CN110629222A - Etching method of nano silver wire transparent conductive film with shadow eliminating function - Google Patents
Etching method of nano silver wire transparent conductive film with shadow eliminating function Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/02—Local etching
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/12—Gaseous compositions
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Abstract
The invention discloses a method for etching a nano silver wire transparent conductive film with a shadow eliminating function. The method has the advantages that the etching process is controlled, so that most of the etching area is kept while the etching area is not conductive, the haze difference between the etching area and the non-etching area is reduced, and the shadow eliminating purpose is achieved.
Description
Technical Field
The invention relates to a novel etching method of a nano silver wire transparent conductive film with a shadow eliminating function.
Background
The transparent conductive film is an important optical device in the display field, and the ITO transparent conductive film is most widely applied at present. However, ITO transparent conductive films have the disadvantages of poor bending performance, high sheet resistance, complex vacuum sputtering process for film preparation, and the like, so in recent years, related research and development workers have developed novel transparent conductive films such as nano metal conductive films, carbon nanotube conductive films, graphene films, and the like which replace ITO transparent conductive films in succession, wherein the nano silver wire transparent conductive films become the most effective substitute materials for ITO conductive films due to excellent performance, low cost, and simple preparation process.
As an important optical device applied to the fields of displays, touch screens and the like, a nano silver wire transparent conductive film usually needs to be etched, and the etched transparent conductive film is divided into an electrode region (non-etching region) and a non-electrode region (etching region). At present, the etching process of the nano silver wire transparent conductive film mainly comprises laser etching and exposure development, wherein: the laser etching efficiency is low, the equipment cost is high, and the etching mark of the prepared conductive film is serious; the exposure and development efficiency is high, but the problem of serious etching marks is existed like laser etching. If the etching mark is serious, a large haze difference exists between the electrode area and the non-electrode area of the etched transparent conductive film, so that the electrode area boundary can be observed by naked eyes. If the transparent conductive film is directly applied to a display screen, the visual effect of the touch screen is reduced, so that the transparent conductive film needs to be subjected to shadow elimination treatment to eliminate the visibility of the edge of the electrode area by naked eyes.
Disclosure of Invention
In order to avoid the defects of the prior art, the invention provides the method for etching the nano silver wire transparent conductive film, which is simple to operate and high in efficiency, and aims to enable the etched conductive film to have a shadow eliminating function.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for etching a nano silver wire transparent conductive film with a shadow eliminating function is characterized by comprising the following steps:
(1) arranging a photosensitive adhesive layer on the surface of the nano silver wire transparent conductive film and patterning the photosensitive adhesive layer, wherein the formed patterned photosensitive adhesive layer comprises a complete transmission area (namely a non-adhesive area) and a complete shielding area (namely an adhesive area); the complete transmission area corresponds to an etching area of the conductive film, and the complete shielding area corresponds to a non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then, introducing an etching medium into the etching cavity to etch the conductive film;
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by alkali washing, and then washing and drying to obtain the patterned nano silver wire transparent conductive film with the shadow eliminating function.
Further, in the step (1), the method for disposing a photosensitive adhesive layer on the surface of the silver nanowire transparent conductive film and patterning the photosensitive adhesive layer comprises: coating photosensitive glue on the surface of the conductive film and drying the conductive film, or directly pasting film-shaped photosensitive glue on the surface of the conductive film, then covering a mask plate provided with a required pattern on the surface of the photosensitive glue, and exposing and developing to form a patterned photosensitive glue layer; or directly printing photosensitive glue on the surface of the conductive film through gravure printing and drying to form the patterned photosensitive glue layer. Further, the method comprises the following steps: the photosensitive glue can be positive photosensitive glue or negative photosensitive glue; the mask can be a film sheet or a chromium plate. Furthermore, the developing solution used for developing is NaOH aqueous solution or KOH aqueous solution with the mass concentration of 0.1-1 wt%.
Further, in the step (2), the etching medium is a physical etching medium or a reactive etching medium. Further, the method comprises the following steps: the physical etching medium is oxygen, helium, nitrogen, argon or hydrogen; the reactive etching medium is HCl, HBr, HI and H2S、BCl3、SF6、CF4、Cl2、Br2Or I2。
Further, in the step (2), the etching conditions are as follows: the temperature of the etching cavity is 40-90 ℃, the pressure of the etching cavity is 10-100Mpa, the frequency of the alternating voltage is not lower than 10KHz, and the etching time is 1s-10 s.
