Preparation method of high-generation silicon-based panel photoresist stripping liquid

Abstract

The invention discloses a preparation method of an advanced silicon-based panel photoresist stripping solution, and belongs to the technical field of stripping solution preparation and production, the preparation method comprises the following steps: S1, preparing raw materials: 10%-15% of monoethanolamine, 22%-32% of butanol, 0.5%-1.5% of citric acid, 15.5%-25.5% of dimethyl sulfoxide, 15.5%-25.5% of diethylene glycol monomethyl ether and 0.5%-1.5% of benzotriazole; s2, monoethanolamine and butanol are added into a reaction kettle to be stirred at the stirring speed of 200 r / min-300 r / min, citric acid is added into the reaction kettle to be stirred after stirring and mixing are conducted, stirring continues to be conducted for 15 min-20 min after citric acid is added, the temperature of the reaction kettle is kept at 23 DEG C, and the compound solvent system can rapidly swell and dissolve various positive and negative photoresists; comprising a stubborn photoresist after high-temperature hard baking and ion implantation, and the stripping efficiency is high; and a buffer system formed by MEA and citric acid is matched with the efficient BTA corrosion inhibitor, so that the corrosion rate on copper, aluminum, molybdenum, indium tin oxide and other films is extremely low, and a precise circuit is effectively protected.

Description

Technical Field

[0001] This invention belongs to the field of stripping solution preparation and production technology, and particularly relates to a method for preparing a photoresist stripping solution for high-generation silicon-based panels. Background Technology

[0002] Silicon-based panels refer to silicon-based OLED products (such as silicon-based OLED microdisplays), which differ from conventional AMOLED devices that use amorphous silicon, microcrystalline silicon, or low-temperature polycrystalline silicon thin-film transistors as backplanes. They use monocrystalline silicon chips as a substrate, and the pixel size of OLED displays is one-tenth that of traditional display devices, resulting in significantly higher resolution. Silicon-based OLED display panels (monocrystalline silicon chips) can utilize existing mature integrated circuit CMOS technology, enabling not only the active addressing matrix of OLED display pixels but also the implementation of various driving control circuits such as SRAM memory on the silicon-based OLED display panel. This reduces external wiring, increases reliability, and achieves lightweight design.

[0003] Silicon-based OLEDs possess numerous superior characteristics, including self-emissiveness, high resolution, high contrast, wide color gamut, wide viewing angle, fast response, high luminous efficiency, low power consumption, thinness, light weight, small size, and portability. Silicon-based OLEDs are well-suited for near-eye display smart devices, such as AR / VR, head-mounted video players, head-mounted home theaters, head-mounted virtual reality simulators, head-mounted game consoles, pilot helmet systems, infrared night vision devices, and head-mounted medical rescue and diagnostic systems. However, for high-generation lines such as 8.5 generations and above, issues like incomplete stripping and poor stripping uniformity can arise. Therefore, we propose a method for preparing photoresist stripping solutions for high-generation silicon-based panels. Summary of the Invention

[0004] This invention provides a method for preparing a photoresist stripping solution for high-generation silicon-based panels to solve the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a method for preparing a photoresist stripping solution for high-generation silicon-based panels, comprising the following steps:

[0006] S1. Prepare raw materials: 10%–15% monoethanolamine, 22%–32% butanol, 0.5%–1.5% citric acid, 15.5%–25.5% dimethyl sulfoxide, 15.5%–25.5% diethylene glycol monomethyl ether, and 0.5%–1.5% benzotriazole;

[0007] S2. Add monoethanolamine and butanol to the reaction vessel and stir at a speed of 200 r / min to 300 r / min. After mixing, add citric acid to the reaction vessel and stir. After the citric acid is added, continue stirring for 15 min to 20 min, and keep the temperature of the reaction vessel at 23℃. Citric acid and monoethanolamine react fully to generate citrate ethanolamine salt and form a homogeneous system.

[0008] S3. Add benzotriazole to the system prepared in step S2 to carry out the reaction. During the reaction, keep the stirring speed at 200 r / min to 300 r / min, keep the temperature at 23℃, and stir for 20 min to 30 min until the benzotriazole is completely dissolved and dispersed.

[0009] S4. When the benzotriazole in step S3 is completely dissolved and dispersed, add dimethyl sulfoxide and diethylene glycol monomethyl ether slowly to the reaction vessel by pouring through a metering pump and stirring. After the materials are added, increase the stirring speed to 300 r / min to 400 r / min, keep the temperature of the reaction vessel at 23°C, and continue stirring for 45 min to 60 min until the entire solution is completely clear, transparent, and free of any suspended matter or stratification.

