Optical-grade OLED supporting film and production process thereof

Abstract

The invention discloses an optical-grade OLED (Organic Light Emitting Diode) supporting film and a production process thereof, and belongs to the technical field of electronic products, modified organic silicon resin is added into an adhesive solution adopted by the optical-grade OLED supporting film, and the modified organic silicon resin is prepared by polymerizing allyl glycidyl ether and hydrogen-containing double-end-socket tetramethyl dihydrodisiloxane together, then adding an initiator, and then adding an initiator, the preparation method comprises the following steps: carrying out polymerization on organic silicon glycidyl ether, perfluorooctyl acrylic acid and carboxylated composite powder to obtain organic silicon glycidyl ether, carrying out ring opening on epoxy bonds in the organic silicon glycidyl ether, and reacting with carboxyl groups in the perfluorooctyl acrylic acid and the carboxylated composite powder to generate ester bonds; the carboxylated composite powder can be uniformly dispersed in the modified organic silicon resin, so that the cohesive force of the adhesive liquid can be enhanced, the bonding strength of the adhesive liquid can be improved, the ultraviolet aging resistance of the OLED supporting film can be effectively improved, the oxidative degradation of a polymer in the supporting film can be reduced, and the warping phenomenon can be prevented.

Description

Technical Field

[0001] The present invention belongs to the technical field of electronic products, and specifically relates to an optical-grade OLED support film and a production process thereof. Background Art

[0002] With the rapid development of flexible display technology, organic light-emitting diodes (OLEDs) have become a core component of the next-generation display due to their ultra-thin, self-luminous, and bendable properties. In the multi-layer structure of flexible OLED devices, optical-grade support films, as key substrates or encapsulation layers, must simultaneously meet stringent requirements such as high transmittance, ultra-low haze, high thermal stability, and excellent mechanical flexibility.

[0003] The Chinese invention patent application with announcement number CN112680135B discloses a support film for an OLED module and a preparation method thereof, comprising a first substrate layer, an antistatic low-viscosity pressure-sensitive adhesive layer, a second substrate layer, a high-viscosity pressure-sensitive adhesive layer and an antistatic release film layer. The antistatic effect is achieved by coating a high-viscosity pressure-sensitive adhesive on the antistatic PET surface. The high-viscosity pressure-sensitive adhesive layer does not contain an antistatic agent component, thereby avoiding the antistatic agent from reducing the bonding strength of the adhesive layer, and at the same time ensuring that the high-viscosity pressure-sensitive adhesive of the support film has a low tearing static voltage, wherein the pressure-sensitive adhesive is any one of polyurethane pressure-sensitive adhesive, acrylic pressure-sensitive adhesive, silicone pressure-sensitive adhesive, rubber pressure-sensitive adhesive, hot-melt pressure-sensitive adhesive, etc.

[0004] In automotive displays, the OLED module in the display screen uses a support film. However, under high temperatures and direct sunlight in summer, the acrylic or polyurethane in the pressure-sensitive adhesive layer will undergo photodegradation, resulting in a decrease in the cohesive strength of the adhesive layer. After long-term exposure to this environment, the peel strength of the pressure-sensitive adhesive layer will decrease, resulting in local separation between the OLED display screen and the support film, and warping. Summary of the Invention

[0005] The purpose of the present invention is to provide an optical-grade OLED support film and its production process. The fluorine atoms of perfluorooctyl acrylic acid and the titanium dioxide and antimony tin oxide in the carboxylated composite powder synergistically improve the UV aging resistance of the OLED support film, reduce the oxidative degradation of the polymer in the support film, prevent the occurrence of warping, and also increase the light transmittance to meet the use requirements of the OLED module of the display screen under high temperature and strong light.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] An optical-grade OLED support film structurally comprises: a PET transparent protective film, a CPI substrate film, a processing layer, an adhesive layer and a PET blue protective film.

[0008] A production process for an optical-grade OLED support film comprises: first covering one side of a CPI substrate film with a transparent PET protective film, applying a treatment layer liquid to the other side of the CPI substrate film, drying the film, then applying an adhesive liquid to the treatment layer, drying the film, and attaching a blue PET protective film to the adhesive layer. The adhesive liquid is prepared by the following steps:

[0009] Step 1: When preparing nano titanium dioxide powder by a sol-gel method, nano tin antimony oxide powder is doped to obtain nano composite powder.

