A hardening solution, an apf hardening film and a preparation method

Abstract

This application provides a curing liquid, an APF curing film, and a preparation method thereof, relating to the field of optical film technology. The curing liquid of this application comprises, by weight parts: 10-20 parts of a first acrylic resin; 2-10 parts of a second acrylic resin; 2-8 parts of a diluent monomer; 0.05-0.5 parts of filler; 0.5-3 parts of a photoinitiator; and 10-90 parts of solvent. The first acrylic resin contains hydrophilic groups, and the second acrylic resin contains polyether segments, polyester segments, and high molecular weight alkyl C6-C... 12 At least one of the long chain segments. The hardening liquid, APF hardening film, and preparation method of the embodiments of this application can be used to harden multilayer structure films such as APF base films with low corrosion; the obtained APF hardening film can be directly bonded to the frame adhesive in subsequent processes, and is not prone to wrinkles and cracks, thus meeting the requirements of practical use.

Description

Technical Field

[0001] This application relates to the field of optical film technology, and more specifically, to a curing liquid, an APF curing film, and a preparation method thereof. Background Technology

[0002] An APF (Advanced Polarizing Film) is a multilayer film structure that combines birefringent materials with Bragg reflective films to achieve light reflection in a specific direction. APFs are typically formed by alternating layers of refractive and dielectric layers on a substrate layer. The core layer consists of alternating layers of birefringent material and a homogeneous dielectric layer. Total internal reflection of light in a specific direction is achieved through the refractive index difference. This structure can replace traditional linear polarizers, effectively blocking light from a specific direction while maintaining light transmittance.

[0003] In the field of display technology, APF (Optical Part Formulator) base film is used as an optical film in liquid crystal display modules to enhance display effects. The APF base film is typically laminated together with an absorptive polarizer onto the lower glass substrate of the display to improve backlight utilization efficiency. During use, the APF base film is often bonded using frame adhesive, but the substrate itself is not chemically resistant. Furthermore, with the increasing thinning of polarizers, when thin APF base films are stacked with prism films in the backlight module, they are prone to rupture, thus affecting backlight performance. Therefore, the APF base film needs to undergo a hardening treatment to give it a certain degree of chemical resistance and hardness.

[0004] However, using conventional hardening liquid for hardening treatment can easily corrode chemically insensitive substrates, causing peeling, whitening, and other phenomena; it can also affect the subsequent frame adhesive bonding; in addition, since the APF base film is a multi-layered film, it is very easy for wrinkles and cracks to occur during later use. Summary of the Invention

[0005] The purpose of this application is to provide a hardening liquid, an APF hardening film, and a preparation method, which can be used to harden multilayer structure films such as APF base films with minimal corrosion; the obtained APF hardening film can be directly bonded to the frame adhesive in subsequent processes, and is not prone to wrinkles and cracks, thus meeting practical application requirements.

[0006] In a first aspect, embodiments of this application provide a hardening liquid, the components of which, by weight, include: 10-20 parts of the first acrylic resin; 2-10 parts of the second acrylic resin; Dilute the monomer to 2-8 parts; 0.05-0.5 parts of filler; Photoinitiator 0.5-3 parts; Solvent 10-90 parts; The first acrylic resin contains hydrophilic groups, and the second acrylic resin contains polyether segments, polyester segments, and high molecular weight alkyl C6-C... 12 At least one of the long-chain segments; the solvent includes at least one of benzene-based solvents and ether-based solvents.

