CN109830327B - Preparation method of transparent conductive electrode - Google Patents
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Abstract
The invention relates to the technical field of conductive electrodes, in particular to a preparation method of a transparent conductive electrode. The preparation method of the transparent conductive electrode comprises the following steps: 1) laying a nano metal conducting layer on the surface of a transparent base material; 2) carrying out graphical shielding on the nano metal conducting layer in the step 1) to form a blocking layer on the surface of the nano metal conducting layer, wherein the unmasked nano metal conducting layer forms a reaction area; 3) and introducing gas containing a doped etchant or injecting impurity ions into the reaction area, so that the nano metal conducting layer of the reaction area reacts with the gas containing the doped etchant or is doped with the impurity ions to form a non-conducting area, and obtaining the transparent conducting electrode after the reaction is finished. According to the preparation method of the transparent conductive electrode, the characteristics that the nano metal material has large specific surface area, is easy to adsorb impurities, is easy to break and lose conductivity are utilized, directional doping is carried out, the patterned transparent electrode is formed, and the preparation method is simple and low in cost.
Description
Technical Field
The invention relates to the technical field of conductive electrodes, in particular to a preparation method of a transparent conductive electrode.
Background
At present, the materials of the transparent electrode mainly include transparent conductive oxide films, carbon nanotubes, graphene, conductive polymers, metal grids, metal nanowires, and the like. ITO transparent electrodes have occupied a large part of the market by virtue of their high transparency and high conductivity. However, the ITO electrode needs to be prepared by vacuum vapor deposition, and contains rare element indium, so that the cost is high, and the ITO is brittle and cannot be used in flexible devices. Therefore, people are looking for other transparent electrode materials, and the nano metal wire is favored due to the lower cost, higher performance and good adaptability to flexible devices, and becomes the product with the highest market acceptance. And the nano metal wire conductive material can obtain better applicability by matching with graphene, carbon nano tubes, conductive polymers and metal oxide semiconductor materials.
In practical applications in the fields of liquid crystal displays, OLEDs (organic electroluminescence), touch screens, solar cells, etc., patterned transparent conductive electrodes are often required to perform various functions. For the existing transparent conductive material, various patterning methods are available in the prior art, including laser ablation, chemical etching method of yellow light process, chemical etching of silk-screen etching paste, ink-jet printing etching solution and other methods. The methods all cause the large difference of optical performance between the etching area and the non-etching area, and have the defects of large pollution to the environment, complex preparation process and high preparation cost.
The invention of China patent with application publication No. CN103187118A, a method for manufacturing the conductive film and a touch screen thereof, provides a method for preparing the conductive film, firstly, a groove is arranged on a substrate by using a nano-imprinting method, nano-slurry formed by nano-metal particles and nano-metal wires is filled in the groove, a metal grid with the width of 5-10um and the thickness of 0.5-2um is obtained by sintering, at the moment, the nano-silver particles or wires are converted into a material with micron-scale dimension, the chemical activity of the material is greatly reduced, the material is similar to a silver block material, therefore, the etching needs to be carried out by firstly oxidizing into silver oxide and then vulcanizing in hydrogen sulfide gas; wherein, the oxidation is formed by soaking or coating hydrogen peroxide or acid solution, which belongs to the liquid-solid reaction in the solution; although the second step uses gas as a reactant to react with the silver oxide in the metal grid to obtain the non-conductive metal compound, the gas is not directly reacted with the nano metal, the characteristics of large specific surface area of the nano material, high chemical activity and easy doping of the nano metal wire are not utilized, the preparation process is complex, and the yield cannot be ensured.
Chinese patent No. CN 105788760B, entitled "method for manufacturing transparent conductive electrode", provides a method for forming a patterned electrode from a transparent conductive material through a gas etching reaction, in which a template is used to prevent reaction gas from entering other parts, and after the etching is finished, the template can be easily removed, but in the production process, a transparent conductive electrode processing device is required, and the manufacturing process is complicated and slow.
