CN113861854A - Adhesive film for image display device and image display device - Google Patents
Adhesive film for image display device and image display device Download PDFInfo
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- CN113861854A CN113861854A CN202111127894.7A CN202111127894A CN113861854A CN 113861854 A CN113861854 A CN 113861854A CN 202111127894 A CN202111127894 A CN 202111127894A CN 113861854 A CN113861854 A CN 113861854A
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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
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/33—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements being semiconductor devices, e.g. diodes
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- G—PHYSICS
- G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
- G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
- G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
- G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
- G09F9/35—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements being liquid crystals
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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
- C09J2433/00—Presence of (meth)acrylic polymer
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Abstract
The invention discloses an adhesive film for an image display device and the image display device, the glass transition temperature of the adhesive film is-23-0 ℃, and the tan delta at 25-100 ℃ is 0.42-0.84, the glass transition temperature is the temperature at which the tan delta shows the peak value within-40-80 ℃, the tan delta is the value obtained by dividing the loss modulus by the storage modulus, and the adhesive film comprises the following components: 1) acrylic derivative polymer, and acrylic derivative polymer packageComprises the following raw materials: C4-C18 acrylate monomer, hydrophilic monomer and basic monomer; 2) and the photoinitiator comprises a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator. The adhesive film has good filling property and storage stability, good reliability after ultraviolet post-curing, and can inhibit high temperature and high humidity (85)oC/85% RH), air bubbles, floating, peeling, and the like.
Description
Technical Field
The invention relates to an adhesive film for an image display device and an image display device.
Background
As an example of a typical image display device (fig. 1), a Liquid Crystal Display (LCD) or LED display device is exemplified, and as can be seen from fig. 1, in order to obtain a good display effect, the adhesive film should have a good filling capability to fill the ink level difference without generating bubbles. Meanwhile, in the long-time storage process, the adhesive film should not overflow to cause defects. Further, when the display device is used for a vehicle, an outdoor measuring instrument, a mobile phone, a personal computer, or the like, the use environment in which the adhesive film is adhered becomes very severe, and the adhesive force of the adhesive film is reduced when the members are bonded, and bubbles, peeling, or the like are likely to occur. Therefore, there is an increasing demand for highly durable pressure-sensitive adhesive sheets that do not generate bubbles, peeling, and the like in the application environment.
In response to this requirement, JP20040279833, JP20070284292, CN103403119B and CN104254583B exemplify adhesive material compositions which are exposed to high temperature and high humidity for a long time, and which do not cause foaming, floating, peeling, etc. at the bonding interface, but it is difficult to achieve both good filling properties and good storage stability of the resulting adhesive film.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an adhesive film for an image display device, which has good filling property and storage stability.
In order to achieve the purpose, the invention adopts the technical scheme that: an adhesive film for an image display device, the adhesive film having a glass transition temperature of-23 to 0 ℃ and a tan δ of 0.42 to 0.84 at 25 to 100 ℃, the glass transition temperature being a temperature at which tan δ shows a peak within-40 to 80 ℃, the tan δ being a value obtained by dividing a loss modulus by a storage modulus, the adhesive film comprising the following components:
1) an acrylic derivative polymer comprising the following raw materials: C4-C18 acrylate monomer, hydrophilic monomer and basic monomer;
2) a photoinitiator which comprises a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator,
wherein the adding amount of the alkaline monomer is 0.5-15% of the mass of the acrylic derivative polymer raw material.
Here, the adhesive film is obtained by polymerizing an acrylic derivative polymer and a photoinitiator, and the polymerization method includes, but is not limited to, uv curing without solvent, thermal curing, and solvent thermal polymerization.
In the ultraviolet curing process, the light source can be, but is not limited to, LED lamp, low-pressure mercury lamp, medium-pressure mercury lamp, high-pressure mercury lamp, etc., and the ultraviolet irradiation device is used for irradiating ultraviolet rays with intensity of 0.65-1mW/cm2。
Preferably, the acrylic derivative polymer comprises the following raw materials in percentage by mass: 75-89.5% of C4-C18 acrylate monomer, 10% of hydrophilic monomer and the balance of basic monomer.
