CN107557787B - Etching solution for nano-silver conductive film and preparation method of patterned nano-silver conductive film - Google Patents
Etching solution for nano-silver conductive film and preparation method of patterned nano-silver conductive film Download PDFInfo
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Abstract
The invention provides an etching solution for a nano silver conductive film, which comprises the following components: 1-30 parts of an etchant, 70-90 parts of a solvent and 0-10 parts of an additive, wherein the etchant has no direct oxidation to silver at normal temperature and can be complexed with silver ions; therefore, the etching solution only cuts off the conductive network in the etching area, but does not etch the area, so that the conductive action of the nano silver conductive film in the etching area disappears while the etching trace is reduced, and the difference between the shapes of the etching area and the non-etching area is small, thereby the optical characteristics are basically consistent.
Description
Technical Field
The invention relates to a preparation method of a transparent conductive film, in particular to an etching solution for a nano-silver conductive film and a preparation method of a patterned nano-silver conductive film.
Background
The nano-silver transparent conductive film has flexible characteristics, so that the nano-silver transparent conductive film has wide application in the fields of flexible display, touch sensors, solar cells, wearable equipment and the like. In the above application, a patterning process is required for the nano silver conductive film, and a common process includes: laser etching, screen printing of etching paste, etc.
The laser etching process is a common process, and functional patterns are prepared by a laser machine after silver paste is printed; however, the laser etching equipment is expensive, the efficiency is low, the operation is limited by the size problem of a laser machine, and only the patterning of a single-sided conductive film can be prepared. The screen printing process comprises the working procedures of printing, baking, washing and the like of etching paste; the functional pattern can be prepared only by baking and triggering for a long time after the paste is printed and etched, the adjustable window of the baking condition and the appearance effect of the process is small, and the efficiency is only higher than that of laser etching. These two processes can only work on a single sheet, and cannot implement roll-to-roll operations like the yellow light process. Therefore, it is highly desirable to develop an etching process with higher efficiency.
In view of the above, it is desirable to provide an etching solution based on a nano silver conductive film and a patterning preparation method thereof to solve the above problems.
Disclosure of Invention
The invention aims to provide an etching solution for a nano silver conductive film and a preparation method of a patterned nano silver conductive film.
In order to achieve the above object, the present invention provides an etching solution for a nano silver conductive film, comprising: 1-30 parts of an etchant, 70-90 parts of a solvent and 0-10 parts of an additive, wherein the etchant has no direct oxidation to silver at normal temperature and can be complexed with silver ions.
As a further improvement of the invention, the etchant is at least one of thiocyanic acid and salts thereof, thiocyanate, isothiocyanic acid and salts thereof, isothiocyanate, long-chain polyol, sulfide and polyamine.
As a further improvement of the invention, the solvent is at least one of ethylene glycol, deionized water, methanol and ethanol.
As a further improvement of the invention, the additive is at least one of a surfactant, a pH regulator and a defoaming agent.
As a further improvement of the invention, the surfactant is at least one of dioctyl sodium sulfosuccinate, sodium octadecyl sulfate, sodium dodecyl sulfate and stearic acid.
In order to achieve the above object, the present invention further provides a method for preparing a patterned nano silver conductive film, comprising the following steps: preparing a patterned protective layer on the nano silver conductive film; soaking the nano silver conductive film with the protective layer in the etching solution, and standing for 10-1000 s at normal temperature; taking the nano silver conductive film out of the etching solution, placing the nano silver conductive film in UV equipment to trigger the etching solution, and etching the area which is not protected by the protective layer; and cleaning the residual etching solution and the protective layer after the etching is finished to form the patterned nano silver conductive film.
As a further improvement of the invention, the protective layer is formed of ink, sapphire, photoresist or peelable glue.
In order to achieve the above object, the present invention further provides a method for preparing a patterned nano silver conductive film, comprising the following steps: soaking a nano silver conductive film in the etching solution of any one of claims 1 to 5, and standing for 10 to 1000 seconds at normal temperature; taking the nano silver conductive film out of the etching solution, placing the nano silver conductive film in UV equipment with a preset patterned film to trigger the etching solution, etching the nano silver conductive film corresponding to the light-transmitting area of the film, and not etching the nano silver conductive film corresponding to the non-light-transmitting area of the film; and cleaning the residual etching solution after the etching is finished to form the patterned nano silver conductive film.