Disclosure of Invention
The invention aims to provide a preparation method of a transparent conductive electrode, which is simpler in preparation process, can effectively improve the preparation speed of the transparent conductive electrode and has more excellent shadow eliminating effect.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a transparent conductive electrode comprises the following steps:
1) laying a nano metal conducting layer on the surface of a transparent base material;
2) carrying out graphical shielding on the nano metal conducting layer in the step 1) to form a blocking layer on the surface of the nano metal conducting layer, wherein the unmasked nano metal conducting layer forms a reaction area;
3) introducing a gas doping etching agent or injecting impurity ions into the reaction area in the step 2), so that the nano metal conducting layer of the reaction area reacts with the gas containing the doping etching agent or is doped with the impurity ions to form a non-conducting area, and obtaining the transparent conducting electrode after the reaction is finished.
The gas containing the doped etchant comprises a carrier gas and the doped etchant, wherein the carrier gas is one or more of air, nitrogen, oxygen and inert gas; the doped etching agent is any one or more of ozone, water vapor, hydrogen peroxide, organic amine, ammonia gas, carbon dioxide, organic acid, nitrogen oxide, inorganic volatile acid, sulfur vapor, hydrogen sulfide, sulfur oxide and sulfur-containing compound vapor.
The carrier gas is in a normal gas state or a plasma gas state.
The doped etchant is in a normal gas state or a plasma gas state.
The impurity ions are any one or more of carbon, nitrogen, oxygen, boron, helium, phosphorus, iron, aluminum, zinc, cobalt, tin and nickel.
The transparent substrate is any one of a transparent polyethylene terephthalate film, a transparent polyimide resin film, polycarbonate, glass and polymethacrylic resin.
The method for laying the nano metal conducting layer on the surface of the transparent substrate in the step 1) comprises the following steps: and depositing the nano metal dispersion liquid on the transparent substrate by coating or spraying to form a latticed conducting layer in a mutually overlapping mode.
The nano metal dispersion liquid is one or more of simple substance nano silver, nickel, copper, palladium, platinum, gold, cobalt, iron and aluminum.
The nano metal adopted by the nano metal dispersion liquid is any one of a nano metal wire, a nano metal rod and a nano metal band. The diameter of the nano metal is 1-200nm, and the length is 1-200 um.
Preferably, the nano metal dispersion liquid is a dispersion liquid of nano silver wires, and the diameter of the nano silver wires is 10-100nm, and the length of the nano silver wires is 5-100 mu m. The nano metal silver wire is of a single crystal structure and has excellent conductivity.
The barrier layer in the step 2) is any one or more of ultraviolet radiation loss adhesive tape, peelable adhesive, easy-to-pull adhesive and single-sided pressure-sensitive adhesive tape. The barrier layer has good gas permeation resistance, and can achieve good barrier effect without adding filler or anti-permeation agent.
The blocking layer in the step 2) comprises a blocking agent, wherein the blocking agent is removable ink, transparent resin or photoresist.
The barrier layer further comprises an auxiliary agent, wherein the auxiliary agent is any one or two of a permeation-resistant filler and an etching resistant agent; the anti-permeation filler is any one or more of metal powder, metal oxide, carbon material, nano silicon dioxide, boron nitride and calcium carbonate, and the anti-etching agent is glucose or vitamin C.
The metal powder is one or more of aluminum powder, copper powder, iron powder, zinc powder and nickel powder; the metal oxide is one or more of aluminum oxide, manganese dioxide, titanium dioxide and indium tin oxide; the carbon material is one or more of graphene, graphite, carbon black and carbon fiber.