Further, in the step (3), the alkali liquor used for alkali washing is NaOH aqueous solution or KOH aqueous solution with the mass concentration of 3-10 wt%.
Further, in the step (3), the drying temperature is 80-120 ℃ and the drying time is 20-60 s.
The etching method of the invention can prepare the nano silver wire transparent conductive film with the shadow eliminating function, and the principle is as follows: at present, the common structure of the nano silver wire transparent conductive film is a conductive layer and a protective layer, the protective layer is obtained by curing different kinds of resin, has high crosslinking degree, is not a completely compact structure, and has certain permeability. After the etching medium is treated by the plasma, the components comprise various steam, molecules, electrons, ions, free radicals and the like, so that the surface plasma concentration is increased, and the etching medium has certain permeability; the etching medium reacts with the nano silver wire preferentially, so that the etching medium can not only corrode the nano silver wire exposed on the surface of the conductive film, but also directly permeate into the etching area of the conductive film to corrode the nano silver wire, so that the etching area is changed from conducting to non-conducting. By controlling the etching time, the main components of the etched area are still remained at the original position after the etched area becomes non-conductive, so that the haze difference between the etched area and the non-etched area is small and invisible to naked eyes, and the purpose of shadow elimination is achieved.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the etching method, most of the etching area is kept while the etching area is not conductive, so that the haze difference between the etching area and the non-etching area is reduced, and the purpose of shadow elimination is achieved;
2. the etching condition of the invention is lower than the requirement of the semiconductor field, and the invention is easy to realize the industrial production.
Drawings
FIG. 1 is a graph showing the effect of comparative example 1 after wet etching;
FIG. 2 is a graph showing the effects of example 1 after plasma etching;
FIG. 3 is an enlarged view of an etched area after plasma etching in example 1.
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 operation procedures are given, but the scope of the present invention is not limited to the following examples.
The conductive films used in the following examples are all the w jf25 type conductive films (for better observation of the shadow-eliminating performance, a low sheet resistance type conductive film with slightly high haze, which is 1.8% of the haze of the w jf25 conductive film) of co-fertilizer microcrystalline material science and technology ltd.
The method for judging the etching traces in the following examples is as follows: and (3) visually observing whether the boundary of the etching area and the non-etching area of the patterned conductive film has etching marks or testing the haze of the etching area and the non-etching area, and calculating the haze difference (the haze of the etching area can be tested by etching the whole conductive film, the haze of the non-etching area is the haze of the conductive film, and the larger the haze difference between the etching area and the non-etching area is, the more serious the visual etching marks are).
Comparative example 1
In the comparative example, the etching treatment is performed on the transparent conductive film of the nano silver wire by wet etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) soaking the conductive film with the patterned photosensitive adhesive layer in an acid solution (the mass ratio of water, 36.5 wt% of hydrochloric acid and 65-68 wt% of nitric acid is 15: 15: 4) to perform acid-washing etching;
(3) and after etching, removing the patterned photosensitive adhesive layer on the surface by alkaline washing with 5 wt% NaOH aqueous solution, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Example 1
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then, introducing an etching medium argon into the etching cavity, and etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 1.5 s);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Example 2
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then introducing an etching medium H into the etching chamber2S, steam is used for etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 1.5S);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Example 3
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then introducing an etching medium I into the etching chamber2Steam is used for etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 1.5 s);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Example 4
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then introducing an etching medium I into the etching chamber2Steam is used for etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 5 s);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Comparative example 2
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then introducing an etching medium I into the etching chamber2Steam is used for etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 15 s);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
Comparative example 3
In this embodiment, the etching process is performed on the transparent conductive film of the silver nanowire by plasma etching, and the steps are as follows:
(1) laminating a film-shaped photosensitive adhesive (Hitachi chemical PH-2325) on the surface of the WJF25 conductive film by using a film laminating machine; covering a film with a required pattern on the surface of the photosensitive glue layer, and carrying out UV parallel light irradiation by using an exposure machine; then removing the film on the surface of the photosensitive glue layer, and developing by using 0.7 wt% of NaOH aqueous solution to form a patterned photosensitive glue layer;
the patterned photosensitive glue layer comprises a complete transmission area and a complete shielding area; the completely transparent area corresponds to the etching area of the conductive film, and the completely shielding area corresponds to the non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then introducing an etching medium I into the etching chamber2Steam is used for etching the conductive film (the etching temperature is 50 ℃, the etching cavity pressure is 50MPa, the alternating voltage frequency is 20KHz, and the etching time is 30 s);
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by using 5 wt% of NaOH aqueous solution through alkaline washing, then washing with water for 10s, and drying at 100 ℃ for 30s to obtain the patterned nano silver wire transparent conductive film.
