A polyimide film surface modifier and its preparation method and application
By introducing quaternary aminated polyethylene imidazole and other components into the polyimide film surface modifier, phenol groups and amine groups are directly generated on the surface of the PI film, solving the high cost and performance instability of traditional plasma treatment, achieving efficient and low-cost metallization treatment, meeting the requirements of high-frequency applications.
Patent Information
- Application Number
- CN202310359889.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-06
- Publication Date
- 2025-08-19
- Estimated Expiration
- 2043-04-06
AI Technical Summary
The prior art has high cost and capacity limitations in the metallization treatment of polyimide film surfaces, and the material performance after traditional plasma treatment is unstable, making it difficult to meet the roughness and anchoring effect requirements of high-frequency applications.
A polyimide film surface modifier is used, including quaternary aminated polyethylene imidazole, inorganic salt, alkylphenol polyoxyethylene ether, reducing agent and alcohol amine, and phenol groups are generated on the surface of the PI film through chemical modification treatment, which directly replaces plasma physical modification, reduces costs and enhances the surface chemical modification ability.
Metalization treatment with full coverage in a short time is achieved, which enhances the adhesion between the PI film surface and the deposited metal, reduces the processing cost, and is applicable on a variety of substrates, avoiding the complexity of traditional processes.
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Figure CN116426022B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of polyimide film surface modifiers, in particular to a polyimide film surface modifier and a preparation method and application thereof. Background Art
[0002] Polyimide (PI) film is a high-performance polyimide material with the characteristics of high-temperature stability, high mechanical strength, high chemical stability, and excellent electrical properties. It is widely used in electronics, aerospace and other fields. According to the requirements of use, the surface of the polyimide film usually needs to be metallized.
[0003] Traditional polyimide (PI) metallization utilizes a plasma dry process for functionalization, including degreasing, roughening (physical etching), and surface modification (physical modification). Finally, copper is deposited on the PI film surface using an electroless copper plating process. Prior to degreasing and pore shaping, the polyimide (PI) film must be soaked in a PI conditioning agent, typically using a potassium hydroxide solution to chemically etch and modify the PI surface. KOH modification forms amide and carboxylic acid groups on the PI film surface, and the material's physical and chemical properties, such as dielectric properties and hygroscopicity, are no longer equivalent to those of polyimide, raising concerns about its reliability in high-end applications.
[0004] Furthermore, most current PI films utilize a two-layer, adhesive-free, flexible copper foil substrate, 2L / FCCL, eliminating the need to address adhesive overflow. Furthermore, due to the increasing availability of smaller routing widths and high-frequency applications, the surface roughness of the PI film must be limited, with the average roughness unable to exceed the wavelength of high-frequency communications. Therefore, the substrate's surface chemical modification capabilities must be significantly enhanced to compensate for the reduced anchoring effect caused by the reduced roughness and achieve the required adhesion between the PI film and the deposited copper. Therefore, to address the high cost and capacity limitations of dry plasma treatment while enhancing the functionality of PI film surface chemical modification, there is an urgent need to develop a novel PI film surface modification composition that replaces the dual functions of plasma treatment and conditioning agent immersion. Summary of the Invention
[0005] Based on this, the purpose of the present invention is to provide a polyimide film surface modifier, a preparation method and application thereof. After the polyimide film surface is metallized (Cu, Ni) treated with the polyimide film surface, the polyimide film surface modifier can obtain full coverage in a relatively short time, and can produce more phenolic and amine chemical groups on the PI film surface. It can directly avoid plasma physical modification treatment and does not require the use of PI adjusters. It can be directly added to the whole hole groove for use, thereby reducing the cost of metallization treatment of the polyimide film surface.
[0006] In order to solve the above technical problems of the present invention, the present invention provides the following technical solutions:
[0007] One aspect of the present invention is to provide a polyimide film surface modifier, which comprises, in terms of concentration:
[0008]
[0009] The rest was deionized water.
