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CN-121978864-A - Photosensitive resin high refractive index regulating and controlling method

CN121978864ACN 121978864 ACN121978864 ACN 121978864ACN-121978864-A

Abstract

The invention discloses a method for regulating and controlling a high refractive index of photosensitive resin, which comprises the steps of adding a refractive index regulator into a photosensitive resin system at 10-25 ℃ and performing ultrasonic treatment to obtain a photosensitive resin composition, wherein the refractive index regulator is alkyl orthosilicate and/or tetraalkyl titanate, curing the photosensitive resin composition through ultraviolet irradiation, and regulating curing parameters to calibrate the refractive index of the photosensitive resin composition. The photosensitive resin composition and the photosensitive resin high-refractive index regulating method provided by the invention have the advantages that the raw material components are simple, the preparation is convenient, the regulation and control of the high refractive index of 2.0 and above can be realized by the regulating and controlling action of the refractive index regulator, and the refractive index matching requirements of different optical scenes are met.

Inventors

  • CHEN YU
  • REN ZHENWEI
  • CHEN HUICHENG
  • LUO CHENGZHAO

Assignees

  • 苏州大学

Dates

Publication Date
20260505
Application Date
20251223

Claims (10)

  1. 1. A method for regulating and controlling a high refractive index of a photosensitive resin, comprising the steps of: (1) Adding a refractive index regulator into a photosensitive resin system at 10-25 ℃ and performing ultrasonic treatment to obtain a photosensitive resin composition, wherein the photosensitive resin system comprises, by weight, 50-60 parts of a base resin, 20-30 parts of a reactive diluent, 3-6 parts of a photoinitiator, 10-20 parts of a solvent and 1-5 parts of an auxiliary agent, the base resin is one or more selected from epoxy acrylate, polyurethane acrylate and polyester acrylate, the refractive index regulator is alkyl orthosilicate and/or tetraalkyl titanate, and the mass ratio of the photosensitive resin system to the refractive index regulator is (80-95) (5-20); (2) The photosensitive resin composition is cured by ultraviolet irradiation, and the refractive index of the photosensitive resin composition is calibrated by adjusting curing parameters, wherein the curing parameters comprise the ultraviolet intensity of 500-800 mJ/cm 2 , the curing time of 5-10 s and the curing temperature of 15-20 ℃.
  2. 2. The method for controlling the high refractive index of a photosensitive resin according to claim 1, wherein in the step (1), the alkyl orthosilicate is one or more selected from the group consisting of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate, and the tetraalkyl titanate is one or more selected from the group consisting of tetrabutyl titanate, tetraethyl titanate and tetraisopropyl titanate.
  3. 3. The method for controlling a high refractive index of a photosensitive resin according to claim 1, wherein in the step (1), the ultrasonic treatment of 10 to 20min is performed at a frequency of 45 to 60 kHz.
  4. 4. The method for controlling the high refractive index of a photosensitive resin according to claim 1, wherein in the step (1), when the refractive index adjuster is an alkyl orthosilicate, the alkyl orthosilicate is added to the photosensitive resin system at 10-25 ℃ and the photosensitive resin composition is obtained after ultrasonic treatment.
  5. 5. The method for controlling a high refractive index of a photosensitive resin according to claim 1, wherein in the step (1), when the refractive index modifier is a tetraalkyl titanate, a part of the photosensitive resin system and the tetraalkyl titanate are mixed at a mass ratio of (1.5-2.5): 1 at 10-25 ℃ to obtain a photosensitive resin mixed solution, and then the photosensitive resin mixed solution is mixed with another part of the photosensitive resin system, so that the mass ratio of the total mass of the photosensitive resin system and the tetraalkyl titanate is (80-95): (5-20), and the photosensitive resin composition is obtained after ultrasonic treatment.
  6. 6. The method of controlling a high refractive index of a photosensitive resin according to claim 1, wherein in the step (2), the refractive index of the cured photosensitive resin composition is measured in a wavelength range of 400 to 800 nm, and the refractive index of the cured photosensitive resin composition is not less than 2.0.
  7. 7. The photosensitive resin composition is characterized by comprising 50-60 parts by weight of a base resin, 20-30 parts by weight of a reactive diluent, 3-6 parts by weight of a photoinitiator, 10-20 parts by weight of a solvent and 1-5 parts by weight of an auxiliary agent, wherein the base resin is one or more selected from epoxy acrylate, polyurethane acrylate and polyester acrylate, the refractive index regulator is alkyl orthosilicate and/or tetraalkyl titanate, and the mass ratio of the photosensitive resin system to the refractive index regulator is (80-95): 5-20.
  8. 8. The photosensitive resin composition according to claim 7, wherein the refractive index modifier has a particle diameter of 50to 100 nm and a dispersity of 90% or more.
  9. 9. The photosensitive resin composition according to claim 7, wherein the reactive diluent is trimethylolpropane triacrylate and/or dipropylene glycol diacrylate, the photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-propanone and/or phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, the auxiliary agent comprises a leveling agent and an antioxidant, and the mass ratio of the leveling agent to the antioxidant is 1 (0.5-1.5).
  10. 10. Use of a photosensitive resin composition according to any one of claims 7-9 in AR/VR optical module assembly, display device diffusion film preparation, optical fiber sensing system packaging, optical element bonding or micro-nano structure molding.

