KR101440396B1 - Method for fabricating transparent conductive film using conductive nano-sized wires - Google Patents
Method for fabricating transparent conductive film using conductive nano-sized wires Download PDFInfo
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- KR101440396B1 KR101440396B1 KR1020140019642A KR20140019642A KR101440396B1 KR 101440396 B1 KR101440396 B1 KR 101440396B1 KR 1020140019642 A KR1020140019642 A KR 1020140019642A KR 20140019642 A KR20140019642 A KR 20140019642A KR 101440396 B1 KR101440396 B1 KR 101440396B1
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- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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Abstract
Description
The present invention relates to a method of manufacturing a transparent conductive film using a conductive nanowire, and more particularly, to a method of manufacturing a transparent conductive film using conductive nanowires by forming a conductive nanowire network by bonding or intersecting conductive nanowires To a method of manufacturing a transparent conductive film having characteristics of excellent electrical conductivity.
In order to be used as a transparent electrode, it is advantageous that the sheet resistance is low, the electric conductivity is high, and the light transmittance in the branch ray region is as high as 70% or more. When the conductive nanowires are layered on a transparent substrate such as glass or plastic to form a network like a net, the transparent electrode having excellent conductivity can be manufactured by high light transmittance and high electrical conductivity.
In order to form a transparent flexible electrode, it is important to maintain a unique characteristic while maintaining a low sheet resistance and excellent electrical conductivity. However, electrodes using conductive nanowires are more important because they can have such properties.
However, when electrodes are formed using conductive nanowires, the contact characteristics between the conductive nanowires are improved through heat treatment to improve the sheet resistance. However, in such a heat treatment process, deterioration of electric conductivity occurs due to oxidation of a conductive material. On the other hand, when electrodes are formed using conductive nanowires, there is a need to improve the contact characteristics between the flexible substrate and the conductive nanowires.
Conductive nanowires include metallic nanowires such as silver, gold, and copper, and carbon-based nanowires such as carbon nanotubes and graphene, and silver nanowires are typically used.
For example, in the case of forming an electrode using a silver nanowire, when the electrode is exposed to the atmosphere, a silver oxide film having a shape of Ag 2 O, AgO, AgO 2 or the like may be formed immediately upon meeting with oxygen. In particular, when an electrode using a silver nanowire is exposed to oxygen in the atmosphere for a long time, the color of silver changes from gray to black, and the electric resistance is rapidly increased to 500 times or more. This oxidation of silver significantly lowers the reliability of the transparent electrode.
In order to reduce the electrical resistance of the conductive nanowire network, the present invention provides a transparent electrode including a conductive nanowire network layer connected to each other by improving the adhesion between the contact points of the conductive nanowires By improving the crystallinity of the individual nanowires, it is possible to improve the electrical characteristics of the nanowires rather than when the nanowires are present in an amorphous phase or in a poly crystal having many grain boundaries, and at the same time to increase the surface adhesion of the conductive nanowires to the flexible substrate .
According to an aspect of the present invention, there is provided a method of manufacturing a transparent conductive film using conductive nanowires, the method comprising: (a) coating an ink composition containing a conductive nanowire on a substrate; (b) irradiating the coated ink composition with an electron beam to fuse the conductive nanowires together to form a conductive nanowire network, thereby completing a conductive nanowire layer having high electrical conductivity; And,
The conductive nanowire may be one of a metallic nanowire of a metal such as silver, gold, copper and the like, and a carbon nanowire such as a carbon nanotube, a graphene and the like.
In the method for manufacturing a transparent conductive film according to the above-described characteristics, it is preferable that the ink composition contains ethanol glycol as a solvent and PVP (polyvinylpyrrolidone) and KBr as additives, and the substrate is made of PET (polyethylene terephthalate) It is preferably PEN (polyethylene naphthalene), PI (polyimide), COP (cyclic olefin polymer) film, or PC (polycarbonate).
The method of manufacturing a transparent conductive film according to the above-described characteristic may further comprise the step of pre-treating the surface of the substrate with an electron beam or the step of forming a protective layer for preventing oxidation on the surface of the conductive nanowire layer after the step (b) It is more preferable that the antioxidant protective layer is composed of a polymer material including cellulose, urethane, etc., and a transparent oxide composed of one of silicon oxide and aluminum oxide, or a mixed layer thereof.
