Photosensitive dry film material and preparation method thereof
By using modified silica and epoxy double sealing heads in photosensitive dry film materials, the flexible -Si-O-Si-link and benzene ring structure is introduced, and the performance degradation caused by plasticizer migration is solved, and the mechanical properties and stability of the material are significantly improved.
Patent Information
- Application Number
- CN202411053771.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-01
- Publication Date
- 2025-03-21
- Estimated Expiration
- 2044-08-01
AI Technical Summary
When existing photosensitive dry film materials are used in high temperature, ultraviolet, humid and oxidized environments, plasticizers are prone to migrating, resulting in a degradation of performance.
By using modified silica and epoxy double caps in photosensitive dry film materials, flexible-Si-O-Si-link and benzene ring structures are introduced to enhance the toughening effect, and compatibility and dispersion are improved by modifying silica.
The tensile strength, elongation and hardness of the photosensitive dry film material are significantly improved, and its stability and performance under different environmental conditions are enhanced.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of photosensitive dry films and relates to a photosensitive dry film material and a preparation method thereof. Background Art
[0002] Photosensitive dry film, also known as photoresist dry film, consists of three parts: 1. The polyester film layer has a certain hardness, plays a protective role and serves as a photosensitive layer carrier; 2. The photosensitive layer / resist layer, as the main part of the photosensitive dry film, has the main functions of resisting etching, electroplating and masking; 3. The polyethylene film layer mainly acts as a protective film to isolate dust and avoid damage to the photosensitive layer caused by mechanical scratches or film rolling. Among them, the photosensitive layer is mainly composed of a polymer adhesive, a photopolymerizable compound, a photoinitiator and an auxiliary agent. The auxiliary agent is generally a plasticizer, a thermal inhibitor, a colorant, etc. The existing photosensitive dry film adds a plasticizer to improve its performance. It can improve the rheology of the polymerization system or reduce the brittle components. Typical plasticizers include dioctyl phthalate, butyl benzyl phthalate, di-sec-octyl phthalate and dibutyl phthalate, etc., but the ester organic compound usually does not react chemically with the polymer, but increases the plasticity of the dry film through physical action, and it is generally a non-volatile high-boiling point liquid, which is extremely difficult to volatilize and will remain in the system. When it is used in an environment of high temperature, ultraviolet rays, humidity, oxidation, etc., the plasticizer in the system will migrate, which is easy to cause a decrease in the performance of the photosensitive dry film. Summary of the invention
[0003] The object of the present invention is to provide a photosensitive dry film material having excellent tensile strength, elongation at break and hardness.
[0004] The purpose of the present invention can be achieved through the following technical solutions:
[0005] A photosensitive dry film material comprises the following components by weight: 60-65 parts of acrylate, 20-24 parts of photosensitive monomer, 8-10 parts of modified silicon dioxide, 1.5-2.3 parts of plasticizer and 0.4-0.6 parts of photoinitiator.
[0006] As a preferred technical solution of the present invention, the photosensitive monomer is triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.0-2.5:3.3-3.8:4-5.
[0007] The invention discloses a method for preparing the acrylic ester, comprising the following steps: in an inert atmosphere, after mixing a solvent and an initiator, adding tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate, heating and stirring, to obtain an acrylic resin;
[0008] As a preferred technical solution of the present invention, the inert atmosphere is a nitrogen atmosphere; the heating and stirring is stirring at a temperature of 70-75°C for 5-6h; the mass ratio of the solvent, initiator, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 28-30: 0.40-0.42: 3.3-3.5: 2.0-2.3: 0.30-0.34: 4.2-4.6; the solvent is diethylene glycol methyl ethyl ether; and the initiator is azobisisobutyronitrile.
[0009] The invention discloses a preparation method of the plasticizer, which comprises the following steps: mixing epoxy double-capped end and aminostyrene, adding a catalyst, heating and stirring, and obtaining the plasticizer.
[0010] As a preferred technical solution of the present invention, in the preparation of the plasticizer, the heating and stirring is stirring at a speed of 300-400 r / min and 50-60° C. for 1-2 hours; the catalyst is one or more of stannous octoate, dibutyltin dilaurate and dibutyltin dimaleate; in the preparation method of the plasticizer, the molar ratio of the epoxy double head and aminostyrene is 1:2.0-2.2; and the aminostyrene is 4-aminostyrene.