[0010] S5. The transparent liquid obtained in step S4 is filtered through a 0.1μm polytetrafluoroethylene filter to remove trace particulate impurities, thus obtaining the high-generation silicon-based panel photoresist stripping liquid.

[0011] Furthermore, in step S1, the inside of the reactor is rinsed with ultrapure IPA. After rinsing three times, the reactor is purged with high-purity nitrogen for 10 minutes to dry the inside of the reactor.

[0012] Furthermore, in step S2, solid citric acid is added slowly and evenly. This process is an exothermic reaction and requires cooling of the reactor by jacketed cooling water.

[0013] Furthermore, in step S3, two-thirds of the total amount of diethylene glycol monomethyl ether and benzotriazole are placed in another small container and stirred at 30°C to 40°C until completely dissolved to prepare a premixed solution for later use.

[0014] The beneficial effects of this invention are:

[0015] 1. The compound solvent system can quickly swell and dissolve various positive and negative photoresists, including stubborn photoresists after high-temperature hard baking and ion implantation, with high stripping efficiency; the buffer system formed by MEA and citric acid, combined with the highly efficient BTA corrosion inhibitor, has an extremely low corrosion rate on thin films such as copper, aluminum, molybdenum, and indium tin oxide, effectively protecting precision circuits.

[0016] 2. High stability: The components are highly compatible and do not easily decompose, volatilize, or discolor during long-term storage and in high-temperature bath environments, resulting in a long service life and reduced production costs.

[0017] 3. Environmental protection and safety: Compared with pure amine systems, the volatility and irritating odor are significantly reduced, making the working environment more friendly.

[0018] 4. Suitable for high-generation lines: Its superior performance fully meets the stringent requirements of G8.6, G10.5 and even higher generation large-scale production lines for the uniformity, stability and reliability of the stripping fluid. Detailed Implementation

[0019] To further understand the content, features, and effects of this invention, the following embodiments are provided in detail below.

[0020] Example 1:

[0021] A method for preparing a photoresist stripping solution for a high-generation silicon-based panel includes the following steps;

[0022] S1. Prepare raw materials: 10% monoethanolamine, 22% butanol, 1.0% citric acid, 15.5% dimethyl sulfoxide, 15.5% diethylene glycol monomethyl ether and 1.5% benzotriazole;

[0023] The inside of the reactor was rinsed with ultrapure water three times. After rinsing, the reactor was purged with high-purity nitrogen for 10 minutes to replace the air.

[0024] S2. Add monoethanolamine and butanol to the reaction vessel and stir at a speed of 200 r / min to 300 r / min. After mixing, add citric acid to the reaction vessel and stir slowly and evenly. This process is an exothermic reaction, so the reaction vessel needs to be cooled by jacketed cooling water. After the citric acid is added, continue stirring for 15 min to 20 min, and keep the temperature of the reaction vessel at 23℃. Citric acid and monoethanolamine react fully to form citrate ethanolamine salt, forming a homogeneous system.

[0025] S3. First, put two-thirds of the total amount of diethylene glycol monomethyl ether and benzotriazole into another small container and stir at 30℃~40℃ until completely dissolved to prepare a premixed solution for later use. Add the benzotriazole mixed solution to the system prepared in step S2 to carry out the reaction. During the reaction, keep the stirring speed at 200r / min~300r / min, keep the temperature at 23℃, and stir for 20min~30min until the benzotriazole is completely dissolved and dispersed.

[0026] S4. When the benzotriazole in step S3 is completely dissolved and dispersed, add dimethyl sulfoxide and diethylene glycol monomethyl ether slowly to the reaction vessel by pouring through a metering pump and stirring. After the materials are added, increase the stirring speed to 300 r / min to 400 r / min, keep the temperature of the reaction vessel at 23°C, and continue stirring for 45 min to 60 min until the entire solution is completely clear, transparent, and free of any suspended matter or stratification.

[0027] S5. The transparent liquid obtained in step S4 is filtered through a 0.1μm polytetrafluoroethylene filter to remove trace particulate impurities, thus obtaining the high-generation silicon-based panel photoresist stripping liquid.