[0010] Step 2: Modify the nanocomposite powder to obtain a carboxylated composite powder, then graft allyl glycidyl ether and hydrogen-containing double-headed tetramethyldihydrodisiloxane together to obtain silicone glycidyl ether, and polymerize the silicone glycidyl ether, perfluorooctyl acrylic acid and the carboxylated composite powder together to obtain a modified silicone resin.

[0011] Step 3: Mix nitrile rubber 1072cgx, 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, ion scavenger IXE-100, antioxidant G200, accelerator EVERRNOX-10, PVP-K30 tackifying resin, KH-550, and modified silicone resin, and disperse at high speed at 30-40°C for 5-6 hours to obtain an adhesive liquid.

[0012] Furthermore, the nanocomposite powder is prepared by the following steps:

[0013] Antimony tin oxide powder with a particle size of 5-20 nm, anhydrous ethanol and tetraethyl titanate are added to a reactor and ultrasonically dispersed for 30-40 minutes. A hydrochloric acid-ethanol mixture with a concentration of 1.2 mol / L is dripped into the reactor at 40-45° C. and 300-500 r / min. Deionized water is then added, and the mixture is reacted at 140-150° C. for 8-9 hours. The mixture is cooled to room temperature, filtered, washed and dried to obtain a nanocomposite powder.

[0014] Furthermore, the dosage ratio of antimony tin oxide powder, anhydrous ethanol, tetraethyl titanate, hydrochloric acid ethanol mixture and deionized water is 0.3-0.5 g: 24-25 mL: 36-40 mL: 20-25 mL: 11-15 mL.

[0015] Furthermore, the carboxylated composite powder is prepared by the following steps:

[0016] The amino nanocomposite powder and ethanol solution are added to a reaction kettle, ultrasonically dispersed for 15-20 minutes, and then glutaric anhydride is added. The mixture is reacted at 50-60° C. and 600-800 r / min for 3-4 hours. The mixture is filtered, washed, and dried to obtain a carboxylated composite powder.

[0017] Furthermore, the usage ratio of the amino nanocomposite powder, the ethanol solution and the glutaric anhydride is 30-50 g: 2-3 L: 30-40 g.

[0018] Furthermore, the amination nanocomposite powder is prepared by the following steps:

[0019] Add nanocomposite powder, 3-aminopropyltriethoxysilane, anhydrous toluene and deionized water into a reaction kettle, ultrasonically disperse for 5-10 minutes, then dropwise add triethylamine, react at 110-120°C and 300-500 r / min for 5-6 hours, cool to room temperature, filter, and wash to obtain amino nanocomposite powder.

[0020] Furthermore, the usage ratio of the nanocomposite powder, 3-aminopropyltriethoxysilane, anhydrous toluene, deionized water and triethylamine is 50-60 g: 20-30 mL: 1-1.5 L: 10-15 mL: 5-10 mL.

[0021] Furthermore, organosilicon glycidyl ether is prepared by the following steps:

[0022] Allyl glycidyl ether and Karstedt catalyst were added to a reactor, stirred for 10-15 minutes under nitrogen protection, 65-70°C, and 300-500 r / min, and then hydrogen-containing double-headed tetramethyldihydrogen disiloxane was added dropwise. The reaction was carried out at 85-90°C for 6-8 hours. Activated carbon was added, the mixture was filtered, and distilled under reduced pressure to obtain organosilicon glycidyl ether.

[0023] Furthermore, the usage ratio of allyl glycidyl ether, Karstedt catalyst, and hydrogen-containing double-capped tetramethyldihydrogen disiloxane is 100-150 g: 0.5-1 mg: 200-300 g.

[0024] Furthermore, the modified silicone resin is prepared by the following steps:

[0025] Add silicone glycidyl ether into a reaction kettle, add a mixed solution of perfluorooctyl acrylic acid, carboxylated composite powder, tetrabutylammonium bromide and 4-methoxyphenol at 80-82°C and 300-500 r / min, and react at 90-105°C and 500-800 r / min for 3-4 hours to obtain a modified silicone resin.

[0026] Furthermore, the mass ratio of organosilicon glycidyl ether, perfluorooctyl acrylic acid, carboxylated composite powder, tetrabutylammonium bromide and 4-methoxyphenol is 100-150:230-250:20-30:2.5-2.7:0.66-1.

[0027] Furthermore, the mass ratio of nitrile rubber 1072cgx, 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, ion capture agent IXE-100, antioxidant G200, promoter EVERRNOX-10, PVP-K30 tackifying resin, KH-550 and modified silicone resin is 40-45:10-15:0.5-1:0.5-1:1-2:7-10:5-7:50-60.

