CN113355028A - Light-cured material, display panel and preparation method thereof - Google Patents
Light-cured material, display panel and preparation method thereof Download PDFInfo
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- CN113355028A CN113355028A CN202110778547.4A CN202110778547A CN113355028A CN 113355028 A CN113355028 A CN 113355028A CN 202110778547 A CN202110778547 A CN 202110778547A CN 113355028 A CN113355028 A CN 113355028A
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- photoinitiator
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- titanocene
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- KOMDZQSPRDYARS-UHFFFAOYSA-N cyclopenta-1,3-diene titanium Chemical compound [Ti].C1C=CC=C1.C1C=CC=C1 KOMDZQSPRDYARS-UHFFFAOYSA-N 0.000 claims abstract description 41
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- GLGHTHUJSZZNMW-UHFFFAOYSA-N cyclopenta-2,4-dien-1-ylmethylbenzene titanium(2+) Chemical compound [Ti++].C(c1ccccc1)[c-]1cccc1.C(c1ccccc1)[c-]1cccc1 GLGHTHUJSZZNMW-UHFFFAOYSA-N 0.000 claims description 3
- UFULAYFCSOUIOV-UHFFFAOYSA-N cysteamine Chemical compound NCCS UFULAYFCSOUIOV-UHFFFAOYSA-N 0.000 claims description 3
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- HUVAFPHSQFFCID-UHFFFAOYSA-N 5-chlorocyclopenta-1,3-diene titanium(2+) Chemical compound [Ti++].Cl[c-]1cccc1.Cl[c-]1cccc1 HUVAFPHSQFFCID-UHFFFAOYSA-N 0.000 claims description 2
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 2
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- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 abstract 1
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- NNAHKQUHXJHBIV-UHFFFAOYSA-N 2-methyl-1-(4-methylthiophen-2-yl)-2-morpholin-4-ylpropan-1-one Chemical compound CC1=CSC(C(=O)C(C)(C)N2CCOCC2)=C1 NNAHKQUHXJHBIV-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
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- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 2
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- HIAILPSESUQYPI-UHFFFAOYSA-N ethyl 2-cyano-3-(2,6-dimethylanilino)-3-sulfanylprop-2-enoate Chemical compound CCOC(=O)C(C#N)=C(S)NC1=C(C)C=CC=C1C HIAILPSESUQYPI-UHFFFAOYSA-N 0.000 description 2
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- HZNVUJQVZSTENZ-UHFFFAOYSA-N 2,3-dichloro-5,6-dicyano-1,4-benzoquinone Chemical compound ClC1=C(Cl)C(=O)C(C#N)=C(C#N)C1=O HZNVUJQVZSTENZ-UHFFFAOYSA-N 0.000 description 1
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- ZWWOMKXBDJOGGW-UHFFFAOYSA-N C1=CC=C[C-]1C1=CC=CC=C1.C1=CC=C[C-]1C1=CC=CC=C1.F.[Ti+2] Chemical compound C1=CC=C[C-]1C1=CC=CC=C1.C1=CC=C[C-]1C1=CC=CC=C1.F.[Ti+2] ZWWOMKXBDJOGGW-UHFFFAOYSA-N 0.000 description 1
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- OCQVVXJUPFJXIZ-UHFFFAOYSA-N carbon monoxide;cyclopenta-1,3-diene;cyclopentane;titanium Chemical group [Ti].[O+]#[C-].[O+]#[C-].C=1C=C[CH-]C=1.[CH-]1[CH-][CH-][CH-][CH-]1 OCQVVXJUPFJXIZ-UHFFFAOYSA-N 0.000 description 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/842—Containers
- H10K50/8426—Peripheral sealing arrangements, e.g. adhesives, sealants
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The application discloses a light-cured material, a display panel and a preparation method thereof. The material comprises a resin matrix, a reactive diluent, a photoinitiator and a chain transfer agent. The resin matrix is selected from acrylics, or acrylics and epoxies. The photoinitiator comprises titanocene and/or peroxides, and can also comprise a small amount of ultraviolet light. The reactive diluent is selected from acrylic and/or epoxy. The chain transfer agent is a mercapto compound. The curing reaction that this application mainly adopts visible light initiating agent to initiate the resin matrix and take place under visible light shines can avoid only adopting the phenomenon that the OLED display panel inner structure that ultraviolet curing caused is damaged by the ultraviolet ray, also can avoid the phenomenon that the temperature is too high and the OLED display panel inner structure that leads to is damaged by the heat in the induced curing process of ultraviolet ray, is favorable to improving OLED display panel's yields and prolongs its life.
Description
Technical Field
The application relates to the technical field of display, in particular to a photocuring material, a display panel and a preparation method thereof.
Background
An Organic Light Emitting Diode (OLED) has a multi-layer Organic thin film structure. Compared with a Liquid Crystal Display (LCD), the OLED device does not need to rely on backlight, can self-emit light, and has the advantages of being light and thin, high in response speed, low in power consumption and the like, so that the OLED device is widely applied to the market.
The existing rigid OLED device is often packaged by using ultraviolet curing glue which is cured under the irradiation of ultraviolet light. As shown in fig. 1, an Ultraviolet curing adhesive 300(Ultraviolet curing adhesive) is applied on the cover plate 100, and then the cover plate is bonded to the display substrate 200, and after bonding, the display substrate is sent to an Ultraviolet curing device 400 for Ultraviolet curing. Under the irradiation of the ultraviolet light emitted from the ultraviolet curing device 400, the ultraviolet curing adhesive 300 is cured, so that the cover plate 100 and the display substrate 200 are tightly combined together, thereby achieving the purpose of packaging the rigid OLED product.
However, the irradiation of ultraviolet light may cause irreversible damage to the internal structure of the OLED device, thereby reducing the yield thereof. In addition, the ultraviolet curing adhesive 300 releases heat in the curing process, so that the temperature rises, the final temperature is 60-80 ℃, the heat increases the environmental temperature during packaging, the precise structure inside the OLED device is also affected, and the service life of the OLED device is further adversely affected.
Disclosure of Invention
The application provides a light-cured material, a display panel and a preparation method thereof. The light curing material can be cured under the irradiation of visible light, so that the display substrate and the cover plate can be encapsulated. The damage of the internal structure of the OLED device caused by the irradiation of ultraviolet light when the ultraviolet curing glue is used for packaging can be avoided, and the improvement of the yield of the rigid OLED device is facilitated.
