CN108008606B - Stripping liquid for photosensitive dry film and production method and application thereof - Google Patents
Stripping liquid for photosensitive dry film and production method and application thereof Download PDFInfo
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- CN108008606B CN108008606B CN201711420013.4A CN201711420013A CN108008606B CN 108008606 B CN108008606 B CN 108008606B CN 201711420013 A CN201711420013 A CN 201711420013A CN 108008606 B CN108008606 B CN 108008606B
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- stripping
- dry film
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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
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
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- General Physics & Mathematics (AREA)
- Photosensitive Polymer And Photoresist Processing (AREA)
- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
- Manufacturing Of Printed Circuit Boards (AREA)
Abstract
The invention discloses a photosensitive dry filmThe stripping solution comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.4-1.25mol/L, the content of inorganic alkali is 0.5-2g/L, and the adding volume of the organic alkali accounts for 2-5% of the stripping liquid. The invention takes organic base as a main component for stripping the film to react with a dry film polymer, and simultaneously, a certain amount of inorganic base component is added to supplement OH in the process of stripping the film‑The concentration of (c); the alcohol ether solvent with high boiling point can better play the role of permeating and swelling the dry film. The aromatic azole chelate additive is a film forming substance with specific affinity with metal, so that the oxidation corrosion of the surface of the conductive film layer in the film stripping process is avoided. The dry film stripping device is simple and safe in configuration, strong in dry film stripping capability under the normal spraying and stamping operation condition, and high in production efficiency and yield.
Description
Technical Field
The invention belongs to the field of touch screen production, relates to a membrane stripping liquid used in a flexible capacitive touch screen yellow light production process, and particularly relates to a membrane stripping liquid used for a photosensitive dry film, and a production method and application thereof.
Background
The photosensitive dry film is a key material for processing micro patterns and manufacturing microelectronic devices and printed circuit boards as an ultraviolet light induced anti-acid etching material, and is widely applied to the field of photoelectric display industry. The photosensitive dry film currently used in production is generally negative, i.e., the exposed part will undergo high molecular crosslinking polymerization to form a resist layer. And finally stripping and removing the film of the dry film of the exposure polymerization part in a yellow light process, and finally finishing the manufacture of the peripheral wires and the transparent electrode patterns of the touch screen.
CN101177657 discloses a film removing liquid additive for printed circuit boards and a production method thereof, CN101166397 discloses a method for stripping photosensitive films of flexible printed circuit boards; CN105676603A discloses a printed circuit board membrane removing liquid and a preparation method and a use method thereof; the above solutions relate to the field mainly in the printed circuit board industry, and are different for the substrate material objects to which the dry film is attached.
CN106707702 discloses a stripping solution for copper-plated alloy indium tin oxide conductive films and a preparation method thereof, wherein organic alkali is easy to form alkali mist to volatilize in the heating circulating spraying process, and in addition, the air oxygen atmosphere of an air draft and spraying system exists in a groove body in the production operation process, the following side reactions can occur to cause corrosion to a copper layer or other metal layers:
Cu+OH-+O2→[Cu(OH)4]2-+H2O。
at present, most manufacturers take NaOH or KOH solution with certain concentration as stripping liquid medicine to strip the dry film, and compared with the prior art, the method can save certain cost. The dry film with high photosensitive fineness can not be peeled off due to large foaming amount in the process of peeling the dry film by NaOH or KOH solution, the reverse-adhered substrate film surface causes poor residue due to large viscosity of alkali liquor in the peeling process, white spots possibly cause poor cleaning difficulty, and the conductive film is easy to corrode. The production efficiency and yield are low.
Disclosure of Invention
The invention aims to solve the technical problem of providing a stripping liquid for a photosensitive dry film and a production method and application thereof; the film stripping speed is high, the efficiency is high, and other surfaces cannot be damaged.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the utility model provides a shell membrane liquid for sensitization dry film which characterized in that: comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.4-1.25mol/L, the content of inorganic alkali is 0.5-2g/L, and the adding volume of the organic alkali accounts for 2-5% of the stripping liquid.