[0028] Beneficial effects of the present invention:

[0029] 1. The adhesive liquid used in the optical-grade OLED support film of the present invention is added with a modified silicone resin. The modified silicone resin is obtained by first polymerizing allyl glycidyl ether and hydrogen-containing double-headed tetramethyldihydrogen disiloxane to obtain silicone glycidyl ether, and then polymerizing silicone glycidyl ether, perfluorooctyl acrylic acid and carboxylated composite powder. The strong electronegative property of the fluorine atoms of perfluorooctyl acrylic acid reduces the electron cloud density of the molecular chain and reduces ultraviolet light absorption. At the same time, the titanium dioxide in the carboxylated composite powder can also block and absorb ultraviolet rays. The antimony tin oxide therein mainly absorbs UVB and can also transfer electrons, reduce the electron-hole of titanium dioxide, and inhibit the generation of free radicals. The three can work together to effectively improve the anti-ultraviolet aging performance of the OLED support film, reduce the oxidative degradation of the polymer in the support film, prevent warping, and also improve the light transmittance to meet the use requirements of the display OLED module under high temperature and strong light.

[0030] 2. The epoxy bonds in the silicone glycidyl ether of this invention undergo ring-opening and react with the carboxyl groups in perfluorooctyl acrylate and the carboxylated composite powder to form ester bonds. This allows the carboxylated composite powder to be evenly dispersed in the modified silicone resin, helping to enhance the cohesion of the adhesive solution and improve its bonding strength. The long perfluorinated chains of perfluorooctyl acrylate reduce the hygroscopicity of the adhesive layer, balance the elastic modulus of the cross-linked system, and synergize with the carboxylated composite powder to improve interfacial stress transfer efficiency, thereby enhancing the durability of the adhesive layer.

[0031] 3. The adhesive liquid of the present invention also contains 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt, which is composed of cations and anions and achieves conductivity through ion dissociation and migration. The carboxylated composite powder is obtained by uniformly doping antimony tin oxide powder into titanium dioxide during the preparation of nano-titanium dioxide, then modifying it with 3-aminopropyltriethoxysilane to introduce amino groups, and then introducing carboxyl groups through glutaric anhydride. During the preparation of titanium dioxide, the antimony tin oxide powder is doped. The like charges between antimony tin oxide and titanium dioxide repel each other, inhibiting the van der Waals attraction between the particles and reducing agglomeration, so that the antimony tin oxide is uniformly embedded in the titanium dioxide. The antimony tin oxide can form free electron carriers, reducing surface resistance. After being compounded with titanium dioxide and then polymerized with silicone glycidyl ether, it can be evenly distributed in the cross-linked structure of the modified silicone resin, and can still maintain a stable conductive effect under low humidity.

[0032] The combined use of 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt and carboxylated composite powder can form an electron-ion dual conductive path, improving the antistatic properties of the adhesive liquid, thereby improving the overall antistatic properties of the OLED support film, helping to avoid electrostatic breakdown of the display pixel unit, and also reducing dust absorption, helping to keep the display clean. DETAILED DESCRIPTION

[0033] The following will be combined with specific embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0034] Example 1: This example provides an optical-grade OLED support film, which is prepared by the following steps:

[0035] S1: 0.4 g of antimony tin oxide powder with a particle size of 5-20 nm (commercially available, model: DK445, purchased from Beijing Dekedao Gold Technology Co., Ltd.), 24.5 mL of anhydrous ethanol and 38 mL of tetraethyl titanate were added to a reactor and ultrasonically dispersed for 35 minutes. 22.5 mL of a 1.2 mol / L hydrochloric acid-ethanol mixture was dropwise added to the reactor at 42°C and 400 r / min. Then 13 mL of deionized water was added to the reactor and reacted at 145°C for 8 hours. Antimony tin oxide can be evenly mixed in titanium dioxide. The mixture was cooled to room temperature and filtered. The precipitate was washed 4 times with dichloromethane, dried to constant weight at 55°C, and ground to obtain a nanocomposite powder.

[0036] S2: 55 g of nanocomposite powder, 25 mL of 3-aminopropyltriethoxysilane, 1.25 L of anhydrous toluene and 12.5 mL of deionized water were added to a reactor and ultrasonically dispersed for 7 minutes. Then, 7.5 mL of triethylamine was added dropwise and reacted at 115°C and 400 r / min for 5.5 hours. The mixture was cooled to room temperature and centrifuged. The precipitate was washed four times with acetone and freeze-dried to obtain an amino-containing nanocomposite powder.