[0007] In the above technical solution, the components of the hardening liquid include a first acrylic resin and a second acrylic resin. The first acrylic resin contains hydrophilic groups, and the second acrylic resin contains polyether segments, polyester segments, and high molecular weight alkyl C6-C... 12 The curing solution, containing long-chain flexible segments, is used to harden multilayer membranes such as the APF base film. The curing solution then solidifies to form a hardened layer. By introducing hydrophilic groups and flexible segments into the two acrylic resins mentioned above, the curing solution exhibits good water absorption, ensuring that the water bonding and dyne value of the hardened APF membrane meet certain requirements, allowing for direct subsequent frame bonding. Furthermore, it has low shrinkage, effectively reducing wrinkles and cracks caused by shrinkage of the layers in the hardened APF base film and other multilayer membranes under high and low temperature conditions, as well as high temperature and high humidity conditions. The solvent contains a certain amount of weakly corrosive solvents (benzene-based solvents and ether solvents), which reduces the corrosion of the APF base film and other multilayer membranes during the curing process.

[0008] Meanwhile, the curing liquid also contains a small amount of filler, which can separate the APF base film from the prism film in the backlight module. This can effectively solve the problem of rupture and adhesion caused by the lamination of the thin APF base film and the prism film in the backlight module under high and low temperature conditions and high temperature and high humidity conditions.

[0009] In one possible implementation, the hydrophilic groups in the first acrylic resin include one or more of hydroxyl, amino, carboxyl, and amide groups.

[0010] In one possible implementation, the filler comprises one or more of polymethylsilsesquioxane, silica, magnesium oxide, aluminum oxide, zirconium oxide, calcium oxide, barium sulfate, calcium sulfate, and strontium sulfate; And / or, the particle size of the filler is 0.5-3 μm, optionally 1-2 μm.

[0011] In the above technical solution, micron-level fillers are selected, which can effectively solve the problems of rupture and adhesion caused by the lamination of the APF base film and the prism film in the backlight module.

[0012] In one possible implementation, the solvent further includes at least one of ester solvents and ketone solvents.

[0013] In the above technical solution, the solvent also contains a certain amount of corrosive solvent (ester solvent, ketone solvent) to ensure the formation of the hardening liquid.

[0014] In one possible implementation, the diluting monomer comprises one or more of pentaerythritol hexaacrylate, pentaerythritol triacrylate, ethoxyethyl acrylate, trimethylolpropane triacrylate, hexanediol diacrylate, isobornyl acrylate, trimethylolpropane trimethacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate, and triisocyanurate triacrylate.

[0015] In one possible implementation, the photoinitiator is selected from one or more of cleavage-type initiators and hydrogen-abstracting initiators; the cleavage-type initiators include 2-hydroxy-2-methylphenylacetone, 1-hydroxycyclohexylbenzophenone, 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)butanone, and phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide; the hydrogen-abstracting initiators include benzophenone, 4-methylbenzophenone, and 2,4,6-trimethylbenzophenone.

[0016] In one possible implementation, the solvent includes one or more of ethyl acetate, butyl acetate, toluene, xylene, propylene glycol methyl ether, dipropylene glycol methyl ether, acetone, butanone, cyclohexanone, methyl isobutyl ketone, isopropanol, and isobutanol.

[0017] Secondly, embodiments of this application provide a method for preparing the hardening liquid provided in the first aspect, which involves mixing the components of the hardening liquid to form a hardening liquid.

[0018] Thirdly, embodiments of this application provide an APF curing film, which includes an APF base film and a curing layer, wherein the curing layer is formed by curing with the curing liquid provided in the first aspect.

[0019] In one possible implementation, the thickness of the APF base film can be 25-60 μm; The thickness of the hardened layer is 1-5 μm.

[0020] Fourthly, embodiments of this application provide a method for preparing the APF hardened film provided in the third aspect, which involves coating the surface of the APF base film with the hardening liquid and then curing it.

[0021] In one possible implementation, the curing method includes: first, heat drying, followed by UV curing, wherein the heat drying temperature is 40-90°C, and the UV curing energy is 250-350 mJ / cm².2 . Detailed Implementation

[0022] APF (Advanced Polarizing Film) is a multilayer film structure that combines birefringent materials with Bragg reflective films to achieve light reflection in a specific direction. During use, the APF base film is often bonded using adhesive, but the APF base film itself is not chemically resistant; furthermore, with the increasing thinning of polarizers, thin APF base films are prone to puncture. Therefore, a hardening treatment is required for the APF base film, typically by coating its surface with a hardening liquid, thereby giving it a certain degree of chemical resistance and hardness.