[0010] Among them, quaternized polyvinyl imidazole can make the resin pore wall positively charged, which is convenient for the adsorption of palladium, and can also serve as a wetting agent.
[0011] Further, the amine is diethylenetriamine;
[0012] The inorganic salt is at least one of sodium chloride, potassium chloride and magnesium chloride.
[0013] Diethylenetriamine has the function of cleaning the oxide layer on the board surface; inorganic salt is a co-solvent and also has a cleaning effect, which can corrode the oxide layer on the board surface.
[0014] Furthermore, the alkylphenol polyoxyethylene ether is at least one of OP-10, TX-100, and TX-10. Alkylphenol polyoxyethylene ether is a nonionic surfactant with stable properties and acid and alkali resistance, and has good wetting, penetration, emulsification and washing effects.
[0015] Further, the reducing agent is hydrazine hydrate;
[0016] The alcoholamine is at least one of monoethanolamine, diethanolamine and triethanolamine. The alcoholamine can increase the brightness of the copper surface.
[0017] Preferably, the volume ratio of the reducing agent to the alcoholamine is 1:1-1.8.
[0018] Furthermore, the inorganic base is one or both of potassium hydroxide and sodium hydroxide. The inorganic base can induce the hydrolysis of polyimide, converting the less hydrophilic PI film into a more hydrophilic PAA layer, which is beneficial for the wettability of the copper plating solution. At the same time, the nitrogen-containing amide group and oxygen-containing carboxylic acid group can increase the adsorption capacity of palladium and enhance the adhesion between the copper plating and the PI film bottom layer.
[0019] The inventors found that by adding amines, inorganic bases and reducing agents to the polyimide film surface modifier and controlling the addition ratio of reducing agent to amines to be 1:1-1.8, the plasma physical modification treatment can be directly avoided, thereby reducing the operating cost and labor cost of the PI film surface metallization treatment.
[0020] Another aspect of the present invention is to provide a method for preparing the above-mentioned polyimide film surface modifier, comprising the following steps:
[0021] S1. Dissolve the inorganic base in deionized water to prepare a solution with a mass concentration of 20%, cool it, and set aside;
[0022] S2. Add an appropriate amount of deionized water to the production tank, add a reducing agent, stir evenly, and cool to room temperature; add amines, stir for 20-40 minutes, and cool to room temperature; continue to add inorganic salts, stir for 8-15 minutes until completely dissolved, to obtain a mixed solution;
[0023] S3. Add the 20% inorganic base solution obtained in S1 to the mixed solution obtained in S2, stir evenly, add alcoholamines and quaternized polyvinyl imidazole, and after they are fully dissolved, add alkylphenol polyoxyethylene ether, stir evenly, add water to the liquid level, filter, and package to obtain a polyimide membrane surface modifier.
[0024] Furthermore, in S3, the filtration is performed using a 5" filter cotton core for 1-3 hours.
[0025] The present invention also provides the use of the aforementioned polyimide film surface modifier in the metallization treatment of polyimide films. During the metallization treatment of polyimide film surfaces, the polyimide film surface modifier can generate a larger number of phenolic and amine chemical groups on the PI film surface. This can directly replace plasma physical modification and eliminates the need for a PI adjuster (strong base). The modifier can be directly added to the pore-sizing tank for use, thus simultaneously functioning as a pore-sizing agent and reducing the cost of PI film surface metallization.
[0026] Beneficial effects of the present invention:
[0027] 1. After the polyimide film surface modifier provided by the present invention is used to metallize the surface of the polyimide film, a large number of phenyl, phenol and amine chemical groups are generated on the surface of the PI film, which show strong affinity to various substrates through hydrophobic interactions, hydrogen bonds and coordination bonds. These phenol and amine groups have high hydrophilicity and complexing ability for palladium and copper atoms. The adsorbed palladium catalyst is tightly bonded to the substrate through the modified intermediate adhesive layer, producing a more stable and stronger adhesion with the deposited chemical copper metal.