In order to achieve the purpose, the following technical scheme is adopted in the application:
the application provides a photocuring material which comprises the following components in parts by weight:
60-80 parts of resin matrix;
20-40 parts of a reactive diluent;
0.5-2 parts of a photoinitiator;
0.5-2 parts of a chain transfer agent; and
0-5 parts of an auxiliary agent.
The above "parts" represent the proportion of parts by weight of each component, and do not represent the percentage by weight of the parts by weight of each component in the photocurable material. Specifically, the term "20 to 40 parts of reactive diluent" means that the resin matrix and the reactive diluent are (60 to 80): (20 to 40), "0.5 to 2 parts of photoinitiator" means that the resin matrix and the photoinitiator are (60 to 80): (0.5 to 2), "0.5 to 2 parts of chain transfer agent" means that the resin matrix and the chain transfer agent are (60 to 80): (0.5 to 2), "and" 0 to 5 parts of auxiliary agent "means that the auxiliary agent may or may not be added, based on the resin matrix. The proportions mentioned are based on the resin matrix and the proportions of the other various components relative to the resin matrix can be freely adjusted within the ranges listed. The adjustment of the ratio of one component does not affect the adjustment of the ratio of the other component. The parts by weight mentioned below are the same. The actual weight of each part is not particularly limited, and may be, for example, 1g to 1kg, or may be adjusted depending on the scale of pilot plant, actual production, etc., as long as the ratio between the compositions is secured.
Wherein the resin matrix is selected from acrylic resin or a mixture of acrylic resin and epoxy resin. The acrylic resin is selected from the group consisting of those having the formula (C)3H4O2)nThe range of n is an integer from 200 to 1600, or is selected from fluorine-silicon modified acrylic resin (namely, the acrylic resin is subjected to fluorine-silicon modification). The epoxy resin is selected from the group consisting of those having the molecular formula (C)11H12O3)mM is an integer ranging from 5 to 30. When the resin matrix is a mixture of an acrylic resin and an epoxy resin, the ratio of the acrylic resin to the epoxy resin may be (2-4): 1 by weight. In other embodiments, the resin matrix may be present in an amount of from 62 to 78 parts by weight (based on weight), from 65 to 75 parts by weight, or from 68 to 72 parts by weight. Illustratively, if the resin matrix is 62 to 78 parts by weight, the ratio of the other components to the resin matrix may be: resin matrix and active diluent (62-78) to (22-38), resin matrix and photoinitiator (62-78) to (1-1.5), resin matrix and chain transfer agent (1-1.5)(62-78) to (1-1.5), and the light curing material also comprises an auxiliary agent, wherein the resin matrix and the auxiliary agent are (62-78) to (0.5-5). When the resin matrix is in other weight portions, the same is true.
The reactive diluent is selected from any one or a mixture of more of 1, 6-hexanediol diacrylate (HDDA), dipropylene glycol diacrylate (DPGDA), tripropylene glycol diacrylate (TPGDA), 1, 4-butanediol diglycidyl ether and hydroxyl cyclic ether (oxetane). The hydroxycyclic ethers are predominantly oxetanes, and are classified as monofunctional oxetanes and difunctional oxetanes. In other embodiments, the reactive diluent is present in an amount of 0.5 to 1.5 parts by weight.
The photoinitiator is selected from any one or two of a titanocene initiator and a peroxide initiator, or is selected from any one or two of the titanocene initiator and the peroxide initiator and the ultraviolet light photoinitiator.
In some embodiments, the titanocene-based initiator is selected from any one or a mixture of bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene (photoinitiator PI784), bis 2, 6-difluoro-3-pyrrolylphenyltitanocene (photoinitiator 784), titanocene dichloride, diphenyltitanocene fluoride, titanocene dicarbonyl, titanocene dibenzyl, and titanocene bis (trichloroacetic acid).
In some embodiments, the peroxide-based initiator is selected from any one or a mixture of benzophenone peroxyformate, xanthone peroxyformate, 2-methylindenone peroxyformate, benzothiazole peroxyformate, and t-butyl peroxy (2-ethylhexanoate).
In some embodiments, the uv photoinitiator is selected from any one or a mixture of diphenyl (2,4, 6-Trimethylbenzoyl) Phosphine Oxide (TPO), 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-methyl-1- [ 4-methylthiophenyl ] -2-morpholinyl-1-propanone, 1-hydroxy-cyclohexyl-phenyl-methanone, (1-hydroxycyclohexyl) (4- (2-hydroxyethoxy) phenyl) methanone, and hexafluorophosphate.
In some embodiments, when the photoinitiator is a mixture of a titanocene-based initiator and a peroxide-based initiator, the weight parts ratio of the titanocene-based initiator to the peroxide-based initiator is (1-5) to 1.
In some embodiments, when the photoinitiator is a mixture of any one or two of a titanocene initiator and a peroxide initiator and an ultraviolet light photoinitiator, the ratio of the weight part of any one or two of the titanocene initiator and the peroxide initiator to the weight part of the ultraviolet light photoinitiator is (8-10) to 1.
In other embodiments, the photoinitiator may be present in an amount of 1 to 1.5 parts by weight.
The chain transfer agent is a mercapto compound. The mercapto compound may be any one or a mixture of several selected from the group consisting of mercaptoethanol, mercaptopropionic acid, mercaptoethylamine, pentaerythritol tetrakis (3-mercaptobutanoate), isooctyl 3-mercaptopropionate, fluoro-bis (prop-2-yloxy) -mercaptophosphane, N- (2-mercaptoethyl) -ethyl carbamate propyl thiocarbonate, (3-prop-2-ylphenyl) N-methyl-N-mercapto-carbamate, 1, 4-butanediol bis (mercaptoacetate), 4' -dimercaptodiphenylsulfide dimethacrylate, ethyl 2-cyano-3-mercapto-3- (phenylamino) -2-acrylate, and ethyl 2-cyano-3- [ (2, 6-dimethylphenyl) amino ] -3-mercaptoacrylate. In other embodiments, the weight part of the chain transfer agent may also be 1 to 1.5 parts.
The auxiliary agent is selected from one or more of antioxidant, compatilizer, viscosity regulator and the like. In other embodiments, the amount of the additive may be 0.5 to 3 parts by weight, or 1 to 2 parts by weight.
The final viscosity of the photocurable material may be 2000 ± 200 mpa.s. The light-cured material can be applied as an interlayer bonding agent of a display panel.