[0023] Using conventional curing solutions to harden the APF base film can affect the subsequent frame adhesive bonding process. The applicant's analysis revealed that the APF base film needs to meet certain requirements for water bonding and dyne value after the curing solution is applied to ensure that the APF base film will not affect the subsequent frame adhesive bonding process after the curing treatment.

[0024] On the other hand, after conventional curing treatment, environmental testing (such as high-temperature environment testing and high-temperature and high-humidity environment testing) results show that the APF base film is extremely prone to wrinkling and cracking. The applicant found that this is because: as a multilayer film structure, the APF base film is prone to wrinkling and cracking due to the large stress differences between the layers.

[0025] Therefore, it is necessary to design a curing liquid that can be used to harden APF base film, so that the treated APF base film will not affect the subsequent frame adhesive bonding process, and will not easily develop wrinkles and cracks, thus meeting the requirements of actual use.

[0026] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0027] The following provides a detailed description of the hardening liquid, APF hardening film, and preparation method of the embodiments of this application.

[0028] This application provides a curing liquid, which, by weight, comprises: 10-20 parts of a first acrylic resin; 2-10 parts of a second acrylic resin; 2-8 parts of a diluent monomer; 0.05-0.5 parts of a filler; 0.5-3 parts of a photoinitiator; and 10-90 parts of a solvent. The first acrylic resin contains hydrophilic groups, and the second acrylic resin contains flexible segments, such as polyether segments, polyester segments, and high molecular weight alkyl C6-C segments. 12 At least one of the long-chain segments; the solvent includes at least one of benzene-based solvents and ether-based solvents. Exemplarily, the components of the curing liquid, by weight, include: 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts of a first acrylic resin or any intermediate number between two of the above values; 2 parts, 4 parts, 6 parts, 8 parts, 10 parts of a second acrylic resin or any intermediate number between two of the above values; 2 parts, 4 parts, 6 parts, 8 parts of a diluent monomer or any intermediate number between two of the above values; 0.05 parts, 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts of filler or any intermediate number between two of the above values; 0.5 parts, 1 part, 2 parts, 3 parts of photoinitiator or any intermediate number between two of the above values; and 10 parts, 30 parts, 50 parts, 70 parts, 90 parts of solvent or any intermediate number between two of the above values.

[0029] In this application, the first acrylic resin is an ultraviolet (UV) curable resin, belonging to the oligomer category of light-curable resins; the first acrylic resin can be a polyurethane acrylic resin or a polyester acrylic resin; the polyurethane acrylic resin (PUA) contains acrylate functional groups (CH2=CR-C(O)-O-, R=-H or -CH3) and urethane groups (-NH-C(O)-O-); the polyester acrylic resin is composed of polyester segments and acrylate segments linked by chemical bonds. The first acrylic resin contains hydrophilic groups, also known as polar groups, which refer to atoms or groups of atoms that can form hydrogen bonds, ion-dipole interactions, or other strong polar interactions with water molecules.

[0030] In this application, the second acrylic resin contains flexible segments, such as polyether segments, polyester segments, and high molecular weight alkyl C6-C segments. 12 At least one of the long chain segments. Specifically, C6-C 12 Long-chain segments refer to segments containing 6-12 consecutive -CH2- groups, that is, segments containing 6, 7, 8, 9, 10, 11, or 12 consecutive -CH2- groups. In this application, the second acrylic resin does not contain hydrophilic groups.

