CN115678440B - OCA optical cement for 3D curved screen and preparation method and application thereof - Google Patents
OCA optical cement for 3D curved screen and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of OCA (optically clear adhesive) optical cement, in particular to OCA optical cement for a 3D curved screen, and a preparation method and application thereof. The OCA optical cement for the 3D curved screen is mainly prepared from the following components in parts by weight: 100 parts of oligomer, 0.1 to 1 part of first photoinitiator, 0.5 to 1 part of thermal cross-linking agent, 8978 parts of functional assistant 1~5 parts and 0.1 to 1 part of silane coupling agent; the oligomer is mainly prepared from the following components in parts by weight: 30-85 parts of methoxypolyethylene glycol (550) monomethacrylate, 10-40 parts of tetrahydrofuran acrylate, 5-20 parts of hydroxyethyl acrylate, 10-30 parts of glycidyl methacrylate, 2-10 parts of 1,6-hexanediol diacrylate and 0.1-1.5 parts of a second photoinitiator. The OCA optical cement has high filling property, can prevent bubbles from rebounding, and has high bonding performance and the like.
Description
Technical Field
The invention relates to the technical field of OCA (optically clear adhesive) optical cement, in particular to OCA optical cement for a 3D curved screen, and a preparation method and application thereof.
Background
From the structure of the touch screen, the screen can be roughly divided into three parts, namely a protective glass, the touch screen and a liquid crystal display screen from top to bottom. The three parts are bonded and attached by glue, generally, two times of bonding and attaching are needed, and one time of bonding and attaching is carried out between the protective glass and the touch screen, namely TP attaching; the other time of attaching is between the display screen and the touch screen, namely, the attaching is complete. The most mature glue for sticking at present is OCA optical glue. The OCA optical cement has the characteristics of being colorless and transparent, having the light transmittance of more than 90 percent, being capable of being cured at room temperature or middle temperature, having small curing shrinkage and the like, and is generally applied to the lamination of touch display screens, touch display screens and other modules.
From 2016 to 2017, the market is basically adopting a full screen design with the same width from top to bottom. In the meantime, in order to realize a full-screen, research and development staff continuously try new schemes, so that a 3D curved screen is provided, and the 3D curved screen can further extend the vision of people out of the screen on the basis of the left and right ultra-narrow borders, and enjoy a wider picture feeling. The achieved display effect is better than that of no frame, the constraint of the frame on the visual field can be relieved, and the visual enjoyment beyond the screen is brought, so that the purpose of creating better full-screen display effect is achieved. The common screen is a pure plane, and as shown in fig. 1, the screen does not have any arc design; and 3D curved screens, as shown in FIG. 2, adopt an arc design for both the middle and the edge. Nowadays, the mainstream smart phones are mostly popular to adopt a 3D curved screen design.
In the prior art, no matter be ordinary screen or 3D curved surface screen, all choose OCA optical cement for use as the material of bonding protective glass, touch-sensitive screen and liquid crystal display, 3D curved surface screen leads to its segment difference height because it has certain radian, needs have the OCA optical cement of better filling effect, simultaneously because the reason of radian, easily causes OCA to continuously receive the effect of internal stress, finally leads to the risk of coming unstuck, specifically as shown in FIG. 3. Therefore, it is urgently needed to develop an OCA optical cement suitable for a 3D curved screen to prolong the service life of the whole touch element.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide OCA optical cement for a 3D curved screen, which aims to solve the technical problems of poor filling effect, degumming and the like caused by the fact that the OCA optical cement in the prior art is not suitable for the 3D curved screen.
The invention also aims to provide a preparation method of the OCA optical cement for the 3D curved screen.
The invention further aims to provide application of the OCA optical cement for the 3D curved screen.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the OCA optical cement for the 3D curved screen is mainly prepared from the following components in parts by weight:
100 parts of oligomer, 0.1 to 1 part of first photoinitiator, 0.5 to 1 part of thermal cross-linking agent, 8978 parts of functional assistant, 8978 parts of zxft 8978 parts of silane coupling agent;
the oligomer is mainly prepared from the following components in parts by weight:
30 to 85 parts of methoxy polyethylene glycol (550) monomethacrylate, 10 to 40 parts of tetrahydrofuran acrylate, 5 to 20 parts of hydroxyethyl acrylate, 10 to 30 parts of glycidyl methacrylate, 2 to 10 parts of 1,6-hexanediol diacrylate and 0.1 to 1.5 parts of a second photoinitiator;
the functional assistant comprises any one or more of acrylamide, tert-butyl acrylamide amidosulfonic acid, N-dimethylacrylamide and trimethyl ammonium chloride methacrylamide propyl ester.
In a particular embodiment of the invention, the preparation of the oligomer comprises: under the protective atmosphere, the mixture of the components is subjected to UV photopolymerisation.