The barrier layer can remove printing ink, transparent resin and photoresist, has certain permeability to gas, and is doped with anti-permeation filler if necessary, on one hand, the filler is compact and has high barrier property to gas, and can prevent the gas containing a doped etching agent from permeating the barrier layer to corrode the conducting layer; on the other hand, a portion of the filler may act as a catalyst, such as manganese dioxide, which when the gaseous etchant is ozone, may catalytically decompose to oxygen that is not available for the doping reaction, further preventing gases containing the doped etchant from permeating through the barrier layer to corrode the conductive layer. The anti-etching agent is glucose or vitamin C, is a reducing agent, and the oxidizing etching gas permeated into the anti-etching agent reacts with the glucose or the vitamin C to be consumed so that the oxidizing etching gas cannot etch the conductive layer below the barrier layer.
The barrier layer is formed by any one of screen printing, pad printing, gravure printing, planographic printing, letterpress printing, ink-jet printing, hot stamping, thermal transfer printing, spraying, brushing, coating, patterned dispensing, patterned exposure developing and attaching.
The barrier layer in the step 2) is removed or partially removed or retained by heating and the like after the preparation of the transparent conductive electrode is finished.
The reaction temperature of the nano metal conducting layer in the reaction area in the step 3) and the gas containing the doped etching agent is 0-300 ℃.
Step 3) reacting the nano metal conducting layer in the reaction area with the gas containing the doped etching agent or doping the nano metal conducting layer with impurity ions, doping the reaction area with heteroatoms such as oxygen, sulfur, phosphorus, boron, nitrogen, fluorine, chlorine, bromine, iodine and the like or impurity ions such as carbon, nitrogen, oxygen, boron, helium, phosphorus, iron, aluminum, zinc, cobalt, tin, nickel and the like, destroying the crystal structure of the nano metal wire, destroying the continuity of an energy band and increasing the resistance of a single nano metal wire; or the doped atoms destroy the mechanical structure of the nano metal wire, and the nano metal wire is broken to form discrete short rods; macroscopically rendered non-conductive or weakly conductive.
And 3) implanting impurity ions in the step 3) by adopting an ion implantation technology and equipment in the prior art.
The method comprises the steps of firstly carrying out graphical shielding on a nano conductive layer to form a barrier layer and a reaction area, then directly reacting with a nano metal wire in the reaction area through gas containing a doped etching agent or injected with impurity ions to enable the active point of the nano metal wire to carry out doping reaction, and losing excellent conductivity of the reacted nano metal wire, wherein macroscopically, the difference of the resistance values of a channel in the reaction area and a channel in an unreacted area is larger than 1000 times, so that a usable patterned electrode is obtained.
According to the preparation method of the transparent conductive electrode, a template and other transparent conductive electrode processing devices are not needed, the conductive layer is subjected to graphical shielding by using the blocking layer, and the patterned metal grid is formed by directionally doping the nano metal material which has the characteristics of large specific surface area, easiness in impurity adsorption and easiness in conductivity loss; the preparation method of the transparent conductive electrode is simple, the cost is low, the optical properties of the reaction area and the blocking area are close, and the prepared transparent conductive electrode has good optical properties.
Drawings
FIG. 1 is a schematic flow chart of a method for manufacturing a transparent conductive electrode in example 1 of the present invention;
FIG. 2(a) is a scanning electron micrograph of a region in which oxygen doping does not occur in example 1; (b) scanning electron microscope images of the reaction region after oxygen doping;
FIG. 3(a) is a scanning electron micrograph of a region in which sulfur doping does not occur in example 2; (b) scanning electron microscopy of the reaction zone after sulfur doping.