[0031] In this embodiment, the curing liquid comprises a first acrylic resin and a second acrylic resin. The first acrylic resin contains hydrophilic groups, and the second acrylic resin contains flexible segments. After using this curing liquid to cure the multilayer structure film, including the APF base film, the curing liquid solidifies to form a cured layer. By introducing hydrophilic groups and flexible segments through the above two oligomers, it possesses good water absorption, ensuring that the water bonding and dyne value of the cured APF film meet certain requirements, allowing for direct subsequent frame bonding. Furthermore, it exhibits low shrinkage, effectively reducing wrinkles and cracks caused by shrinkage of each layer under high and low temperature conditions and high temperature and humidity conditions. Moreover, the solvent contains a certain amount of weakly corrosive solvents (benzene-based solvents, ether-based solvents), which can reduce the corrosion of the multilayer structure film, including the APF base film, during the curing process.

[0032] Meanwhile, the curing liquid also contains a small amount of filler, which can separate the APF base film from the prism film in the backlight module. This can effectively solve the problem of rupture and adhesion caused by the lamination of the thin APF base film and the prism film in the backlight module under high and low temperature conditions and high temperature and high humidity conditions.

[0033] In one possible implementation, the hydrophilic group includes one or more of the following: hydroxyl (-OH), amino (-NH2), carboxyl (-COOH), and amide (-CONH).

[0034] In this embodiment, the hydrophilic groups of the first acrylic resin are selected from the above-mentioned range, and the source of the acrylic resin is readily available.

[0035] In one embodiment, the first acrylic resin is selected from Kunshan Nairliang L612 (which is a polyester acrylic resin and contains hydrophilic groups: hydroxyl and carboxyl groups); the second acrylic resin is selected from Sartoma CN9001NS (which contains flexible segments: polyether segments).

[0036] In one possible implementation, the filler includes one or more of polymethylsilsesquioxane, silica, magnesium oxide, aluminum oxide, zirconium oxide, calcium oxide, barium sulfate, calcium sulfate, and strontium sulfate. Polymethylsilsesquioxane (PMSQ) is a multifunctional silicon-based micropowder, an organic-inorganic hybrid polymer with the general molecular formula (CH3SiO2). 1.5 ) n The particle size of the filler is 0.5-3μm, and can be selected as 1-2μm. For example, the particle size of the filler is 0.5μm, 1μm, 1.5μm, 2μm, 2.5μm, 3μm or any intermediate value between the two above.

[0037] In this embodiment, micron-sized fillers are selected, which can effectively solve the problems of rupture and adhesion caused by the stacking of the APF base film and the prism film in the backlight module.

[0038] In this application, the solvent includes at least one of the following: benzene-based solvents and ether-based solvents. For example, the solvent includes at least one of toluene, xylene, propylene glycol methyl ether, and dipropylene glycol methyl ether.

[0039] In one possible implementation, the solvent further includes a corrosive solvent: at least one of ester solvents and ketone solvents. Exemplarily, the solvent also includes at least one of ethyl acetate, butyl acetate, acetone, butanone, cyclohexanone, and methyl isobutyl ketone.

[0040] In another possible implementation, the solvent may also include a non-corrosive solvent: an alcohol solvent, and, for example, at least one of isopropanol and isobutanol.

[0041] In one possible implementation, the diluting monomer includes one or more of pentaerythritol hexaacrylate, pentaerythritol triacrylate, ethoxyethyl acrylate, trimethylolpropane triacrylate, hexanediol diacrylate, isobornyl acrylate, trimethylolpropane trimethacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate, and triisocyanurate triacrylate.

[0042] In one possible implementation, the photoinitiator is selected from one or more of the cleavage-type initiators and hydrogen-abstraction-type initiators; Among them, the cleavage initiators include one or more of the following: 2-hydroxy-2-methylphenylacetone (1173), 1-hydroxycyclohexylbenzophenone (184), 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone (907), 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (photoinitiator TPO), 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)butanone (369), and phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide (819); Among them, hydrogen abstraction initiators include one or more of benzophenone (BP), 4-methylbenzophenone, and 2,4,6-trimethylbenzophenone.