In the method of manufacturing a transparent conductive film according to the above-described characteristic, the method of manufacturing the transparent conductive film may further include forming a buffer layer for enhancing adhesion between the conductive nanowire layer and the substrate before the step (a) It is more preferable that the buffer layer is formed by coating one or more of Si, Ti and Al on the surface of the substrate.
(C) forming a conductive coating layer on the surface of the conductive nanowire layer in the method of manufacturing a transparent conductive film according to the above-described features.
In the method of manufacturing the transparent conductive film according to the above-described characteristic, the step (b) may be performed by adjusting the intensity of the electron beam so as to maintain a temperature higher than the melting point of the conductive nanowire and below the temperature and the substrate transition temperature , It is preferable that the substrate is adjustable so that the irradiation time of the electron beam is shortened by irradiating the electron beam in a pulse shape with the transition temperature or higher.
In the method for manufacturing a transparent conductive film according to the above-described features, it is preferable that the step (b) is repeatedly carried out by cooling the substrate together with the electron beam irradiation, or by irradiating the electron beam and cooling the substrate.
In the method of manufacturing a transparent conductive film according to the above-described characteristic, it is preferable that the step (b) applies a (+) electric field to the substrate at the time of electron beam irradiation.
According to the present invention, a conductive nanowire network is distributed on a lower transparent substrate, and in particular, a plurality of embedded conductive nanowires are effectively transformed from an amorphous phase to a crystalline state or from a polycrystal to a single crystal by electron beam treatment, Since the bonding and fusion are performed between the wires, electrons can be smoothly moved without increasing the resistance due to grain boundaries in the nanowire without increasing contact resistance, and thus have high electrical conductivity characteristics.
Since the electron beam treatment is performed in a very short time of several minutes to several tens of seconds in vacuum, the oxidation of the conductive material, which may occur during the heat treatment process according to the conventional manufacturing method, can be originally blocked. Also, since the conductive nanowire and the substrate surface temperature are instantaneously raised by the electron beam treatment, fusion between the conductive nanowire and the substrate is improved, so that the adhesion between the nanowire and the substrate can be improved. If a metal layer capable of forming an eutectic alloy exists between the nanowire material and the nanowire under the nanowire in order to improve adhesion with the substrate, adhesion enhancement due to adhesion of nanowires can be more easily achieved.
In order to confirm the improvement of conductivity by the electron beam treatment in the manufacturing method according to the present invention, a silver nanowire layer was formed as a conductive nanowire layer for each of different concentrations on a substrate by a screen printing method, Table 1 shows the sheet resistance before and after the electron beam treatment in the state that the nanowire layer is completed. The concentration of the nanowires was 0.1 wt%, 0.5 wt%, 1 wt%, 5 wt%, and 10 wt%, respectively, for the electron beam at 900 eV for 5 minutes, and # 1, # 2, # 3, % to be.
As shown in Table 1 below, it can be easily seen that the sheet resistance has been reduced by the electron beam treatment. Thus, it can be understood that the electron conductivity of the silver nanowire layer is improved by the electron beam treatment.
4 (a) and 4 (b) are SEM photographs of the silver nanowire layer before and after electron beam treatment for the case of # 4. It can be seen from FIG. 4 that the fusion between the silver nanowires is increased by the electron beam treatment.
Accordingly, it is possible to manufacture a transparent conductive film using a conductive nanowire having a very high light transmittance according to the present invention. Such a method for manufacturing a transparent conductive film can be widely applied to a touch screen panel, a flexible display, and the like.
1 is a flowchart illustrating a method of manufacturing a transparent conductive film according to a first embodiment of the present invention.
2 is a flowchart showing a method of manufacturing a transparent conductive film according to a second embodiment of the present invention.
3 is a flowchart illustrating a method of manufacturing a transparent conductive film according to a third embodiment of the present invention.
4 (a) and 4 (b) are SEM photographs of the nanowire layer formed by the manufacturing method according to the present invention before and after electron beam treatment.
