CN110781600A - Nano-silver wire flexible transparent conductive film easy for electrode patterning and patterning method thereof - Google Patents
Nano-silver wire flexible transparent conductive film easy for electrode patterning and patterning method thereof Download PDFInfo
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- CN110781600A CN110781600A CN201911045579.2A CN201911045579A CN110781600A CN 110781600 A CN110781600 A CN 110781600A CN 201911045579 A CN201911045579 A CN 201911045579A CN 110781600 A CN110781600 A CN 110781600A
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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Abstract
The invention discloses a nano silver wire flexible transparent conductive film easy for electrode patterning and a patterning method thereof. The OC photoresist integrating the nano silver wire protection function and the developing solution corrosion resistance function and the developing etching solution integrating the developing OC photoresist and the etching lower nano silver wire function are matched, so that the process step of patterning the electrode of the flexible transparent conducting film of the nano silver wire through a yellow light process is greatly simplified, the production efficiency and the product yield are improved, and the OC photoresist is very suitable for manufacturing touch screens, OLEDs and Micro-LED electrode patterns in panel factories.
Description
Technical Field
The invention belongs to the field of nano-silver wire transparent conductive films, and particularly relates to a nano-silver wire flexible transparent conductive film easy for electrode patterning and a patterning method thereof.
Background
The transparent conductive film is widely applied to the fields of touch display screens, sensors, solar cells, light emitting diodes and the like as an important functional material. Indium Tin Oxide (ITO) has been widely used as a transparent conductive electrode for a long time because of its excellent conductivity, light transmittance and high stability, but ITO has some defects that are difficult to overcome, such as brittleness, difficulty in applying to the flexible touch field, shortage of metal indium resources, high price, high investment in magnetron sputtering equipment for ITO coating, and the like. Therefore, in recent years, materials such as conductive metal oxide, graphene, carbon nanotube, conductive polymer material and metal nanowire have been developed to replace ITO, wherein silver nanowire is considered to be the most likely transparent conductive material for replacing ITO in the future due to its good light transmittance, conductivity, flexibility and simple preparation process.
The application of the prior nano silver wire transparent conductive film in the field of touch control is mature day by day, and the main process steps comprise: and patterning the electrode of the nano silver wire conducting layer by utilizing a laser etching or yellow light process, then attaching the nano silver wire transparent conducting film to the optical transparent adhesive OCA, and then attaching the composite film to the liquid crystal display module or the OLED display module to manufacture the touch screen. The manufacturing of the conducting layer pattern is mature by applying a laser etching scheme, but the laser etching also has the problems of expensive processing equipment, long time consumption and the like at present. The yellow light process can be operated in a production line, and laser etching equipment is not required to be purchased, so that the yellow light process is particularly suitable for manufacturing electrode patterns in panel factories.
The production steps of electrode patterning of the nano silver wire conducting layer by the traditional yellow light process comprise: 1. coating a layer of photoresist on the surface of the silver nanowire conducting layer and drying; 2. carrying out local selective exposure on the photoresist by using a mask plate; 3. developing the exposed/non-exposed region of the photoresist by using a developing solution; 4. etching the exposed nano silver wire conducting layer by using etching liquid; 5. stripping the photoresist in the non-exposure/exposure area above the nano silver line by using a stripping liquid; 6. and coating a layer of OC protective resin on the surface of the nano silver wire conducting layer with the etched pattern. This step is very cumbersome.
Disclosure of Invention
The invention discloses a nano silver wire flexible transparent conductive film easy for electrode patterning and a patterning method thereof, aiming at providing an OC photoresist integrating the nano silver wire protection function and the developer corrosion resistance function and a matched developing etching solution integrating the developing OC photoresist and the etching lower nano silver wire function, so as to simplify the process steps of electrode patterning and improve the production efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention firstly discloses a flexible transparent conducting film of a nano silver wire, which is easy to pattern an electrode, and is characterized in that: the nano silver wire flexible transparent conductive film is characterized in that a nano silver wire conductive layer is arranged on the surface of a flexible substrate, and an OC photoresist layer is formed on the surface of the nano silver wire conductive layer by coating an OC photoresist;
the OC photoresist comprises the following components in parts by weight:
further, the light-cured resin is at least one of sartomer CN8007NS urethane acrylate, CN8011NS urethane acrylate, CN9010NS urethane acrylate and CN9110NS urethane acrylate.
Further, the developing resin is at least one of dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate and 2- (diisopropylamino) ethyl methacrylate with tertiary amino groups.
Further, the photoinitiator is at least one of 2-hydroxy-2 methyl-1-phenyl acetone, a photoinitiator 754 and a photoinitiator 1173.