As a specific embodiment, the C4-C18 acrylate monomer includes but is not limited to one or more of butyl (meth) acrylate, isooctyl (meth) acrylate, isobornyl (meth) acrylate, isobutyl (meth) acrylate, tert-butyl (meth) acrylate, cyclohexyl (meth) acrylate, n-octyl (meth) acrylate, dodecyl (meth) acrylate, stearyl (meth) acrylate and isostearyl (meth) acrylate, and the C4-C18 acrylate monomer is added in an amount of 50-95% of the mass of the acrylic derivative polymer raw material.
As a specific embodiment, the hydrophilic monomer includes but is not limited to one or more of hydroxyethyl acrylate, 2-hydroxypropyl acrylate and 4-hydroxybutyl acrylate, and the amount of the hydrophilic monomer added is 5-30%, preferably 10% of the mass of the acrylic derivative polymer raw material.
As a specific embodiment, the basic monomer includes but is not limited to one or more of (meth) acrylamide, (meth) acryloyl morpholine, N-dimethylacrylamide, and the addition amount of the basic monomer is 0.5-15% of the mass of the acrylic derivative polymer raw material.
As a specific embodiment, the hydrogen abstraction type ultraviolet light initiator includes but is not limited to one or more of 4-methyl benzophenone, 4-acrylyl oxybenzoic acid benzophenone, and the amount of the hydrogen abstraction type ultraviolet light initiator is 0.1-1% of the amount of the acrylic derivative polymer.
As a specific embodiment, the cleavage type uv initiator includes, but is not limited to, one or more of benzoin derivatives, benzil ketal derivatives, dialkoxyacetophenones, α -hydroxyalkylphenylketones, α -aminoalkylphenones, acylphosphine hydrides, esterified oxime ketone compounds, aryl peroxy ester compounds, halogenated methyl aryl ketones, organic sulfur-containing compounds, and benzoyl formate, and is used in an amount of 0.1 to 2%, preferably 0.5%, based on the mass of the acrylic derivative polymer.
As a specific embodiment, the adhesive film comprises the following components:
1) the acrylic acid derivative polymer comprises the following raw materials in percentage by mass: 75-89.5% of C4-C18 acrylate monomer, 10% of hydrophilic monomer and the balance of alkaline monomer;
2) the photoinitiator adopts a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator, wherein the cracking type ultraviolet initiator adopts benzil dimethyl ether, the hydrogen abstraction type ultraviolet initiator adopts 4-acrylyl oxybenzoic acid benzophenone or 4-methyl benzophenone, and the adding amount of the hydrogen abstraction type ultraviolet initiator is 0.1-1% of the mass of the acrylic derivative polymer;
and the adhesive film has a glass transition temperature of-23 to 0 ℃ and a tan delta of 0.42 to 0.84 at 25 to 100 ℃, the glass transition temperature being a temperature at which tan delta shows a peak value within-40 to 80 ℃, the tan delta being a value obtained by dividing a loss modulus by a storage modulus. Here, the amount of the cleavage type ultraviolet initiator added is preferably 0.5% of the amount of the acrylic derivative polymer.
A second object of the present invention is to provide an image display device having a layer on the visible side to which the image display device is adhered with an adhesive film.
A third object of the present invention is to provide an image display device having the adhesive film for an image display device between a transparent protective plate and a touch panel or between a transparent protective plate and an image display unit.
There is also provided a method of manufacturing an image display device, comprising: the adhesive sheet for an image display device is used to bond the transparent protective plate to the touch panel, the touch panel to the image display unit, or the transparent protective plate to the image display unit.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the adhesive film for image display device is polymerized by acrylic derivative polymer and photoinitiator, has glass transition temperature of-23-0 deg.C and tan delta of 0.42-0.84 at 25-100 deg.C, has good filling property and storage stability, and has good reliability after UV post-curing, and can inhibit bubbles, floating, peeling and the like at high temperature and high humidity (85 deg.C/85% RH).
Drawings
Fig. 1 is a schematic diagram showing a cross-sectional structure of an example of a conventional image display device;
wherein: 1. a transparent protective plate (glass or plastic substrate); 2. the adhesive layer is used for attaching the transparent protective plate and the display module; 3. a display module (LCD module or LED module).
Detailed Description
The technical solution of the present invention is further illustrated below with reference to specific examples.