The present application also provides a display panel, which includes: display substrate, apron and anchor coat. The bonding layer is positioned between the display substrate and the cover plate and is respectively attached to the display substrate and the cover plate, so that a sandwich structure is formed. The bonding layer is formed at least by the curing reaction of the light-cured material initiated by light irradiation. The illumination is mainly visible light. If the light-curing material also contains a small amount of ultraviolet light photoinitiator, then the mixed irradiation of visible light and ultraviolet light can also be adopted, but the ultraviolet light is required to avoid damaging the precise structure inside the display panel.
The application also provides a preparation method of the display panel, which comprises the following steps:
(1) forming the photocuring material between the display substrate and the cover plate, and pressing the display substrate and the cover plate;
(2) and (2) irradiating the product obtained in the step (1) at a certain temperature by adopting visible light, or performing mixed irradiation by adopting visible light and ultraviolet light to initiate a curing reaction, and obtaining the display panel after the curing reaction is finished.
Wherein, the temperature in the step (2) may be 25 ℃ to 35 ℃.
The wavelength range of visible light can be 400-700nm, and the radiation illumination can be 20-30mW/cm2Or 22-28mW/cm2The irradiation time can be 40s to 90s, or 60s to 80s, the irradiation distance is 10-20cm, and the energy and distance can be adjusted according to actual requirements in subsequent different application processes. When visible light is adopted for irradiation, the curing rate needs to reach the same level as that of the traditional ultraviolet light curing, and the determination can be carried out by testing the gel rate.
The wavelength range of the ultraviolet light is 200-375nm, and the radiation illumination can be 31-40mW/cm2The irradiation time is 10s to 30s, the irradiation distance is 10-20cm, and the irradiation distance of the ultraviolet rays and the irradiation distance of the visible light should be equal; the energy and distance can be adjusted according to actual requirements in different subsequent application processes.
The duration of the curing reaction can be between 50s and 120s, but also between 60s and 90 s.
The application adopts visible light irradiation, can slowly release heat in the curing process, but the temperature of releasing heat produced during curing of the device is not more than 45 degrees and is lower than the temperature (more than 60 degrees) in the ultraviolet curing process by more than about 15 degrees, so that the technology of the application does not need an additional cooling process.
Due to the adoption of the technical scheme, the application has the following technical effects:
the photo-curing material contains the photo-initiator which is mainly or completely a visible light type initiator, and the photo-curing material can initiate the curing reaction of a resin matrix under the irradiation of visible light through the matching of the photo-initiator with the resin matrix containing double bonds, a chain transfer agent and other components, so that the packaging between laminates of the OLED display panel is realized. Because this application mainly or all adopts the visible light irradiation to initiate the curing reaction of resin matrix, can avoid only adopting ultraviolet irradiation to initiate the inherent defect of curing reaction, consequently, this application can avoid only adopting the phenomenon that the OLED display panel inner structure that ultraviolet curing caused is damaged by ultraviolet ray, also can avoid the phenomenon that the OLED display panel inner structure that the induced curing in-process temperature of ultraviolet ray is too high (if more than 60 degrees) and leads to is damaged by the heat, thereby this application is favorable to improving OLED display panel's yields and prolongs its life.
Experimental detection proves that the temperature in the ultraviolet light induced curing process can reach more than 60 ℃, the temperature rise is caused by natural heat release in the ultraviolet light induced curing process, and the temperature is easy to thermally damage a precise structure in the OLED display panel; in addition, the temperature can be reduced by more than 15 degrees compared with ultraviolet curing by adopting visible light irradiation. Therefore, the temperature of the components in the curing process is about 45 degrees, and the phenomenon of thermal damage cannot occur.
Drawings
The technical solution and other advantages of the present application will become apparent from the detailed description of the embodiments of the present application with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of a UV-cured packaged display panel in the prior art;
fig. 2 is a schematic view of a visible light curing package display panel according to the present application.
The reference numbers are:
a cover plate 100, a display substrate 200, an ultraviolet curing adhesive 300, and an ultraviolet curing device 400.
A cover plate 10, a display substrate 20, a bonding layer 30, a visible light curing instrument 40 (or an ultraviolet-visible light curing instrument 40).
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
[ Photocurable Material ]
The application provides a light-cured material, which at least comprises the following components in parts by weight: 60-80 parts of resin matrix, 20-40 parts of reactive diluent, 0.5-2 parts of photoinitiator, 0.5-2 parts of chain transfer agent and 0-5 parts of auxiliary agent. The minimum weight part of the above-mentioned auxiliary is 0, indicating that this component may not be added. The parts by weight of the above components are merely ratios, and therefore the sum of the parts by weight of the components may be 100 parts or may not be 100 parts. When the photocurable material contains only the above components, the sum of the parts by weight of the above components is 100 parts. When the photocurable material contains other additives (such as pigments, fillers, etc.) which do not assist the curing function in addition to the above components, the sum of the parts by weight of the above components may be other than 100 parts.
< resin matrix >
The resin matrix may be selected from an acrylic resin, or a mixture of an acrylic resin and an epoxy resin. If the resin matrix is a mixture of an acrylic resin and an epoxy resin, the weight ratio of the acrylic resin to the epoxy resin may be (2-4) to 1 or 3 to 1.
The acrylic resin may be selected from those having the formula (C)3H4O2)nThe acrylic resin of (a) may be any one or a mixture of several kinds, and may also be selected from fluorosilicone-modified acrylic resins. The acrylic resin is a polymer obtained by polymerizing acrylic acid as a monomer. The value of n varies depending on the degree of polymerization. n may range from an integer from 200 to 1600. If the molecular weight of the acrylic resin is too small, the double bond content is too small,the curing speed is too slow or curing does not easily occur. If the molecular weight of the acrylic resin is too large, the double bond content is too large, the stability of itself is lowered, and long-term storage is not facilitated, and therefore, it is preferable that the range of n is selected as an integer in the range of 200 to 1600. However, in some other embodiments of the present application, n may range from 300 to 1500, from 400 to 1200, from 500 to 1000, from 600 to 900, and from 700 to 800. Illustratively, the acrylic resin may be selected from (C)3H4O2)200、(C3H4O2)600And (C)3H4O2)800Any one of (A), (B), (C) and (C) may be used as the component (A)3H4O2)200And (C)3H4O2)600A mixture of both, optionally selected from (C)3H4O2)800And (C)3H4O2)600Mixtures of both, of course, may also be selected from (C)3H4O2)200、(C3H4O2)600And (C)3H4O2)800The mixture of the three components. The same applies to the rest cases. The acrylic resin does not include an acrylic derivative resin, however, in other embodiments of the present application, an amount of the acrylic derivative resin (as a compatibilizer or viscosity modifier in an auxiliary agent, etc.) may be added to the mixed components of the photocurable material.