Detailed Description
Example 1
The preparation method of the transparent conductive electrode of the embodiment, as shown in fig. 1, includes the following steps:
1) coating a mixed dispersion liquid of nano silver wires, modified cellulose and a surfactant on a transparent PET (polyethylene terephthalate) film by a wire rod in a scraping way, and drying to prepare a nano silver wire conducting layer; the diameter of the nano silver wire is 10-100 nm; the sheet resistance of the nano silver wire conducting layer is 50 ohm/sq;
2) manufacturing a patterned silk screen printing plate: silk-screen printing a patterned blocking layer on the surface of the nano silver wire conducting layer, wherein the blocking layer is composed of blocking agent transparent UV resin, anti-permeation filler nano silicon dioxide and manganese dioxide, the blocking layer is formed by UV lamp curing, a single-side pressure-sensitive adhesive tape is pasted at the position of an electrode outgoing line for protection, and the unmasked nano silver wire conducting layer forms a reaction area;
3) placing the silver wire into a gas doping device with controllable temperature, airflow and reaction gas concentration, introducing ozone by taking air as carrier gas to carry out doping reaction with the nano silver wire conducting layer in the reaction area, wherein the doping reaction temperature is 60 ℃, partial positions of the nano silver wires are converted into silver oxide due to the doping reaction of oxygen atoms, the whole conductivity is greatly reduced, and the silver wires can be broken at the reaction point position due to the stress in the nano silver wires, in the figure 2, (a) is a scanning electron microscope image of an area without oxygen doping, and (b) is a scanning electron microscope image of the reaction area after oxygen doping, as can be seen by comparing the figures 2(a) and (b), the middle of the silver wires after oxygen doping shows a dark point (oxidized into silver oxide), and the silver wires can be broken at the reaction point position; macroscopically, the resistance value ratio of the reaction area to the blocking area is larger than 1000; the undoped area is protected by the barrier layer, and the nano silicon dioxide in the barrier layer can improve the air tightness of the transparent UV resin and prevent the subsequent gas ozone containing the doped etching agent from permeating the transparent UV resin; even if a small amount of ozone permeates, the manganese dioxide filler can be used as a catalyst to decompose the ozone into oxygen which cannot be doped for reaction, so that the conductive layer below the barrier layer is further protected, and the conductive layer below the barrier layer is ensured to have good conductivity;
4) and taking out after the reaction is finished, and removing the single-sided pressure sensitive adhesive tape to obtain the patterned transparent conductive electrode.
Example 2
The preparation method of the transparent conductive electrode of the embodiment comprises the following steps:
1) extruding and coating mixed dispersion liquid of a nano silver wire, modified cellulose and a surfactant on a transparent colorless PI (polyimide resin) film after corona through a slit, and drying to prepare a nano silver wire film conducting layer; the diameter of the nano silver wire is 10-100 nm;
2) compounding a photoresist film containing nano copper powder and silicon dioxide filler on the surface of the nano silver wire film conducting layer, forming a photoresist barrier layer through exposure and development, and forming a reaction area on the unmasked nano silver wire conducting layer;
3) putting the silver nanowire into gas doping equipment with controllable temperature, airflow and reaction gas concentration, introducing trace hydrogen sulfide gas by taking high-pressure air as carrier gas, and performing a synergistic reaction of hydrogen sulfide, oxygen and nano silver on the surface of the nano silver wire in a reaction area, wherein the doping temperature is 120 ℃, and the high-activity point position of the nano silver wire part in the reaction area is converted into silver sulfide; and removing the photoresist layer by using a sodium hydroxide solution after the reaction is finished, thus obtaining the patterned transparent conductive electrode. As the silver wire is doped with sulfur, the conductivity is further reduced, the nano silver wire in the doped region loses the conductivity, the scanning electron microscope image of the reaction region after sulfur doping is shown in figure 3(b), and the scanning electron microscope image of the region without sulfur doping reaction is shown in figure 3 (a).
Example 3
The preparation method of the transparent conductive electrode of the embodiment comprises the following steps:
1) extruding and coating a mixed dispersion solution of a nano silver wire, modified cellulose and a surfactant on the transparent PET film subjected to corona through a slit, and drying to prepare a nano silver wire film conductive layer;
2) compounding a photoresist film containing nano silicon dioxide on the surface of the nano silver wire conducting layer, forming a photoresist barrier layer through exposure and development, and forming a reaction area in an unmasked area;
3) placing the thin film material into ion implantation equipment, wherein ion sources are boron trifluoride, phosphane, arsane and the like, forming boron B ions and impurity ions through ionization, purifying the boron B ions and the impurity ions through a magnetic analyzer, accelerating the required boron ions through an electric field to obtain high kinetic energy, performing deflection injection molding on the surface of a conductive layer of a nano silver wire thin film through an electromagnetic field, performing doping reaction on a boron element and the conductive layer of a reaction region, directly influencing the continuous structure of silver single crystals through doping of the boron element, reducing the conductivity, and removing a photoresist layer through a sodium hydroxide solution to obtain the patterned transparent conductive electrode.