Further, the inorganic base is one or more of sodium hydroxide, potassium hydroxide and ammonia water.
Further, the organic base is one or more of ethanolamine, ethylenediamine, triethylene tetramine and polyethylene polyamine.
Further, the solvent is one or more of diethylene glycol monobutyl ether, propylene glycol butyl ether, cyclohexanediol monomethyl ether and N-methylpyrrolidone, and the volume percentage of the solvent is 1.0-5.0%
Further, the additive is aromatic azole or sugar alcohol chelate, and the content of the additive is 0.5-5g/L
In a preferred scheme, the inorganic base in the stripping liquid is potassium hydroxide, the using amount of the inorganic base is 0.8g/L, the organic base is ethanolamine and ethylenediamine, and the volume percentage of the ethanolamine and the ethylenediamine is 2.5%; the solvent is diethylene glycol monobutyl ether, the volume percentage is 1.5%, and the additive is aromatic azole chelate: 2g/L, and the balance of water.
The method for preparing the stripping liquid comprises the steps of taking the raw materials according to the proportion, and uniformly mixing to obtain the stripping liquid for the photosensitive dry film. The mixing equipment is an acid and alkali resistant PE liquid preparation tank.
The invention also relates to application of the stripping liquid in a process for producing a flexible touch screen.
Further, the stripping production conditions are temperature: 45-50 ℃, spray pressure: 0.5-2.0Kg/cm2The dry film peeling point is that when the dry film is peeled: 20-40 s.
The invention also relates to application of the film stripping liquid in a roll-to-roll yellow light film stripping process. The yellow light production process comprises the steps of sputtering indium tin oxide thin film, copper and copper alloy on a flexible PET substrate, then pressing a dry film, exposing, developing, etching (etching copper and ITO conductive patterns), and stripping the film; and then pressing a dry film, exposing, developing for the second time, etching and stripping the film to complete the manufacture of the electrode pattern of the touch screen. The traditional stripping liquid is generally prepared by caustic soda, and is particularly widely applied to the manufacturing industries of PCBs, FPCs and the like. However, the high-concentration caustic soda easily causes damage to the metal surface and is easy to foam during production to cause peeling of dry film winding equipment rollers and other mechanisms, so that the potential safety hazard of production and low yield are serious.
The invention takes organic base as a main component for stripping the film to react with a dry film polymer, and simultaneously, a certain amount of inorganic base component is added to supplement OH in the process of stripping the film-Concentration (base equivalent). The selected alcohol ether solvent with high boiling point can better play the role of permeating and swelling the dry film. The aromatic azole chelate additive is a film forming substance with specific affinity with metal, thereby ensuring that the surface of a conductive film layer (such as copper and copper alloy) can not be oxidized and corroded in the film stripping process. The components of the stripping liquid can be well dissolved with water, the preparation is simple and safe, the capability of stripping a dry film under the normal spraying and stamping operation condition is strong, and the production efficiency and the yield are high. The method is designed for peeling the dry film on the surface of the flexible conductive film, is particularly suitable for flexible roll-to-roll yellow light film peeling production and application, and realizes the step of peeling the dry film.