The epoxy resin is selected from the group consisting of those having the molecular formula (C)11H12O3)mAny one or a mixture of several of the epoxy resins of (a). The value of m varies depending on the degree of polymerization. n may be an integer of 5 to 30, an integer of 7 to 27, an integer of 9 to 25, a further integer of 10 to 23, a further integer of 11 to 22, and a further integer of 15 to 20. The molecular weight of the epoxy resin should not be too large. If the molecular weight is too large, the fluidity is poor and it is difficult to obtain a resin composition having a high fluidityUniform coating on the surface of each laminate is achieved, and uniform curing is difficult to achieve. In addition, if the molecular weight is too large, the curing rate is slow, and it is difficult to satisfy the requirements. Illustratively, the epoxy-based resin may be selected from (C)11H12O3)5、(C11H12O3)11、(C11H12O3)20And (C)11H12O3)30Any one of (A), (B), (C) and (C) may be used as the component (A)11H12O3)5And (C)11H12O3)20May also be selected from (C)11H12O3)5、(C11H12O3)11、(C11H12O3)20And (C)11H12O3)30A mixture of (a). The epoxy resin should generally be a thermosetting resin to prevent the rigid OLED device from plasticizing in the heat-generating state, thereby avoiding failure. The epoxy resin does not include the epoxy resin derivative, however, in other embodiments of the present application, an amount of the epoxy resin derivative (as a compatibilizer or viscosity regulator in the additive, etc.) may be added to the mixed components of the photocurable material. The resin matrix is 60-80 parts by weight, however, in other embodiments of the present disclosure, the resin matrix may be 62-78 parts by weight, 65-75 parts by weight, or 68-70 parts by weight.
< reactive Diluent >
The reactive diluent is a low molecular weight compound (having a molecular weight of 500 or less, including 500) which can reduce the viscosity of the mixture system and can also participate in the curing reaction of the acrylic resin or the acrylic resin and the epoxy resin to form a part of the crosslinked network structure of the cured product. The reactive diluent can be any one or a mixture of more of 1, 6-hexanediol diacrylate (HDDA), dipropylene glycol diacrylate (DPGDA), tripropylene glycol diacrylate (TPGDA), 1, 4-butanediol diglycidyl ether, and hydroxyl cyclic ether (oxetane).
The reactive diluent is 20-40 parts by weight, however, in other embodiments of the present application, the reactive diluent may be 22-38 parts by weight, or 25-35 parts by weight, or 27-32 parts by weight, or more 29-30 parts by weight.
< photoinitiator >
The photoinitiator is selected from any one or two of a titanocene initiator and a peroxide initiator, or is selected from any one or two of the titanocene initiator and the peroxide initiator and the ultraviolet light photoinitiator.
When the photoinitiator is the mixture of the titanocene initiator and the peroxide initiator, the weight ratio of the titanocene initiator to the peroxide initiator can be (1-5) to 1, or (2-5) to 1, or (2.2-4.8) to 1, or (2.5-4.5) to 1, or (3-4) to 1. Both the titanocene initiator and the peroxide initiator belong to visible light initiators. At this time, the curing reaction may be initiated entirely by irradiation with visible light.
When the photoinitiator is the mixture of any one or two of a titanocene initiator and a peroxide initiator and an ultraviolet light photoinitiator, the weight ratio of the weight parts of any one or two of the titanocene initiator and the peroxide initiator to the weight parts of the ultraviolet light photoinitiator can be (8-10) to 1, also can be (8.2-9.8) to 1, also can be (8.5-9.5) to 1, and further can be 9 to 1. In this case, a curing reaction may be initiated by a mixed irradiation of visible light and ultraviolet light. The energy of the ultraviolet lamp can be adjusted to be lower energy, and the energy of the visible lamp can be adjusted to be higher energy, so that the curing process is mainly carried out under the irradiation of visible light. This can minimize the damaging effects of ultraviolet light on delicate devices inside the rigid OLED device.
The above-mentioned titanocene photoinitiator may be selected from any one or a mixture of several of bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene (photoinitiator PI784), bis 2, 6-difluoro-3-pyrrolylphenyltitanocene (photoinitiator 784), dichlorotitanocene, fluorinated diphenyltitanocene, dicarbonyl titanocene, dibenzyltitanocene and bis (trichloroacetic acid) titanocene.
The peroxide photoinitiator may be any one or a mixture of benzophenone peroxyformate, xanthone peroxyformate, 2-methylindenone peroxyformate, benzothiazole peroxyformate and tert-butyl peroxy (2-ethylhexanoate). The titanium dioxide photoinitiator and the peroxide photoinitiator belong to visible light initiators and can initiate the curing reaction of a resin matrix under the irradiation of visible light and a certain temperature environment.
The ultraviolet light photoinitiator may be any one or a mixture of several selected from diphenyl (2,4, 6-Trimethylbenzoyl) Phosphine Oxide (TPO), 2-hydroxy-2-methyl-1-phenyl-1-propanone, 2-methyl-1- [ 4-methylthiophenyl ] -2-morpholinyl-1-propanone, 1-hydroxy-cyclohexyl-phenyl ketone, (1-hydroxycyclohexyl) (4- (2-hydroxyethoxy) phenyl) ketone and hexafluorophosphate. The hexafluorophosphate may include sodium hexafluorophosphate, lithium hexafluorophosphate, potassium hexafluorophosphate, and the like.
The photoinitiator is present in an amount of 0.5 to 2 parts by weight, however, in other embodiments of the present disclosure, the photoinitiator may be present in an amount of 0.8 to 1.8 parts by weight, 1 to 1.5 parts by weight, and 1.2 to 1.3 parts by weight.
< chain transfer agent >
The chain transfer agent is used to control the chain length of the polymer during the curing reaction and may be a mercapto compound. The mercapto compound may be selected from the group consisting of mercaptoethanol, mercaptopropionic acid, mercaptoethylamine, pentaerythritol tetrakis (3-mercaptobutanoate), isooctyl 3-mercaptopropionate, fluoro-bis (prop-2-yloxy) -mercaptophosphane, N- (2-mercaptoethyl) -ethyl carbamate propyl thiocarbonate, (3-prop-2-ylphenyl) N-methyl-N-mercapto-carbamate, 1, 4-butanediol bis (mercaptoacetate), 4' -dimercaptodiphenylsulfide dimethacrylate, 2-cyano-3-mercapto-3- (phenylamino) -2-acrylic acid ethyl ester, 2-cyano-3- [ (2, 6-dimethylphenyl) amino ] -3-mercaptoacrylic acid ethyl ester, Any one or more of sulfydryl-containing acrylate.
