CN111378412A - Light-cured adhesive composition for shading and edge sealing of display module and preparation method thereof - Google Patents
Light-cured adhesive composition for shading and edge sealing of display module and preparation method thereof Download PDFInfo
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- CN111378412A CN111378412A CN201911066644.XA CN201911066644A CN111378412A CN 111378412 A CN111378412 A CN 111378412A CN 201911066644 A CN201911066644 A CN 201911066644A CN 111378412 A CN111378412 A CN 111378412A
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- 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
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses a photocuring adhesive composition for shading and edge sealing of a display module and a preparation method thereof, wherein the photocuring adhesive composition comprises the following components in parts by weight based on 100 parts by weight of the adhesive composition: component A is 25-70 parts of aliphatic polyurethane acrylate prepolymer; and (B) component: 5-20 parts of epoxy acrylate prepolymer; component C is 10-40 parts of one or more aliphatic acrylate monomers; component D is 12-45 parts of monofunctional acrylate monomer containing nitrogen atom structure; component E is 0.2 to 5 portions of tackifying promoter containing sulfur or phosphorus atom structure; component F is 1.0 to 8 portions of two or more cracking type photoinitiators; and the component G is 0.05 to 3 parts of carbon black or carbon black premix taking UV monomer as a carrier. The invention can give consideration to the problems of optical density and deep curing; the adhesive has excellent adhesive force to glass and stainless steel, is very suitable for assembling large-size television module materials, improves the problem of stickiness on the surface of cured glue, is more environment-friendly and healthy, and is convenient for construction and customer use.
Description
Technical Field
The invention relates to the technical field of compositions, in particular to a photocuring adhesive composition for shading and edge sealing of a display module and a preparation method thereof.
Background
Rapid development of modern technologies has advanced the touch technology, especially for updating iterations of consumer display electronic devices. The display module is generally classified as an LCD liquid crystal module or an OLED module. With the progress and development of technology, display devices are thinner and larger in size. In the production and assembly process of the display module, high-performance glue needs to be used in many places to perform the bonding function, and new requirements are provided for auxiliary materials of the adhesive. In order to pursue thinner and more beautiful appearance design, the original mode of mechanical fixation or plate fixation is directly replaced by adhesive.
Taking a large-sized tv display module as an example, in order to seek beauty, the edge of the tv display module is gradually fixed by black light-shielding UV glue instead of the original plate, so that the display module is thinner and lighter (see fig. 1). The back of the display module is sometimes made of stainless steel to improve the impact resistance of the television, which puts various severe requirements on the glue. Firstly, the glue has good light shading performance, and light cannot overflow when the display module is lightened. Meanwhile, the glue needs to have enough curing depth, the curing depth of the glue at the bonding part can reach 400 microns, and the inside is required to be completely cured. One surface of the glue is exposed and leaked outside, so that the surface drying is required to be excellent to prevent pollution; after the adhesive is cured, the adhesive is required to have excellent bonding force and reliability such as overhigh temperature, high humidity, high and low temperature cycle and the like.
The bonding force of the common UV adhesive cannot meet the bonding requirement of glass and stainless steel substrates; and when the curing depth exceeds 200um, it is difficult to achieve excellent light-shielding properties, such as an optical density of 1 or more. To solve this problem, many use reactive polyurethane hot melt adhesive (PUR) technology or dual cure UV colloidal systems. The PUR technology is often required to be heated to more than 90 ℃ for use during construction, certain pressure maintaining time and initial strength forming time are required after glue dispensing, the working efficiency is greatly influenced, and particularly the assembly of large-size television module equipment is realized. The dual curing system such as a UV/heat or UV/moisture curing system, whether heat or moisture, greatly reduces the production efficiency and increases the process complexity, so a photo-curing adhesive composition for shading and edge sealing of a display module and a preparation method thereof are designed to solve the problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a photocuring adhesive composition for shading and edge sealing of a display module.