The method for manufacturing a transparent conductive film according to the present invention is characterized in that an ink composition containing a conductive nanowire is coated on a substrate and then an electron beam is irradiated to improve electrical conductivity of the transparent conductive film. Hereinafter, a method of manufacturing a transparent conductive film according to the present invention will be described in detail with reference to the accompanying drawings.
1 is a flowchart illustrating a method of manufacturing a transparent conductive film according to a first embodiment of the present invention. Referring to FIG. 1, a method of manufacturing a transparent conductive film according to a first embodiment of the present invention includes coating a substrate with an ink composition containing conductive nanowires (S100), and irradiating the substrate with an electron beam to form conductive nano- And forming a wire network to complete the conductive nanowire layer (S110).
The conductive nanowire may be one of a metallic nanowire of a metallic material such as silver, gold, copper and the like, and a carbon nanowire such as a carbon nanotube or a graphene. It is preferable that the ink composition contains ethanol glycol as a solvent and PVP (polyvinylpyrrolidone) and KBr as an additive.
The substrate is preferably PET (polyethylene terephthalate), PEN (polyethylene naphthalene), PI (polyimide), COP (cyclic olefin polymer) film, or PC (polycarbonate).
The method for manufacturing a transparent conductive film may further include a step of pretreating the surface of the substrate with an electron beam, thereby further improving the adhesion of the surface of the substrate.
The method of manufacturing the transparent conductive film may further include a step of forming a conductive nanowire layer by irradiating electron beams, and then coating a protective layer on the surface of the conductive nanowire layer, thereby preventing oxidation of the conductive nanowires. At this time, the protective film may be composed of a polymer material including cellulose, urethane, etc., a transparent oxide such as silicon oxide or aluminum oxide, a mixture thereof, or a mixture of a polymer and a transparent oxide.
When the electron beam is irradiated, the electron collides against the nanowire instantaneously to increase the surface temperature at an extremely short time. Therefore, the temperature condition above the melting point of the conductive nanowire and the transition temperature of the substrate in the substrate holder to be cooled , Or adjust the intensity of the electron beam so that the substrate is kept at a transition temperature or higher, but the electron beam is irradiated in a pulse shape so that the irradiation time of the electron beam can be shortened.
On the other hand, it is preferable to prevent the temperature of the substrate from rising by repeating the steps of cooling the substrate at the time of electron beam irradiation, or irradiating the electron beam and cooling the substrate.
In addition, it is preferable that electrons of the electron beam are mainly irradiated to the conductive nanowires by applying a (+) electric field to the substrate at the time of electron beam irradiation so that more fusion between the conductive nanowires and the substrate is generated.
Hereinafter, methods for generating an electron beam for electron beam irradiation will be described in detail. As an electron beam generating method, a hot filament method in which a tungsten filament is heated and a negative DC voltage is applied to the tungsten filament to emit a hot electron, and a method in which a shielded plasma is generated and electrons are pulled to accelerate can be used.
The hot filament method is a method in which an alternating current is applied to a filament such as tungsten to heat it, and a negative DC electrode is applied to the filament, thereby releasing a thermoelectron having energy. This method has a problem that the substrate can be heated by the heat of the filament itself and the filament is easily broken after being heated and the filament is oxidized to a gas such as oxygen, And can act as a source of contamination to the substrate, and there is a problem that the uniformity of the electron beam is lowered for processing in a large area. However, it is suitable for testing small size at low cost.
On the other hand, a method of generating a plasma, shielding it, and extracting electrons from it to accelerate can compensate for the shortcomings of the hot filament method described above, It is possible to uniformly process a large area, which is advantageous for industrial applications. In this case, various power sources such as MF, HF, RF, UHF and Microwave can be used to generate plasma according to the AC frequency. Capacitor, Inductive, ICP, ECR, Helical, Helicon, Hollow cathode, hot filament, and high pressure plasma such as atmospheric plasma can be used. In particular, when an atmospheric pressure plasma is used, it may be carried out in an inert gas or nitrogen atmosphere to prevent oxidation of silver nanowires.
