold is also increasing gradually.
On flexible PC substrate, prepare transparent graphene conductive film
Get 1mg/ml graphene oxide solution 5ml, add wherein 25ml ethanol.In ultrasonic a moment, get 2ml homogeneous solution and join in airbrush watering can.Clean PC substrate is ultrasonic, with post-drying, put on warm table and be warmed up to 100 ℃.Now utilize the airbrush that is associated with air pump that above-mentioned solution is injected on the flexible PC substrate that area is 5 * 5cm, jet length is 10cm left and right, and air pump air pressure is 35psi.Graphene oxide consumption is 2ml, and concentration is 0.17mg/ml.Finally, successfully prepared graphene oxide film (so as Fig. 3).Prepared graphene oxide film utilizes 0.5mlHI acid stifling, and it is reduced.Now substrate P C substrate temperature is 100 ℃, and final prepared graphene film square resistance is 16.4k Ω, and transmittance is 64.1%.
Claims (7)
1. directly in flexible substrates, prepare a spraying method for transparent graphene conductive film, it is characterized in that, the method adopts following steps:
(1) preparation water-ethanol-graphene oxide dispersion liquid, controls the concentration of graphene oxide at 0.1～2mg/ml, and the volume ratio of water and ethanol is 1: 1～1: 10, and sonic oscillation obtains water-ethanol-graphene oxide dispersion liquid of dispersed and good stability;
(2) flexible base, board is cleaned and dried in baking oven under ultrasonic, guarantee flexible base, board surface clean, dustless;
(3) flexible base, board is heated on hot-plate and approaches flexible base, board softening temperature;
(4) water-ethanol-graphene oxide dispersion liquid is joined in the airbrush that is connected with air pump, be ejected on flexible base, board, obtain graphene oxide film;
(5) graphene oxide film is reduced, prepare transparent graphene conductive film.
2. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 1, is characterized in that, described flexible base, board is that transparent material is made the flexible base, board obtaining.
3. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 2, is characterized in that, the preferred PC of described flexible base, board or PET transparent material are made the flexible base, board obtaining.
4. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 1, is characterized in that, described flexible base, board softening temperature is 20-200 ℃.
5. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 1, is characterized in that, described flexible base, board softening temperature is preferably 80-120 ℃.
6. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 1, is characterized in that, airbrush, when spraying water-ethanol-graphene oxide dispersion liquid, is 5～20cm apart from the distance of flexible base, board.
7. a kind of spraying method of directly preparing transparent graphene conductive film in flexible substrates according to claim 1, is characterized in that, airbrush is when spraying water-ethanol-graphene oxide dispersion liquid, and the injection air pressure of employing is 20～80psi.
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| CN105761774A (en) * | 2014-12-19 | 2016-07-13 | 北京生美鸿业科技有限公司 | Novel electrode material applicable to intelligent liquid crystal dimming film and preparation method thereof |
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| CN107887076A (en) * | 2017-10-27 | 2018-04-06 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of graphene conductive film |
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| CN110407201A (en) * | 2019-09-11 | 2019-11-05 | 华北理工大学 | A kind of graphene film and its preparation method and application |
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| CN105761774A (en) * | 2014-12-19 | 2016-07-13 | 北京生美鸿业科技有限公司 | Novel electrode material applicable to intelligent liquid crystal dimming film and preparation method thereof |
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| CN105084858B (en) * | 2015-08-07 | 2018-05-18 | 常州富烯科技股份有限公司 | A kind of preparation method of graphene film |
| CN105582751A (en) * | 2015-12-17 | 2016-05-18 | 常州碳星科技有限公司 | Filter element and preparing method and application thereof |
| CN105582751B (en) * | 2015-12-17 | 2018-05-22 | 常州碳星科技有限公司 | Filter core and its preparation method and application |
| CN105951302A (en) * | 2016-06-08 | 2016-09-21 | 海南大学 | Method for preparing oil-water separation nanofiber membrane |
| CN105951302B (en) * | 2016-06-08 | 2020-10-27 | 海南大学 | Method for preparing oil-water separation nanofiber membrane |
| CN108242452A (en) * | 2016-12-27 | 2018-07-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Photonic integrated device and preparation method thereof |
| CN107887076A (en) * | 2017-10-27 | 2018-04-06 | 成都天航智虹知识产权运营管理有限公司 | A kind of preparation method of graphene conductive film |
| CN110407201A (en) * | 2019-09-11 | 2019-11-05 | 华北理工大学 | A kind of graphene film and its preparation method and application |
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