Example 4
The preparation method of the transparent conductive electrode of the embodiment comprises the following steps:
1) coating a mixed dispersion liquid of a nano silver wire, modified cellulose and a surfactant on a transparent polymethacrylic resin film by a wire rod in a scraping way, and drying to prepare a nano silver wire conducting layer; the diameter of the nano silver wire is 10-100 nm;
2) manufacturing a patterned silk screen printing plate: silk-screen printing a patterned blocking layer on the surface of the nano silver wire conducting layer, wherein the blocking layer is composed of blocking agent transparent UV resin and anti-etching agent glucose, the blocking layer is formed by UV lamp curing, a single-side pressure-sensitive adhesive tape is pasted at the position of an electrode outgoing line for protection, and the non-shielded nano silver wire conducting layer forms a reaction area;
3) putting the silver wire into gas doping equipment with controllable temperature, airflow and reaction gas concentration, introducing ozone by taking nitrogen and oxygen mixed gas as carrier gas to carry out doping reaction with the conductive layer of the nano silver wire in the reaction area, wherein the doping reaction temperature is 80 ℃, partial position of the nano silver wire is converted into silver oxide due to the doping reaction of oxygen atoms, the whole conductivity is greatly reduced, and the silver wire can be broken at the position of the reaction point due to the stress in the nano silver wire; due to the protection effect of the barrier layer, the conducting layer below the barrier layer is not doped with oxygen atoms, so that the barrier layer has good conductivity; even if a small amount of ozone permeates through the UV resin, the glucose in the barrier layer reacts with the ozone to consume the permeated ozone, so that the influence of ozone permeation on the conductive layer is avoided;
4) and taking out after the doping reaction is finished, and removing the single-sided pressure sensitive adhesive tape to obtain the patterned transparent conductive electrode.
Example 5
The preparation method of the transparent conductive electrode of the embodiment comprises the following steps:
1) coating a mixed dispersion liquid of a nano silver wire, modified cellulose and a surfactant on a transparent polymethacrylic resin film by a wire rod in a scraping way, and drying to prepare a nano silver wire conducting layer; the diameter of the nano silver wire is 10-100 nm;
2) manufacturing a patterned silk screen printing plate: silk-screen printing a patterned blocking layer on the surface of the nano silver wire conducting layer, wherein the blocking layer is composed of blocking agent transparent UV resin, the blocking layer is formed by UV lamp curing, a single-sided pressure sensitive adhesive tape is pasted at the position of an electrode outgoing line for protection, and the unmasked nano silver wire conducting layer forms a reaction area;
3) introducing mixed hydrogen sulfide gas by taking high-pressure air as carrier gas, converting the carrier gas and a doping agent into plasma gas by using a jet plasma spray gun, sweeping the surface of the conductive film, wherein the doping reaction temperature is 80 ℃, partial positions of the nano silver wires are converted into silver sulfide due to the doping reaction of sulfur atoms, the overall conductivity is greatly reduced, and the silver wires can be broken at the positions of reaction points due to the stress in the nano silver wires; due to the protection effect of the barrier layer, the conducting layer below the barrier layer is not doped, so that the conductive layer has good conductivity;
4) and taking out after the doping reaction is finished, and removing the single-sided pressure sensitive adhesive tape to obtain the patterned transparent conductive electrode.