[0011] The present invention discloses a method for preparing the modified silicon dioxide, comprising the following steps:
[0012] 1) placing nano-silicon dioxide in anhydrous ethanol and stirring and mixing, adding a silane coupling agent and mixing, heating and stirring, filtering and removing the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain a preform;
[0013] 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica.
[0014] As a preferred technical solution of the present invention, in step 1), the stirring and mixing is stirring at a speed of 600-1000r / min for 30-45min; the heating and stirring is stirring at a temperature of 60-75°C for 5-8h; the alcohol washing is washing with anhydrous ethanol for 3 times; and the temperature of the vacuum drying is 70-80°C.
[0015] As a preferred technical solution of the present invention, in step 1), the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 15-18:50-60:4-6; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 80-100nm.
[0016] As a preferred technical solution of the present invention, in step 2), the wavelength of the ultraviolet irradiation is 365nm; the stirring and mixing is stirring at a speed of 300-400r / min and a temperature of 35-45°C for 3-5h; the alcohol washing is washing with anhydrous ethanol for 3 times; and the temperature of the vacuum drying is 70-80°C.
[0017] As a preferred technical solution of the present invention, in step 2), the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 12-15:40-50:2.4-3.0:1.8-2.0:0.5-0.8:0.12-0.14; the photoinitiator is photoinitiator 651.
[0018] As a preferred technical solution of the present invention, the epoxy double cap is 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane.
[0019] Beneficial effects of the present invention:
[0020] The present invention modifies the epoxy double head so that it participates in the polymerization reaction in the dry film system and introduces a flexible -Si-O-Si- chain link and a rigid benzene ring structure, which can absorb energy when subjected to impact force, thereby achieving a strengthening and toughening effect. In addition, the present invention modifies silicon dioxide to increase its compatibility and dispersibility in the dry film system, thereby improving the tensile strength, elongation at break and hardness of the film material. DETAILED DESCRIPTION
[0021] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the specific implementation methods, structures, features and effects of the present invention are described in detail below in combination with the embodiments.
[0022] Example 1
[0023] A photosensitive dry film material comprises the following components in parts by weight: 60 parts of acrylate, 20 parts of photosensitive monomer, 8 parts of modified silicon dioxide, 1.5 parts of plasticizer and 0.4 parts of photoinitiator; wherein the photosensitive monomer is triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.0:3.3:4; and the photoinitiator is IRGACURE OXE03.
[0024] The preparation method of the acrylic acid ester comprises the following steps: in a nitrogen atmosphere, after mixing a solvent and an initiator, adding tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate, stirring at 70°C for 5 hours, to obtain an acrylic resin; the mass ratio of diethylene glycol methyl ethyl ether, azobisisobutyronitrile, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 28:0.40:3.3:2.0:0.30:4.2;
[0025] The preparation method of the plasticizer comprises the following steps: mixing epoxy double-capped plasticizer and aminostyrene, adding stannous octoate and stirring at 300 r / min and 50° C. for 1 hour to obtain the plasticizer; wherein the molar ratio of the epoxy double-capped plasticizer to 4-aminostyrene is 1:2.0;
[0026] The preparation method of the modified silicon dioxide comprises the following steps:
[0027] 1) Place nano-silicon dioxide in anhydrous ethanol and stir and mix, add a silane coupling agent and mix, heat and stir, filter and remove the filtrate, wash with alcohol, and vacuum dry to constant weight to obtain a preform; wherein the stirring and mixing is stirring at a speed of 600 r / min for 30 minutes; the heating and stirring is stirring at a temperature of 60° C. for 5 hours; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 70° C., the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 15:50:4; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 80 nm.
[0028] 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, mixing the mixture, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica; wherein the wavelength of the ultraviolet irradiation is 365 nm; the stirring and mixing is stirring at a speed of 300 r / min and a temperature of 35° C. for 3 hours; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 70° C.; the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 12:40:2.4:1.8:0.5:0.12; and the photoinitiator is photoinitiator 651.
[0029] Example 2
[0030] A photosensitive dry film material comprises the following components in parts by weight: 62 parts of acrylate, 21 parts of photosensitive monomer, 8.7 parts of modified silicon dioxide, 1.8 parts of plasticizer and 0.45 parts of photoinitiator; wherein the photosensitive monomer is triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.2:3.5:4.3; and the photoinitiator is IRGACURE OXE03.