In order to achieve the purpose, the invention adopts the following technical scheme:
the light-cured adhesive composition for the shading and edge sealing of the display module comprises the following components in parts by weight based on 100 parts by weight of the adhesive composition: component A is 25-70 parts of aliphatic polyurethane acrylate prepolymer; and (B) component: 5-20 parts of epoxy acrylate prepolymer; component C is 10-40 parts of one or more aliphatic acrylate monomers; component D is 12-45 parts of monofunctional acrylate monomer containing nitrogen atom structure; component E is 0.2 to 5 portions of tackifying promoter containing sulfur or phosphorus atom structure; component F is 1.0 to 8 portions of two or more cracking type photoinitiators; and the component G is 0.05 to 3 parts of carbon black or carbon black premix taking UV monomer as a carrier.
Preferably, the component A comprises 25 to 70 parts of aliphatic polyurethane acrylate prepolymer, wherein the aliphatic polyurethane acrylate prepolymer is derived from polyester or polyether or any copolymer thereof, the weight average molecular weight is greater than or equal to 10000, the functionality is less than or equal to 3, preferably 30 to 65 parts by weight, and the functionality is less than or equal to 2;
the component B: 5-20 parts of epoxy acrylate prepolymer, the glass transition temperature is more than or equal to 60 ℃, and the functionality is less than or equal to 2; preferably 6 to 18 parts by weight, and the glass transition temperature is more than or equal to 80 ℃;
the component C is 10-40 parts of one or more aliphatic acrylate monomers, the glass transition temperature of the monomers is higher than 40C, and the functionality is less than or equal to 2; preferably 12 to 35 parts by weight, the glass transition temperature of the monomer is higher than 60 ℃;
the component D is 12-45 parts, preferably 13-30 parts, of monofunctional acrylate monomer containing a nitrogen atom structure, wherein the nitrogen atom corresponds to a tertiary amine or secondary amine structure;
the component E comprises 0.2 to 5 parts of tackifying promoter containing sulfur or phosphorus atom structure, preferably 0.3 to 4.0 parts by weight of tackifying promoter containing sulfydryl or phosphate structure;
the component F comprises 1.0-8 parts of two or more cracking type photoinitiators, preferably 1.5-6.0 parts by weight, and at least one long-wavelength cracking type photoinitiator, wherein the maximum absorption wavelength of the long-wavelength cracking type photoinitiator is more than 405 nm;
the component G is 0.05 to 3 parts of carbon black or carbon black premix taking UV monomer as a carrier, and preferably 0.10 to 2.5 parts by weight.
Preferably, the acrylate group may be at any position on the polymer molecular chain, preferably at a terminal position of the polymer molecular chain.
Preferably, component C is 10-40 parts of one or more aliphatic acrylate monomers including isobornyl acrylate, dicyclopentenyloxyethyl acrylate, dicyclopentadienyl acrylate, acrylic acid, hexanediol diacrylate, 1, 4-butanediol diacrylate, diethylene glycol diacrylate, 1, 3-butanediol diacrylate, dipropylene glycol diacrylate, neopentyl glycol diacrylate, and any combination thereof.
Preferably, the component D comprises 12 to 45 parts of monofunctional acrylate monomer containing a nitrogen atom structure, and the monomer comprises N-vinyl pyrrolidone, N-dimethylacrylamide, N-diethylacrylamide, morpholine acrylate, N-isopropylacrylamide, N-hydroxyethyl acrylamide, N-dimethylaminopropyl acrylamide, diacetone acrylamide and any combination thereof.
Preferably, the component E comprises 0.2 to 5 parts of tackifying promoter containing sulfur or phosphorus atom structure, and the sulfur-containing tackifying promoter comprises: gamma-mercaptopropyltrimethoxysilane, dodecyl mercaptan, 2-ethylhexyl thioglycolate, 2-bisethanethiol, ethylene glycol di-and trimethylolpropane tri-ester.