In order to achieve the above object, the present invention further provides a method for preparing a patterned nano silver conductive film, comprising the following steps: adding the etching solution of any one of claims 1 to 5 into a nano-silver coating solution, and forming a nano-silver conductive film on a substrate from the nano-silver coating solution; placing the nano-silver conductive film in UV equipment with a preset patterned film to trigger etching liquid, etching the nano-silver conductive film corresponding to the light transmission area of the film, and not etching the nano-silver conductive film corresponding to the non-light transmission area of the film; and forming a patterned nano silver conductive film.
As a further improvement of the invention, the time for triggering the etching solution by the UV equipment is 10S-1000S.
The invention has the beneficial effects that: the etchant for the nano-silver conductive film has no direct oxidability to silver at normal temperature and can be complexed with silver ions, and can cut off the conductive network of the nano-silver conductive film instead of etching a large area after being heated in air or irradiated by UV light; therefore, the etching solution only cuts off the conductive network in the etching area, but does not etch the area, so that the conductive action of the nano silver conductive film in the etching area disappears while the etching trace is reduced, and the difference between the shapes of the etching area and the non-etching area is small, thereby the optical characteristics are basically consistent.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail below with reference to specific embodiments.
The etching solution based on the nano silver conductive film comprises the following components: 1-30 parts of etchant, 70-90 parts of solvent and 0-10 parts of additive; the etchant has no direct oxidation to silver at normal temperature and can be complexed with silver ions, but can cut off the conductive network of the nano silver conductive film after heating or UV light irradiation, rather than etch away a large area. In addition, the etching speed can be regulated and controlled through temperature or UV light irradiation, and the reaction degree can be regulated and controlled through reaction time.
The etchant is at least one of thiocyanic acid and salts thereof, thiocyanate, isothiocyanic acid and salts thereof, isothiocyanate, long-chain polyol, sulfide and polyamine. Although the etchant cannot react with silver at normal temperature, the silver is oxidized by an oxygen source in the environment when the etchant is heated or irradiated by UV light, the etchant is complexed with silver ions to cut off a conductive network in an etching area, the etching area is not etched in a large area, the etching trace is reduced, and meanwhile, the conductive action of a nano silver conductive film in the etching area disappears, so that the shape difference between the etching area and a non-etching area is small, and the optical characteristics are basically consistent.
Common thiocyanates include methyl thiocyanate, methyl dithiocyanate, phenyl thiocyanate, and the like. Isothiocyanates and salts thereof, isothiocyanates, where the group R coordinated to N is an alkyl group, such as: allyl isothiocyanate, 2-N, N-dimethyl-2, 3-dithiocyano propylamine and the like, and common isothiocyanates are: sulforaphane, allyl isothiocyanate, benzyl isothiocyanate, phenethyl isothiocyanate, etc.
Taking the conductive film formed by the silver nanowires as an example, the etchant cuts off partial areas of the silver nanowires, but more than 90% of the silver nanowires are reserved, and the nano silver is not etched in a large area, so that the difference between the shapes of the nanowires in the etched area and the nanowires in the non-etched area is small, the optical characteristics of the two areas are basically consistent, and the difference between the electricity of the two areas is large.
The solvent is at least one of ethylene glycol, deionized water, methanol and ethanol.
The additive is at least one of a surfactant, a pH regulator and a defoaming agent.
The surfactant is at least one of dioctyl sodium sulfosuccinate, sodium octadecyl sulfate, sodium dodecyl sulfate and stearic acid.
The etching solution and the preparation method thereof of the present invention are described below with reference to specific examples:
example 1: the etching solution comprises 10 parts of propane diamine, 70 parts of deionized water, 10 parts of ethylene glycol and 10 parts of surfactant. Wherein, the propane diamine is used as an etchant, the deionized water is used as a solvent, and the ethylene glycol has the moisture-preserving function and can reduce the volatility of the etching solution.