[0031] The preparation method of the acrylic acid ester comprises the following steps: in a nitrogen atmosphere, after mixing a solvent and an initiator, adding tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate, stirring at a temperature of 72° C. for 5.3 hours, to obtain an acrylic resin; the mass ratio of diethylene glycol methyl ethyl ether, azobisisobutyronitrile, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 29:0.41:3.4:2.1:0.31:4.3;
[0032] The preparation method of the plasticizer comprises the following steps: mixing epoxy double-capped plasticizer and aminostyrene, adding stannous octoate, stirring at a speed of 330 r / min and 53° C. for 1.3 h, and obtaining the plasticizer; wherein the molar ratio of the epoxy double-capped plasticizer to 4-aminostyrene is 1:2.1;
[0033] The preparation method of the modified silicon dioxide comprises the following steps:
[0034] 1) Place nano-silicon dioxide in anhydrous ethanol and stir and mix, add a silane coupling agent and mix, heat and stir, filter and remove the filtrate, wash with alcohol, and vacuum dry to constant weight to obtain a preform; wherein the stirring and mixing is stirring at a speed of 730 r / min for 35 minutes; the heating and stirring is stirring at a temperature of 65° C. for 6 hours; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 73° C., the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 16:53:4.7; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 87 nm.
[0035] 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, mixing the mixture, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica; wherein the wavelength of the ultraviolet irradiation is 365 nm; the stirring and mixing is stirring at a speed of 330 r / min and a temperature of 38° C. for 3.7 h; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 73° C.; the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 13:43:2.6:1.9:0.6:0.13; and the photoinitiator is photoinitiator 651.
[0036] Example 3
[0037] A photosensitive dry film material comprises the following components in parts by weight: 63 parts of acrylate, 23 parts of photosensitive monomer, 9.3 parts of modified silicon dioxide, 2 parts of plasticizer and 0.5 parts of photoinitiator; wherein the photosensitive monomer is triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.3:3.6:4.7; and the photoinitiator is IRGACURE OXE03.
[0038] The preparation method of the acrylic acid ester comprises the following steps: in a nitrogen atmosphere, after mixing a solvent and an initiator, adding tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate, stirring at a temperature of 73° C. for 5.7 hours, to obtain an acrylic resin; the mass ratio of diethylene glycol methyl ethyl ether, azobisisobutyronitrile, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 29:0.41:3.4:2.2:0.34:4.5;
[0039] The preparation method of the plasticizer comprises the following steps: mixing epoxy double-capped plasticizer and aminostyrene, adding stannous octoate and stirring at 360 r / min and 57° C. for 1.7 h to obtain the plasticizer; wherein the molar ratio of the epoxy double-capped plasticizer to 4-aminostyrene is 1:2.1;
[0040] The preparation method of the modified silicon dioxide comprises the following steps:
[0041] 1) Place nano-silicon dioxide in anhydrous ethanol and stir and mix, add a silane coupling agent and mix, heat and stir, filter and remove the filtrate, wash with alcohol, and vacuum dry to constant weight to obtain a preform; wherein the stirring and mixing is stirring at a speed of 860r / min for 40min; the heating and stirring is stirring at a temperature of 70°C for 7h; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 77°C, the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 17:57:5.3; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 90nm.
[0042] 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica; wherein the wavelength of the ultraviolet irradiation is 365nm; the stirring and mixing is stirring at a speed of 360r / min and a temperature of 42°C for 4.5h; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 77°C; the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 14:47:2.8:1.9:0.7:0.13; and the photoinitiator is photoinitiator 651.
[0043] Example 4
[0044] A photosensitive dry film material comprises the following components in parts by weight: 65 parts of acrylate, 24 parts of photosensitive monomer, 10 parts of modified silicon dioxide, 2.3 parts of plasticizer and 0.6 parts of photoinitiator; wherein the photosensitive monomer is triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.5:3.8:5; and the photoinitiator is IRGACURE OXE03.