[0043] This application also provides a method for preparing the hardening liquid of the aforementioned embodiments, which involves mixing the components of the hardening liquid to form a hardening liquid.

[0044] As one embodiment, the method for preparing the curing liquid in this application includes: mixing a first acrylic resin, a second acrylic resin, a diluent monomer, and a solvent evenly, and then adding filler and photoinitiator to mix and obtain the curing liquid.

[0045] This application provides an APF curing film, which includes an APF base film and a curing layer, wherein the curing layer is formed by curing the curing liquid of the aforementioned embodiment.

[0046] In this application, the core structural layer of the APF base film is composed of two alternating layers of materials, achieving light reflection in a specific direction through multi-layer periodic arrangement. The working principle of the APF base film is based on the alternating combination of birefringent materials and homogeneous dielectric materials. By controlling the film layer thickness and refractive index difference, light in a specific polarization direction is transmitted, while light in another direction is reflected. Structurally, the APF base film typically consists of hundreds to thousands of ultrathin dielectric layers, each with a thickness of only about 0.1 micrometers. These layered structures form an optical interference effect through periodic arrangement, achieving a theoretical reflectivity of up to 99% in the visible light range (380-780nm).

[0047] In one embodiment, a hardened layer is disposed on at least one side surface of the APF base film, which is stacked with the prism film in the backlight module.

[0048] In one possible implementation, the thickness of the APF base film can be 25-60 μm. Optionally, the thickness of the APF base film can be 25-30 μm, 33-40 μm, or 55-60 μm. For example, the thickness of the APF base film is 25 μm, 30 μm, 33 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, or any intermediate value between two of the above.

[0049] In one possible implementation, the thickness of the hardening layer is 1-5 μm. For example, the thickness of the hardening layer is 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, or any intermediate value between two of the above.

[0050] In this embodiment, the curing solution of the present application is used for curing treatment, introducing hydrophilic groups and flexible segments to solve the problems of multilayer membranes under high temperature and high humidity conditions, such as the curing treatment problem of APF base membranes. The resulting APF cured membrane has excellent adhesion, a pencil hardness of 500g*HB, a water contact angle ≤90°, and a dyne value of ≥30; the appearance of the membrane surface remains unchanged under high and low temperature conditions as well as high temperature and high humidity conditions.

[0051] This application provides a method for preparing an APF hardening film according to the aforementioned embodiments. The APF hardening film includes an APF base film and a hardening layer stacked together. The corresponding preparation method is to coat the surface of the APF base film with a hardening liquid and then cure it.

[0052] In this embodiment, the APF hardening film is formed by coating a layer of hardening liquid onto the surface of the APF base film and then curing it to form a hardened layer.

[0053] In one possible implementation, the curing method includes: first, heat drying, followed by UV curing; the heat drying temperature is 40-90℃, and the UV curing energy is 250-350 mJ / cm². 2 For example, the heat drying temperature is 40°C, 50°C, 60°C, 70°C, 80°C, 90°C, or any two of the above values; the UV curing energy is 250 mJ / cm². 2 270mJ / cm 2 300mJ / cm 2 320mJ / cm 2 350mJ / cm 2 Or the midpoint between any two of the above values.

[0054] In some embodiments of this application, the curing liquid of this application can be used for surface curing treatment of APF base film. The structure of APF base film can be referred to the film structure in patent CN1170382A-Multilayer Optical Thin Film. In other embodiments, the curing liquid of this application can also be used for surface curing treatment of other multilayer structure films, such as the surface curing treatment of brightness enhancement film and the corresponding brightness enhancement curing film formed by patent CN101189546B-Brightness enhancement film. It can also solve the problem of high temperature and high humidity faced by the multilayer structure film.

[0055] The features and performance of this application will be further described in detail below with reference to the embodiments.