Preferably, component F is 1.0-8 parts of two or more cleavage type photoinitiators, preferably 1.5-6.0 parts by weight, and at least comprises one cleavage type photoinitiator with the maximum absorption wavelength less than 390 nm;
a preparation method of a light-cured adhesive composition for shading and edge sealing of a display module comprises the following steps:
s1, respectively taking out three parts of the component B and the component C, uniformly mixing by using a dispersion machine, and adding carbon black into the mixture;
s2, uniformly mixing and dispersing, grinding by a three-roller machine, and discharging to obtain premix after the particle size is less than 20 mu m;
s3, sequentially adding the premix in the S2 and the rest of components (total 100g) into a plastic barrel with the capacity of 150g, putting the plastic barrel into a mixer with the model of a SpeedMixer DAC 150.1FVZr, and dispersing and mixing at high speed for 10 minutes at 2500 rpm;
s4, filtering the obtained mixture by using a 10-micron filter screen.
Preferably, the whole feeding and three-dimensional mixing process is carried out in a way of avoiding light and the temperature is below 60 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention is different from a reaction type polyurethane hot melt adhesive (PUR) technology or a dual-curing UV colloid system, and has the following advantages when in use:
1. the glue dispensing method can be applied to the assembly of the electronic module, and the edge sealing of the module by the glue can be instantly realized;
2. the formula design focuses on balancing the bonding of glass and stainless steel;
3. the good curing depth of the adhesive is kept under the condition of keeping the low transmittance of the adhesive;
4. the glue has excellent temperature resistance and humidity resistance, and can be subjected to harsh environment measurement of module equipment;
5. in the design of the adhesive formula, the heterozygosis epoxy acrylate mode is adopted, so that the problem of stickiness of the surface of the cured glue is solved;
6. the light-curable glue is a single-component solvent-free product, is environment-friendly and healthy, and is convenient for construction and customer use.
Drawings
Fig. 1 is a schematic structural diagram of the application of the black light-shielding UV glue in a large-sized television according to the background art of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The light-cured adhesive composition for the shading and edge sealing of the display module comprises the following components in parts by weight based on 100 parts by weight of the adhesive composition: component A is 25-70 parts of aliphatic polyurethane acrylate prepolymer; and (B) component: 5-20 parts of epoxy acrylate prepolymer; component C is 10-40 parts of one or more aliphatic acrylate monomers; component D is 12-45 parts of monofunctional acrylate monomer containing nitrogen atom structure; component E is 0.2 to 5 portions of tackifying promoter containing sulfur or phosphorus atom structure; component F is 1.0 to 8 portions of two or more cracking type photoinitiators; the component G is 0.05 to 3 portions of carbon black or carbon black premix taking UV monomer as a carrier;
the component A comprises 25-70 parts of aliphatic polyurethane acrylate prepolymer, wherein the aliphatic polyurethane acrylate prepolymer is derived from polyester or polyether or any copolymer thereof, the weight average molecular weight is greater than or equal to 10000, the functionality is less than or equal to 3, preferably 30-65 parts by weight, and the functionality is less than or equal to 2, wherein the acrylate group can be at any position on the polymer molecular chain, preferably at the terminal position of the polymer molecular chain. Wherein the "average functionality" refers to the average number of acrylates in one molecular chain. Typical commercial resins are CN962, CN996NS, CN9031, CN9893, CN959, CN9001, CN9009, CN 986; EBECRYL 113, EBECRYL 4833 from Allenx; UV 3000B, UV 3200B from Nippon Gohsei corporation, etc.;
the component B: 5-20 parts of epoxy acrylate prepolymer, the glass transition temperature is more than or equal to 60 ℃, and the functionality is less than or equal to 2; preferably 6 to 18 parts by weight, and has a glass transition temperature of 80C or higher, and typical commercial resins include NEOPOL 8315, NEOPOL 8319, NEOPOL 8312, NEOPOL 8351, NEOPOL 8352, NEOPOL 8353, NEOPOL 8357, NEOPOL 8358, etc., available from UPICA corporation of Japan; HY-5004 bisphenol A epoxy modified diacrylate ester in Jiangmen Hongye chemical industry and any combination thereof;