The preparation method of the etching solution comprises the following steps: at normal temperature and normal pressure, uniformly stirring and dispersing the propane diamine, the deionized water, the ethylene glycol and the surfactant to obtain the etching solution with the etching function.
Example 2: the etching solution comprises 5 parts of sodium sulfide, 80 parts of deionized water and 5 parts of pH regulator, wherein the sodium sulfide is used as an etching agent, and the deionized water is used as a solvent.
The preparation method of the etching solution comprises the following steps: and stirring and uniformly dispersing sodium sulfide, deionized water and a pH regulator at normal temperature and normal pressure to obtain the etching solution with the etching function.
Example 3: the etching solution comprises 10 parts of thiocyanate, 80 parts of deionized water and 10 parts of ethylene glycol. The thiocyanate serves as an etchant, the deionized water serves as a solvent, and the ethylene glycol has a moisturizing effect and can reduce the volatility of the etching solution.
The preparation method of the etching solution comprises the following steps: under normal temperature and pressure, the thiocyanate, the deionized water, the glycol and the surfactant are stirred and uniformly dispersed to obtain the etching solution with the etching function.
Example 4: the etching solution comprises 20 parts of polyethylene glycol-600 and 80 parts of deionized water. Wherein, the polyethylene glycol-600 is used as an etchant, and the deionized water is used as a solvent.
The preparation method of the etching solution comprises the following steps: and (3) stirring and uniformly dispersing the polyethylene glycol-600, the deionized water and the surfactant at normal temperature and normal pressure to obtain the etching solution with the etching function.
The invention also provides a method for preparing the patterned transparent conductive film by using the etching solution, which comprises triggering the etching solution in a specific etching area by using a protective layer with a specific pattern or UV light emitted by a UV device from a film, cutting off the conductive network of the nano-silver conductive film in the etching area, and not completely etching the nano-silver conductive film, so that the etching trace in the etching area is small, the shape difference between the etching area and the non-etching area is small, the optical performance is basically consistent, but the difference of the electrical performance is large.
According to the method, a key process of patterning the nano-silver conductive film can be realized through one UV device, and the problems of small process window and low laser etching efficiency of screen printing etching paste triggering etching performance-low etching mark appearance effect balance are solved in actual production.
A method for preparing a patterned nano-silver conductive film using the above nano-silver conductive film-based etching solution will be specifically described below.
The method comprises the following steps: preparing a patterned protective layer on the nano-silver conductive film, specifically arranging one of patterned ink, blue resist, photoresist or peelable glue on the nano-silver conductive film to form the protective layer capable of preventing the etching solution from etching the nano-silver conductive film; soaking the nano silver conductive film with the protective layer in the etching solution, and standing for 10-1000 s at normal temperature; taking the nano silver conductive film out of the etching solution, draining the etching solution on the surface, placing the nano silver conductive film in UV equipment for 10-1000 s, and triggering the etching solution by UV light to etch an unprotected area; and after the etching is finished, cleaning the protective layer and the residual etching solution to form the patterned nano-silver conductive film with the specific conductive pattern area. UV light irradiation promotes the speed of oxidation of the silver nanowires, and the etching speed is accelerated.
The second method comprises the following steps: soaking the nano silver conductive film in the etching solution, and standing for 10-1000 s at normal temperature; taking the nano silver conductive film out of the etching solution, draining the etching solution on the surface, and placing the nano silver conductive film in UV equipment with a preset patterned film for 10-1000 s; triggering the etching solution by UV light, etching the nano silver conductive film corresponding to the light-transmitting area of the film, and not etching the nano silver conductive film corresponding to the non-light-transmitting area of the film; and cleaning the residual etching solution after the etching is finished to form the patterned nano silver conductive film with the specific conductive pattern area.
The third method comprises the following steps: adding the etching solution into the nano-silver coating solution, and forming a nano-silver conductive film on the substrate by using the nano-silver coating solution; placing the nano-silver conductive film in UV equipment with a preset patterned film for 10-1000 s, preferably for 30-1000 s, triggering the etching solution by UV light, etching the nano-silver conductive film corresponding to the light-transmitting area of the film, and not etching the nano-silver conductive film corresponding to the non-light-transmitting area of the film; thereby forming a patterned nano silver conductive film.