In a specific embodiment of the invention, the glass transition temperature Tg of the oligomer is-60 to 10 ℃, preferably-35 to 5 ℃.
In a specific embodiment of the present invention, the oligomer has a viscosity of 500 to 10000cps at 25 ℃; the weight average molecular weight of the oligomer is 50000 to 2500000 daltons.
In a specific embodiment of the present invention, the mass ratio of the methoxypolyethylene glycol (550) monomethacrylate to the glycidyl methacrylate is (3~5): 1.
In a particular embodiment of the invention, the first photoinitiator is a hydrogen abstraction type radical photoinitiator. Further, the first photoinitiator comprises any one or more of benzophenone, 4-phenylbenzophenone, 2,4,6-trimethylbenzophenone, and isopropyl thioxanthone.
In a particular embodiment of the invention, the second photoinitiator is a cleavage-type free-radical photoinitiator. Further, the second photoinitiator comprises any one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, methyl benzoylformate, 2-hydroxy-2-methylphenylpropane-1-one, 1-hydroxy-cyclohexylbenzophenone, and 2-benzyl-2-dimethylamino-1-1 (4-morpholinobenzyl) butanone-1.
In a specific embodiment of the invention, the thermal crosslinker comprises any one or more of 2,2-azo-bis- (2-methylbutyronitrile), azobisisobutyronitrile, aziridine crosslinking agent CX-100, aziridine crosslinking agent XR-100, and aziridine crosslinking agent GY-225.
In a specific embodiment of the present invention, the silane coupling agent includes any one or more of vinyltriethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, methyldimethoxysilane and methyltriethoxysilane.
The invention also provides a preparation method of the OCA optical cement for the 3D curved-surface screen, which comprises the following steps:
and mixing the components in proportion, and performing ultraviolet curing to obtain the OCA optical cement.
In a specific embodiment of the present invention, the conditions of the uv curing include: the wavelength is 280 to 420nm, and the energy is 500 to 5000mj/cm 2 。
In a specific embodiment of the invention, the thickness of the OCA optical cement is 25-400 μm.
The invention also provides application of any one of the OCA optical cement for the 3D curved screen in preparation of the 3D curved screen.
In the embodiment of the invention, the OCA optical cement and the display module to be bonded are filled and bonded, and then are thermally crosslinked and cured. Further, the thermal crosslinking curing conditions include: the temperature is 60 to 110 ℃, the time is 30 to 120min, and the pressure is 1.5 to 6kg.
Compared with the prior art, the invention has the beneficial effects that:
(1) The OCA optical cement has high filling property, can wet the ink section difference displayed on the filling cover plate, can release internal and external stresses through post-crosslinking curing, has certain strength to support the damage of the curved surface stress to the cement without generating or rebounding bubbles, has high bonding property, and effectively solves the problem of bubble return of components after being attached;
(2) The OCA optical cement has the advantages of simple preparation process, safety, environmental protection, less flow, low cost and contribution to industrial production; in addition, the OCA optical adhesive is solvent-free, has no VOC emission, and has excellent economic benefit, production benefit and environmental protection benefit;
(3) The OCA optical cement is particularly suitable for the lamination of the 3D curved screen due to the consideration of the performances in various aspects, and can remarkably improve the performance and the service life of elements with the 3D curved screen.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of a common screen in the prior art;
fig. 2 is a schematic structural view of a 3D curved screen in the prior art;
fig. 3 is a schematic diagram of degumming in a 3D curved screen in the prior art.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. 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 invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "first", "second", and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
The OCA optical cement for the 3D curved screen is mainly prepared from the following components in parts by weight:
100 parts of oligomer, 0.1 to 1 part of first photoinitiator, 0.5 to 1 part of thermal cross-linking agent, 8978 parts of functional assistant, 8978 parts of zxft 8978 parts of silane coupling agent;
the oligomer is mainly prepared from the following components in parts by weight:
30 to 85 parts of methoxy polyethylene glycol (550) monomethacrylate, 10 to 40 parts of tetrahydrofuran acrylate, 5 to 20 parts of hydroxyethyl acrylate, 10 to 30 parts of glycidyl methacrylate, 2 to 10 parts of 1,6-hexanediol diacrylate and 0.1 to 1.5 parts of a second photoinitiator;
the functional assistant comprises any one or more of acrylamide, tert-butyl acrylamide amidosulfonic acid, N-dimethylacrylamide and trimethyl ammonium chloride methacrylamide propyl ester.
In different embodiments, in the OCA optical cement for the 3D curved screen, when the oligomer is 100 parts by weight, the amount of each component can be as follows:
the first photoinitiator may be used in amounts of 0.1 parts, 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, and the like;
the amount of the thermal crosslinking agent may be 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, etc.;
the amount of the functional aid may be 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, etc.;
the silane coupling agent may be used in an amount of 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part, 1 part, etc.