Hereinafter, a method of forming the conductive nanowire layer according to the present invention and measuring the surface resistance thereof will be described. For the preparation of the conductive nanowire with a large diagonal ratio, 40 ml of ethanol glycol, 0.67 g of polyvinylpyrrolidone (PVP) polymer and 0.02 g of KBr additive were mixed and stirred and heated to 170 ° C. At this time, PVP helps to grow into a wire shape by obstructing the specific growth surface of the conductive nanowire, and the additive KBr helps the ion concentration of the conductive material in the solution to be kept constant. Next, ball milling of the finely ground conductive powder (0.02 g) is added to the stable solution to form an initial precursor. The metallic conductive powder used here is a chloride compound such as AgCl, AuCl, CuCl and the like, and a chloride compound such as AgCl, AuCl, CuCl or the like is used as the powder of the conductive material of the carbon series. Then, about 10 minutes later, nitrate (0.44 g) such as AgNO 3 , AuNO 3 or CuNO 3 was added. At this time, nitric acid salts such as AgNO 3 , AuNO 3 , and CuNO 3 may be first dissolved in ethylene glycol and put in a solution state. In order to separate pure conductive nanowires from ethylene glycol and PVP in the grown conductive nanowire solution, they were diluted with pure water or ethanol at a ratio of 1: 3 and then centrifuged and washed. Since the separation was not smoothly performed at a time, the above procedure was repeated 3 to 4 times. The separated conductive nanowires were dispersed in methanol solution to a concentration of conductive nanowires of 0.1 to 10 wt% in a solution, and coated on a transparent PET substrate using a screen printing method to form a conductive nanowire network. The conductive nanowire network formed on the transparent PET substrate showed a surface resistance of 250 ~ 1000 Ω / □ as measured by 4 point probe.
Carbon-based conductive nanowires were formed by coating a carbon nanotube or graphene on a transparent PET substrate using a screen printing method using a solution of water or an organic solvent dispersed in the conductive nanowire network. The carbon nanotubes can be obtained by treating carbon dioxide in a high-pressure and high-temperature process, or can be produced by plasma treatment, arc treatment, laser ablation treatment, or the like, of carbon lumps such as graphite. In the case of the above graphene, the graphite may be peeled off using scotchate or the like, or the ground graphite particles may be subjected to plasma treatment. The prepared carbon nanotubes or graphenes are dispersed in an organic solvent such as water or methanol or ethanol using a dispersing surface treatment and a dispersing agent.
In order to improve the contact characteristics between the conductive nanowires, electron beam irradiation was performed. After the electron beam irradiation, the contact resistance was measured. As a result, the surface resistance was 150 to 300? / ?. This means that contact properties between the conductive nanowires are improved by electron beam irradiation and the crystallinity of the nanowires is improved, thereby increasing the electric conductivity.
As a representative conductive nanowire material, silver has a melting point of about 961 ° C. In order to melt the contact point between silver nanowires, heat treatment at a high temperature is inevitable. However, such a high-temperature heat treatment not only affects the shape of the silver nanowire but also adversely affects the lower transparent substrate, thereby causing fatal damage to the substrate. Therefore, it is important to improve the contact characteristics between the silver nanowires without affecting the underlying transparent substrate. In the case of electron beam processing, since the electron beam instantaneously hits the surface, only the temperature of the surface irradiated with the electron beam rises and does not affect the lower substrate placed on the cooled substrate holder.
The nanowire solution is applied to a transparent substrate by a coating method such as screen printing or the like, and then a drying process is performed to remove the solvent. In order to prevent oxidation of the silver nanowires after the drying process, a polymer or transparent oxide protective layer is formed on the silver nanowire layer. In this method, electron beam irradiation is performed in a vacuum chamber or an inert gas atmosphere before forming the polymer or transparent oxide protective layer. After the treatment, a protective layer is formed. Since the volatilization of the solvent proceeds very rapidly in vacuum, it is possible to shorten the processing time in a conventional drying furnace and to prevent the oxidation of silver nanowires that may occur during the drying process. In the silver nanowire layer from which the solvent is removed, since the contact properties between the nanowires are still poor, it is possible to transform the shape of the silver nanowire from a cylindrical shape to a flat pancake shape through electron beam irradiation. So that the light transmittance is improved. Silver nanowires irradiated with electron beams are melted by local electron beam irradiation only on the surface. In this case, the contact force between the nanowires is improved and the crystallinity of the silver wire is improved to improve the overall electrical conductivity.