An adhesive film for an image display device, the adhesive film comprising the following components:
1) an acrylic derivative polymer comprising the following raw materials: C4-C18 acrylate monomer, hydrophilic monomer and basic monomer;
2) a photoinitiator which comprises a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator,
wherein the adding amount of the alkaline monomer is 0.5-15% of the mass of the acrylic derivative polymer raw material,
the adhesive film has a glass transition temperature of-23 to 0 ℃ and a tan delta of 0.42 to 0.84 at 25 to 100 ℃, the glass transition temperature is a temperature at which tan delta shows a peak value within-40 to 80 ℃, and the tan delta is a value obtained by dividing a loss modulus by a storage modulus.
Specifically, the C4-C18 acrylate monomer includes, but is not limited to, one or more of butyl (meth) acrylate, isooctyl (meth) acrylate, isobornyl (meth) acrylate, isobutyl (meth) acrylate, tert-butyl (meth) acrylate, cyclohexyl (meth) acrylate, n-octyl (meth) acrylate, dodecyl (meth) acrylate, octadecyl (meth) acrylate, and isostearyl (meth) acrylate, and the addition amount thereof is 50-95% of the mass of the raw material of the acrylic derivative polymer.
The hydrophilic monomer comprises one or more of 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate and 4-hydroxybutyl acrylate, and the adding amount of the hydrophilic monomer is 5-30% of the mass of the acrylic derivative polymer raw material.
The basic monomer includes but is not limited to one or more of (meth) acrylamide, (meth) acryloyl morpholine and N, N-dimethylacrylamide, and the adding amount of the basic monomer is 0.5-15% of the mass of the acrylic derivative polymer raw material.
< preparation of acrylic derivative Polymer >
Production example 1
75.5g of isooctyl acrylate, 14g of isobornyl acrylate, 10g of hydroxyethyl acrylate, and 0.5g of (meth) acrylamide were charged into a reaction vessel equipped with a cooling tube, a thermometer, a stirring device, a dropping funnel, and a nitrogen injection tube, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing with nitrogen gas with an air volume of 100 mL/minute. Then, while maintaining the temperature at 50 ℃, 0.06g of azobisisoheptonitrile was dissolved in 15.1g of isooctyl acrylate, 2.8g of isobornyl acrylate, 2g of hydroxyethyl acrylate, and 0.1g of (meth) acrylamide as additional monomers to prepare a solution, and the solution was added to the reaction vessel 4 to 6 times in 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer a.
Production example 2
75.5g of isooctyl acrylate, 7g of isobornyl acrylate, 10g of hydroxyethyl acrylate, 2.5g of (meth) acrylamide and 5g of (meth) acryloylmorpholine were charged into a reaction vessel equipped with a cooling tube, a thermometer, a stirrer, a dropping funnel and a nitrogen-injecting tube, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing with nitrogen gas with an air volume of 100 mL/minute. Then, while maintaining the temperature at 50 ℃, 0.06g of azobisisoheptonitrile was dissolved in 15.1g of isooctyl acrylate, 1.4g of isobornyl acrylate, 2g of hydroxyethyl acrylate, 0.5g of (meth) acrylamide and 1g of (meth) acryloylmorpholine as additional monomers to prepare a solution, and the solution was added to the reaction vessel 4 to 6 times within 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer B.
Production example 3
A reaction vessel equipped with a cooling tube, a thermometer, a stirring device, a dropping funnel and a nitrogen injection tube was charged with 70g of isooctyl acrylate, 5g of isobornyl acrylate, 10g of hydroxyethyl acrylate, 1g of (meth) acrylamide and 14g of (meth) acryloylmorpholine, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing with nitrogen gas with an air volume of 100 mL/minute. Thereafter, while maintaining the temperature at 50 ℃, a solution prepared by dissolving azobisisoheptonitrile in an amount of 0.06g was used as additional monomers including isooctyl acrylate 14g, isobornyl acrylate 1g, hydroxyethyl acrylate 2g, (meth) acrylamide 0.2g and (meth) acryloylmorpholine 2.8g, and the solution was charged into a reaction vessel 4 to 6 times in 1 hour, and after the completion of the charging, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer C.