Example 6
The preparation method of the transparent conductive electrode of the embodiment comprises the following steps:
1) coating a mixed dispersion liquid of a nano silver wire, modified cellulose and a surfactant on a transparent polymethacrylic resin film by a wire rod in a scraping way, and drying to prepare a nano silver wire conducting layer; the diameter of the nano silver wire is 10-100 nm;
2) manufacturing a patterned silk screen printing plate: silk-screen printing a patterned blocking layer on the surface of the nano silver wire conducting layer, wherein the blocking layer is composed of blocking agent transparent UV resin, the blocking layer is formed by UV lamp curing, a single-sided pressure sensitive adhesive tape is pasted at the position of an electrode outgoing line for protection, and the unmasked nano silver wire conducting layer forms a reaction area;
3) introducing mixed ozone gas by taking high-pressure air as carrier gas, heating the mixed gas by using a hot air spray gun, and blowing the surface of the conductive film, wherein the doping reaction temperature is 50 ℃, the overall conductivity is greatly reduced due to the oxidation doping reaction, and the silver wire can be broken at the position of a reaction point due to the stress in the nano silver wire; due to the protection effect of the barrier layer, the conducting layer below the barrier layer is not doped, so that the conductive layer has good conductivity;
4) and taking out after the doping reaction is finished, and removing the single-sided pressure sensitive adhesive tape to obtain the patterned transparent conductive electrode.
Various other modifications and changes may be made by those skilled in the art based on the above-described technical solutions and concepts, and all such modifications and changes should fall within the scope of the claims of the present invention.
Claims (8)
1. A preparation method of a transparent conductive electrode is characterized by comprising the following steps:
1) laying a nano metal conducting layer on the surface of a transparent base material;
2) carrying out graphical shielding on the nano metal conducting layer in the step 1) to form a blocking layer on the surface of the nano metal conducting layer, wherein the unmasked nano metal conducting layer forms a reaction area;
3) injecting impurity ions into the reaction area in the step 2), doping the nano metal conducting layer of the reaction area with the impurity ions to form a non-conducting area, and obtaining a transparent conducting electrode after the reaction is finished;
the impurity ions are any one or more of carbon, nitrogen, oxygen, boron, helium and phosphorus.
2. The method for preparing a transparent conductive electrode according to claim 1, wherein the method for disposing the nanometal conductive layer on the surface of the transparent substrate in the step 1) comprises: and depositing the nano metal dispersion liquid on the transparent substrate by coating or spraying to form a latticed conducting layer in a mutually overlapping mode.
3. The method for preparing the transparent conductive electrode according to claim 2, wherein the nano metal dispersion is a dispersion of one or more of elemental nano silver, nickel, copper, palladium, platinum, gold, cobalt, iron and aluminum.
4. The method of claim 2, wherein the nano metal dispersion is a dispersion of nano silver wires having a diameter of 10 to 100nm and a length of 5 to 100 μm.
5. The method for preparing a transparent conductive electrode according to claim 1, wherein the barrier layer in step 2) is any one or more of an ultraviolet radiation loss adhesive tape, a peelable adhesive, an easy-to-pull adhesive, and a single-sided pressure sensitive adhesive tape.
6. The method for preparing a transparent conductive electrode according to claim 1, wherein the barrier layer in step 2) comprises a barrier agent, and the barrier agent is removable ink, transparent resin or photoresist.
7. The method for preparing the transparent conductive electrode according to claim 6, wherein the barrier layer further comprises an auxiliary agent, and the auxiliary agent is any one or two of a permeation-resistant filler and an etching-resistant agent; the anti-permeation filler is any one or more of metal powder, metal oxide, carbon material, nano silicon dioxide, boron nitride and calcium carbonate, and the anti-etching agent is glucose or vitamin C.
8. The method of claim 1, wherein the barrier layer is formed by any one of screen printing, pad printing, gravure printing, lithography printing, letterpress printing, inkjet printing, hot stamping, thermal transfer printing, spraying, brushing, coating, patterned dispensing, patterned exposure and development, and lamination.
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| CN112191847B (en) * | 2020-09-22 | 2021-07-16 | 燕山大学 | Steel sample sintering forming method for artificially implanting inclusions |
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