[0045] The preparation method of the acrylic acid ester comprises the following steps: in a nitrogen atmosphere, after mixing a solvent and an initiator, adding tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate, stirring at a temperature of 75° C. for 6 hours, to obtain an acrylic resin; the mass ratio of diethylene glycol methyl ethyl ether, azobisisobutyronitrile, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 30:0.42:3.5:2.3:0.34:4.6;
[0046] The preparation method of the plasticizer comprises the following steps: mixing epoxy double-capped end and 4-aminostyrene, adding stannous octoate and stirring at 400 r / min and 60° C. for 2 hours to obtain the plasticizer; wherein the molar ratio of the epoxy double-capped end to 4-aminostyrene is 1:2.2;
[0047] The preparation method of the modified silicon dioxide comprises the following steps:
[0048] 1) Place nano-silicon dioxide in anhydrous ethanol and stir and mix, add a silane coupling agent and mix, heat and stir, filter and remove the filtrate, wash with alcohol, and vacuum dry to constant weight to obtain a preform; wherein the stirring and mixing is stirring at a speed of 1000 r / min for 45 minutes; the heating and stirring is stirring at a temperature of 75° C. for 8 hours; the alcohol washing is washing with anhydrous ethanol for 3 times; the vacuum drying temperature is 80° C., the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 18:60:6; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 100 nm.
[0049] 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, mixing the mixture, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica; wherein the wavelength of the ultraviolet irradiation is 365 nm; the stirring and mixing is stirring at a speed of 400 r / min and a temperature of 45° C. for 5 hours; the alcohol washing is washing with anhydrous ethanol for 3 times; the temperature of the vacuum drying is 80° C.; the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 15:50:3.0:2.0:0.8:0.14; and the photoinitiator is photoinitiator 651.
[0050] Comparative Example 1
[0051] Compared with Example 4, Comparative Example 1 is different in that aniline replaces 4-aminostyrene, and the other components, preparation steps and parameters are the same.
[0052] Comparative Example 2
[0053] Compared with Example 4, Comparative Example 2 is different in that 4-aminostyrene is not used, and the other components, preparation steps and parameters are the same.
[0054] Comparative Example 3
[0055] Compared with Example 4, Comparative Example 3 is different in that vinyltrimethoxysilane is not used, and the remaining components, preparation steps and parameters are the same.
[0056] Comparative Example 4
[0057] Compared with Example 4, Comparative Example 4 is different in that n-butyl phosphate is not used, and the remaining components, preparation steps and parameters are the same.
[0058] Comparative Example 5
[0059] Compared with Example 4, Comparative Example 5 is different in that glycidyl methacrylate is not used, and the other components, preparation steps and parameters are the same.
[0060] The dry film materials obtained from Examples 1-4 and Comparative Examples 1-5 were tested as follows. The test results are shown in Table 1.
[0061] Mechanical properties test: The tensile strength and elongation at break of the film cured by the photosensitive composition were measured using a UTM5000 electronic universal testing machine. Samples with a size of 20 mm × 10 mm × 0.5 mm were used, and the crosshead speed was set to 10 mm / min. Each sample was measured three times, and the average value was calculated as the final result.
[0062] Hardness test: Test and rating are carried out in accordance with GB / T 6739-1996. The higher the rating number, the better the performance.
[0063] Table 1
[0064]
[0065]
[0066] From the test results in Table 1, it can be seen that compared with Comparative Examples 1-5, the mechanical properties of the photosensitive dry film material prepared in Examples 1-4 after curing into a film are significantly better than those of Comparative Examples 1-5.
[0067] From the comparative analysis of Examples 1-4 and Comparative Examples 1-2 in combination with Table 1, it can be seen that the lack of the benzene ring structure and active vinyl group of aminostyrene leads to a decrease in the mechanical properties of the film after formation. This is because the vinyl and benzene ring structures are grafted onto the epoxy double head, enabling it to participate in the polymerization reaction in the system and increase the interfacial bonding force between it and other components. At the same time, the introduction of flexible -Si-O-Si- chain segments has the effect of enhancing toughness, thereby improving the mechanical properties of the film material.
[0068] From the comparative analysis of Examples 1-4 and Comparative Example 3 in combination with Table 1, it can be seen that the lack of vinyltrimethoxysilane to modify the silica and the lack of introduction of vinyl groups reduce the coverage rate of styrene and glycidyl methacrylate on the silica, and its compatibility in the dry film system is reduced, and the mechanical properties of the film material are reduced.