In various embodiments, the oligomer may be used in the following amounts, in parts by weight:
the methoxypolyethylene glycol (550) monomethacrylate may be used in amounts of 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts, 80 parts, 85 parts, and the like;
the amount of tetrahydrofuran acrylate may be 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, etc.;
hydroxyethyl acrylate may be used in amounts of 5 parts, 8 parts, 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, and the like;
glycidyl methacrylate can be used in amounts of 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 22 parts, 25 parts, 28 parts, 30 parts, and the like;
1,6-hexanediol diacrylate may be used in amounts of 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.;
the second photoinitiator may be used in an amount of 0.1 parts, 0.2 parts, 0.5 parts, 0.8 parts, 1 part, 1.2 parts, 1.5 parts, and the like.
In a preferred embodiment of the invention, the oligomer is made essentially of the following components in parts by weight:
30-55 parts of methoxy polyethylene glycol (550) monomethacrylate, 20-40 parts of tetrahydrofuran acrylate, 8-18 parts of hydroxyethyl acrylate, 10-12 parts of glycidyl methacrylate, 1,6-hexanediol diacrylate 2~5 and 0.1-0.9 part of a second photoinitiator.
In a particular embodiment of the invention, the preparation of the oligomer comprises: under the protective atmosphere, the mixture of the components is subjected to UV photopolymerisation. Furthermore, in the UV light polymerization, the energy of the UV light polymerization is 500-5000 mj/cm 2 。
In practice, the polymerization is carried out using suitable UV light to give oligomers of corresponding viscosity. The energy parameter of UV illumination polymerization is adjustable, and the target viscosity is obtained.
In a specific embodiment of the invention, the glass transition temperature Tg of the oligomer is-60 to 10 ℃, preferably-35 to 5 ℃.
As in the various embodiments, the oligomer may have a glass transition temperature Tg of-60 ℃, -50 ℃, -40 ℃, -30 ℃, -20 ℃, -10 ℃, 0 ℃, 10 ℃, etc.
In a specific embodiment of the present invention, the oligomer has a viscosity of 500 to 10000cps at 25 ℃; the weight average molecular weight of the oligomer is 50000 to 2500000 daltons.
As in various embodiments, the oligomer may have a viscosity at 25 ℃ of about 500CPS, 1000CPS, 2000CPS, 3000CPS, 4000CPS, 5000CPS, 6000CPS, 7000CPS, 8000CPS, 9000CPS, 10000CPS, or the like, preferably 500 to 3000CPS, such as 800 to 2000CPS.
As in various embodiments, the oligomer can have a weight average molecular weight of 50000 daltons, 100000 daltons, 200000 daltons, 300000 daltons, 400000 daltons, 500000 daltons, 600000 daltons, 700000 daltons, 800000 daltons, 900000 daltons, 1000000 daltons, 2000000 daltons, 2500000 daltons, and the like.
In a specific embodiment of the present invention, the mass ratio of the methoxypolyethylene glycol (550) monomethacrylate to the glycidyl methacrylate is (3~5): 1.
In various embodiments, the mass ratio of the methoxypolyethylene glycol (550) monomethacrylate to the glycidyl methacrylate can be 3: 1, 3.2: 1, 3.5: 1, 3.8: 1, 4: 1, 4.2: 1, 4.5: 1, 4.8: 1, 5: 1, and so forth.
According to the invention, by adjusting the proportion of the monomethacrylate of the soft monomer methoxy polyethylene glycol (550) to the hard monomer glycidyl methacrylate, on one hand, the Tg of the oligomer is adjusted, so that the phenomenon that the Tg is too low to cause easy glue overflow is avoided, and the phenomenon that the Tg is too high to influence the poor filling performance is also avoided; meanwhile, the adhesive is matched with components such as tetrahydrofuran acrylate and the like, and the adhesive property of the obtained optical adhesive is ensured.
In a particular embodiment of the invention, the first photoinitiator is a hydrogen abstraction-type radical photoinitiator. Further, the first photoinitiator comprises any one or more of benzophenone, 4-phenylbenzophenone, 2,4,6-trimethylbenzophenone, and isopropylthioxanthone.
In a particular embodiment of the invention, the second photoinitiator is a cleavage-type free-radical photoinitiator. Further, the second photoinitiator comprises any one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, methyl benzoylformate, 2-hydroxy-2-methylphenylpropane-1-one, 1-hydroxy-cyclohexylbenzophenone, and 2-benzyl-2-dimethylamino-1-1 (4-morpholinobenzyl) butanone-1.