Such an electron beam irradiation process is easy to control the amount of energy by using an electron beam source, and it is possible to improve the surface contact force of the conductive nanowires for a short period of time for irradiation for several seconds at a few minutes. In addition, since the irradiation depth of the electron beam is very shallow from several nanometers to several tens nanometers, there is a fundamental difference from the process of heat-treating the entire material including the transparent substrate. The long sintering process is accompanied by the diffusion of oxygen and the oxidation of conductive nanowires, and oxidation of silver such as Ag 2 O, AgO and AgO 2 , oxidation of gold such as Au 2 O and AuO, copper oxide such as Cu 2 O and CuO, There may be a problem that the formation of the oxide of the carbon-based nanowire accelerates. In order to prevent this, it is possible to improve the contact characteristics between the conductive nanowires of the conductive nanowire network without damaging the transparent substrate through a usual heat treatment by performing electron beam irradiation in vacuum. Subsequent formation of a polymeric or transparent oxide protective layer may result in a very good conductive nanowire transparent electrode.
Hereinafter, a method of manufacturing a transparent conductive film according to a second embodiment of the present invention will be described.
2 is a flowchart sequentially illustrating a method of manufacturing a transparent conductive film according to a second embodiment of the present invention. Referring to FIG. 2, a method for fabricating a transparent conductive film according to an embodiment of the present invention includes forming a buffer layer on a substrate surface (Step 210), coating an ink composition containing conductive nanowires on the buffer layer (Step 220) (Step 230), forming a conductive coating layer on the surface of the conductive nanowire layer (step 240), forming a conductive nanowire network by fusing the conductive nanowires to the conductive coating layer (Step 250) on the protective layer.
Hereinafter, each of the above-described steps will be described in detail.
The step of forming the buffer layer on the surface of the substrate (step 210) is to improve the adhesion between the conductive nanowire to be deposited in the post-process and the substrate, and a material such as Si, Ti, Lt; RTI ID = 0.0 > A < / RTI > When a buffer layer is formed on the surface of the substrate and the conductive nanowires are deposited on the buffer layer, an alloy of the conductive nanowire material and the Si, Ti, and Al materials is generated in a fine surface contact region by electron beam irradiation at a subsequent step The same alloys undergo eutectic reaction, which makes it easier to improve the adhesion by lowering the melting point of the conductive nanowire material or Si, Ti, Al materials.
The temperature of the substrate surface caused by the electron beam irradiation rapidly increases the temperature of the buffer layer such as Si, Ti, and Al formed on the surface of the substrate rapidly in a situation where the substrate is not deformed by thermal diffusion to the entire substrate, The adhesion at the contact point with the nanowire is increased and the adhesion is accelerated more easily by the reaction of the process. Therefore, the adhesion problem with the substrate surface of the existing nanowire can be solved. Such a rapid high-temperature heat treatment is a method that can not be achieved due to limited temperature rise due to deformation of the substrate in the conventional heat treatment method, and can be performed only by the heating characteristics of the surface temperature such as an electron beam.
In addition, the substrate on which the conductive nanowires are deposited is irradiated with an electron beam in a vacuum chamber or an inert gas atmosphere to complete a nanowire layer (
At this time, the conductive nanowire layer and the conductive coating layer may be further fused by further performing the electron beam treatment after forming the conductive coating layer, thereby further improving the electric conductivity.
Next, a step (step 250) of forming an antioxidation protective layer on the surface of the conductive coating layer is a post-treatment step after the electron beam irradiation. In order to prevent oxidation of the conductive nanowire layer, a polymer material such as cellulose, urethane, Oxide or the like, or a mixture thereof.
Hereinafter, a method for manufacturing a transparent conductive film according to a third embodiment of the present invention will be described.