Further, the leveling agent is a leveling agent BYK-333, purchased from Bick China Limited.
Further, the silver stabilizer is at least one of dodecyl mercaptan, hexadecyl mercaptan and octadecyl mercaptan.
Further, the solvent is at least one of butanone, ethyl acetate and ethylene glycol.
Further, the preparation method of the OC photoresist comprises the following steps: weighing the raw materials according to the proportion, firstly adding a solvent into the photocuring resin, stirring at the speed of 500r/min for 20-30 min, then adding the developing resin, the flatting agent, the silver stabilizer and the photoinitiator while stirring, and continuously stirring for 20min to obtain the OC photoresist.
The manufacturing method of the flexible transparent conducting film of the nano silver wire comprises the following steps: firstly, coating the nano silver wire conductive ink on the surface of a flexible transparent substrate, and then drying the flexible transparent substrate for 2min at 120-150 ℃ by using a tunnel furnace to prepare a nano silver wire conductive layer; and then coating a layer of OC photoresist on the surface of the nano silver wire conducting layer, drying for 2min under the vacuum condition of 0.1MPa, and baking for 2min at the temperature of 80-130 ℃ to form an OC photoresist layer, thus obtaining the nano silver wire flexible transparent conducting film which is stored in a dark place. The coating process can be a dimple coating process or a slit extrusion coating process. The nano silver wire conductive ink can be any conductive ink containing nano silver wires and used for manufacturing a conductive film.
The invention also discloses a method for patterning the electrode of the flexible transparent conducting film of the nano silver wire, which comprises the following steps:
(1) setting a mask plate according to the required electrode pattern, wherein a light-transmitting area of the mask plate corresponds to an electrode pattern area, and a non-light-transmitting area of the mask plate corresponds to a non-electrode pattern area which needs to be removed by etching;
then, exposing the lightproof and stored flexible transparent conductive film of the nano silver wires by using the mask plate through UV illumination;
preferably, the UV wavelength of the UV illumination is 340-380 nm, and the energy is 100-300 mJ/cm
2And the time is 30-60 s;
(2) soaking the exposed flexible transparent conductive film of the nano silver wire in a developing etching solution for 1-3 min to develop the OC photoresist of the non-exposure area, etching the conductive layer of the nano silver wire of the non-exposure area, and then cleaning and drying the conductive layer of the nano silver wire by deionized water to obtain the conductive layer of the nano silver wire and the OC photoresist layer after electrode patterning;
(3) carrying out post-baking on the nano silver wire flexible transparent conductive film after the electrode patterning, and/or carrying out UV curing under the protection of nitrogen so as to further improve the protection function of the OC photoresist layer, namely finishing the treatment; preferably, the post-baking is baking at 120-200 ℃ for 5 min.
Further, the pH value of the developing etching solution is 1-5, and the developing etching solution comprises the following components in parts by weight:
the developing etching solution is prepared by dissolving nitric acid and acetic acid in water, mixing uniformly, then sequentially adding hydrogen peroxide, ammonia water and ethanol, and mixing uniformly.
Compared with the prior art, the invention has the beneficial effects that:
the invention greatly simplifies the process steps of patterning the electrode of the flexible transparent conducting film of the nano silver wire by the yellow light process, improves the production efficiency and the product yield and is very suitable for manufacturing the electrode patterns of a touch screen, an OLED and a Micro-LED in a panel factory by providing the OC photoresist integrating the nano silver wire protection function (isolating external water vapor, oxygen-containing atmosphere and sulfur-containing atmosphere to protect the conducting layer of the nano silver wire) and the developing solution erosion resistance function (protecting the conducting layer of the nano silver wire below from erosion of the developing solution) and the developing etching solution integrating the developing OC photoresist and the etching function of the nano silver wire below.
Detailed Description
The present invention is described in detail below with reference to examples, which are carried out on the premise of the technical solution of the present invention, and detailed embodiments and specific procedures are given, but the scope of the present invention is not limited to the following examples.
The flexible substrate used in the following examples was a PET film.
Manufacturing method of flexible transparent conducting film of nano silver wire
The following examples and comparative examples used the following formulation of silver nanowire conductive ink:
0.13% of nano silver wire (WJAG 1);
0.2% of dispersing film-forming assistant (hydroxyethyl cellulose)
Deionized water 0ppm 99.67%
The preparation method comprises the following steps: deionized water, nano silver wire WJAG1 (wire diameter 20nm, length-diameter ratio 1000-.
Comparative example
The formulation of the UV protectant used in this example is as follows:
the preparation method comprises the following steps: weighing the raw materials according to the ratio, firstly adding a solvent into CN9010NS resin, stirring at the speed of 500r/min for 25min, then adding BYK-333 and a photoinitiator 1173 while stirring, and continuously stirring for 20min to obtain the UV protection solution.