the component C is 10-40 parts of one or more aliphatic acrylate monomers, the glass transition temperature of the monomers is higher than 40C, and the functionality is less than or equal to 2; preferably 12 to 35 parts by weight, and a monomer having a glass transition temperature of greater than 60C, typically isobornyl acrylate, dicyclopentenyloxyethyl acrylate, dicyclopentadienyl acrylate, acrylic acid, hexanediol diacrylate, 1, 4-butanediol diacrylate, diethylene glycol diacrylate, 1, 3-butanediol diacrylate, dipropylene glycol diacrylate, neopentyl glycol diacrylate, and any combination thereof;
the component D is 12-45 parts, preferably 13-30 parts by weight of monofunctional acrylate monomer containing a nitrogen atom structure, wherein the nitrogen atom corresponds to a tertiary amine or secondary amine structure, and typical monomers comprise N-vinyl pyrrolidone, N-dimethylacrylamide, N-diethylacrylamide, morpholine acrylate, N-isopropylacrylamide, N-hydroxyethyl acrylamide, N-dimethylaminopropyl acrylamide, diacetone acrylamide and any combination thereof;
0.2-5 parts of tackifying promoter containing sulfur or phosphorus atom structure, preferably 0.3-4.0 parts by weight, tackifying promoter containing sulfydryl or phosphate structure, typical commercial sulfur-containing tackifying promoter is as follows: gamma-mercaptopropyltrimethoxysilane, dodecyl mercaptan, 2-ethylhexyl thioglycolate, 2- (1, 2-ethanediylbiooxo) bisethanethiol, ethylene glycol di (3-mercaptopropionate), trimethylolpropane tri (3-mercaptopropionate); typical tackifying aids containing phosphorus atom structures include SR 9050 and SR 9051 of Sartomer company; EB 168, EB 170, EB 171, by Allnex corporation, and any combination thereof;
the component F comprises 1.0-8 parts of two or more cracking type photoinitiators, preferably 1.5-6.0 parts by weight, and at least one long-wavelength cracking type photoinitiator, wherein the maximum absorption wavelength of the long-wavelength cracking type photoinitiator is more than 405nm, so that the deep curing of the light-curable adhesive is facilitated; at least contains a cracking type photoinitiator with the maximum absorption wavelength less than 390nm, which is beneficial to the surface curing of the adhesive; typical deep-cure initiators are:
omnirad TPO: 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide
Omnirad TPO-L: 2,4, 6-Trimethylbenzoylphenylphosphonic acid ethyl ester
Omnirad 819: [ bis (2, 4, 6-trimethylbenzoyl) phenylphosphine oxide ]
Initiators for surface curing such as:
omnirad 651: benzoinum dimethyl ether
Omnirad MBF: benzoic acid methyl ester
Omnirad 907: [ 2-methyl-1- (4-methylmercaptophenyl) -2-morpholinopropanone-1 ]
Omnirad 369: [ 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1 ]
Omnirad 184: (1-hydroxy-cyclohexylbenzophenone)
Omnirad 1173: (2-hydroxy-2-methyl-phenylacetone-1)
Omnirad 2959: (2-hydroxy-2-methyl-p-hydroxyethyl etheryl-phenyl-acetone-1);
the component G is 0.05 to 3 parts by weight of carbon black or carbon black premix taking UV monomer as a carrier, preferably 0.10 to 2.5 parts by weight;
the following photo-curing adhesive performance parameters were obtained:
example one
The adhesive composition was formulated as follows:
all parts are parts by weight based on 100 parts by weight of the adhesive composition.
The preparation method of the photocuring adhesive composition for the shading and edge sealing of the display module comprises the following steps:
s1, respectively taking out three parts of the component B and the component C, uniformly mixing by using a dispersion machine, and adding carbon black into the mixture;
s2, uniformly mixing and dispersing, grinding by a three-roller machine, and discharging to obtain premix after the particle size is less than 20 mu m;
s3, sequentially adding the premix in the S2 and the rest of components (total 100g) into a plastic barrel with the capacity of 150g, putting the plastic barrel into a mixer with the model of a SpeedMixer DAC 150.1FVZr, and dispersing and mixing at high speed for 10 minutes at 2500 rpm;
s4, filtering the obtained mixture by using a 10-micron filter screen;
wherein, the whole feeding and three-dimensional mixing process is carried out in a dark place at a temperature below 60 ℃;
after preparation, it was tested and verified:
1. viscosity measurement
Which refers to Brookfield viscosity (Brookfield), is measured using ASTM D1084, at a test temperature of 25 ℃.