The amount of the chain transfer agent added is not preferably too large or too small. If the amount of the chain transfer agent added is too large, the shorter the chain of the cured polymer, the smaller the viscosity, and it is difficult to achieve a preferable curing effect. If the amount of the chain transfer agent added is too small, it is difficult to ensure a good curing effect, thereby adversely affecting the sealing tightness. Therefore, the amount of the chain transfer agent to be added is preferably in the range of 0.5 to 2 parts. However, in other embodiments herein, the weight portion of the chain transfer agent may be from 0.7 to 1.8 parts, from 1 to 1.5 parts, and from 1.2 to 1.4 parts.
< auxiliary agent >
The auxiliary agent plays a role in assisting curing, and can be selected from any one or a mixture of several of antioxidant, compatilizer, viscosity regulator and the like. The kind of the antioxidant, the compatibilizer, and the viscosity modifier is not particularly limited, and may be added as appropriate as long as other reactions which are not detrimental to the curing reaction do not occur with other components in the mixed system of the photocurable material of the present application. The assistant is 0-5 parts by weight, however, in other embodiments of the present application, the assistant can be 1-4 parts by weight, and can also be 2-3 parts by weight.
The final viscosity of the photocurable material should be maintained at 2000 ± 200mPa · s (mPa · s) regardless of whether a viscosity modifier is added. The photo-curing material under the viscosity is easy to coat on the surface of a display substrate or a cover plate, and is favorable for smooth curing reaction of each component in a system under the irradiation of visible light or the mixed irradiation of the visible light and a part of ultraviolet light, thereby realizing packaging. Therefore, the light-cured material can be used as an interlayer bonding agent of the display panel to realize bonding between various laminates (including a display substrate or a cover plate) of the display panel.
[ method for producing photocurable Material ]
The application provides a preparation method of a photocuring material, which comprises the following steps:
(1) mixing 60-80 parts of resin matrix with 20-40 parts of reactive diluent to obtain a first product;
(2) and sequentially adding 0.5-2 parts of photoinitiator, 0.5-2 parts of chain transfer agent and 0-5 parts of auxiliary agent into the first product, mixing and preparing into a mixture with the viscosity of 2000 +/-200 mpa.s, thus obtaining the photocuring material. If the weight part of the auxiliary agent is 0, the auxiliary agent is not added.
The light-cured material can be prepared in advance, then stored in a sealed light-proof and heat-insulating environment, and coated when in use, or prepared at any time on site. Since the light-curable material is easily deteriorated by a curing reaction under irradiation of visible light, the light-shielding environment is required for the storage environment.
[ display Panel ]
The present application also provides a display panel, which includes: the display device comprises a display substrate, a cover plate and a bonding layer arranged between the display substrate and the cover plate.
Wherein, the display substrate is integrated with a glass substrate and a display module. The bonding layer is respectively attached to the display substrate and the cover plate and is formed by at least the curing reaction of the photocuring material initiated by light irradiation.
[ method for producing display Panel ]
The application also provides a preparation method of the display panel, which comprises the following steps:
(1) forming a light-cured material between the display substrate and the cover plate, and pressing the display substrate and the cover plate;
(2) and (2) irradiating the product obtained in the step (1) at a certain temperature by adopting visible light, or irradiating the product by adopting visible light and ultraviolet light in a mixing way, and obtaining the display panel after the curing reaction is finished.
In step (1), the light-curable material may be coated on the lower surface of the display substrate or the upper surface of the cover plate.
In the step (1), after the coating is finished, the display substrate and the cover plate need to be pressed together with a certain pressure, so that the light-cured material is tightly attached to the display substrate and the cover plate.
In step (1), the temperature may be 25 ℃ to 35 ℃ or 27 ℃ to 32 ℃. This temperature primarily serves to initiate the initiation of the curing reaction. When the curing reaction starts, the temperature of the whole mixture system can be further increased due to the heat generated by the curing reaction, so that the curing reaction is further promoted, and finally, the complete curing is realized. Temperature measurement experiments prove that the application adopts visible light irradiation, the ambient temperature in the curing process is not more than 45 degrees, and the ambient temperature in the curing process adopting ultraviolet light irradiation in the prior art is more than 60 degrees. Therefore, the temperature during curing of the OLED display panel is obviously lower than that during curing of the prior art, and the phenomenon that the internal structure of the OLED display panel is thermally damaged due to overhigh temperature cannot occur in the curing process.
In the step (1), the wavelength range of the visible light may be 400-700nm, may also be 450-650nm, and may also be 500-600 nm. The power of the radiation illumination can be 20-30mW/cm2Or 28mW/cm2The irradiation time is 40s to 90s, or 60s, and the irradiation distance is 10-20 cm.
In the step (1), the wavelength range of the ultraviolet light is 200-375nm, and the radiation illumination is 31-40mW/cm2The irradiation time is 10 to 30s and the irradiation distance is 10-20cm, which is equal to the distance when visible light is irradiated.
In step (1), the duration of the curing reaction is 60 to 90 s.
The present application is further described below with reference to specific examples.
Example one
The present embodiment provides a photocurable material, including: 60 parts of resin matrix, 37 parts of reactive diluent, 1 part of photoinitiator, 1 part of chain transfer agent and 1 part of auxiliary agent.
Wherein the resin matrix has a molecular formula of (C)3H4O2)500And (C)3H4O2)1000A mixture of acrylic resins of (a). The reactive diluent is 1, 6-hexanediol diacrylate (HDDA). The photoinitiator is a mixture of a titanocene initiator (bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene) and a peroxide initiator (benzophenone peroxyformate), and the weight part ratio of the titanocene initiator to the peroxide initiator is 1: 1. The chain transfer agent is acrylate containing sulfhydryl. The auxiliary agent is a compatilizer. The kind of the compatibilizing agent is not particularly limited as long as it can perform a compatibilizing action.
The preparation method of the light-cured material of the embodiment comprises the following steps:
(1) mixing 60 parts of resin matrix with 37 parts of reactive diluent, and uniformly mixing by ultrasonic to obtain a first product;
(2) and sequentially adding 1 part of photoinitiator, 1 part of chain transfer agent and 1 part of auxiliary agent into the first product, and mixing to prepare a mixture with the viscosity of 2000mpa.s, thereby obtaining the photocuring material of the embodiment.