[0037] S3: 40 g of amino-type nanocomposite powder and 2.5 L of ethanol solution were added to a reactor, ultrasonically dispersed for 17 min, and then 35 g of glutaric anhydride was added. The reaction was carried out at 55°C and 700 rpm for 3.5 h. The mixture was centrifuged and filtered. The precipitate was washed six times with anhydrous ethanol and freeze-dried to obtain a carboxylated composite powder.

[0038] S4: 125 g of allyl glycidyl ether and 0.75 mg of Karstedt catalyst were added to the reactor, stirred for 12 min under nitrogen protection, 67 ° C and 400 r / min, and then 250 g of hydrogen-containing double-headed tetramethyldihydrogen disiloxane was dropped into it. The temperature was raised to 87 ° C at a rate of 10 ° C / h and the reaction was carried out for 7 h. The Si-H bond in the hydrogen-containing double-headed tetramethyldihydrogen disiloxane reacted with the carbon-carbon double bond at the end of allyl glycidyl ether to form a Si-C bond. Activated carbon adsorption catalyst was added and decolorized, filtered, and distilled under reduced pressure to obtain silicone glycidyl ether.

[0039] S5: 125 g of silicone glycidyl ether was added to a reactor, and a uniformly mixed solution of 240 g of perfluorooctyl acrylic acid, 25 g of carboxylated composite powder, 2.6 g of tetrabutylammonium bromide and 0.8 g of 4-methoxyphenol was added at 81°C and 400 r / min. The mixture was reacted at 97°C and 650 r / min for 3.5 hours. The epoxy bond in the silicone glycidyl ether was ring-opened and reacted with the carboxyl group in the perfluorooctyl acrylic acid and the carboxylated composite powder to form an ester bond, thereby obtaining a modified silicone resin.

[0040] S6: 42.5 g of nitrile rubber 1072cgx, 12.5 g of 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, 0.75 g of ion scavenger IXE-100, 0.75 g of antioxidant G200, 1.5 g of accelerator EVERRNOX-10, 8.5 g of PVP-K30 tackifying resin, 6 g of KH-550 and 55 g of modified silicone resin were added to a reactor and dispersed using a high-speed disperser at 35° C. for 5.5 h to obtain an adhesive liquid.

[0041] S7: Covering one side of the CPI substrate film with a transparent PET protective film, applying a treatment layer liquid to the other side of the CPI substrate film, drying it to form a treatment layer, then applying an adhesive liquid on the treatment layer, drying it to form an adhesive layer, and attaching a blue PET protective film to the adhesive layer to obtain an optical-grade OLED support film;

[0042] The thicknesses of the PET transparent protective film, CPI substrate film, treatment layer, adhesive layer and PET blue protective film are 25 μm, 75 μm, 10 μm, 15 μm and 25 μm, respectively.

[0043] The raw materials of the treatment layer liquid include 30g zirconium oxide, 10g 3-methyl-2-pentanone, 10g methyl ether, 15g 1-methoxy-2-propanol, 12g cyclohexanone, 25g CMC2200, and 1g pentaerythritol triacrylate.

[0044] Example 2: This example provides an optical-grade OLED support film, which is prepared by the following steps:

[0045] S1: 0.3 g of antimony tin oxide powder with a particle size of 5-20 nm (commercially available, model: DK445, purchased from Beijing Dekedaojin Technology Co., Ltd.), 24 mL of anhydrous ethanol and 36 mL of tetraethyl titanate were added to a reactor and ultrasonically dispersed for 30 minutes. 20 mL of a 1.2 mol / L hydrochloric acid-ethanol mixture was dripped into the reactor at 40°C and 300 r / min. Then 11 mL of deionized water was added to the reactor and reacted at 140°C for 8 hours. Antimony tin oxide can be evenly mixed in titanium dioxide. The mixture was cooled to room temperature and filtered. The precipitate was washed three times with dichloromethane, dried to constant weight at 50°C, and ground to obtain a nanocomposite powder.

[0046] S2: 50 g of nanocomposite powder, 20 mL of 3-aminopropyltriethoxysilane, 1 L of anhydrous toluene and 10 mL of deionized water were added to a reactor and ultrasonically dispersed for 5 minutes. Then, 5 mL of triethylamine was added dropwise and reacted at 110°C and 300 r / min for 5 hours. The mixture was cooled to room temperature and centrifuged. The precipitate was washed three times with acetone and freeze-dried to obtain an amino-containing nanocomposite powder.