In a specific embodiment of the invention, the thermal crosslinker comprises any one or more of 2,2-azo-bis- (2-methylbutyronitrile), azobisisobutyronitrile, aziridine crosslinker CX-100, aziridine crosslinker XR-100, and aziridine crosslinker GY-225.
The OCA optical adhesive disclosed by the invention has the advantages that a certain heat cross-linking agent is added into the components of the OCA optical adhesive, so that the optical adhesive can be cross-linked and cured under a certain condition, the modulus of the OCA optical adhesive film can be improved, the residual of internal stress can be eliminated, the adhesive is supported by a certain strength to damage curved surface stress, bubbles cannot be generated or rebound, and the phenomena of delamination and foaming are prevented.
In a specific embodiment of the present invention, the silane coupling agent includes any one or more of vinyltriethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, methyldimethoxysilane and methyltriethoxysilane.
The OCA optical adhesive disclosed by the invention can further enhance the bonding strength of an interface under the action of a silane coupling agent, and effectively solves the problem that components and parts are back-foamed after being attached.
The invention also provides a preparation method of the OCA optical cement for the 3D curved-surface screen, which comprises the following steps:
and mixing the components in proportion, and performing ultraviolet curing to obtain the OCA optical cement.
In a specific embodiment of the present invention, the conditions of the uv curing include: the wavelength is 280 to 420nm, and the energy is 500 to 5000mj/cm 2 。
In actual operation, the ultraviolet curing conditions can be adjusted according to actual conditions, and the components are fully cured by ultraviolet.
In a specific embodiment of the invention, the thickness of the OCA optical cement is 25 to 400 μm.
As in the different embodiments, the thicknesses of the OCA optical glues may be 25 μm, 50 μm, 75 μm, 100 μm, 150 μm, 200 μm, 250 μm, 300 μm, 350 μm, 400 μm, and so on.
The invention also provides an application of any one of the OCA optical cement for the 3D curved screen in preparation of the 3D curved screen.
In the embodiment of the invention, the OCA optical cement and the display module to be bonded are filled and bonded, and then are thermally crosslinked and cured. Further, the thermal crosslinking curing conditions include: the temperature is 60 to 110 ℃, the time is 30 to 120min, and the pressure is 1.5 to 6kg.
In practical operation, after bonding, thermal crosslinking curing is realized in the defoaming process.
In the conditions of the thermal crosslinking curing, the temperature may be 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃ and the like, the time may be 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min and the like, and the pressure may be 1.5kg, 2kg, 2.5kg, 3kg, 3.5kg, 4kg, 4.5kg, 5kg, 5.5kg, 6kg and the like, as in the different embodiments.
Example 1
The embodiment provides an OCA optical cement for a 3D curved screen, which is mainly prepared from the following components in parts by weight: 100 parts of oligomer, 0.2 part of benzophenone, 0.5 part of 2,2-azo-bis- (2-methylbutyronitrile), 2 parts of acrylamide and 0.2 part of vinyl triethoxysilane.
The preparation method of the OCA optical cement comprises the following steps:
mixing the components in proportion to prepare a mixed solution, coating the mixed solution into a sandwich structure of a release film/mixed solution/release film after vacuumizing, and curing by an ultraviolet lamp under the curing conditions that: the wavelength is 280 to 420nm, and the energy is 500mj/cm 2 Preparing OCA optical cement with the film thickness of 175 mu m; and carrying out thermal crosslinking curing on the prepared OCA optical cement in a defoaming furnace under the conditions of 110 ℃, 40min and 3kg of pressure.
The preparation of the oligomer of this example included: after 30 parts by weight of methoxypolyethylene glycol (550) monomethacrylate, 40 parts by weight of tetrahydrofuran acrylate, 18 parts by weight of hydroxyethyl acrylate, 10 parts by weight of glycidyl methacrylate, 1,6-hexanediol diacrylate, 2 parts by weight of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide were mixed and polymerized by UV light to form an oligomer having a viscosity of 800CPS (25 ℃), a weight average molecular weight of 90000 daltons, and a Tg of-20 ℃. Wherein the energy of UV light polymerization is 2000-5000 mj/cm 2 And increasing the temperature by 8 to 20 ℃.
Example 2
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the OCA optical cement has different component types or dosage.
The OCA optical cement of the present embodiment is mainly prepared from the following components in parts by weight: 100 parts of oligomer, 0.3 part of 4-phenylbenzophenone, 0.6 part of azobisisobutyronitrile, 2.5 parts of tert-butyl acrylamide sulfonic acid and 0.1 part of dimethyl dimethoxy silane.
Example 3
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the OCA optical cement has different component types or dosage.