In order to improve the volatilization state of the stripping liquid and inhibit the oxidation of a metal layer, the invention adopts a proper amount of inorganic base and organic base as the alkali components of the stripping liquid, and adds alcohol ether solvents which can be mutually soluble with the organic base and have higher boiling points to solve the relevant problems. On one hand, the equivalent weight of the stripping liquid alkali in the production process can not be reduced too fast; on the other hand, increasing the viscosity of the solution system or adding a high boiling point alcohol ether solvent will reduce the risk of oxygen-absorbing corrosion of the metal layer, and will also achieve the film stripping effect of the fine line pattern portion better and more efficiently. By using the stripping liquid, the components have good intersolubility with water, the conductive indium tin oxide, copper metal and other films cannot be damaged, stripping residues are decomposed uniformly and finely, no surface residue is left after stripping and washing, the production capacity can be improved, and dry film residues decomposed in the stripping process cannot cause the rewinding of rollers and the reverse sticky film surface. The membrane stripping condition can be carried out under normal production conditions, and the preparation and production processes are safe and efficient. The stripping liquid can not attack metal film layers such as copper and the like and indium tin oxide conductive film layers in the operation modes of heating and circulating spraying, has the technical characteristics of high stripping speed, high efficiency, long effective period of use and the like, and the effective period of use can reach 7-15 days.
The stripping solution can also be applied to stripping a dry film on the surface of a conductive film (the thickness of the conductive layer of a printed circuit board is generally 10-15 microns) with a 10-100 nanometer thickness layer without corroding the surface layer of the film, and can well realize fine circuits: the surface dry film with the line width and the line distance (L/S) of 15 mu m/15 mu m is stripped, and the production efficiency of stripping the film is higher.
Drawings
FIG. 1 is a graph showing the change of the reflectivity of the surface of a copper layer after the film stripping liquid of the invention is continuously sprayed for stripping for 5 min.
FIG. 2 is a diagram showing the film stripping effect of the stripping liquid of the present invention on the surface of the copper circuit layer.
Detailed Description
The invention will be further elucidated with reference to the following examples. These examples are to be construed as merely illustrative and not limitative of the remainder of the disclosure. After reading the description of the invention, one skilled in the art can make various changes and modifications to the invention, and such equivalent changes and modifications also fall into the scope of the invention defined by the claims.
Example 1: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.52mol/L, specifically, the inorganic alkali is sodium hydroxide, and the content is 0.5 g/L; the organic alkali is ethanolamine and ethylenediamine, and the volume percentage content is respectively 2% and 2%; the solvent is N-methyl pyrrolidone, and the volume percentage content is 1%; the additive is aromatic azole chelate, and the adding amount is 0.5 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 2: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 1.14mol/L, specifically, the inorganic alkali is sodium hydroxide, and the content is 2 g/L; the organic alkali is ethanolamine, and the volume percentage content is 5 percent respectively; the solvent is diethylene glycol monobutyl ether, and the volume percentage content is 5%; the additive is aromatic azole chelate, and the adding amount is 5 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 3: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.58mol/L, specifically, the inorganic alkali is potassium hydroxide, and the content is 2 g/L; the organic alkali is ethanolamine and polyethylene polyamine, and the volume percentage content is respectively 2.5 percent and 2.5 percent; the solvent is propylene glycol butyl ether and cyclohexanediol monomethyl ether, and the volume percentage content is 1 percent and 3 percent respectively; the additive is sugar alcohol chelate, and the adding amount is 3 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 4: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.56mol/L, specifically, the inorganic alkali is potassium hydroxide, and the content is 1 g/L; the organic alkali is ethanolamine and ethylenediamine, and the volume percentage content is 1.5 percent and 1 percent respectively; the solvent is diethylene glycol monobutyl ether and propylene glycol butyl ether, and the volume percentage content is 1.5 percent and 1 percent respectively; the additive is aromatic azole chelate, and the adding amount is 2.5 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 5: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.47mol/L, specifically, the inorganic alkali is sodium hydroxide and ammonia water, and the contents are 0.5g/L and 0.5g/L respectively; the organic alkali is ethylenediamine, triethylene tetramine and polyethylene polyamine, and the volume percentage content is 1.5%, 0.5% and 0.5% respectively; the solvent is diethylene glycol monobutyl ether and propylene glycol butyl ether, and the volume percentage content is 1.5 percent and 1 percent respectively; the additive is aromatic azole chelate, and the addition amount is 2 g/L; injecting pure water to supplement the water to 100 percent, and fully and uniformly stirring the mixture in an acid and alkali resistant PE liquid preparation tank according to the figure 1 to obtain the photosensitive dry film stripping liquid.