[0028] 2. The polyimide film surface modifier provided by the present invention has a coupling bridging component that can couple chemical copper metal with substrate-modified organic matter. This bridging layer fills the chemical group vacancies in the adhesive layer, increases the coverage of the deposited copper and strengthens the bonding ability.
[0029] 3. After the polyimide film surface modifier provided by the present invention is used for metallization (Cu, Ni) treatment of the polyimide film surface, full coverage can be obtained in a relatively short time, and more phenolic and amine chemical groups can be generated on the surface of the PI film. The plasma physical modification treatment can be directly exempted, and there is no need to use a PI adjuster (strong base). It can be directly added to the pore-forming tank for use, and has the function of a pore-forming agent, thereby reducing the cost of metallization treatment of the PI film surface. In addition, there is no need to be particularly careful about the introduction of moisture during the treatment process, and the subsequent water washing process is easier.
[0030] 4. The polyimide film surface modifier provided by the present invention can be applied to PCB hard boards, FPC soft boards and soft-rigid boards without distinguishing slots or production lines. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying any creative work.
[0032] Figure 1 This is the SEM image of copper crystals on the PI board treated in Experimental Example 1;
[0033] Figure 2 This is the PI board hole wall lift-off image processed in Experimental Example 1;
[0034] Figure 3 This is the backlight detection image of the PI board processed in Test Example 1;
[0035] Figure 4 This is the PI board hole wall floating image processed in Comparative Example 1;
[0036] Figure 5 This is a backlight detection image of the PI board processed in Comparative Example 1;
[0037] Figure 6 This is the PI board hole wall lifting image processed in Comparative Example 3;
[0038] Figure 7 This is the backlight detection picture of the PI board treated in comparative example 3. DETAILED DESCRIPTION
[0039] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below in conjunction with the drawings and specific implementation methods of the embodiments of the present invention.
[0040] The experimental methods in the following examples are conventional methods unless otherwise specified. The reagents or instruments involved in the present invention without indicating the manufacturer are all common commercial products and can be purchased from the market.
[0041] Example 1:
[0042] Preparation of polyimide membrane surface modifier:
[0043] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0044] S2. Add an appropriate amount of deionized water to the production tank, add 18 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 2 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0045] S3. Add 40 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 25 mL of triethanolamine and 7 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 2 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0046] Example 2:
[0047] Preparation of polyimide membrane surface modifier:
[0048] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0049] S2. Add an appropriate amount of deionized water to the production tank, add 20 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 95 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 3 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0050] S3. Add 45 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 30 mL of triethanolamine and 7.5 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 2 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0051] Example 3:
[0052] Preparation of polyimide membrane surface modifier:
[0053] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0054] S2. Add an appropriate amount of deionized water to the production tank, add 20 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 100 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 2.5 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0055] S3. Add 45 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 30 mL of triethanolamine and 8.0 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 3.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 3 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0056] Example 4:
[0057] Preparation of polyimide membrane surface modifier:
[0058] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0059] S2. Add an appropriate amount of deionized water to the production tank, add 20 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 95 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 3.0 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0060] S3. Add 45 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 35 mL of triethanolamine and 8.0 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 3.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 3 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0061] Example 5:
[0062] Preparation of polyimide membrane surface modifier:
[0063] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0064] S2. Add an appropriate amount of deionized water to the production tank, add 25 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 100 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 3.5 g of sodium chloride, stir for 12 min until completely dissolved, to obtain a mixed solution;
[0065] S3. Add 43 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 35 mL of triethanolamine and 7.5 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 3.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 3 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0066] Example 6:
[0067] Preparation of polyimide membrane surface modifier:
[0068] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0069] S2. Add an appropriate amount of deionized water to the production tank, add 25 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 4.0 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0070] S3. Add 50 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 35 mL of triethanolamine and 8.0 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 3.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 3 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0071] Example 7:
[0072] Preparation of polyimide membrane surface modifier:
[0073] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0074] S2. Add an appropriate amount of deionized water to the production tank, add 25 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 100 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 4.0 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0075] S3. Add 50 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 35 mL of triethanolamine and 8.0 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 3.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 3 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0076] Example 8:
[0077] Preparation of polyimide membrane surface modifier:
[0078] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0079] S2. Add an appropriate amount of deionized water to the production tank, add 18 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 2 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0080] S3. Add 40 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 25 mL of triethanolamine and 7 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 2 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0081] Example 9:
[0082] Preparation of polyimide membrane surface modifier:
[0083] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0084] S2. Add an appropriate amount of deionized water to the production tank, add 18 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 20 min, and cool to room temperature; continue to add 2 g of sodium chloride and stir for 15 min until completely dissolved to obtain a mixed solution;
[0085] S3. Add 40 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Add 25 mL of triethanolamine and 7 g of quaternized polyvinyl imidazole and dissolve them fully. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 1 hour. Dispense the mixture to obtain a polyimide membrane surface modifier.