The OCA optical cement of the present embodiment is mainly prepared from the following components in parts by weight: 100 parts of oligomer, 0.5 part of 2,4,6-trimethylbenzophenone, 0.8 part of azobisisobutyronitrile, 3 parts of N, N-dimethylacrylamide and 0.3 part of 3- (methacryloyloxy) propyltrimethoxysilane.
Example 4
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the OCA optical cement has different component types or dosage.
The OCA optical cement of the present embodiment is mainly prepared from the following components in parts by weight: 100 parts of oligomer, 0.8 part of 2,4,6-trimethylbenzophenone, 1 part of azobisisobutyronitrile, 3.5 parts of N, N-dimethylacrylamide and 0.5 part of 3- (methacryloyloxy) propyltrimethoxysilane.
Example 5
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the oligomer composition was different.
The preparation of the oligomer of this example included: after 40 parts by weight of methoxypolyethylene glycol (550) monomethacrylate, 28 parts by weight of tetrahydrofuran acrylate, 16 parts by weight of hydroxyethyl acrylate, 12 parts by weight of glycidyl methacrylate, 4 parts by weight of 1,6-hexanediol diacrylate and 0.2 part by weight of methyl benzoylformate are mixed, they are polymerized by UV light to form an oligomer having a viscosity of 1000CPS (25 ℃), a weight average molecular weight of 110000 daltons and a Tg of-28 ℃.
Example 6
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the oligomer composition was different.
The preparation of the oligomer of this example included: 45 parts of methoxy polyethylene glycol (550) monomethacrylate, 30 parts of tetrahydrofuran acrylate, 10 parts of hydroxyethyl acrylate, 12 parts of glycidyl methacrylate, 3 parts of 1,6-hexanediol diacrylate and 0.4 part of 2-hydroxy-2-methylphenyl propane-1-one in parts by weight are mixed and polymerized by UV light to form an oligomer with the viscosity of 1500CPS (25 ℃), the weight-average molecular weight of 180000 daltons and the Tg of-30 ℃.
Example 7
The present embodiment provides an OCA optical cement for a 3D curved screen, which is specifically referred to in embodiment 1, and the difference is only that: the oligomer composition was different.
The preparation of the oligomer of this example included: 55 parts of methoxy polyethylene glycol (550) monomethacrylate, 20 parts of tetrahydrofuran acrylate, 8 parts of hydroxyethyl acrylate, 12 parts of glycidyl methacrylate, 5 parts of 1,6-hexanediol diacrylate and 0.9 part of 2-hydroxy-2-methylphenyl propane-1-one in parts by weight are mixed and polymerized by UV light to form an oligomer with the viscosity of 2000CPS (25 ℃), the weight-average molecular weight of 000 daltons and the Tg of-25032 ℃.
Example 8
The present embodiment provides an OCA optical cement for a 3D curved screen, specifically referring to embodiment 1, which is different only in that: the oligomer composition was different.
The preparation of the oligomer of this example included: 48 parts of methoxy polyethylene glycol (550) monomethacrylate, 30 parts of tetrahydrofuran acrylate, 10 parts of hydroxyethyl acrylate, 9 parts of glycidyl methacrylate, 3 parts of 1,6-hexanediol diacrylate and 0.4 part of 2-hydroxy-2-methylphenyl propane-1-one in parts by weight are mixed and polymerized by UV light to form an oligomer with the viscosity of 2000CPS (25 ℃), the weight-average molecular weight of 000 daltons and the Tg of-25034 ℃.
Example 9
The present embodiment provides an OCA optical cement for a 3D curved screen, specifically referring to embodiment 1, which is different only in that: the oligomer composition was different.
The preparation of the oligomer of this example included: 42 parts of methoxy polyethylene glycol (550) monomethacrylate, 30 parts of tetrahydrofuran acrylate, 10 parts of hydroxyethyl acrylate, 15 parts of glycidyl methacrylate, 3 parts of 1,6-hexanediol diacrylate and 0.4 part of 2-hydroxy-2-methylphenyl propane-1-one in parts by weight are mixed and polymerized by UV light to form an oligomer with the viscosity of 2000CPS (25 ℃), the weight-average molecular weight of 000 daltons and the Tg of-25029 ℃.
Comparative example 1
Comparative example 1 reference example 1 is made with the difference that: the oligomer composition was different.
The preparation method of the oligomer of comparative example 1 includes: 50 parts of methoxypolyethylene glycol (550) monomethacrylate, 30 parts of hydroxyethyl acrylate, 17 parts of glycidyl methacrylate, 3 parts of 1,6-hexanediol diacrylate and 0.1 part of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide in parts by weight are mixed and polymerized by UV light to form an oligomer with a viscosity of 900CPS (25 ℃), a weight-average molecular weight of 95000 daltons and a Tg of-38 ℃.