[0028] Example 2:

[0029] S1. Prepare raw materials: 10% monoethanolamine, 32% butanol, 0.5% citric acid, 25.5% dimethyl sulfoxide, 25.5% diethylene glycol monomethyl ether and 1.5% benzotriazole;

[0030] The inside of the reactor was rinsed with ultrapure water three times. After rinsing, the reactor was purged with high-purity nitrogen for 10 minutes to replace the air.

[0031] S2. Add monoethanolamine and butanol to the reaction vessel and stir at a speed of 200 r / min to 300 r / min. After mixing, add citric acid to the reaction vessel and stir slowly and evenly. This process is an exothermic reaction, so the reaction vessel needs to be cooled by jacketed cooling water. After the citric acid is added, continue stirring for 15 min to 20 min, and keep the temperature of the reaction vessel at 23℃. Citric acid and monoethanolamine react fully to form citrate ethanolamine salt, forming a homogeneous system.

[0032] S3. First, put two-thirds of the total amount of diethylene glycol monomethyl ether and benzotriazole into another small container and stir at 30℃~40℃ until completely dissolved to prepare a premixed solution for later use. Add the benzotriazole mixed solution to the system prepared in step S2 to carry out the reaction. During the reaction, keep the stirring speed at 200r / min~300r / min, keep the temperature at 23℃, and stir for 20min~30min until the benzotriazole is completely dissolved and dispersed.

[0033] S4. When the benzotriazole in step S3 is completely dissolved and dispersed, add dimethyl sulfoxide and diethylene glycol monomethyl ether slowly to the reaction vessel by pouring through a metering pump and stirring. After the materials are added, increase the stirring speed to 300 r / min to 400 r / min, keep the temperature of the reaction vessel at 23°C, and continue stirring for 45 min to 60 min until the entire solution is completely clear, transparent, and free of any suspended matter or stratification.

[0034] S5. The transparent liquid obtained in step S4 is filtered through a 0.1μm polytetrafluoroethylene filter to remove trace particulate impurities, thus obtaining the high-generation silicon-based panel photoresist stripping liquid.

[0035] Example 3:

[0036] S1. Prepare raw materials: 15% monoethanolamine, 32% butanol, 1.5% citric acid, 15.5% dimethyl sulfoxide, 25.5% diethylene glycol monomethyl ether and 1.5% benzotriazole;

[0037] The inside of the reactor was rinsed with ultrapure water three times. After rinsing, the reactor was purged with high-purity nitrogen for 10 minutes to replace the air.

[0038] S2. Add monoethanolamine and butanol to the reaction vessel and stir at a speed of 200 r / min to 300 r / min. After mixing, add citric acid to the reaction vessel and stir slowly and evenly. This process is an exothermic reaction, so the reaction vessel needs to be cooled by jacketed cooling water. After the citric acid is added, continue stirring for 15 min to 20 min, and keep the temperature of the reaction vessel at 23℃. Citric acid and monoethanolamine react fully to form citrate ethanolamine salt, forming a homogeneous system.

[0039] S3. First, put two-thirds of the total amount of diethylene glycol monomethyl ether and benzotriazole into another small container and stir at 30℃~40℃ until completely dissolved to prepare a premixed solution for later use. Add the benzotriazole mixed solution to the system prepared in step S2 to carry out the reaction. During the reaction, keep the stirring speed at 200r / min~300r / min, keep the temperature at 23℃, and stir for 20min~30min until the benzotriazole is completely dissolved and dispersed.

[0040] S4. When the benzotriazole in step S3 is completely dissolved and dispersed, add dimethyl sulfoxide and diethylene glycol monomethyl ether slowly to the reaction vessel by pouring through a metering pump and stirring. After the materials are added, increase the stirring speed to 300 r / min to 400 r / min, keep the temperature of the reaction vessel at 23°C, and continue stirring for 45 min to 60 min until the entire solution is completely clear, transparent, and free of any suspended matter or stratification.

[0041] S5. The transparent liquid obtained in step S4 is filtered through a 0.1μm polytetrafluoroethylene filter to remove trace particulate impurities, thus obtaining the high-generation silicon-based panel photoresist stripping liquid.

[0042] In this technical solution:

[0043] Monoethanolamine: As the main alkali agent, it provides an alkaline environment and breaks the polymer chains of photoresist through saponification. It is the main source of peeling force, and its content control is crucial. Too high a content can easily corrode metals, while too low a content will result in insufficient peeling ability.