The manufacturing method of the flexible transparent conductive film of the nano silver wire comprises the following steps:
(1) coating the nano silver wire conductive ink on the surface of a flexible transparent substrate by a micro-concave coating process, and then drying at 130 ℃ for 2min by using a tunnel furnace to obtain a nano silver wire conductive layer;
(2) coating a layer of UV protective solution on the surface of the silver nanowire conductive layer by a micro-concave coating process, drying under 0.1MPa vacuum for 2min, baking at 120 ℃ for 2min, and finally performing UV curing under the protection of nitrogen (the UV wavelength is 360nm, and the energy is 300 mJ/cm)
2And 10s), obtaining the flexible transparent conducting film of the nano silver wire.
Example 1
The OC photoresist formulation used in this example is as follows:
the preparation method comprises the following steps: weighing the raw materials according to the proportion, firstly adding a solvent into CN9010NS resin, stirring at the speed of 500r/min for 25min, then adding dimethylaminoethyl methacrylate, BYK-333, dodecyl mercaptan and a photoinitiator 1173 while stirring, and continuously stirring for 20min to obtain the OC photoresist.
The manufacturing method of the flexible transparent conductive film of the nano silver wire comprises the following steps:
(1) coating the nano silver wire conductive ink on the surface of a flexible transparent substrate by a micro-concave coating process, and then using a tunnel furnace
Drying at 130 ℃ for 2min to obtain a nano silver wire conductive layer;
(2) coating a layer of OC photoresist on the surface of the nano silver wire conducting layer by a micro-concave coating process, drying for 2min under the vacuum of 0.1MPa, and baking for 2min at the temperature of 120 ℃ to obtain the nano silver wire flexible transparent conducting film, and storing in a dark place.
Example 2
The OC photoresist formulation used in this example is as follows:
the preparation method comprises the following steps: weighing the raw materials according to the proportion, firstly adding a solvent into CN9010NS resin, stirring at the speed of 500r/min for 25min, then adding diethylaminoethyl methacrylate, BYK-333, dodecyl mercaptan and a photoinitiator 1173 while stirring, and continuously stirring for 20min to obtain the OC photoresist.
The manufacturing method of the flexible transparent conductive film of the nano silver wire comprises the following steps:
(1) coating the nano silver wire conductive ink on the surface of a flexible transparent substrate by a micro-concave coating process, and then drying at 130 ℃ for 2min by using a tunnel furnace to obtain a nano silver wire conductive layer;
(2) coating a layer of OC photoresist on the surface of the nano silver wire conducting layer by a micro-concave coating process, drying for 2min under the vacuum of 0.1MPa, and baking for 2min at the temperature of 120 ℃ to obtain the nano silver wire flexible transparent conducting film, and storing in a dark place.
Example 3
The OC photoresist formulation used in this example is as follows:
the preparation method comprises the following steps: weighing the raw materials according to the proportion, firstly adding a solvent into CN9010NS resin, stirring at the speed of 500r/min for 25min, then adding 2- (diisopropylamino) ethyl methacrylate, BYK-333, dodecyl mercaptan and a photoinitiator 1173 while stirring, and continuously stirring for 20min to obtain the OC photoresist.
The manufacturing method of the flexible transparent conductive film of the nano silver wire comprises the following steps:
(1) coating the nano silver wire conductive ink on the surface of a flexible transparent substrate by a micro-concave coating process, and then drying at 130 ℃ for 2min by using a tunnel furnace to obtain a nano silver wire conductive layer;
(2) coating a layer of OC photoresist on the surface of the nano silver wire conducting layer by a micro-concave coating process, drying for 2min under the vacuum of 0.1MPa, and baking for 2min at the temperature of 120 ℃ to obtain the nano silver wire flexible transparent conducting film, and storing in a dark place.
For testing the performance, the conductive film obtained in each of the above examples was UV-cured under nitrogen (UV wavelength of 360nm, energy of 300 mJ/cm)
210s) to compare the performance of the conductive film obtained in each example after exposure in subsequent electrode patterning, with the performance of the existing flexible transparent conductive film structure for nano-silver wires provided in the comparative example. The results are shown in Table 1.
Table 1: comparison of Performance of conductive films obtained in comparative example and examples
As can be seen from table 1, the OC photoresist layer in the flexible transparent conductive film of silver nanowires of the present invention does not affect the performance of the conductive film.