The etching conditions and the performance ratio of the patterned transparent conductive film with silver nanowires obtained in the above examples and comparative examples are shown in table 1.
Table 1: comparison of comparative and example Performance
From the comparison of the comparative examples and the examples, it can be seen that: after wet etching, the haze difference between an etching area and a non-etching area of the conductive film is large, and etching marks at the boundary are obvious; different etching media are used for plasma etching, etching time is controlled, etching marks at the boundary of an etched area and a non-etched area of the conductive film after etching are not obvious, the haze difference between the etched area and the non-etched area is increased along with the prolonging of the etching time, the etching marks are more and more obvious, and therefore the etching process needs to be controlled.
The above-described embodiments are only a few examples of the present invention, and do not limit the present invention in any way, and all persons skilled in the art can make modifications or changes to the present invention by using the methods and technical contents shown above without departing from the technical scope of the present invention; however, any modification or modification of the above embodiments is within the scope of the present invention, which does not depart from the technical scope of the present invention.
Claims (8)
1. A method for etching a nano silver wire transparent conductive film with a shadow eliminating function is characterized by comprising the following steps:
(1) arranging a photosensitive adhesive layer on the surface of the nano silver wire transparent conductive film and patterning the photosensitive adhesive layer, wherein the formed patterned photosensitive adhesive layer comprises a complete transmission area and a complete shielding area; the complete transmission area corresponds to an etching area of the conductive film, and the complete shielding area corresponds to a non-etching area of the conductive film;
(2) transferring the conductive film with the patterned photosensitive adhesive layer into a plasma etching cavity, and vacuumizing; then, introducing an etching medium into the etching cavity to etch the conductive film;
(3) and conveying the etched conductive film out of the plasma etching cavity, removing the patterned photosensitive adhesive layer on the surface by alkali washing, and then washing and drying to obtain the patterned nano silver wire transparent conductive film with the shadow eliminating function.
2. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 1, wherein: in the step (1), the method for arranging the photosensitive adhesive layer on the surface of the nano silver wire transparent conductive film and patterning the photosensitive adhesive layer comprises the following steps:
coating photosensitive glue on the surface of the conductive film and drying the conductive film, or directly pasting film-shaped photosensitive glue on the surface of the conductive film, then covering a mask plate provided with a required pattern on the surface of the photosensitive glue, and exposing and developing to form a patterned photosensitive glue layer;
or directly printing photosensitive glue on the surface of the conductive film through gravure printing and drying to form the patterned photosensitive glue layer.
3. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 2, characterized in that: the developing solution used for developing is NaOH aqueous solution or KOH aqueous solution with the mass concentration of 0.1-1 wt%.
4. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 1, wherein: in the step (2), the etching medium is a physical etching medium or a reactive etching medium.
5. The method for etching the silver nanowire transparent conductive film with the shadow eliminating function according to claim 4, wherein the etching process comprises the steps of; the physical etching medium is oxygen, helium, nitrogen, argon or hydrogen; the reactive etching medium is HCl, HBr, HI and H2S、BCl3、SF6、CF4、Cl2、Br2Or I2。
6. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 1, wherein: in the step (2), the etching conditions are as follows: the temperature of the etching cavity is 40-90 ℃, the pressure of the etching cavity is 10-100Mpa, the frequency of the alternating voltage is not lower than 10KHz, and the etching time is 1s-10 s.
7. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 1, wherein: in the step (3), the alkali liquor used for alkali washing is NaOH aqueous solution or KOH aqueous solution with the mass concentration of 3-10 wt%.
8. The method for etching a transparent conductive film with a silver nanowire having a shadow-eliminating function according to claim 1, wherein: in the step (3), the drying temperature is 80-120 ℃ and the drying time is 20-60 s.
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Cited By (1)
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| CN112309634A (en) * | 2020-09-24 | 2021-02-02 | 苏州思尔维纳米科技有限公司 | Etching mark optimization method and conductive film |
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