Production example 4
A reaction vessel equipped with a cooling tube, a thermometer, a stirring device, a dropping funnel and a nitrogen injection tube was charged with 66g of isooctyl acrylate, 10g of isobornyl acrylate, 10g of hydroxyethyl acrylate, 2g of (meth) acrylamide and 12g of (meth) acryloylmorpholine, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing with nitrogen gas with an air volume of 100 mL/minute. Then, while maintaining the temperature at 50 ℃, using 13.2g of isooctyl acrylate, 2g of isobornyl acrylate, 2g of hydroxyethyl acrylate, 0.4g of (meth) acrylamide and 2.4g of (meth) acryloylmorpholine as additional monomers, 0.06g of azobisisoheptonitrile was dissolved therein to prepare a solution, and the solution was added to the reaction vessel 4 to 6 times within 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer D.
Production example 5
76g of isooctyl acrylate, 14g of isobornyl acrylate, and 10g of hydroxyethyl acrylate were charged into a reaction vessel equipped with a cooling tube, a thermometer, a stirring device, a dropping funnel, and a nitrogen-injecting tube, and the mixture was heated from room temperature (25 ℃ C.) to 50 ℃ for 15 minutes while replacing the nitrogen with an air volume of 100 mL/minute. Then, while maintaining the temperature at 50 ℃, 0.06g of azobisisoheptonitrile was dissolved in 15.2g of isooctyl acrylate, 2.8g of isobornyl acrylate, and 2g of hydroxyethyl acrylate as additional monomers to prepare a solution, and the solution was added to the reaction vessel 4 to 6 times in 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer E.
Production example 6
A reaction vessel equipped with a cooling tube, a thermometer, a stirrer, a dropping funnel and a nitrogen injection tube was charged with 66g of isooctyl acrylate, 10g of hydroxyethyl acrylate, 4g of (meth) acrylamide and 20g of (meth) acryloylmorpholine, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing the nitrogen with 100 mL/minute of air flow. Then, while maintaining the temperature at 50 ℃, a solution was prepared by dissolving 0.06g of azobisisoheptonitrile in 13.2g of isooctyl acrylate, 2g of hydroxyethyl acrylate, (meth) acrylamide, and 4g of (meth) acryloylmorpholine as additional monomers, and the solution was added to the reaction vessel 4 to 6 times in 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylate polymer F.
Production example 7
Adding 75.5G of isooctyl acrylate, 7G of isobornyl acrylate, 10G of hydroxyethyl acrylate and 2.5G of (methyl) acrylamide into a reaction vessel with a stirring device and a nitrogen injection pipe, carrying out nitrogen replacement with the air volume of 100 mL/min while uniformly stirring, irradiating by using a 365nm LED lamp until the viscosity reaches about 10000cp, then closing the nitrogen, and introducing compressed air for 2min to obtain an acrylate polymer G.
Production example 8
0.3g of isooctyl thioglycolate, 75.5g of isooctyl acrylate, 7g of isobornyl acrylate, 10g of hydroxyethyl acrylate, 2.5g of (meth) acrylamide, and 5g of (meth) acryloylmorpholine were charged into a reaction vessel equipped with a cooling tube, a thermometer, a stirring device, a dropping funnel, and a nitrogen gas injection tube, and heated from room temperature (25 ℃) to 50 ℃ for 15 minutes while replacing with nitrogen gas with an air flow of 100 mL/minute. Then, while maintaining the temperature at 50 ℃, 0.06g of azobisisoheptonitrile was dissolved in 15.1g of isooctyl acrylate, 1.4g of isobornyl acrylate, 2g of hydroxyethyl acrylate, 0.5g of (meth) acrylamide and 1g of (meth) acryloylmorpholine as additional monomers to prepare a solution, and the solution was added to the reaction vessel 4 to 6 times within 1 hour, and after the addition was completed, the reaction was further carried out for 1 hour to obtain an acrylic ester polymer H.
< sample compounding and adhesive sheet production >
Example 1
100g of the acrylic derivative polymer A obtained in production example 1, 0.5g of benzil dimethyl ether and 0.3g of 4-acryloyloxybenzoic acid phenone (4ABP) were weighed, and dissolved uniformly under stirring and then degassed under a vacuum of 0.95MPa for 2 hours to obtain an adhesive resin composition for adhesive sheets.