[0047] S3: 30 g of amino-type nanocomposite powder and 2 L of ethanol solution were added to a reactor, ultrasonically dispersed for 15 min, and then 30 g of glutaric anhydride was added. The mixture was reacted at 50°C and 600 rpm for 3 h. The mixture was centrifuged and filtered. The precipitate was washed five times with anhydrous ethanol and freeze-dried to obtain a carboxylated composite powder.

[0048] S4: 100 g of allyl glycidyl ether and 0.5 mg of Karstedt catalyst were added to the reactor, stirred for 10 min under nitrogen protection, 65 ° C and 300 r / min, and then 200 g of hydrogen-containing double-headed tetramethyldihydrogen disiloxane was dropped into it. The temperature was raised to 85 ° C at a rate of 10 ° C / h and the reaction was carried out for 6 h. The Si-H bond in the hydrogen-containing double-headed tetramethyldihydrogen disiloxane reacted with the carbon-carbon double bond at the end of allyl glycidyl ether to form a Si-C bond. Activated carbon adsorption catalyst was added and decolorized, filtered, and distilled under reduced pressure to obtain silicone glycidyl ether.

[0049] S5: 100 g of silicone glycidyl ether was added to a reactor, and a uniformly mixed solution of 230 g of perfluorooctyl acrylic acid, 20 g of carboxylated composite powder, 2.5 g of tetrabutylammonium bromide and 0.66 g of 4-methoxyphenol was added at 80°C and 300 r / min. The mixture was reacted at 90°C and 500 r / min for 3 h. The epoxy bond in the silicone glycidyl ether was ring-opened and reacted with the carboxyl group in the perfluorooctyl acrylic acid and the carboxylated composite powder to form an ester bond, thereby obtaining a modified silicone resin.

[0050] S6: 40 g of nitrile rubber 1072cgx, 10 g of 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, 0.5 g of ion scavenger IXE-100, 0.5 g of antioxidant G200, 1 g of accelerator EVERRNOX-10, 7 g of PVP-K30 tackifying resin, 5 g of KH-550 and 50 g of modified silicone resin were added to a reactor and dispersed using a high-speed disperser at 30° C. for 5 h to obtain an adhesive liquid.

[0051] S7: Covering one side of the CPI substrate film with a transparent PET protective film, applying a treatment layer liquid to the other side of the CPI substrate film, drying it to form a treatment layer, then applying an adhesive liquid on the treatment layer, drying it to form an adhesive layer, and attaching a blue PET protective film to the adhesive layer to obtain an optical-grade OLED support film;

[0052] The thicknesses of the PET transparent protective film, CPI substrate film, treatment layer, adhesive layer and PET blue protective film are 25 μm, 75 μm, 10 μm, 15 μm and 25 μm, respectively.

[0053] The raw materials of the treatment layer liquid include 30g zirconium oxide, 10g 3-methyl-2-pentanone, 10g methyl ether, 15g 1-methoxy-2-propanol, 12g cyclohexanone, 25g CMC2200, and 1g pentaerythritol triacrylate.

[0054] Example 3: This example provides an optical-grade OLED support film, which is prepared by the following steps:

[0055] S1: 0.5 g of antimony tin oxide powder with a particle size of 5-20 nm (commercially available, model: DK445, purchased from Beijing Dekedaojin Technology Co., Ltd.), 25 mL of anhydrous ethanol and 40 mL of tetraethyl titanate were added to a reactor and ultrasonically dispersed for 40 minutes. 25 mL of a 1.2 mol / L hydrochloric acid-ethanol mixture was dripped into the reactor at 45°C and 500 r / min. Then 15 mL of deionized water was added to the reactor and reacted at 150°C for 9 hours. Antimony tin oxide can be evenly mixed in titanium dioxide. The mixture was cooled to room temperature and filtered. The precipitate was washed 5 times with dichloromethane, dried to constant weight at 60°C, and ground to obtain a nanocomposite powder.

[0056] S2: 60 g of nanocomposite powder, 30 mL of 3-aminopropyltriethoxysilane, 1.5 L of anhydrous toluene and 15 mL of deionized water were added to a reactor and ultrasonically dispersed for 10 min. 10 mL of triethylamine was then added dropwise. The mixture was reacted at 120°C and 500 rpm for 6 h. The mixture was cooled to room temperature and centrifuged. The precipitate was washed five times with acetone and freeze-dried to obtain an amino-containing nanocomposite powder.