Example 6: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.62mol/L, specifically, the inorganic alkali is sodium hydroxide, and the content is respectively 2 g/L; the organic alkali is ethanolamine, ethylenediamine and polyethylene polyamine, and the volume percentage content is respectively 1%, 0.5% and 2%; the solvent is cyclohexanediol monomethyl ether and N-methyl pyrrolidone, and the volume percentage content is 3.5 percent and 0.5 percent respectively; the additive is sugar alcohol chelate, and the adding amount is 5 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 7: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.56mol/L, specifically, the inorganic alkali is sodium hydroxide, and the content is 1.25g/L respectively; the organic alkali is ethanolamine and ethylenediamine, and the volume percentage content is respectively 2 percent and 0.5 percent; the solvent is diethylene glycol monobutyl ether, and the volume percentage content is 3.0 percent respectively; the additive is aromatic azole chelate, and the adding amount is 3 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 8: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.54mol/L, specifically, the inorganic alkali is sodium hydroxide, and the content is 1.0g/L respectively; the organic alkali is ethanolamine and triethylene tetramine, and the volume percentage content is respectively 2% and 1.5%; the solvent is cyclohexanediol monomethyl ether, and the volume percentage content is 3.5 percent respectively; the additive is aromatic azole chelate, and the addition amount is 2 g/L; and (3) injecting pure water to supplement the solution to 100%, and fully and uniformly stirring the solution in an acid and alkali resistant PE liquid preparation tank to obtain the photosensitive dry film stripping solution.
Example 9: a stripping liquid for a photosensitive dry film comprises inorganic base, organic base, solvent, additive and water; the inorganic alkali in the stripping liquid is potassium hydroxide with the dosage of 0.8g/L, the organic alkali is ethanolamine and ethylenediamine, and the volume percentage of the ethanolamine and the ethylenediamine is 2.5 percent; the solvent is diethylene glycol monobutyl ether, the volume percentage is 1.5%, and the additive is aromatic azole chelate: 2g/L, and the balance of water.
1. For the stripping solutions in examples 1 to 8, in the roll-to-roll production process of a Sensor (copper wire type touch screen), the films are stripped according to the following process conditions, and the production effects are shown in table 1 below:
TABLE 1
2. 2000m film-stripping production by roll-to-roll equipment2After the material, the peel ability and appearance are shown in table 2:
TABLE 2
3. The stripping solution prepared in example 2 was used to test the attack resistance of the metal copper layer to the chemical solution, and the surface sheet resistance of the copper layer and the change in the resistance of the copper wire of the touch panel are shown in the following tables 3 and 4, respectively: the sheet resistance of the copper surface and the resistance change rate of the copper wire line of the touch screen are very small, and the metal copper layer is not corroded to cause the abnormity of resistance increase, so that the production requirement of the copper wire touch screen can be completely met.
TABLE 3
TABLE 4
4. And continuously spraying and stripping the film for 5min by roll-to-roll production equipment, wherein the change condition of the surface reflectivity of the copper layer is shown in figure 1, and the reflection and the color before and after stripping are basically unchanged, so that the conclusion shows that the conventional film stripping production process can completely meet the requirement of production quality.
5. FIG. 2 is a diagram showing the stripping effect of the stripping solution of the present invention on the surface of copper wiring layer
The film stripping effect, the dry film stripping capability and the circuit layer are not corroded. The Film stripping liquid medicine has no attack on a metal copper layer, the sheet resistance and the line resistance change rate are very small, and the Film surface appearance effect after stripping is very good.