[0056] Example 1 This embodiment provides an APF hardening film, the preparation process of which is as follows: (1) Weigh the raw materials by weight as follows: 14 parts of primary acrylic resin (specifically Kunshan Nairliang L612); 6 parts of secondary acrylic resin (specifically Sartoma CN9001NS); 8 parts of diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of filler (specifically Yuansheng New Materials UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether). The first acrylic resin, the second acrylic resin, the diluent monomer, and the solvent were mixed evenly, and then filler and photoinitiator were added to prepare a curing liquid.

[0057] (2) The above-mentioned curing liquid was applied to the APF base film (3M base film, thickness 38μm) to form a coating. The coating was first dried at 85℃ for 2 min, and then cured with UV at an energy of 300mJ / cm. 2UV curing yields an APF hardened film, wherein the thickness of the hardened layer formed by the curing liquid coating is 4 μm.

[0058] Example 2 This embodiment provides an APF curing film, the preparation process of which differs from that of Example 1 in that: In this embodiment, (1) by weight, the following raw materials are weighed: 18 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 2 parts of the second acrylic resin (specifically Sartoma CN9001NS); 7 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0059] Example 3 This embodiment provides an APF curing film, the preparation process of which differs from that of Example 1 in that: In this embodiment, (1) by weight, the following raw materials are weighed: 10 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 10 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0060] Example 4 This embodiment provides an APF curing film, the preparation process of which differs from that of Example 1 in that: In this embodiment, (1) by weight, the following raw materials are weighed: 14 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 6 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.5 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0061] Example 5 This embodiment provides an APF curing film, the preparation process of which differs from that of Example 1 in that: In this embodiment, (1) by weight, the following raw materials are weighed: 14 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 6 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 3 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0062] Example 6 This embodiment provides an APF curing film, the preparation process of which differs from that of Embodiment 1 in that: in this embodiment, the first acrylic resin is specifically selected from Kunshan Nairliang L615 (which is a polyurethane acrylic resin and contains hydrophilic groups: amino).

[0063] Example 7 This embodiment provides an APF curing film, the preparation process of which differs from that of Embodiment 1 in that: in this embodiment, the second acrylic resin is specifically selected as Sartoma CN2302 (which contains flexible segments: polyester segments), and finally an APF curing film is obtained.

[0064] Example 8 This embodiment provides an APF hardening film, the preparation process of which differs from that of Embodiment 1 in that: in this embodiment, the filler is specifically selected as silica powder (Tosoh SS-50F from Japan), with an average particle size of 2μm, and finally an APF hardening film is obtained.

[0065] Comparative Example 1 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 20 parts of first acrylic resin (specifically Kunshan Nairliang L612); 8 parts of diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of filler (specifically Yuansheng New Material UltraShield962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally an APF curing film is obtained.

[0066] Comparative Example 2 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 20 parts of second acrylic resin (specifically, Sartoma CN9001NS); 8 parts of diluent monomer (specifically, pentaerythritol hexaacrylate); 0.1 parts of filler (specifically, UltraShield962 from Yuansheng New Materials, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of photoinitiator (specifically, 1-hydroxycyclohexyl benzophenone); 70 parts of solvent (specifically, 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally, an APF curing film is obtained.

[0067] Comparative Example 3 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 14 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 6 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0068] Comparative Example 4 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 14 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 6 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically butyl acetate), and finally the APF curing film is obtained.

[0069] Comparative Example 5 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 5 parts of the first acrylic resin (specifically Kunshan Nairliang L612); 15 parts of the second acrylic resin (specifically Sartoma CN9001NS); 8 parts of the diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of the filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of the photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of the solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally the APF curing film is obtained.