[0057] S3: 50 g of amino-type nanocomposite powder and 3 L of ethanol solution were added to a reactor, ultrasonically dispersed for 20 min, and then 40 g of glutaric anhydride was added. The reaction was carried out at 60°C and 800 rpm for 4 h. The mixture was centrifuged and filtered. The precipitate was washed 8 times with anhydrous ethanol and freeze-dried to obtain a carboxylated composite powder.

[0058] S4: 150 g of allyl glycidyl ether and 1 mg of Karstedt catalyst were added to the reactor, stirred for 15 min under nitrogen protection, 70 ° C and 500 r / min, and then 300 g of hydrogen-containing double-headed tetramethyldihydrogen disiloxane was dropped into it. The temperature was raised to 90 ° C at a rate of 10 ° C / h and the reaction was carried out for 8 h. The Si-H bond in the hydrogen-containing double-headed tetramethyldihydrogen disiloxane reacted with the carbon-carbon double bond at the end of allyl glycidyl ether to form a Si-C bond. Activated carbon adsorption catalyst was added and decolorized, filtered, and distilled under reduced pressure to obtain silicone glycidyl ether.

[0059] S5: 150 g of silicone glycidyl ether was added to a reactor, and a uniformly mixed solution of 250 g of perfluorooctyl acrylic acid, 30 g of carboxylated composite powder, 2.7 g of tetrabutylammonium bromide and 1 g of 4-methoxyphenol was added at 82°C and 500 r / min. The mixture was reacted at 105°C and 800 r / min for 4 hours. The epoxy bond in the silicone glycidyl ether was ring-opened and reacted with the carboxyl group in the perfluorooctyl acrylic acid and the carboxylated composite powder to form an ester bond, thereby obtaining a modified silicone resin.

[0060] S6: 45 g of nitrile rubber 1072cgx, 15 g of 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, 1 g of ion scavenger IXE-100, 1 g of antioxidant G200, 2 g of accelerator EVERRNOX-10, 10 g of PVP-K30 tackifying resin, 7 g of KH-550 and 60 g of modified silicone resin were added to a reactor and dispersed using a high-speed disperser at 40° C. for 6 h to obtain an adhesive liquid.

[0061] S7: Covering one side of the CPI substrate film with a transparent PET protective film, applying a treatment layer liquid to the other side of the CPI substrate film, drying it to form a treatment layer, then applying an adhesive liquid on the treatment layer, drying it to form an adhesive layer, and attaching a blue PET protective film to the adhesive layer to obtain an optical-grade OLED support film;

[0062] The thicknesses of the PET transparent protective film, CPI substrate film, treatment layer, adhesive layer and PET blue protective film are 25 μm, 75 μm, 10 μm, 15 μm and 25 μm, respectively.

[0063] The raw materials of the treatment layer liquid include 30g zirconium oxide, 10g 3-methyl-2-pentanone, 10g methyl ether, 15g 1-methoxy-2-propanol, 12g cyclohexanone, 25g CMC2200, and 1g pentaerythritol triacrylate.

[0064] Comparative Example 1: Based on Example 1, the carboxylation composite powder was removed in step S5, and the remaining steps remained unchanged to prepare an optical-grade OLED support film.

[0065] Comparative Example 2: Based on Example 1, the antimony tin oxide powder was removed from step S1 to prepare nano titanium dioxide powder and replace the subsequent nano composite powder. The remaining steps remained unchanged to prepare an optical-grade OLED support film.

[0066] Comparative Example 3: Based on Example 1, commercially available acrylic acid (purchased from Jinan Xinchen Chemical Co., Ltd.) was used instead of perfluorooctyl acrylic acid in step S5, and the other steps remained unchanged to prepare an optical-grade OLED support film.

[0067] Comparative Example 4: Based on Example 1, 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide salt was removed from step S6, and the remaining steps remained unchanged to prepare an optical-grade OLED support film.

[0068] The optical-grade OLED support films in Examples 1-3 and Comparative Examples 1-3 were subjected to performance tests, and the test results are as follows:

[0069] Anti-UV aging performance: The UV aging test was conducted in an artificial aging chamber. The aging procedure was set according to the cycle 1 in the ASTM G154-06 standard. The optical grade OLED support film sample was placed in an accelerated aging chamber with multiple lamps and exposed to 0.89W / m 2 The samples were irradiated with UVA-340 fluorescent light (UVA-340) at 340 nm irradiance. All samples were irradiated with UV light at 60°C for 8 hours, followed by condensation at 50°C for 4 hours, and this cycle was repeated multiple times. After artificial aging for 24 hours, 300 hours, and 600 hours, the samples were removed to analyze changes in the tensile properties of the optical-grade OLED support film during the aging process.