The light-cured material of the embodiment is used for packaging a display panel, and the packaging method comprises the following steps:
(1) coating the light-cured material on the surface of the cover plate to enable the coating surface to be attached to the display substrate, and then pressing the display substrate and the cover plate together at a certain pressure to form a sandwich structure;
(2) preheating the temperature of a visible light curing instrument to 30 ℃, sending the sandwich structure obtained in the step (1) into the visible light curing instrument, and irradiating by adopting visible light at the temperature of 30 ℃ to enable the light curing material to have a curing reaction. As the curing reaction is exothermic, the temperature of the entire mixture system is further increased, thereby driving the curing reaction to proceed and ultimately achieving full cure. And obtaining the display panel after the curing reaction is finished. In the embodiment, the whole process of the curing reaction ensures that the whole temperature is not more than 80 ℃, and compared with the whole temperature (more than 60 ℃) of the curing reaction initiated by ultraviolet rays under the same condition, the temperature is reduced by at least 15 ℃ and is about 45 ℃.
The results show that the cover plate and the display substrate can be tightly bonded together after the curing reaction is finished. In addition, the detection of the internal devices shows that the fine structure in the display substrate is not damaged, and the display effect meets the product quality standard.
Example two
The present embodiment provides a photocurable material, including: 67 parts of resin matrix, 29 parts of reactive diluent, 1 part of photoinitiator, 1 part of chain transfer agent and 2 parts of auxiliary agent.
Wherein the resin matrix is fluorine-silicon modified acrylic resinThe acrylic resin is modified by adopting organic silicon and organic fluorine monomers, and the mass ratio of the organic silicon to the organic fluorine monomers to the acrylic resin is 2: 1: 97. Wherein the acrylic resin part has a molecular formula of (C)3H4O2)800The acrylic resin of (1). The reactive diluent is dipropylene glycol diacrylate (DPGDA). The photoinitiator is a mixture of a titanocene initiator (bis 2, 6-difluoro-3-pyrrolylphenyltitanocene), a peroxide initiator (tert-butyl peroxy (2-ethylhexanoate)) and an ultraviolet photoinitiator (diphenyl (2,4, 6-trimethylbenzoyl) phosphine oxide, TPO). The weight ratio of the titanocene initiator to the peroxide initiator is 2: 1. The ratio of the sum of the weight parts of the titanocene initiator and the peroxide initiator (both visible light initiators) to the weight part of the ultraviolet light initiator is 10: 1. The chain transfer agent is mercapto-containing acrylate (4,4' -dimercaptodiphenyl sulfide dimethacrylate). The auxiliary agent is a viscosity regulator. The kind of the viscosity modifier is not particularly limited as long as it can perform a compatibilizing action.
The preparation method of the light-cured material of the embodiment comprises the following steps:
(1) mixing 67 parts of resin matrix with 29 parts of reactive diluent, and uniformly mixing by ultrasonic to obtain a first product;
(2) and sequentially adding 1 part of photoinitiator, 1 part of chain transfer agent and 2 parts of auxiliary agent into the first product, and mixing to prepare a mixture with the viscosity of 2000mpa.s, thereby obtaining the photocuring material of the embodiment.
The light-cured material of the embodiment is used for packaging a display panel, and the packaging method comprises the following steps:
(1) coating the light-cured material on the surface of the cover plate to enable the coating surface to be attached to the display substrate, and then pressing the display substrate and the cover plate together at a certain pressure to form a sandwich structure;
(2) preheating the ultraviolet-visible light curing instrument to 30 ℃, sending the sandwich structure obtained in the step (1) into the ultraviolet-visible light curing instrument, and performing mixed irradiation by adopting visible light and ultraviolet light at the temperature of 30 ℃ to enable the light curing material to perform curing reaction. As the curing reaction is exothermic, the temperature of the entire mixture system is further increased, thereby driving the curing reaction to proceed and ultimately achieving full cure. And obtaining the display panel after the curing reaction is finished. The whole process of the curing reaction needs to ensure that the whole temperature does not exceed 80 ℃.
In this embodiment, mainly be that visible light initiates the curing reaction, the inside precision structure of display panel can not destroyed in the visible light irradiation, simultaneously, because the irradiation intensity of visible light is little than the irradiation intensity of ultraviolet ray, can not cause destruction to display panel's inside precision structure basically, consequently, adopt ultraviolet curing and cause the phenomenon of destruction to display panel's inside precision structure among the prior art can be avoided to this embodiment. Temperature measurement experiments prove that in the embodiment, the whole process of the curing reaction ensures that the whole temperature is not more than 80 ℃, and the temperature is reduced by at least 15 ℃ compared with the whole temperature (more than 60 ℃) of the curing reaction initiated by ultraviolet rays under the same condition.
EXAMPLE III
The present embodiment provides a photocurable material, including: 75 parts of resin matrix, 20 parts of reactive diluent, 1 part of photoinitiator, 2 parts of chain transfer agent and 2 parts of auxiliary agent.
Wherein the resin matrix is a mixture of acrylic resin and epoxy resin. Wherein the acrylic resin has a molecular formula of (C)3H4O2)1200The epoxy resin is (C)11H12O3)11. The active diluent is a mixture of 1, 6-hexanediol diacrylate (HDDA) and hydroxy cyclic ether in a mass ratio of 1: 1. The photoinitiator is a mixture of a titanocene initiator (bis 2, 6-difluoro-3-pyrrolylphenyltitanocene), a peroxide initiator (tert-butyl peroxy (2-ethylhexanoate)) and an ultraviolet photoinitiator (diphenyl (2,4, 6-trimethylbenzoyl) phosphine oxide TPO and hexafluorophosphate). The weight ratio of the titanocene initiator to the peroxide initiator is 1: 1. The ratio of the sum of the weight parts of the titanocene initiator and the peroxide initiator to the weight part of the ultraviolet light photoinitiator is 8: 1. Chain transfer agentIs hydrosulfide double methacrylate (4,4' -dimercaptodiphenyl sulfide). The auxiliary agent is a viscosity regulator. The kind of the viscosity modifier is not particularly limited as long as the viscosity modifier can perform a viscosity-modifying function.
The preparation method of the light-cured material of the embodiment comprises the following steps:
(1) mixing 75 parts of resin matrix and 20 parts of reactive diluent to obtain a first product;
(2) and sequentially adding 1 part of photoinitiator, 2 parts of chain transfer agent and 2 parts of auxiliary agent into the first product, and mixing to prepare a mixture with the viscosity of 2100mpa.s, thereby obtaining the photocuring material of the embodiment.