[0086] Performance Testing
[0087] Test Example 1: PI Metallization Treatment
[0088] The polyimide film surface modifier prepared in Example 1 was added to the whole hole groove (the amount of polyimide film surface modifier added was based on the ability to immerse the PI board), and then the PI board was added and immersed at a temperature of 58°C for 5 minutes, followed by water washing, micro-etching (30°C, 120s), water washing, pre-dipping (room temperature, 100s), activation (40°C, 300s), water washing, acceleration (45°C, 120s), water washing, and copper deposition (30°C, 15min). The copper crystallization, pore wall detachment and backlight were then observed.
[0089] After the PI board was metallized with the polyimide film surface modifier prepared in Example 1, the SEM image of copper crystals on the PI board was shown as follows: Figure 1 ,from Figure 1 It can be seen that the copper crystals are fine and dense after the metallization treatment of the polyimide film surface modifier; after the PI metallization treatment, the PI board hole wall floating diagram is shown in Figure 2 , backlight detection diagram see Figure 3 ,from Figure 2 、 3 It can be seen that the PI board treated with metallization of the polyimide film surface modifier has no pore wall floating and the backlight is qualified.
[0090] Comparative Example 1:
[0091] Preparation of polyimide membrane surface modifier:
[0092] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0093] S2. Add an appropriate amount of deionized water to the production tank, add 18 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 2 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0094] S3. Add 40 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 40 mL of triethanolamine and 7 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 2 hours. Then divide the mixture into portions to obtain a polyimide membrane surface modifier.
[0095] The obtained polyimide film surface modifier was used for PI metallization treatment. The specific operation steps of PI metallization treatment were the same as those in Experimental Example 1. The hole wall lift-off diagram of the PI board after metallization treatment is shown in FIG. Figure 4 , backlight detection diagram see Figure 5 ,from Figure 4 、 5 It can be seen that after the PI board is metallized, the hole wall is separated and the backlight is unqualified.
[0096] Comparative Example 2:
[0097] Preparation of polyimide membrane surface modifier:
[0098] S1. Dissolve potassium hydroxide in deionized water to prepare a potassium hydroxide solution with a mass concentration of 20%, cool it, and set aside;
[0099] S2. Add an appropriate amount of deionized water to the production tank, add 18 mL of hydrazine hydrate, stir evenly, and cool to room temperature; add 90 g of diethylenetriamine, stir for 30 min, and cool to room temperature; continue to add 2 g of sodium chloride and stir for 12 min until completely dissolved to obtain a mixed solution;
[0100] S3. Add 40 mL of the 20% potassium hydroxide solution obtained in S1 to the mixed solution obtained in S2 and stir evenly. Then add 10 mL of triethanolamine and 7 g of quaternized polyvinyl imidazole and dissolve them completely. Then add 2.5 g of TX-100 and stir evenly. Add water to 10 L and filter through a 5" filter cotton core for 2 hours. Dispense the mixture to obtain a polyimide membrane surface modifier.