2. Hardness test
In a circular aluminum foil tray (diameter about 4cm), glue (formulation with complete removal of carbon black) was poured to a thickness of about 2 cm. The sample was sufficiently cured for 60 seconds by ultraviolet light using a metal halogen lamp (manufacturer: Loctite, model: UVALOC1000) covering a 200nm-400nm ultraviolet band as a curing light source, with an irradiation energy of about 9000mJ/cm2 and an irradiation power of about 150mW/cm 2.
When the hardness is tested, three adhesive films with the same size and the thickness of 2mm are selected. Hardness values at 6mm thickness were measured by durometer at 25C, 50% relative humidity.
3. Light transmittance and optical density test:
on a 40mm by 60mm by 1.5mm glass plate, the thickness was controlled by a stainless steel wire with a diameter of 0.15mm, about 0.35-0.40g of glue was placed evenly in the center of the glass plate, covered with another 40mm by 60mm by 1.5mm glass plate, the glue was leveled into a ring shape with gentle force, and placed under the above mentioned uv light for sufficient curing for 20 seconds (UVA intensity 150mW/cm 2). The optical transmittance of the glass sheet was measured with a HunterLab desk-top spectrocolorimeter, which was an experimental device, to obtain the optical density by conversion.
4. Test of glue curing depth and glue surface dryness
In a circular aluminum foil tray (diameter about 4cm), glue with a thickness of about 1cm was poured. The sample was sufficiently cured for 20 seconds under ultraviolet light using a metal halogen lamp (manufacturer: Loctite, model: UVALOC1000) covering a 200nm-400nm ultraviolet band as a curing light source, with an irradiation energy of about 3000mJ/cm2 and an irradiation power of about 150mW/cm 2.
After cooling, the hand feeling surface is dry and comfortable; then, the cured film was peeled off, and the cured thickness was measured with a vernier caliper after drying.
5. Bond tensile Strength test
The adhesive composition was coated between a glass sheet and SU303 stainless steel (25mm by 40mm by 4mm) at room temperature to a coating thickness of 150 microns. The obtained sample was irradiated from the surface of a light-transmitting glass with an ultraviolet light source (manufacturer: Loctite Co., model: UVALOC1000) covering an ultraviolet light band of 200nm to 400nm at an irradiation energy of about 3000mJ/cm2 and a radiation power of about 150mW/cm2 for about 20 seconds.
a. Tensile testing at room temperature: the samples were placed in a standard environment at 23C, 50% RH relative humidity and allowed to stand for 24 hours.
b. Aging test after high temperature and high humidity: the samples were placed in a 65C, 90% relative humidity environment and aged for 120 hours. And (5) taking out the sample, and observing whether the sample has cracking, degumming or air bubble problems. The aged samples were then allowed to stand for 24 hours at a standard ambient of 23C, 50% RH relative humidity.
The sample on which the UV curing test was performed was pulled in the direction perpendicular to the surface of the glass sheet in the opposite direction to the stainless steel by using a universal tensile machine (manufacturer: Instron Co., Ltd.; model: Instron 5540) to perform the adhesion tensile strength test at a tensile speed of 10mm per minute under a load of 1000N. The bonding strength (unit: MPa) is obtained by dividing the obtained force value by the lapping area of the glass sheet and the stainless steel.
6. Curing for optical density test:
on a 40mm by 60mm by 1.5mm glass slide, the thickness was controlled with a stainless steel wire with a diameter of 0.1mm, approximately 0.25g of glue was placed evenly in the center of the glass slide, covered with another 40mm by 60mm by 1.5mm glass slide, the glue was leveled into a ring with gentle force, and left to stand under uv light for a full cure of 14 seconds (UVA intensity 150mW/cm 2). The optical transmittance of the glass sheet was measured with a HunterLab desk-top spectrocolorimeter, which was an experimental device, to obtain the optical density by conversion.