The light-cured material of the embodiment is used for packaging a display panel, and the packaging method comprises the following steps:
(1) coating the surface of the cover plate 10 with the photocuring material of the embodiment, enabling the coating surface to be attached to the display substrate, and then pressing the display substrate 20 and the cover plate 10 together at a certain pressure to form a sandwich structure;
(2) preheating the ultraviolet-visible light curing instrument to 30 ℃, sending the sandwich structure obtained in the step (1) into an ultraviolet-visible light curing instrument 40 (shown in figure 2), and performing mixed irradiation by adopting visible light and ultraviolet light at the temperature of 30 ℃ to enable the light curing material to perform curing reaction to form the bonding layer 30. Wherein the uv lamp is adjusted to a minimum energy. As the curing reaction is exothermic, the temperature of the entire mixture system is further increased, thereby driving the curing reaction to proceed and ultimately achieving full cure. And obtaining the display panel after the curing reaction is finished. Temperature measurement experiments prove that in the embodiment, the whole process of the curing reaction ensures that the whole temperature is not more than 80 ℃, and the temperature is reduced by at least 15 ℃ compared with the whole temperature (more than 60 ℃) of the curing reaction initiated by ultraviolet rays under the same condition.
In this embodiment, mainly the visible light initiates the curing reaction, and the inside precision structure of display panel can not destroyed in the visible light irradiation, and consequently, this embodiment can avoid adopting ultraviolet curing among the prior art and cause the phenomenon of destruction to display panel's inside precision structure.
Example four
The present embodiment provides a photocurable material, including: 62 parts of resin matrix, 36 parts of reactive diluent, 1.5 parts of photoinitiator, 0.5 part of chain transfer agent and 0 part of auxiliary agent.
Wherein the resin matrix has a molecular formula of (C)3H4O2)600And (C)3H4O2)1600A mixture of acrylic resins of (a). The mixture of polypropylene resins with different molecular weights is adopted as the resin matrix, so that the degree of interchain crosslinking is better when the resin matrix is cured. The reactive diluent is 1, 6-hexanediol diacrylate (HDDA). The photoinitiator is a titanocene initiator (bis (trichloroacetic acid) titanocene). The chain transfer agent is (3-prop-2-ylphenyl) N-methyl-N-mercapto-carbamate.
The preparation method of the light-cured material of the embodiment comprises the following steps:
(1) mixing 62 parts of resin matrix with 36 parts of reactive diluent, and uniformly mixing by ultrasonic to obtain a first product;
(2) and sequentially adding 1.5 parts of photoinitiator and 0.5 part of chain transfer agent into the first product, and mixing to prepare a mixture with the viscosity of 1800mpa.s, thereby obtaining the photocuring material of the embodiment.
The light-cured material of the embodiment is used for packaging a display panel, and the packaging method comprises the following steps:
(1) coating the light-cured material on the surface of the cover plate to enable the coating surface to be attached to the display substrate, and then pressing the display substrate and the cover plate together at a certain pressure to form a sandwich structure;
(2) preheating the temperature of a visible light curing instrument to 35 ℃, sending the sandwich structure obtained in the step (1) into the visible light curing instrument, and irradiating by adopting visible light at the temperature of 35 ℃ to enable the light curing material to generate a curing reaction. As the curing reaction is exothermic, the temperature of the entire mixture system is further increased, thereby driving the curing reaction to proceed and ultimately achieving full cure. And obtaining the display panel after the curing reaction is finished. Temperature measurement experiments prove that in the embodiment, the whole process of the curing reaction ensures that the whole temperature is not more than 80 ℃, and the temperature is reduced by at least 15 ℃ compared with the whole temperature (more than 60 ℃) of the curing reaction initiated by ultraviolet rays under the same condition.
EXAMPLE five
The present embodiment provides a photocurable material, including: 75 parts of resin matrix, 22 parts of reactive diluent, 2 parts of photoinitiator, 1 part of chain transfer agent and 0 part of auxiliary agent.
Wherein the resin matrix has a molecular formula of (C)3H4O2)400The acrylic resin of (1). The photoinitiator is a titanocene initiator (dibenzyltitanocene). The chain transfer agent is 2-cyano-3-mercapto-3- (phenylamino) -2-ethyl acrylate.
The preparation method of the light-cured material of the embodiment comprises the following steps:
(1) 75 parts of a resin matrix and 22 parts of a reactive diluent are taken as a first product;
(2) and sequentially adding 2 parts of photoinitiator and 1 part of chain transfer agent into the first product, and mixing to prepare a mixture with the viscosity of 2180mpa.s, so as to obtain the photocuring material of the embodiment.
The light-cured material of the embodiment is used for packaging a display panel, and the packaging method comprises the following steps:
(1) coating the light-cured material on the surface of the cover plate to enable the coating surface to be attached to the display substrate, and then pressing the display substrate and the cover plate together at a certain pressure to form a sandwich structure;
(2) preheating the temperature of a visible light curing instrument to 32 ℃, sending the sandwich structure obtained in the step (1) into the visible light curing instrument, and irradiating by adopting visible light at the temperature of 32 ℃ to enable the light curing material to have a curing reaction. As the curing reaction is exothermic, the temperature of the entire mixture system is further increased, thereby driving the curing reaction to proceed and ultimately achieving full cure. And obtaining the display panel after the curing reaction is finished. Temperature measurement experiments prove that in the embodiment, the whole process of the curing reaction ensures that the whole temperature is not more than 80 ℃, and the temperature is reduced by at least 15 ℃ compared with the whole temperature (more than 60 ℃) of the curing reaction initiated by ultraviolet rays under the same condition.
In the above examples, the bulk temperature of the curing process was measured by real-time temperature measurement to ensure that the bulk temperature did not exceed 80 ℃. Experiments prove that the heat quantity caused by the visible light curing process initiated by the visible light curing agent is lower than that caused by the ultraviolet light curing reaction, because the visible light curing time is longer than that of the ultraviolet light curing, the reaction is more stable, and a large amount of energy is not generated because the ultraviolet light is instantly cured like ultraviolet light. Because the temperature is always kept at about 45 ℃ in the visible light curing process and can not reach more than 80 ℃, the cooling treatment is not needed in the curing process. In the actual production process, ultraviolet irradiation is used, the curing temperature is over 60 ℃, but the final curing temperature is required to be ensured not to exceed 80 ℃. If the temperature exceeds 60 ℃ and even reaches more than 80 ℃, cooling methods such as air cooling and the like are adopted for cooling, otherwise, components are inevitably thermally damaged.
In addition, the other purpose of the invention is to avoid the irreversible damage of the OLED device when meeting ultraviolet light, so that a visible light irradiation curing method is adopted.