In summary, the etchant of the etching solution of the present invention does not have an oxidation property to silver at room temperature, and does not etch the nano-silver conductive film at room temperature and normal pressure, after the UV light is triggered, the etchant cuts off the conductive network in the etching area, and does not etch a large area, so that the etching trace is reduced, and the conductive function of the nano-silver conductive film in the etching area is eliminated.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (8)
1. An etching solution for a nano silver conductive film is characterized in that: the method comprises the following steps: the etching agent is characterized by comprising, by weight, 1-30 parts of an etching agent, 70-90 parts of a solvent and 0-10 parts of an additive, wherein the etching agent does not have direct oxidation on silver at normal temperature and can be complexed with silver ions, the etching agent is at least one of thiocyanic acid and salts thereof, thiocyanate, isothiocyanic acid and salts thereof, isothiocyanate, long-chain polyol, sulfide and polyamine, and the solvent is at least one of ethylene glycol, deionized water, methanol and ethanol.
2. The etching solution according to claim 1, wherein: the additive is at least one of a surfactant, a pH regulator and a defoaming agent.
3. The etching solution according to claim 2, wherein: the surfactant is at least one of dioctyl sodium sulfosuccinate, sodium octadecyl sulfate, sodium dodecyl sulfate and stearic acid.
4. A preparation method of a patterned nano-silver conductive film is characterized by comprising the following steps:
preparing a patterned protective layer on the nano silver conductive film;
soaking a nano silver conductive film with a protective layer in the etching solution of any one of claims 1 to 3, and standing for 10 to 1000s at normal temperature;
taking the nano silver conductive film out of the etching solution, placing the nano silver conductive film in UV equipment to trigger the etching solution, and etching the area which is not protected by the protective layer;
and cleaning the residual etching solution and the protective layer after the etching is finished to form the patterned nano silver conductive film.
5. The method of claim 4, wherein the patterned nanosilver conductive film comprises: the protective layer is formed of ink, sapphire, photoresist, or peelable glue.
6. A preparation method of a patterned nano-silver conductive film is characterized by comprising the following steps:
soaking a nano silver conductive film in the etching solution of any one of claims 1 to 3, and standing for 10 to 1000 seconds at normal temperature;
taking the nano silver conductive film out of the etching solution, placing the nano silver conductive film in UV equipment with a preset patterned film to trigger the etching solution, etching the nano silver conductive film corresponding to the light-transmitting area of the film, and not etching the nano silver conductive film corresponding to the non-light-transmitting area of the film;
and cleaning the residual etching solution after the etching is finished to form the patterned nano silver conductive film.
7. A preparation method of a patterned nano-silver conductive film is characterized by comprising the following steps:
adding the etching solution of any one of claims 1 to 3 into a nano-silver coating solution, and forming a nano-silver conductive film on a substrate by using the nano-silver coating solution;
placing the nano-silver conductive film in UV equipment with a preset patterned film to trigger etching liquid, etching the nano-silver conductive film corresponding to the light transmission area of the film, and not etching the nano-silver conductive film corresponding to the non-light transmission area of the film; and forming a patterned nano silver conductive film.
8. The method for preparing a patterned nanosilver conductive film according to any one of claims 4 to 7, wherein: the time for triggering the etching solution by the UV equipment is 10-1000S.
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| KR102659176B1 (en) | 2020-12-28 | 2024-04-23 | 삼성디스플레이 주식회사 | Etching composition for thin film containing silver, method for forming pattern and method for manufacturing a display device using the same |
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Effective date of registration: 20210114 Address after: 215300 unit B, 1st floor, No.5 factory building, Xinxing Industrial Square, 78 Xinglin street, Suzhou Industrial Park, Jiangsu Province Patentee after: NUOVO FILM Inc. Patentee after: SHENZHEN OUPODA TECHNOLOGY Co.,Ltd. Address before: 215300 unit B, 1st floor, No.5 factory building, Xinxing Industrial Square, 78 Xinglin street, Suzhou Industrial Park, Jiangsu Province Patentee before: NUOVO FILM Inc. |