[0070] Comparative Example 6 This comparative example provides an APF curing film, the preparation process of which differs from that of Example 1 in that: in this comparative example, (1) by weight, the following raw materials are weighed: 20 parts of first acrylic resin (specifically Kunshan Nairliang L612); 1 part of second acrylic resin (specifically Sartoma CN9001NS); 8 parts of diluent monomer (specifically pentaerythritol hexaacrylate); 0.1 parts of filler (specifically Yuansheng New Material UltraShield 962, polymethyl silsesquioxane spherical powder with an average particle size of 2μm); 1.6 parts of photoinitiator (specifically 1-hydroxycyclohexyl benzophenone); 70 parts of solvent (specifically 35 parts of butyl acetate + 35 parts of propylene glycol methyl ether), and finally an APF curing film is obtained.

[0071] Performance tests were conducted on the APF hardened films of Examples 1-8 and Comparative Examples 1-6: 1. Water Contact Angle: A tiny volume (typically 1-5 microliters) of ultrapure water is gently added to a clean, flat surface of the membrane to be tested using a precision syringe. An optical system (such as a camera) captures the lateral profile image of the droplet on the solid surface. The image is then analyzed by software to measure the angle between the gas-liquid interface and the solid-liquid interface, i.e., the contact angle.

[0072] 2. Dyne value: Take a clean hardened membrane, lay it flat on a plane, and use a dyne pen with different values ​​to draw 1-2 cm on the hardened surface. The value of the pen that shrinks by no more than 10% within two seconds is the dyne value of the corresponding membrane material.

[0073] III. Stability: High and Low Temperature Testing: The hardened film is attached to a glass plate using OCA adhesive, and then a specific module is bonded to the surface of the hardened film using frame adhesive. The finished structure is kept in a high-temperature environment of 80±5℃ for 30 minutes, and then the temperature is switched to a low-temperature environment of -40±5℃ for 30 minutes within 5 minutes. This constitutes one cycle, and a total of 240 cycles are performed. After the test, the film is removed and allowed to warm up for 2 hours. The film surface is then observed: the target is no cracking, no peeling, and no whitening. High temperature and high humidity: The hardened film is attached to a glass plate using OCA adhesive, and then a specific module is bonded to the surface of the hardened film using frame adhesive. The finished structure is placed in a constant temperature and humidity chamber at 85℃ and 85%RH for 240 hours. After the test, it is removed and allowed to cool for 2 hours, and the film surface is observed: the target is no cracking, no peeling, and no whitening.

[0074] The results are shown in Table 1 below: Table 1 Performance test results of each APF hardened film

[0075] According to the results in Table 1, the APF hardened films formed in Examples 1-8 by using the hardening solution of this application exhibit excellent surface adhesion, with a water contact angle ≤90° and a dyne value of 30-34. Under high and low temperature conditions and high temperature and high humidity conditions, the film appearance remains unchanged (no peeling, no cracking, no whitening). Furthermore, in Examples 1-7, polymethylsilsesquioxane was used as the filler, while in Example 8, silicon dioxide was used. Since inorganic materials are more prone to diffuse reflection, the total reflection effect of the APF hardened films formed in Examples 1-7 is superior to that of the APF hardened film in Example 8.

[0076] The curing solution used in Comparative Example 1 did not contain the second acrylic resin, and the curing solution used in Comparative Example 3 did not contain any filler. Although the resulting APF cured films had a water contact angle ≤90° and a dyne value greater than 30, their appearance changed under high and low temperature conditions and high temperature and high humidity conditions, indicating poor stability. The curing solution used in Comparative Example 2 did not contain the first acrylic resin, and the resulting APF cured films did not meet the standards for water contact angle and dyne value. Furthermore, the appearance of the films changed (peeling) under high temperature and high humidity conditions.

[0077] Moreover, the appearance changes of Comparative Examples 1, 2 and 3 under high and low temperature and high temperature and high humidity conditions are not completely consistent, which indicates that the three raw materials (first acrylic resin, second acrylic resin and filler) have an interactive effect on the overall product performance, rather than a single effect.

[0078] In Comparative Example 4, the curing solution used was not a benzene-based solvent or an ether-based solvent, but an ester-based solvent. Consequently, the resulting APF curing film exhibited peeling and whitening appearance changes, which was due to the severe corrosion of the APF base film by the curing solution.