[0069] From the comparative analysis of Examples 1-4 and Comparative Examples 4-5 in combination with Table 1, it can be seen that the epoxy group contained in glycidyl methacrylate can further improve the dispersibility and compatibility of silica with the plasticizer in the dry film system, and n-butyl phosphate can inhibit the self-polymerization reaction of glycidyl methacrylate. The two work together to effectively improve the reaction grafting rate of silica, introduce more organic groups and active groups on the surface of silica, increase the bonding degree of silica in the dry film system, and improve the mechanical properties.
[0070] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Although the present invention has been disclosed as a preferred embodiment as above, it is not used to limit the present invention. Any technical personnel in this field can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A photosensitive dry film material, characterized in that: The photosensitive dry film material comprises the following components by weight: 60-65 parts of acrylate, 20-24 parts of photosensitive monomer, 8-10 parts of modified silicon dioxide, 1.5-2.3 parts of plasticizer and 0.4-0.6 parts of photoinitiator; wherein the preparation method of the plasticizer comprises the following steps: after mixing epoxy double cap and aminostyrene, adding a catalyst and heating and stirring to obtain the material; the heating and stirring is stirring at a speed of 300-400r / min and 50-60°C for 1-2h; the catalyst is one or more of stannous octoate, dibutyltin dilaurate and dibutyltin dimaleate; the molar ratio of the epoxy double cap and aminostyrene is 1:2.0-2.2; the aminostyrene is 4-aminostyrene; The preparation method of the modified silicon dioxide comprises the following steps: 1) placing nano-silicon dioxide in anhydrous ethanol and stirring and mixing, adding a silane coupling agent and mixing, heating and stirring, filtering and removing the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain a preform; 2) adding anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and a photoinitiator to the preform, stirring and mixing under ultraviolet irradiation, filtering to remove the filtrate, washing with alcohol, and vacuum drying to constant weight to obtain modified silica.
2. A photosensitive dry film material according to claim 1, characterized in that: The photosensitive monomers are triethylene glycol diacrylate, pentaerythritol triacrylate and tetrahydrofuran methacrylate in a mass ratio of 2.0-2.5:3.3-3.8:4-5.
3. The photosensitive dry film material according to claim 1, characterized in that: The preparation method of the acrylic ester comprises the following steps: in an inert atmosphere, a solvent and an initiator are mixed, and tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate are added, and the mixture is heated and stirred to obtain an acrylic resin.
4. A photosensitive dry film material according to claim 3, characterized in that: The inert atmosphere is a nitrogen atmosphere; the heating and stirring is stirring at a temperature of 70-75°C for 5-6 hours; the mass ratio of the solvent, initiator, tricyclodecyl methyl acrylate, methacrylic acid, styrene and glycidyl methacrylate is 28-30: 0.40-0.42: 3.3-3.5: 2.0-2.3: 0.30-0.34: 4.2-4.6; the solvent is diethylene glycol methyl ethyl ether; and the initiator is azobisisobutyronitrile.
5. The photosensitive dry film material according to claim 1, characterized in that: In step 1), the stirring and mixing is stirring at a speed of 600-1000 r / min for 30-45 min; the heating and stirring is stirring at a temperature of 60-75° C. for 5-8 h; the alcohol washing is washing with anhydrous ethanol for 3 times; and the temperature of the vacuum drying is 70-80° C.
6. The photosensitive dry film material according to claim 1, characterized in that: In step 1), the mass ratio of the nano-silicon dioxide, anhydrous ethanol and silane coupling agent is 15-18:50-60:4-6; the silane coupling agent is vinyltrimethoxysilane; and the particle size of the nano-silicon dioxide is 80-100 nm.
7. The photosensitive dry film material according to claim 1, characterized in that: In step 2), the wavelength of the ultraviolet irradiation is 365nm; the stirring and mixing is stirring at a speed of 300-400r / min and a temperature of 35-45°C for 3-5h; the alcohol washing is washing with anhydrous ethanol for 3 times; and the temperature of the vacuum drying is 70-80°C.
8. The photosensitive dry film material according to claim 1, characterized in that: In step 2), the mass ratio of the preform, anhydrous ethanol, styrene, glycidyl methacrylate, n-butyl phosphate and photoinitiator is 12-15:40-50:2.4-3.0:1.8-2.0:0.5-0.8:0.12-0.14; the photoinitiator is photoinitiator 651.
9. A method for preparing the photosensitive dry film material according to any one of claims 1 to 8.
Citation Information
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