The obtained adhesive composition had a viscosity of 8000mpa.s/25 c,
shore A hardness after curing was ShD 45
Optical Density 1.8
Glue bond strength (150 microns): 1.8 MPa.
Bond strength after high temperature high humidity aging (150 microns), 65C, 90% relative humidity 120 hours: 1.62MPa, no bubble in glue, no cracking.
Glue curing depth: 210 micron
Testing the dryness of the surface of the glue: the hand feeling surface dryness after cooling is excellent.
Example two
The adhesive composition was formulated as follows:
all parts are parts by weight based on 100 parts by weight of the adhesive composition.
The viscosity of the obtained adhesive composition was 20000mpa.s/25 c,
shore A hardness after curing was ShD 47
Optical Density 1.6
Glue bond strength (150 microns): 1.5 MPa.
Bond strength after high temperature high humidity aging (150 microns), 65C, 90% relative humidity 120 hours: 1.40MPa, no bubble and no cracking of glue;
glue curing depth: 250 microns;
testing the dryness of the surface of the glue: the hand feeling surface dryness after cooling is excellent.
EXAMPLE III
The adhesive composition was formulated as follows:
all parts are parts by weight based on 100 parts by weight of the adhesive composition.
The obtained adhesive composition had a viscosity of 1300mpa.s/25 c,
shore A hardness after curing was ShD 50
Optical density 2.0
Glue bond strength (150 microns): 3.3 MPa.
Bond strength after high temperature high humidity aging (150 microns), 65C, 90% relative humidity 120 hours: 2.40MPa, no bubble in the glue, and no cracking.
Glue curing depth: 200 micron
Testing the dryness of the surface of the glue: the hand feeling surface dryness after cooling is excellent.
COMPARATIVE EXAMPLE 1
In the same manner as in example 1, an adhesive composition of comparative example 1 was prepared, except that the formulation of the adhesive composition was changed as shown in the following table:
all parts are parts by weight based on 98.04 parts by weight of the adhesive composition after removal of the TMPMP.
The obtained adhesive composition had a viscosity of 8300mpa.s/25 c,
shore A hardness after curing was ShD 44
Optical Density 1.81
Glue bond strength (150 microns): 1.1 MPa.
Testing the dryness of the surface of the glue: the hand feeling surface dryness after cooling is poor.
It is apparent that the adhesive composition of comparative example 1, which uses a mercapto group-containing monomer as a main resin, is excellent in adhesion to stainless steel. On the other hand, the adhesion of comparative example 1 was remarkably reduced after removal, and it was difficult to satisfy the requirement of high strength, and the surface dryness was also deteriorated.
COMPARATIVE EXAMPLE 2 (COMPARATIVE EXAMPLE 1)
In the same manner as in example 1, an adhesive composition of comparative example 2 was prepared, except that the formulation of the adhesive composition was changed as shown in the following table:
all parts are parts by weight based on 100 parts by weight of the adhesive composition.
The adhesive composition obtained had a viscosity of 7400mpa.s/25 c,
shore A hardness after curing was ShD 38
Optical Density 1.50
Glue bond strength (150 microns): 1.6 MPa.
Bond strength after high temperature high humidity aging (150 microns), 65C, 90% relative humidity 120 hours: 1.40MPa, no bubble in glue, and no cracking.
Glue curing depth: 210 microns;
testing the dryness of the surface of the glue: the hand feeling surface dryness after cooling is excellent.
It is apparent that the adhesive composition of comparative example 1, from which the epoxy acrylate was removed from the main resin, had a slightly decreased adhesion to stainless steel, but had a significant deterioration in surface drying.
COMPARATIVE EXAMPLE 3 (COMPARATIVE EXAMPLE 1)
In the same manner as in example 1, an adhesive composition of comparative example 2 was prepared, except that the formulation of the adhesive composition was changed as shown in the following table:
all parts are parts by weight based on 100 parts by weight of the adhesive composition.