[0070] Peel strength: tested using a universal testing machine (Instron 5966) in accordance with IPC-TM-6502.4.6.

[0071] Antistatic performance: The surface resistivity of the optical-grade OLED support film was measured using a digital resistivity meter at a test voltage of 500V and an ambient temperature of 20°C.

[0072] Table 1 Test results of optical grade OLED support film

[0073] project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 24h elongation at break (%) 60.8 61.7 61.4 51.2 58.1 55.1 61.5 300h elongation at break (%) 54.1 54.5 55.1 30.2 49.2 41.8 54.7 600h elongation at break (%) 51.6 52.7 52.1 10.1 38.9 22.5 51.9 Peel strength (N / mm) 0.86 0.90 0.87 0.51 0.86 0.67 0.85 Surface resistivity (Ω / sq) <![CDATA[3.4×10 13 ]]> <![CDATA[3.2×10 13 ]]> <![CDATA[3.5×10 13 ]]> <![CDATA[4.0×10 14 ]]> <![CDATA[4.1×10 14 ]]> <![CDATA[5.8×10 13 ]]> <![CDATA[3.9×10 14 ]]>

[0074] As can be seen from Table 1, when Examples 1-3 are irradiated under ultraviolet light, the 24h elongation at break, the 300h elongation at break, and the 600h elongation at break are all greater than those of Comparative Examples 1, 2, and 3. In step S5 of Comparative Example 1, the carboxylated composite powder is removed, which illustrates that the carboxylated composite powder can enhance the ultraviolet aging resistance of the optical-grade OLED support film. In step S1 of Comparative Example 2, the antimony tin oxide powder is removed to prepare nano titanium dioxide powder. In step S5 of Comparative Example 3, commercially available acrylic acid is used instead of perfluorooctyl acrylic acid, and the ultraviolet aging resistance decreases. This illustrates that the carboxylated composite powder, antimony tin oxide powder, and perfluorooctyl acrylic acid play a synergistic role in improving the ultraviolet aging resistance of the optical-grade OLED support film.

[0075] The peel strength in Examples 1-3 is greater than that in Comparative Examples 1 and 3. In step S5 of Comparative Example 1, the carboxylated composite powder is removed, and in step S5 of Comparative Example 3, commercially available acrylic acid is used instead of perfluorooctyl acrylic acid. This shows that the carboxylated composite powder and perfluorooctyl acrylic acid can jointly enhance the bonding strength of the adhesive liquid, thereby improving the peel strength of the optical-grade OLED support film.

[0076] The surface resistivity in Examples 1-3 is lower than that in Comparative Example 1, Comparative Example 2, and Comparative Example 4. In step S5 of Comparative Example 1, the carboxylated composite powder is removed, and in step S1 of Comparative Example 2, the tin antimony oxide powder is removed to prepare nano titanium dioxide powder. In step S6 of Comparative Example 4, 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt is removed, indicating that zinc tin antimony oxide powder and 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt can synergistically improve the antistatic properties of the optical-grade OLED support film.

[0077] It should be noted that, in this document, terms such as "comprises", "includes" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements that are inherent to such process, method, article or apparatus.

[0078] While the embodiments of the present invention have been shown and described, it will be apparent to those skilled in the art that various changes, modifications, substitutions, and alterations can be made to the embodiments without departing from the principles and spirit of the invention.

Claims

1. A production process for an optical-grade OLED support film, comprising: First, a PET transparent protective film is covered on one side of a CPI substrate film, a treatment layer liquid is applied to the other side of the CPI substrate film and dried, and then an adhesive liquid is applied to the treatment layer and dried, and a PET blue protective film is attached to the adhesive layer. The adhesive liquid is prepared by the following steps: Step 1: When preparing nano titanium dioxide powder by a sol-gel method, nano tin antimony oxide powder is doped to obtain nano composite powder; Step 2: modifying the nanocomposite powder to obtain a carboxylated composite powder, grafting allyl glycidyl ether and hydrogen-containing double-headed tetramethyldihydrogen disiloxane together to obtain silicone glycidyl ether, and polymerizing the silicone glycidyl ether, perfluorooctyl acrylic acid and the carboxylated composite powder together to obtain a modified silicone resin; Step 3: Mix nitrile rubber 1072cgx, 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, ion scavenger IXE-100, antioxidant G200, accelerator EVERRNOX-10, PVP-K30 tackifying resin, KH-550, and modified silicone resin, and disperse at high speed at 30-40°C for 5-6 hours to obtain an adhesive liquid.