Comparative example 2
Comparative example 2 reference example 1, except that: the oligomer composition was different.
The preparation method of the oligomer of comparative example 2 includes: 36.5 parts of methoxy polyethylene glycol (550) monomethacrylate, 49 parts of tetrahydrofuran acrylate, 12 parts of glycidyl methacrylate, 2.5 parts of 1,6-hexanediol diacrylate and 0.1 part of methyl benzoylformate in parts by weight are mixed and polymerized by UV light to form an oligomer with the viscosity of 1100CPS (25 ℃), the weight-average molecular weight of 118000 daltons and the Tg of-26 ℃.
Comparative example 3
Comparative example 3 reference example 1, except that: the oligomer composition was different.
The preparation of the oligomer of comparative example 3 comprises: after 12 parts by weight of methoxy polyethylene glycol (550) monomethacrylate, 41 parts by weight of tetrahydrofuran acrylate, 23 parts by weight of hydroxyethyl acrylate, 18 parts by weight of glycidyl methacrylate, 6 parts by weight of 1,6-hexanediol diacrylate and 0.2 part by weight of methyl benzoylformate are mixed, polymerized by UV light to form an oligomer having a viscosity of 1150CPS (25 ℃), a weight average molecular weight of 140000 daltons and a Tg of-26 ℃.
Comparative example 4
Comparative example 4 reference example 1, except that: the OCA optical cement has different component usage amounts.
The OCA optical cement of comparative example 4 is prepared from the following components in parts by weight: 100 parts of oligomer, 0.2 part of benzophenone, 2 parts of acrylamide and 0.2 part of vinyl triethoxysilane.
Comparative example 5
Comparative example 5 reference example 1, with the difference that: the oligomer composition was different.
The preparation of the oligomer of comparative example 5 comprises: 40 parts of polyethylene glycol (400) diacrylate, 28 parts of tetrahydrofuran acrylate, 16 parts of hydroxyethyl acrylate, 12 parts of glycidyl methacrylate, 4 parts of 1,6-hexanediol diacrylate and 0.2 part of methyl benzoylformate are mixed according to parts by weight, and then polymerized by UV illumination to form an oligomer with the viscosity of 60000CPS (25 ℃), the weight-average molecular weight of 165000 daltons and the Tg of-23 ℃.
Examples of the experiments
To illustrate the properties of the OCA optical glues of the different examples and comparative examples, the following tests were performed on each OCA optical glue.
1. Light transmittance and haze test
And (4) testing standard: GB/T2410-2008 determination of light transmittance and haze of transparent plastics.
The preparation method comprises the following steps: and (3) bonding and defoaming according to a structure of a 5-inch glass cover plate/OCA optical cement/matched ITO sheet, wherein the defoaming process is at 70 ℃,60min and the pressure is 3.5KG.
2. Test of adhesion Property
The preparation method comprises the following steps: and (3) jointing and defoaming according to a 50-micron ink thickness glass cover plate/OCA optical cement/ITO glass structure, wherein the defoaming process is at 70 ℃,60min, the pressure is 3.5KG, and the size is 5 inches. The 50 μm ink step filling performance was evaluated.
3. Mechanical Property test
Testing the adhesive force: GB/T2790-1995 adhesive 180 DEG Peel Strength test method Flexible materials vs. rigid materials.
Modulus test: the dynamic mechanical analyzer measures the modulus of elasticity at 25 ℃. And (3) evaluating the modulus of the product which is not subjected to thermal crosslinking (namely before crosslinking) before the defoaming process and is subjected to crosslinking after the defoaming process, wherein the defoaming process is carried out at 70 ℃ for 60min and the pressure is 3.5KG.
4. General evaluation of aging test
The preparation method comprises the following steps: and (3) bonding and defoaming according to a 50-micron ink thickness glass cover plate/OCA optical cement/ITO glass structure, wherein the defoaming process is at 70 ℃,60min, 3.5KG, and the size is 5 inches. After aging, the sample has no bubble return, no yellowing, no whitening and no warping/glue opening, and the sample passes; if any of the above defects are present, the failure is detected.
The results of the various performance tests are shown in Table 1~2.