The adhesive composition obtained had a viscosity of 9200mpa.s/25 c,
shore A hardness after curing was ShD 39
Optical Density 1.51
Glue bond strength (150 microns): 0.8 MPa.
Bond strength after high temperature high humidity aging (150 microns), 65C, 90% relative humidity 120 hours: 0.76MPa, no bubble in the glue, and no cracking.
Glue curing depth: 210 micron
Testing the dryness of the surface of the glue: the dryness of the hand feeling surface after cooling is normal.
It is apparent that the adhesive composition of comparative example 1, from which the acrylic monomer containing a nitrogen atom was removed, had a remarkably reduced adhesion to stainless steel and also had poor surface drying.
The invention is different from a reaction type polyurethane hot melt adhesive (PUR) technology or a dual-curing UV colloid system, and has the following advantages when in use:
1. the glue dispensing method can be applied to the assembly of the electronic module, and the edge sealing of the module by the glue can be instantly realized;
2. the formula design focuses on balancing the bonding of glass and stainless steel;
3. the good curing depth of the adhesive is kept under the condition of keeping the low transmittance of the adhesive;
4. the glue has excellent temperature resistance and humidity resistance, and can be subjected to harsh environment measurement of module equipment;
5. in the design of the adhesive formula, the heterozygosis epoxy acrylate mode is adopted, so that the problem of stickiness of the surface of the cured glue is solved;
6. the light-curable glue is a single-component solvent-free product, is environment-friendly and healthy, and is convenient for construction and customer use.
The photo-curing adhesive with a special formula developed by the invention can give consideration to the problems of optical density and deep curing; the adhesive has excellent adhesion to glass and stainless steel, and is very suitable for assembling large-size television module materials.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The light-cured adhesive composition for the shading and edge sealing of the display module is based on 100 parts by weight of the adhesive composition, and is characterized by comprising the following components in parts by weight: component A is 25-70 parts of aliphatic polyurethane acrylate prepolymer; and (B) component: 5-20 parts of epoxy acrylate prepolymer; component C is 10-40 parts of one or more aliphatic acrylate monomers; component D is 12-45 parts of monofunctional acrylate monomer containing nitrogen atom structure; component E is 0.2 to 5 portions of tackifying promoter containing sulfur or phosphorus atom structure; component F is 1.0 to 8 portions of two or more cracking type photoinitiators; and the component G is 0.05 to 3 parts of carbon black or carbon black premix taking UV monomer as a carrier.
2. The light-cured adhesive composition for the shading and edge sealing of a display module according to claim 1, wherein the component A comprises 25 to 70 parts of aliphatic polyurethane acrylate prepolymer, wherein the aliphatic polyurethane acrylate prepolymer is derived from polyester or polyether or any copolymer thereof, has a weight average molecular weight of 10000 or more, has a functionality of 3 or less, preferably 30 to 65 parts by weight, and has a functionality of 2 or less;
the component B: 5-20 parts of epoxy acrylate prepolymer, the glass transition temperature is more than or equal to 60 ℃, and the functionality is less than or equal to 2; preferably 6 to 18 parts by weight, and the glass transition temperature is more than or equal to 80 ℃;
the component C is 10-40 parts of one or more aliphatic acrylate monomers, the glass transition temperature of the monomers is higher than 40C, and the functionality is less than or equal to 2; preferably 12 to 35 parts by weight, the glass transition temperature of the monomer is higher than 60 ℃;
the component D is 12-45 parts, preferably 13-30 parts, of monofunctional acrylate monomer containing a nitrogen atom structure, wherein the nitrogen atom corresponds to a tertiary amine or secondary amine structure;
the component E comprises 0.2 to 5 parts of tackifying promoter containing sulfur or phosphorus atom structure, preferably 0.3 to 4.0 parts by weight of tackifying promoter containing sulfydryl or phosphate structure;
the component F comprises 1.0-8 parts of two or more cracking type photoinitiators, preferably 1.5-6.0 parts by weight, and at least one long-wavelength cracking type photoinitiator, wherein the maximum absorption wavelength of the long-wavelength cracking type photoinitiator is more than 405 nm;
the component G is 0.05 to 3 parts of carbon black or carbon black premix taking UV monomer as a carrier, and preferably 0.10 to 2.5 parts by weight.