2. The production process of an optical-grade OLED support film according to claim 1, characterized in that: The nanocomposite powder in step 1 is prepared by the following steps: Antimony tin oxide powder with a particle size of 5-20 nm, anhydrous ethanol and tetraethyl titanate are added to a reactor and ultrasonically dispersed for 30-40 minutes. A hydrochloric acid-ethanol mixture with a concentration of 1.2 mol / L is dripped into the reactor at 40-45° C. and 300-500 r / min. Deionized water is then added, and the mixture is reacted at 140-150° C. for 8-9 hours. The mixture is cooled to room temperature, filtered, washed and dried to obtain a nanocomposite powder.

3. The production process of an optical-grade OLED support film according to claim 2, characterized in that: The dosage ratio of the antimony tin oxide powder, anhydrous ethanol, tetraethyl titanate, hydrochloric acid ethanol mixture and deionized water is 0.3-0.5 g: 24-25 mL: 36-40 mL: 20-25 mL: 11-15 mL.

4. The production process of an optical-grade OLED support film according to claim 1, characterized in that: The carboxylated composite powder in step 2 is prepared by the following steps: Add the amino nanocomposite powder and ethanol solution into a reaction kettle, ultrasonically disperse for 15-20 minutes, then add glutaric anhydride, react at 50-60°C and 600-800 r / min for 3-4 hours, filter, wash, and dry to obtain a carboxylated composite powder; The usage ratio of the amino nano-composite powder, the ethanol solution and the glutaric anhydride is 30-50 g: 2-3 L: 30-40 g.

5. The production process of an optical-grade OLED support film according to claim 4, characterized in that: The amino nanocomposite powder is prepared by the following steps: Add nanocomposite powder, 3-aminopropyltriethoxysilane, anhydrous toluene and deionized water into a reaction kettle, ultrasonically disperse for 5-10 minutes, then dropwise add triethylamine, react at 110-120°C and 300-500 r / min for 5-6 hours, cool to room temperature, filter, and wash to obtain amino nanocomposite powder; The dosage ratio of the nano composite powder, 3-aminopropyltriethoxysilane, anhydrous toluene, deionized water and triethylamine is 50-60 g: 20-30 mL: 1-1.5 L: 10-15 mL: 5-10 mL.

6. The production process of an optical-grade OLED support film according to claim 1, characterized in that: The organosilicon glycidyl ether in step 2 is prepared by the following steps: Allyl glycidyl ether and Karstedt catalyst were added to a reactor, stirred for 10-15 minutes under nitrogen protection at 65-70°C and 300-500 r / min, and then hydrogen-containing double-capped tetramethyldihydrogen disiloxane was added dropwise. The mixture was reacted at 85-90°C for 6-8 hours, and activated carbon was added. The mixture was filtered and distilled under reduced pressure to obtain organosilicon glycidyl ether. The usage ratio of the allyl glycidyl ether, the Karstedt catalyst and the hydrogen-containing double-capped tetramethyldihydrogen disiloxane is 100-150 g: 0.5-1 mg: 200-300 g.

7. The production process of an optical-grade OLED support film according to claim 1, characterized in that: The modified silicone resin in step 2 is prepared by the following steps: Add silicone glycidyl ether into a reaction kettle, add a mixed solution of perfluorooctyl acrylic acid, carboxylated composite powder, tetrabutylammonium bromide and 4-methoxyphenol at 80-82°C and 300-500 r / min, and react at 90-105°C and 500-800 r / min for 3-4 hours to obtain a modified silicone resin.

8. The production process of an optical-grade OLED support film according to claim 7, characterized in that: The mass ratio of the organosilicon glycidyl ether, perfluorooctyl acrylic acid, carboxylated composite powder, tetrabutylammonium bromide and 4-methoxyphenol is 100-150:230-250:20-30:2.5-2.7:0.66-1.

9. The production process of an optical-grade OLED support film according to claim 1, characterized in that: The mass ratio of the nitrile rubber 1072cgx, 1-ethyl-3-methylimidazole bis(trifluoromethanesulfonyl)imide salt, ion capture agent IXE-100, antioxidant G200, accelerator EVERRNOX-10, PVP-K30 tackifying resin, KH-550 and modified silicone resin described in step three is 40-45:10-15:0.5-1:0.5-1:1-2:7-10:5-7:50-60.

10. An optical-grade OLED support film, characterized in that: The optical-grade OLED support film is prepared by the production process of any one of claims 1 to 9.