Electrode patterning of nano silver wire flexible transparent conductive film
The formula of the developing etching solution used in the embodiment is as follows, and the pH value is 2:
the preparation method comprises the following steps: dissolving nitric acid and acetic acid in water, mixing uniformly, then adding hydrogen peroxide, ammonia water and ethanol in sequence, and mixing uniformly to obtain the developing etching solution.
The method for patterning the electrode of the flexible transparent conductive film of the nano-silver wire obtained in the above embodiments 1 to 3 is as follows:
(1) setting a mask plate according to the required electrode pattern, wherein a light-transmitting area of the mask plate corresponds to an electrode pattern area, and a non-light-transmitting area of the mask plate corresponds to a non-electrode pattern area which needs to be etched and removed;
then, using a mask, UV light (UV wavelength of 360nm, energy of 200 mJ/cm)
2And the time is 40s), exposing the nanometer silver wire flexible transparent conducting film which is stored in a dark place;
(2) soaking the exposed flexible transparent conductive film of the nano silver wire in a developing etching solution for 2min to develop the OC photoresist of the non-exposure area, etching the conductive layer of the nano silver wire of the non-exposure area, and then washing and drying the conductive layer of the nano silver wire by deionized water to obtain the conductive layer of the nano silver wire and the OC photoresist layer after electrode patterning;
(3) carrying out UV curing on the nano silver wire flexible transparent conductive film after the electrode patterning under the protection of nitrogen (the UV wavelength is 360nm, and the energy is 300 mJ/cm)
210s) to further enhance the protective function of the OC photoresist layer, i.e., to complete the treatment.
The nano silver wire conducting layer obtained by the method after electrode patterning has clear and sharp edges, no OC photoresist residues and nano silver wire residues, and the developing precision can reach 1 mu m. The patterning method greatly simplifies the process steps of patterning the electrode on the flexible transparent conducting film of the nano silver wire by the yellow light process, and improves the production efficiency and the product yield.
The present invention is not limited to the above exemplary embodiments, and any modifications, equivalent replacements, and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a flexible transparent conducting film of nanometer silver line of easy electrode patterning which characterized in that: the nano silver wire flexible transparent conductive film is characterized in that a nano silver wire conductive layer is arranged on the surface of a flexible substrate, and an OC photoresist layer is formed on the surface of the nano silver wire conductive layer by coating an OC photoresist;
the OC photoresist comprises the following components in parts by weight:
2. the flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the light-cured resin is at least one of sandomar CN8007NS urethane acrylate, CN8011NS urethane acrylate, CN9010NS urethane acrylate and CN9110NS urethane acrylate.
3. The flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the developing resin is at least one of dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate and 2- (diisopropylamino) ethyl methacrylate.
4. The flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the photoinitiator is at least one of 2-hydroxy-2 methyl-1-phenyl acetone, a photoinitiator 754 and a photoinitiator 1173.
5. The flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the leveling agent is a leveling agent BYK-333.
6. The flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the silver stabilizer is at least one of dodecyl mercaptan, hexadecyl mercaptan and octadecyl mercaptan.
7. The flexible transparent conductive film for nanosilver wires susceptible to electrode patterning according to claim 1, characterized in that: the solvent is at least one of butanone, ethyl acetate and ethylene glycol.
8. A method for patterning electrodes of the flexible transparent conductive film with the nano-silver wires as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) setting a mask plate according to the required electrode pattern, wherein a light-transmitting area of the mask plate corresponds to an electrode pattern area, and a non-light-transmitting area of the mask plate corresponds to a non-electrode pattern area which needs to be removed by etching;
then, exposing the lightproof and stored flexible transparent conductive film of the nano silver wires by using the mask plate through UV illumination;
(2) soaking the exposed flexible transparent conductive film of the nano silver wire in a developing etching solution for 1-3 min to develop the OC photoresist of the non-exposure area, etching the conductive layer of the nano silver wire of the non-exposure area, and then cleaning and drying the conductive layer of the nano silver wire by deionized water to obtain the conductive layer of the nano silver wire and the OC photoresist layer after electrode patterning;
(3) and (3) post-baking the nano silver wire flexible transparent conductive film after the electrode patterning, and/or carrying out UV curing under the protection of nitrogen so as to further improve the protection function of the OC photoresist layer, namely finishing the treatment.
9. The method of claim 8, wherein: the pH value of the developing etching solution is 1-5, and the developing etching solution comprises the following components in parts by weight:
40-60 parts of a solvent consisting of water and ethanol in a mass ratio of 1: 1.
10. The method of claim 8, wherein: in the step (3), the post-baking is carried out for 5min at 120-200 ℃.
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| CN113488287A (en) * | 2021-07-22 | 2021-10-08 | 苏州诺菲纳米科技有限公司 | Method for reducing etching trace of nano silver wire conductive film |
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