Description

Photosensitive resin high refractive index regulating and controlling method Technical Field The invention relates to the technical field of photosensitive resin, in particular to a method for regulating and controlling a high refractive index of photosensitive resin. Background The ultraviolet light curing adhesive (comprising photosensitive resin) has the outstanding advantages of high curing rate, high bonding strength, excellent light transmission performance, environmental friendliness and the like, becomes an indispensable core material in the field of optical manufacturing, and is widely applied to key scenes such as AR/VR optical module assembly, display equipment diffusion film preparation, optical fiber sensing system encapsulation, optical element bonding, micro-nano structure molding and the like. In the application, the refractive index matching degree of the photosensitive resin and the refractive index of a substrate or an adjacent component directly determines the core performance of a product, namely the problems of increased light reflection loss, reduced imaging definition, limited viewing angle and the like caused by the mismatching of the refractive index in an AR/VR optical module seriously affect the immersion experience of a user, the optical interference such as rainbow lines, glare and the like is easily caused by the excessive difference of the refractive index of the photosensitive resin and the substrate in the preparation of a diffusion film of display equipment, the uniformity and the comfort of a display picture are reduced, the accuracy of the refractive index of the photosensitive resin is directly related with the end face reflectivity control and the signal to noise ratio in an optical fiber sensing system, which are key factors for guaranteeing the accuracy of sensing data, and the light path deviation possibly caused by the fine deviation of the refractive index in the bonding of a precise optical element affects the integral performance of the optical system. However, the existing photosensitive resin refractive index regulating technology has the defects that firstly, the regulating range is narrow, the flexibility is insufficient, and the high refractive index of more than 2.0 is difficult to reach. In the prior art, the refractive index is improved by adding high aromatic hydrocarbon ring additives such as naphthalene, anthracene derivatives and the like, but the additives are easy to cause the increase of the viscosity of a system and the deterioration of compatibility, and can only realize the adjustment of high refractive index of more than 1.60 and less than 2.00, so that the low refractive index base material cannot be adapted, and the refractive index is improved by the synergic polymerization of thiophene monomers and aromatic ring monomers, but the refractive index is more than 1.6 and is difficult to reach more than 2.0 in China patent CN 117106126A. Secondly, the adjusting precision is low. When the concentration of inorganic nano particles such as titanium dioxide is regulated, the particle agglomeration phenomenon is difficult to avoid, so that the uniformity of the refractive index is reduced, and the light transmittance is obviously reduced. Thirdly, the formula adaptability is poor and the production efficiency is low. Resin components and additive types in the existing photosensitive resin formula system are fixed, the refractive index of organic resin is generally lower than 1.5, and the resin compounding proportion and additive type screening are required to be redesigned according to base materials with different refractive index requirements, so that the formula development period is long and the universality is poor. Disclosure of Invention The invention aims to solve the technical problem that the refractive index regulation of the existing photosensitive resin is difficult to reach more than 2.0, and provides a photosensitive resin high refractive index regulation method which can realize refractive index regulation of 2.0 and more and ensure the dispersion uniformity of a system so as to adapt to the refractive index matching requirements of different optical scenes. The above object of the present invention is achieved by the following technical solutions: The first aspect of the present invention provides a method for controlling a high refractive index of a photosensitive resin, comprising the steps of: (1) Adding a refractive index regulator into a photosensitive resin system at 10-25 ℃ and performing ultrasonic treatment to obtain a photosensitive resin composition, wherein the photosensitive resin system comprises, by weight, 50-60 parts of a base resin, 20-30 parts of a reactive diluent, 3-6 parts of a photoinitiator, 10-20 parts of a solvent and 1-5 parts of an auxiliary agent, the base resin is one or more selected from epoxy acrylate, polyurethane acrylate and polyester acrylate, the refractive index regulator is alkyl orthosilicate