[0044] Dimethyl sulfoxide and diethylene glycol monomethyl ether: as highly polar aprotic solvents, they have excellent solubility and carrying capacity for swollen photoresist, and are miscible with water and organic matter, preventing the re-adhesion of stripping products; the synergistic effect of the two ensures the continuous effectiveness of the stripping solution.

[0045] Butanol: As a co-solvent and penetrant, it can effectively reduce the surface tension of the solution, promote the rapid penetration of active ingredients to the interface between the photoresist and the substrate, and accelerate the stripping of the photoresist; at the same time, it can adjust the boiling point of the system and reduce the volatilization of the main solvent.

[0046] Benzotriazole: an excellent corrosion inhibitor for copper and copper alloys; it can form stable polymeric coordination compounds with copper ions, adsorb onto the metal surface to form a dense protective film, effectively isolating the stripping solution from corroding the metal circuit.

[0047] Citric acid: As a weak organic acid, it is used to precisely adjust the pH value of the system and control the corrosivity within a safe range. On the other hand, its chelating effect can complex metal ions in the solution, prevent side reactions such as catalytic oxidation of metal ions, and improve the service life and stability of the solution.

[0048] Table 1. Stripping solutions used in Examples 1-3

[0049] Example 1 2 3 Alkylamines (m%) 5 26 21 Alcohol (m%) 50 5 35 Metal corrosion resist (m%) 0.01 4 3 Organic acids (m%) 1 0.1 0.1 Organic solvents (m%) 43 65 15

[0050] As can be seen from the above embodiments, the method of the present invention can prepare a compound solvent system that can rapidly swell and dissolve various positive and negative photoresists, including stubborn photoresists after high-temperature hard baking and ion implantation, with high stripping efficiency; the buffer system formed by MEA and citric acid, combined with the highly efficient BTA corrosion inhibitor, has an extremely low corrosion rate on thin films such as copper, aluminum, molybdenum, and indium tin oxide, effectively protecting precision circuits.

[0051] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a photoresist stripping solution for high-generation silicon-based panels, characterized in that: Includes the following steps: S1. Prepare raw materials: 10%–15% monoethanolamine, 22%–32% butanol, 0.5%–1.5% citric acid, 15.5%–25.5% dimethyl sulfoxide, 15.5%–25.5% diethylene glycol monomethyl ether, and 0.5%–1.5% benzotriazole; S2. Add monoethanolamine and butanol to the reaction vessel and stir at a speed of 200 r / min to 300 r / min. After mixing, add citric acid to the reaction vessel and stir. After the citric acid is added, continue stirring for 15 min to 20 min, and keep the temperature of the reaction vessel at 23℃. Citric acid and monoethanolamine react fully to generate citrate ethanolamine salt and form a homogeneous system. S3. Add benzotriazole to the system prepared in step S2 to carry out the reaction. During the reaction, keep the stirring speed at 200 r / min to 300 r / min, keep the temperature at 23℃, and stir for 20 min to 30 min until the benzotriazole is completely dissolved and dispersed. S4. When the benzotriazole in step S3 is completely dissolved and dispersed, add dimethyl sulfoxide and diethylene glycol monomethyl ether slowly to the reaction vessel by pouring through a metering pump and stirring. After the materials are added, increase the stirring speed to 300 r / min to 400 r / min, keep the temperature of the reaction vessel at 23°C, and continue stirring for 45 min to 60 min until the entire solution is completely clear, transparent, and free of any suspended matter or stratification. S5. The transparent liquid obtained in step S4 is filtered through a 0.1μm polytetrafluoroethylene filter to remove trace particulate impurities, thus obtaining the high-generation silicon-based panel photoresist stripping liquid.

2. The method for preparing a photoresist stripping solution for a high-generation silicon-based panel according to claim 1, characterized in that: In step S1, the inside of the reactor is rinsed with ultrapure IPA. After rinsing three times, the reactor is purged with high-purity nitrogen for 10 minutes to dry the inside of the reactor.

3. The method for preparing a photoresist stripping solution for a high-generation silicon-based panel according to claim 1, characterized in that: In step S2, solid citric acid is added slowly and evenly. This process is an exothermic reaction and the reactor needs to be cooled by cooling water in the jacket.

4. The method for preparing a photoresist stripping solution for a high-generation silicon-based panel according to claim 1, characterized in that: In step S3, two-thirds of the total amount of diethylene glycol monomethyl ether and benzotriazole are placed in another small container and stirred at 30°C to 40°C until completely dissolved to prepare a premixed solution for later use.