TABLE 1 results of performance test of OCA optical cement
| Number of | Light transmittance (%) | Haze degree | Adhesion/50 μm ink fill | Adhesive property N/25mm | Modulus before crosslinking KPa | Modulus after crosslinking KPa |
| Example 1 | 92.27 | 0.28 | Defoaming 50-micron ink can be filled | 38 | 81.2 | 118 |
| Example 2 | 92.14 | 0.31 | Defoamable 50 μm ink can be filled | 38 | 86.5 | 120.5 |
| Example 3 | 92.35 | 0.28 | Defoamable 50 μm ink can be filled | 36 | 87.2 | 123.6 |
| Example 4 | 92.16 | 0.32 | Defoamable 50 μm ink can be filled | 40 | 85.4 | 118.8 |
| Example 5 | 92.12 | 0.36 | Defoamable 50 μm ink can be filled | 37 | 83.4 | 115.2 |
| Example 6 | 92.23 | 0.40 | Defoamable 50 μm ink can be filled | 37 | 84.3 | 112.7 |
| Example 7 | 92.20 | 0.38 | Defoamable 50 μm ink can be filled | 39 | 81.7 | 113.4 |
| Example 8 | 92.42 | 0.34 | Defoamable 50 μm ink can be filled | 31 | 86.4 | 117.2 |
| Example 9 | 92.32 | 0.35 | Defoamable 50 μm ink can be filled | 29 | 80.8 | 108.9 |
| Comparative example 1 | 92.30 | 0.41 | Defoamable 50 μm ink can be filled | 34 | 81.8 | 110.4 |
| Comparative example 2 | 92.16 | 0.42 | Defoamable 50 μm ink can be filled | 15 | 83.5 | 112.1 |
| Comparative example 3 | 92.24 | 0.40 | 50-micron ink non-fillable capable of removing bubbles | 35 | 85.0 | 120.4 |
| Comparative example 4 | 92.17 | 0.40 | 50 μm ink refillable with bubble remover | 34 | 82.2 | 82.8 |
| Comparative example 5 | 92.45 | 0.32 | 50 μm ink refillable with bubble remover | 26 | 82.4 | 118.9 |
| J1 | 92.20 | 0.41 | Defoamable 50 μm ink can be filled | 34 | 81.5 | 82.5 |
| J2 | 92.23 | 0.43 | Defoamable 50 μm ink can be filled | 35 | 83.4 | 84.2 |
Remarking: j1 and J2 are commercially available OCA optical cement competitions for 3D curved screens, and the thicknesses of the optical cement competitions are 175 mu m.
TABLE 2 evaluation of aging Properties of OCA after optical clear adhesive application
| Numbering | 85 ℃ 500h | 0.63W/m 2 ， 340nm ， 500h | High and low temperature cycle for 200 rounds | 60 ℃， 90%RH ， 500h |
| Example 1 | By passing | By passing | By passing | By passing |
| Example 2 | By passing | By passing | By passing | By passing |
| Example 3 | By passing | By passing | By passing | By passing |
| Example 4 | By passing | By passing | By passing | By passing |
| Example 5 | By passing | By passing | By passing | By passing |
| Example 6 | By passing | By passing | By passing | By passing |
| Example 7 | By passing | By passing | By passing | By passing |
| Example 8 | By passing | By passing | By passing | By passing |
| Example 9 | By passing | By passing | By passing | By passing |
| Comparative example 1 | By passing | By passing | Return bubble | Return bubble |
| Comparative example 2 | By passing | By passing | Return bubble | Return bubble |
| Comparative example 3 | By passing | By passing | Return bubble | Return bubble |
| Comparative example 4 | By passing | By passing | Return bubble | Return bubble |
| Comparative example 5 | Return bubble | Return bubble | Return bubble | Return bubble |
| J1 | By passing | By passing | Return bubble | By passing |
| J2 | By passing | By passing | Return bubble | By passing |
Remarking: wherein, the 200 rounds of high-temperature and low-temperature circulation refer to that: after the high temperature is 80 ℃/2h, the low temperature is-40 ℃/2h, and the 200 round is carried out.
From the test results in tables 1 and 2, it can be seen that compared with the comparative examples and the commercially available OCA optical adhesives, the optical properties, the adhesion performance and the filling performance of the OCA optical adhesives of the present invention can satisfy the requirements of the OCA optical adhesives. After the OCA optical adhesive is subjected to high-temperature crosslinking and curing, the modulus is obviously improved, the adhesive is more compact, the rebound of bubbles is effectively prevented, particularly, the aging performance after 200 rounds of high-temperature and low-temperature circulation is excellent, the rebound performance is excellent, and the risk of bubble rebound is avoided.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
- The OCA optical cement for the 3D curved screen is characterized by being mainly prepared from the following components in parts by weight:100 parts of oligomer, 0.1 to 1 part of first photoinitiator, 0.5 to 1 part of thermal cross-linking agent, 8978 parts of functional assistant, 8978 parts of zxft 8978 parts of silane coupling agent;the oligomer is mainly prepared from the following components in parts by weight:30 to 85 parts of methoxy polyethylene glycol (550) monomethacrylate, 10 to 40 parts of tetrahydrofuran acrylate, 5 to 20 parts of hydroxyethyl acrylate, 10 to 30 parts of glycidyl methacrylate, 2 to 10 parts of 1,6-hexanediol diacrylate and 0.1 to 1.5 parts of a second photoinitiator;the functional assistant comprises any one or more of acrylamide, tert-butyl acrylamide amidosulfonic acid, N-dimethylacrylamide and trimethyl ammonium chloride methacrylamide propyl ester.