3 is a flowchart sequentially illustrating a method of manufacturing a transparent conductive film according to a third embodiment of the present invention. Referring to FIG. 3, a method of fabricating a transparent conductive film according to an embodiment of the present invention includes forming a buffer layer on a substrate surface (Step 310), coating an ink composition containing conductive nanowires on the buffer layer to form a conductive nanowire layer (Step 320), forming a conductive coating layer on the conductive nanowire layer and forming a composite of the conductive nanowire layer and the conductive coating layer (step 330), irradiating the conductive nanowire layer with the electron beam to melt the conductive nanowires of the conductive nanowire layer Forming a conductive nanowire network and fusing the conductive nanowire layer with the conductive coating layer to improve electrical conductivity (Step 340); and forming an antioxidant protective layer on the conductive coating layer (Step 350).
The method of manufacturing a transparent conductive film according to the present embodiment is characterized in that a conductive coating layer is formed on a conductive nanowire layer to form a composite therebetween, and then an electron beam treatment is performed to improve electrical conductivity. Since the steps in this embodiment are the same as the corresponding steps in the second embodiment, repetitive description will be omitted.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, It will be understood that various changes and modifications may be made without departing from the spirit and scope of the invention. It is to be understood that the present invention may be embodied in many other specific forms without departing from the spirit or essential characteristics thereof.
The method according to the present invention can be widely used in the production of semiconductor devices and the like.
Claims (16)
(b) irradiating the coated ink composition with an electron beam to fuse the conductive nanowires together to form a conductive nanowire network, thereby completing a conductive nanowire layer having electrical conductivity;
When the electron beam is irradiated, the intensity of the electron beam is adjusted so as to maintain a temperature that is higher than the melting point of the conductive nanowire and below the substrate transition temperature, or the electron beam is irradiated with a pulse Wherein the irradiation time of the electron beam is shortened by irradiating the electron beam with the electron beam.
(b) forming a conductive coating layer on the surface of the conductive nanowire layer; And
(c) irradiating the conductive coating layer with an electron beam to fuse the conductive nanowires of the conductive nanowire layer to each other to form a conductive nanowire network, and fusing the conductive nanowire layer and the conductive coating layer;
And forming a transparent conductive film on the transparent conductive film.
(b) irradiating the coated ink composition with an electron beam to fuse the conductive nanowires together to form a conductive nanowire network, thereby completing a conductive nanowire layer having electrical conductivity; And
(c) forming a conductive coating layer on the surface of the conductive nanowire;
And forming a transparent conductive film on the transparent conductive film.
Wherein the antioxidant protective layer is made of a polymer material or a transparent oxide composed of one of silicon oxide and aluminum oxide, or a mixed layer thereof.
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| KR1020140019642A KR101440396B1 (en) | 2014-02-20 | 2014-02-20 | Method for fabricating transparent conductive film using conductive nano-sized wires |
| PCT/KR2014/012743 WO2015126052A1 (en) | 2014-02-20 | 2014-12-23 | Method for manufacturing transparent conductive film using conductive nanowire |
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| KR101737225B1 (en) * | 2015-10-07 | 2017-05-17 | 한국과학기술원 | Transparent, high temperature resistance, highly conductive polyimide film and the fabrication of flexible, transparent, conducting electrodes using the same |
| WO2017099345A1 (en) * | 2015-12-07 | 2017-06-15 | 울산과학기술원 | Method for manufacturing conductive nanowire network using electron beam, and transparent electrode and electronic device employing same |
| KR20190119322A (en) * | 2018-04-12 | 2019-10-22 | 인제대학교 산학협력단 | Manufacturing method of Copper Nanowire Transparent Conductive Electrode using Pulsed laser irradiation |
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| KR101642429B1 (en) * | 2015-05-18 | 2016-07-25 | 울산과학기술원 | Repair method of electronic device |
| KR101737225B1 (en) * | 2015-10-07 | 2017-05-17 | 한국과학기술원 | Transparent, high temperature resistance, highly conductive polyimide film and the fabrication of flexible, transparent, conducting electrodes using the same |
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| KR20190119322A (en) * | 2018-04-12 | 2019-10-22 | 인제대학교 산학협력단 | Manufacturing method of Copper Nanowire Transparent Conductive Electrode using Pulsed laser irradiation |
| KR102050657B1 (en) * | 2018-04-12 | 2019-11-29 | 인제대학교 산학협력단 | Manufacturing method of Copper Nanowire Transparent Conductive Electrode using Pulsed laser irradiation |
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