In a word, the embodiment adopts the visible light curing method, so that the phenomenon of irradiation damage of ultraviolet irradiation to the component structure is avoided, and the phenomenon of thermal damage to the component structure due to the fact that the temperature caused by the ultraviolet light curing method exceeds 60 ℃ can also be avoided, so that the application can avoid two damage types of the component in the curing process.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above detailed description is provided for a resin composition, a display panel and a method for manufacturing the same provided in the embodiments of the present application, and the principles and embodiments of the present application are explained in the present application by applying specific examples, and the description of the above embodiments is only used to help understanding the technical solutions and core ideas of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A photocuring material is characterized by comprising the following components in parts by weight:
resin matrix and active diluent (60-80) to (20-40);
resin matrix and photoinitiator (60-80) to (0.5-2); and
the resin matrix and the chain transfer agent are (60-80) to (0.5-2);
wherein the resin matrix is selected from acrylic resin or a mixture of acrylic resin and epoxy resin;
the photoinitiator is selected from any one or two of a titanocene initiator and a peroxide initiator, or is selected from any one or two of the titanocene initiator and the peroxide initiator and the ultraviolet light photoinitiator;
the chain transfer agent is a mercapto compound.
2. The photocurable material of claim 1 wherein,
the resin matrix and the active diluent are (62-78) to (22-38); and/or
The resin matrix and the photoinitiator are (62-78) to (1-1.5); and/or
The resin matrix and the chain transfer agent are (62-78) to (1-1.5); and/or
The light-cured material also comprises an auxiliary agent, wherein the resin matrix is (62-78) to (0.5-5).
3. The photocurable material of claim 1 wherein said acrylic resin is selected from the group consisting of those of formula (C)3H4O2)nAcrylic acid ofAny one or a mixture of several of resins, wherein n is an integer ranging from 200 to 1600, or is selected from fluorine-silicon modified acrylic resin; and/or
The epoxy resin is selected from (C)11H12O3)mM is an integer ranging from 5 to 30.
4. The photocurable material of claim 1 wherein the resin matrix is a blend of the acrylic resin and the epoxy resin, the acrylic resin and the epoxy resin being present in a weight ratio of (2-4) to 1.
5. The photocurable material of claim 1 wherein the titanocene-based initiator is selected from any one or a mixture of bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene (photoinitiator PI784), bis 2, 6-difluoro-3-pyrrolylphenyltitanocene (photoinitiator 784), dichlorotitanocene, fluorinated diphenyltitanocene, dicarbonyl titanocene, dibenzyltitanocene, and bis (trichloroacetic acid) titanocene; and/or
The peroxide initiator is selected from any one or a mixture of a plurality of benzophenone peroxyformate, xanthone peroxyformate, 2-methylindenone peroxyformate, benzothiazole peroxyformate and tert-butyl peroxy (2-ethyl hexanoate); and/or
The ultraviolet light photoinitiator is selected from any one or a mixture of more of diphenyl (2,4, 6-Trimethylbenzoyl) Phosphine Oxide (TPO), 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl-1- [ 4-methylthiophenyl ] -2-morpholinyl-1-acetone, 1-hydroxy-cyclohexyl-phenyl ketone, (1-hydroxycyclohexyl) (4- (2-hydroxyethoxy) phenyl) ketone and hexafluorophosphate.
6. The photocuring material as claimed in claim 1, wherein the photoinitiator is a mixture of the titanocene initiator and the peroxide initiator, and the weight ratio of the titanocene initiator to the peroxide initiator is (1-5) to 1; or
The photoinitiator is the mixture of any one or two of the titanocene initiator and the peroxide initiator and the ultraviolet light photoinitiator, and the weight ratio of the any one or two of the titanocene initiator and the peroxide initiator to the ultraviolet light photoinitiator is (8-10) to 1.
7. The photocurable material of claim 1 wherein the reactive diluent is selected from any one or more of 1, 6-hexanediol diacrylate (HDDA), dipropylene glycol diacrylate (DPGDA), tripropylene glycol diacrylate (TPGDA), 1, 4-butanediol diglycidyl ether, and hydroxy cyclic ether; and/or
The mercapto compound is selected from any one or a mixture of more of mercaptoethanol, mercaptopropionic acid, mercaptoethylamine, pentaerythritol tetrakis (3-mercaptobutanoate), isooctyl 3-mercaptopropionate, fluoro-bis (prop-2-yloxy) -mercaptophosphane, N- (2-mercaptoethyl) -ethyl carbamate propyl thiocarbonate, (3-prop-2-ylphenyl) N-methyl-N-mercapto-carbamate, 1, 4-butanediol bis (mercaptoacetate), 4' -dimercaptodiphenyl sulfide dimethacrylate, 2-cyano-3-mercapto-3- (phenylamino) -2-ethyl acrylate, and 2-cyano-3- [ (2, 6-dimethylphenyl) amino ] -3-ethyl mercaptoacrylate; and/or
The auxiliary agent is selected from any one or mixture of more of an antioxidant, a compatilizer and a viscosity regulator; and/or
The viscosity of the light-cured material is 2000 +/-200 mpa.s.
8. Use of the photocurable material according to any one of claims 1-6 as an interlayer bonding agent for display panels.
9. A display panel, comprising:
a display substrate;
a cover plate; and
a bonding layer attached to the display substrate and the cover plate, respectively, the bonding layer being formed of at least the photocurable material according to any one of claims 1 to 6.
10. A preparation method of a display panel is characterized by comprising the following steps:
(1) forming a light-cured material between the display substrate and the cover plate, and pressing the display substrate and the cover plate;
(2) irradiating the product obtained in the step (1) by adopting visible light or mixing and irradiating the product by adopting visible light and ultraviolet light to initiate a curing reaction, and obtaining a display panel after the curing reaction is finished;
wherein the light-curable material is the light-curable material according to any one of claims 1 to 6; the temperature is 25 ℃ to 35 ℃; and/or
The wavelength range of the visible light is 400-700nm, and the radiation illumination is 20-30mW/cm2The irradiation time is 40s to 90s, and the irradiation distance is 10-20 cm; and/or
The wavelength range of the ultraviolet light is 200-375nm, and the radiation illumination is 31-40mW/cm2The irradiation time is 10s to 30s, and the irradiation distance is 10-20 cm; and/or
The duration of the curing reaction is 60 to 90 s.
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| CN115651587A (en) * | 2022-11-09 | 2023-01-31 | 深圳市华星光电半导体显示技术有限公司 | Packaging adhesive material, display panel and manufacturing method of display panel |
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Application publication date: 20210907 |