- 2. The OCA optical cement for the 3D curved screen according to claim 1, wherein the glass transition temperature Tg of the oligomer is-60 to 10 ℃;and/or the oligomer has a viscosity of 500 to 10000CPS at 25 ℃; the weight average molecular weight of the oligomer is 50000 to 2500000 daltons.
- 3. The OCA optical cement for a 3D curved screen according to claim 1, wherein the mass ratio of the methoxypolyethylene glycol (550) monomethacrylate to the glycidyl methacrylate is (3~5): 1.
- 4. The OCA optical cement for the 3D curved screen as claimed in claim 1, wherein the first photoinitiator is a hydrogen abstraction type radical photoinitiator;the first photoinitiator comprises any one or more of benzophenone, 4-phenylbenzophenone, 2,4,6-trimethylbenzophenone, and isopropyl thioxanthone.
- 5. The OCA optical cement for the 3D curved screen according to claim 1, wherein the second photoinitiator is a cleavage type free radical photoinitiator;the second photoinitiator comprises any one or more of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, methyl benzoylformate, 2-hydroxy-2-methylphenylpropane-1-one, 1-hydroxy-cyclohexylbenzophenone, and 2-benzyl-2-dimethylamino-1-1 (4-morpholinobenzyl) butanone-1.
- 6. The OCA optical cement for a 3D curved screen according to claim 1, wherein the thermal crosslinking agent comprises any one or more of 2,2-azo-bis- (2-methylbutyronitrile), azobisisobutyronitrile, aziridine crosslinking agent CX-100, aziridine crosslinking agent XR-100, and aziridine crosslinking agent GY-225.
- 7. The OCA optical cement for 3D curved screen according to claim 1, wherein the silane coupling agent comprises any one or more of vinyltriethoxysilane, dimethyldimethoxysilane, vinyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, methyldimethoxysilane and methyltriethoxysilane.
- 8. The method for preparing OCA optical cement for 3D curved screen of 1~7, comprising the steps of:and mixing the components in proportion, and performing ultraviolet curing to obtain the OCA optical cement.
- 9. Root of herbaceous plantThe method of claim 8, wherein the UV curing conditions comprise: the wavelength is 280 to 420nm, and the energy is 500 to 5000mj/cm 2 。
- 10. Use of OCA optical cement for 3D curved screen of any one of claims 1~7 in the preparation of 3D curved screen.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216820A (en) * | 2017-07-17 | 2017-09-29 | 同光（江苏）新材料科技有限公司 | A kind of thermohardening type optical clear hot melt adhesive film and its preparation and applying method |
| CN107353854A (en) * | 2017-07-14 | 2017-11-17 | 东莞市纳利光学材料有限公司 | A kind of OCA optical cements and OCA optical adhesive films |
| CN111363512A (en) * | 2020-03-30 | 2020-07-03 | 嘉兴市海睿新材料有限公司 | 3D ink-jet full-lamination optical adhesive |
| CN112313545A (en) * | 2018-04-27 | 2021-02-02 | 大日本印刷株式会社 | Optical film, polarizing plate and image display device |
| CN114806418A (en) * | 2022-04-06 | 2022-07-29 | 广东鼎立森新材料有限公司 | Preparation and application of OCA (optical clear adhesive) optical cement for touch screen |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102269435B1 (en) * | 2014-07-17 | 2021-06-24 | 헨켈 아게 운트 코. 카게아아 | Photo-curable liquid optically clear adhesive composition and use thereof |
| WO2017154660A1 (en) * | 2016-03-09 | 2017-09-14 | 株式会社カネカ | Radically curable composition and cured product thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353854A (en) * | 2017-07-14 | 2017-11-17 | 东莞市纳利光学材料有限公司 | A kind of OCA optical cements and OCA optical adhesive films |
| CN107216820A (en) * | 2017-07-17 | 2017-09-29 | 同光（江苏）新材料科技有限公司 | A kind of thermohardening type optical clear hot melt adhesive film and its preparation and applying method |
| CN112313545A (en) * | 2018-04-27 | 2021-02-02 | 大日本印刷株式会社 | Optical film, polarizing plate and image display device |
| CN111363512A (en) * | 2020-03-30 | 2020-07-03 | 嘉兴市海睿新材料有限公司 | 3D ink-jet full-lamination optical adhesive |
| CN114806418A (en) * | 2022-04-06 | 2022-07-29 | 广东鼎立森新材料有限公司 | Preparation and application of OCA (optical clear adhesive) optical cement for touch screen |
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