3. The light-curable adhesive composition for the light-shielding edge sealing of a display module according to claim 1, wherein the acrylate group can be located at any position of the polymer molecular chain, preferably at the terminal position of the polymer molecular chain.
4. The photocurable adhesive composition for a black-out edge seal of a display module as set forth in claim 1, wherein said component C is 10-40 parts of one or more aliphatic acrylate monomers comprising isobornyl acrylate, dicyclopentenyloxyethyl acrylate, dicyclopentadienyl acrylate, acrylic acid, hexanediol diacrylate, 1, 4-butanediol diacrylate, diethylene glycol diacrylate, 1, 3-butanediol diacrylate, dipropylene glycol diacrylate, neopentyl glycol diacrylate, and any combination thereof.
5. The photo-curable adhesive composition for a light-shielding edge sealing of a display module according to claim 1, wherein the component D comprises 12-45 parts of a monofunctional acrylate monomer containing a nitrogen atom structure, and the monomer comprises N-vinyl pyrrolidone, N-dimethylacrylamide, N-diethylacrylamide, morpholine acrylate, N-isopropylacrylamide, N-hydroxyethyl acrylamide, N-dimethylaminopropyl acrylamide, diacetone acrylamide, and any combination thereof.
6. The photo-curing adhesive composition for the shading and edge sealing of the display module as claimed in claim 1, wherein the component E comprises 0.2-5 parts of tackifying auxiliary agent with a sulfur or phosphorus atom structure, and the tackifying auxiliary agent with sulfur comprises: gamma-mercaptopropyltrimethoxysilane, dodecyl mercaptan, 2-ethylhexyl thioglycolate, 2-bisethanethiol, ethylene glycol di-and trimethylolpropane tri-ester.
7. The light-curable adhesive composition for the shading and edge sealing of a display module according to claim 1, wherein the component F comprises 1.0 to 8 parts by weight of two or more cleavage type photoinitiators, preferably 1.5 to 6.0 parts by weight, and at least one cleavage type photoinitiator with the absorption maximum wavelength of less than 390 nm.
8. A preparation method of a light-cured adhesive composition for shading and edge sealing of a display module is characterized by comprising the following steps:
s1, respectively taking out three parts of the component B and the component C, uniformly mixing by using a dispersion machine, and adding carbon black into the mixture;
s2, uniformly mixing and dispersing, grinding by a three-roller machine, and discharging to obtain premix after the particle size is less than 20 mu m;
s3, sequentially adding the premix in the S2 and the rest of components (total 100g) into a plastic barrel with the capacity of 150g, putting the plastic barrel into a mixer with the model of a SpeedMixer DAC 150.1FVZr, and dispersing and mixing at high speed for 10 minutes at 2500 rpm;
s4, filtering the obtained mixture by using a 10-micron filter screen.
9. The method for preparing the light-curable adhesive composition for edge sealing and shading of a display module according to claim 8, wherein the light should be protected from light and the temperature should be below 60 ℃ during the whole feeding and three-dimensional mixing process.
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| CN201911066644.XA CN111378412A (en) | 2019-11-04 | 2019-11-04 | Light-cured adhesive composition for shading and edge sealing of display module and preparation method thereof |
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| CN201911066644.XA CN111378412A (en) | 2019-11-04 | 2019-11-04 | Light-cured adhesive composition for shading and edge sealing of display module and preparation method thereof |
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| CN114350303A (en) * | 2021-11-29 | 2022-04-15 | 浙江国能科技有限公司 | Delayed curing UV (ultraviolet) adhesive for bonding optical glass and aluminum sheet |
| CN115109557A (en) * | 2022-07-04 | 2022-09-27 | 安徽众博新材料有限公司 | Electronic packaging UV adhesive with high adhesive force and capable of being rapidly cured |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115109557B (en) * | 2022-07-04 | 2024-03-19 | 安徽众博新材料有限公司 | Fast-curing high-adhesion electronic packaging UV adhesive |
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