Claims (6)
1. The utility model provides a shell membrane liquid for sensitization dry film which characterized in that: is prepared from inorganic base, organic base, solvent, additive and water; wherein the alkali equivalent is 0.4-1.25mol/L, the content of inorganic alkali is 0.5-2g/L, and the inorganic alkali is one or more of sodium hydroxide, potassium hydroxide and ammonia water; the volume of the added organic alkali accounts for 2-5% of the stripping liquid, and the organic alkali is a plurality of kinds of ethanolamine, ethylenediamine, triethylene tetramine and polyethylene polyamine; the solvent is one or more of diethylene glycol monobutyl ether, propylene glycol butyl ether, cyclohexanediol monomethyl ether and N-methyl pyrrolidone, and the volume percentage of the solvent is 1.0-5.0%; the additive is aromatic azole or sugar alcohol chelate, and the content of the additive is 0.5-5 g/L.
2. The stripping solution according to claim 1, characterized in that: the inorganic alkali in the stripping liquid is potassium hydroxide with the dosage of 0.8g/L, the organic alkali is ethanolamine and ethylenediamine, and the volume percentage of the ethanolamine and the ethylenediamine is 2.5 percent; the solvent is diethylene glycol monobutyl ether, the volume percentage is 1.5%, and the additive is aromatic azole chelate: 2g/L, and the balance of water.
3. A method for preparing the stripping liquid according to any one of claims 1-2, comprising the steps of:
the raw materials are taken according to the proportion and are uniformly mixed to obtain the stripping liquid for the photosensitive dry film.
4. Use of the stripping solution according to any one of claims 1-2 in a process for producing a flexible touch screen.
5. Use according to claim 4, characterized in that: the stripping production conditions are temperature: 45-50 ℃, spray pressure: 0.5-2.0Kg/cm2The dry film peeling point is that when the dry film is peeled: 20-40 s.
6. Use of the stripping solution according to any one of claims 1-2 in a roll-to-roll photolithography stripping process.
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| CN113563888A (en) * | 2021-08-24 | 2021-10-29 | 信丰正天伟电子科技有限公司 | Stripping liquid and preparation method thereof |
| CN113741159B (en) * | 2021-08-27 | 2024-05-17 | 漳州思美科新材料有限公司 | PI film stripping liquid, preparation method thereof and stripping method |
| CN114656889A (en) * | 2022-05-07 | 2022-06-24 | 常州亚龙电子科技有限公司 | Stripping liquid for polyimide adhesive film and preparation method thereof |
| CN115820029B (en) * | 2022-12-13 | 2023-10-27 | 广州安达净水材料有限公司 | Film remover for selective dry film/printing ink, and preparation method and application thereof |
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| CN101166397A (en) * | 2006-10-18 | 2008-04-23 | 比亚迪股份有限公司 | A method for removing sensitization film in flexible printed circuit board |
| CN101398639A (en) * | 2007-09-28 | 2009-04-01 | 三星电子株式会社 | Composition for stripping and stripping method |
| CN104102097A (en) * | 2013-04-09 | 2014-10-15 | 东友精细化工有限公司 | Corrosion Resistant Agent And Stripping Agent Composition |
| CN105116696A (en) * | 2015-10-10 | 2015-12-02 | 蓝思科技（长沙）有限公司 | Photoresist stripper and application thereof |
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2017
- 2017-12-25 CN CN201711420013.4A patent/CN108008606B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101166397A (en) * | 2006-10-18 | 2008-04-23 | 比亚迪股份有限公司 | A method for removing sensitization film in flexible printed circuit board |
| CN101398639A (en) * | 2007-09-28 | 2009-04-01 | 三星电子株式会社 | Composition for stripping and stripping method |
| CN104102097A (en) * | 2013-04-09 | 2014-10-15 | 东友精细化工有限公司 | Corrosion Resistant Agent And Stripping Agent Composition |
| CN105116696A (en) * | 2015-10-10 | 2015-12-02 | 蓝思科技（长沙）有限公司 | Photoresist stripper and application thereof |
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