[0079] In Comparative Examples 5-6, the curing liquid used a relatively larger amount of the second acrylic resin and a relatively larger amount of the first acrylic resin, respectively. The appearance of the resulting APF cured film changed accordingly. This shows that the first acrylic resin and the second acrylic resin need to be used in a specific mass ratio.

[0080] In summary, the hardening liquid, APF hardening film, and preparation method of this application embodiment can be used to harden multilayer structure films such as APF base films with minimal corrosion; the obtained APF hardening film can be directly bonded to the frame adhesive in subsequent processes and is not prone to wrinkles and cracks, thus meeting practical application requirements.

[0081] The above description is merely an embodiment of this application and is not intended to limit the scope of protection of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the scope of protection of this application.

Claims

1. A hardening liquid, characterized by, By weight, its components include: 10-20 parts of the first acrylic resin; 2-10 parts of the second acrylic resin; Dilute the monomer to 2-8 parts; 0.05-0.5 parts of filler; Photoinitiator 0.5-3 parts; Solvent 10-90 parts; The first acrylic resin contains hydrophilic groups, including one or more of hydroxyl, amino, carboxyl, and amide groups. The second acrylic resin contains polyether segments, polyester segments, and high molecular weight alkyl C6-C6 segments. 12 The solvent includes at least one of the long-chain segments, and the second acrylic resin does not contain the hydrophilic group; the solvent includes at least one of benzene solvents and ether solvents.

2. The hardening liquid according to claim 1, characterized in that, The filler comprises one or more of polymethylsilsesquioxane, silicon dioxide, magnesium oxide, aluminum oxide, zirconium oxide, calcium oxide, barium sulfate, calcium sulfate and strontium sulfate; And / or, the particle size of the filler is 0.5-3 μm.

3. The hardening liquid according to claim 2, characterized in that The particle size of the filler is 1-2 μm.

4. The hardening solution of claim 1, wherein The solvent also includes at least one of ester solvents and ketone solvents.

5. The hardening solution of claim 1, wherein The diluting monomers include one or more of pentaerythritol triacrylate, ethoxyethyl acrylate, hexanediol diacrylate, isobornyl acrylate, trimethylolpropane trimethacrylate, tripropylene glycol diacrylate, dipropylene glycol diacrylate, trimethylolpropane triacrylate, dipentaerythritol hexaacrylate, and triisocyanurate triacrylate. And / or, the photoinitiator is selected from one or more of cleavage initiators and hydrogen abstraction initiators; the cleavage initiator includes 2-hydroxy-2-methylphenylacetone, 1-hydroxycyclohexylbenzophenone, 2-methyl-1-(4-methylthiophenyl)-2-morpholino-1-propanone, 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)butanone, and phenylbis(2,4,6-trimethylbenzoyl)phosphine oxide; the hydrogen abstraction initiator includes benzophenone, 4-methylbenzophenone, and 2,4,6-trimethylbenzophenone.

6. A method for preparing the hardening solution according to any one of claims 1 to 5, characterized by, It mixes the components of the hardening liquid to form the hardening liquid.

7. An APF hardened film characterized by, It includes an APF base film and a hardening layer, the hardening layer being formed by curing with a hardening liquid as described in any one of claims 1-5.

8. The APF hardened film of claim 7, wherein, The thickness of the APF base film is 25-60 μm; And / or, the thickness of the hardened layer is 1-5 μm.

9. A method for producing the APF hardened film according to claim 7 or 8, characterized by, It involves coating the surface of the APF base film with the curing liquid and then curing it.

10. The method for preparing the APF hardened film according to claim 9, characterized in that, The method for curing comprises: first heat drying, and then UV light curing, the temperature of the heat drying is 40-90℃, the energy of the UV light curing is 250-350mJ / cm 2 .

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