[0101] The obtained polyimide film surface modifier was used for PI metallization treatment, and the specific operation steps of PI metallization treatment were the same as those in Experimental Example 1. The PI board after metallization treatment also showed pore wall separation, and the backlight was unqualified.
[0102] Comparative Example 3:
[0103] The traditional PI metallization treatment process is adopted, and the specific steps are as follows: polyimide film plasma treatment, roughening, PI adjuster treatment (PI adjuster is potassium hydroxide), hole filling (58°C, 5min, the hole filling agent is the common commercially available product DS-122), water washing, micro-etching (30°C, 120s), water washing, pre-dip (room temperature, 100s), activation (40°C, 300s), water washing, acceleration (45°C, 120s), water washing, and copper deposition (30°C, 15min).
[0104] The hole wall of the PI board processed by the traditional PI metallization process is shown in the figure Figure 6 , backlight detection diagram see Figure 7 ,from Figure 6 、 7 It can be seen that the PI board processed by the traditional PI metallization process has no hole wall floating and the backlight is qualified.
[0105] According to the above test method, the polyimide film surface modifiers prepared in Examples 2-9 were used in sequence to perform metallization treatment on the PI board. The results showed that the copper crystals of the PI board after metallization treatment with the polyimide film surface modifiers prepared in Examples 2-9 were fine, there was no pore wall detachment, and the backlight was qualified.
[0106] The preferred embodiments of this patent are described in detail above. However, this patent is not limited to the above embodiments. Other variations or modifications can be made within the knowledge of ordinary technicians in this field. It is not necessary and impossible to list all embodiments here. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of this invention should be included in the scope of protection of the claims of this invention.
Claims
1. A polyimide film surface modifier, characterized in that: In terms of concentration, it includes: Amines: 9.0-10.0 g / L; Quaternized polyvinyl imidazole: 0.7-0.8g / L; Inorganic salts: 0.2-0.4g / L; Alkylphenol polyoxyethylene ether: 0.25-0.35g / L; Reducing agent: 1.8-2.5mL / L; Inorganic alkali: 0.8-1.0g / L; Alcoholamines: 2.5-3.5mL / L; The rest is deionized water; The reducing agent is hydrazine hydrate; The alcoholamine is triethanolamine; The volume ratio of the reducing agent to the alcohol amine is 1: - ; The amine is diethylenetriamine; The inorganic salt is at least one of sodium chloride, potassium chloride and magnesium chloride; The alkylphenol polyoxyethylene ether is at least one of OP-10, TX-100, and TX-10; The inorganic base is one or both of potassium hydroxide and sodium hydroxide.
2. The method for preparing a polyimide film surface modifier according to claim 1, wherein: The steps include: S1. Dissolve the inorganic base in deionized water to prepare a solution with a mass concentration of 20%, cool it, and set aside; S2. Add an appropriate amount of deionized water to the production tank, add a reducing agent, stir evenly, and cool to room temperature; add amines, stir for 20-40 minutes, and cool to room temperature; continue to add inorganic salts, stir for 8-15 minutes until completely dissolved, to obtain a mixed solution; S3. Add the 20% inorganic base solution obtained in S1 to the mixed solution obtained in S2, stir evenly, add alcoholamines and quaternized polyvinyl imidazole, and after they are fully dissolved, add alkylphenol polyoxyethylene ether, stir evenly, add water to the liquid level, filter, and package to obtain a polyimide membrane surface modifier.
3. The preparation method according to claim 2, characterized in that In S3, the filtration is performed using a 5" filter cotton core for 1-3 hours.
4. Use of the polyimide film surface modifier according to claim 1 in metallization treatment of the polyimide film surface.
Citation Information
Patent Citations
KR1016600350000B1