Then, the adhesive resin composition for adhesive sheet obtained in the above was dropped on a polyethylene terephthalate (PET) release film (release surface-contacting adhesive resin composition), and then another PET release film was coveredOn the surface (the release surface was brought into contact with the adhesive resin composition), the adhesive resin composition for adhesive sheets was coated into a sheet form with a roll, and an ultraviolet ray (intensity of 1 mW/cm) was irradiated using an ultraviolet ray irradiation apparatus2The energy is 600mJ/cm2) To obtain a transparent adhesive sheet.
Examples 2 to 6 and comparative examples 1 to 6
As shown in the following table, all the steps were the same as in example 1 except that the kind and amount of the acrylic derivative polymer added or the hydrogen abstraction-type initiator added were different.
Example 7
As shown in the following Table, the ultraviolet intensity for the coating curing step was reduced to 0.65mW/cm except that the acrylic derivative polymer B was added2Except that, all the steps were the same as in example 1.
Example 8
As shown in the following table, all the steps were the same as in example 1 except that the acrylic derivative polymer added was G.
Comparative example 7
100g of the acrylic derivative polymer B obtained in production example 2, 0.5g of benzildimethyl ether, 0.2g of 1, 6-hexanediol diacrylate (HDDA), and 0.3g of 4-acryloyloxybenzophenone (4ABP) were weighed, stirred and dissolved uniformly, and then degassed under a vacuum of 0.95MPa for 2 hours to obtain an adhesive resin composition for an adhesive sheet.
The procedure for preparing an adhesive sheet was as in example 1.
Comparative example 8
100g of the acrylic derivative polymer B obtained in production example 2, 0.5g of benzildimethyl ether, 0.3g of 1, 6-hexanediol diacrylate (HDDA), and 0.3g of 4-acryloyloxybenzophenone (4ABP) were weighed, and after uniformly stirred and dissolved, the mixture was degassed under a vacuum of 0.95MPa for 2 hours to obtain an adhesive resin composition for an adhesive sheet.
The procedure for preparing an adhesive sheet was as in example 1.
Comparative example 9
As shown in the following Table, the intensity of ultraviolet rays for the coating curing step was increased except that the acrylic derivative polymer added was H50mW/cm2Except that, all the steps were the same as in example 1.
The adhesive sheets obtained in the above examples and comparative examples were evaluated in the following manner, and the evaluation results are shown in the following table.
(ii) measurement of glass transition temperature, loss modulus of elasticity and storage modulus of elasticity
An adhesive sheet having a thickness of 0.5mm, a width of 10mm and a length of 10mm was prepared, and a wide-range dynamic viscoelasticity measuring apparatus was used ()
An adhesive sheet having a thickness of 0.5mm, a width of 10mm and a length of 10mm was prepared, and the measurement was carried out in a share sandwich mode at a frequency of 1.0Hz, a measurement temperature range of-40 to 80 ℃ and a temperature rise rate of 5 ℃/min by using a wide-range dynamic viscoelasticity measuring apparatus (Solids Analyzer RSA-II, manufactured by Phenometric Scientific Co., Ltd.).
The glass transition temperature (Tg) in the present application is a temperature at which tan δ exhibits a peak within the above measurement temperature range. When 2 or more tan δ peaks are observed in this temperature range, the glass transition temperature is defined as the temperature at which the tan δ value becomes maximum.
(II) evaluation of filling Property
The prepared adhesive sheet (adhesive film thickness: 150 μm) was attached to a glass cover plate (ink step difference: 30 μm) of a mobile phone in an appropriate size, and was adhered at 25 ℃ under atmospheric pressure with a rubber roller (roller diameter: 50mm, roller width: 210mm) under a load of 2 kg. Then, the display module and the glass cover plate were bonded in a bonding machine (Daizuan TPL-0512MH) under room temperature and 1000Pa and under a pressing condition of 0.2MPa and 10 s. Then, defoaming was performed at 45 ℃ and 0.4MPa for 15min, and the mixture was allowed to stand at room temperature for 24 hours. Whether or not there was any adhesion failure such as air bubbles was observed. If there are bubbles, the filling property is considered to be poor, and if there are no bubbles, the filling property is considered to be passed.
(III) evaluation of storage stability
The storage stability refers to that glue does not overflow in the storage process of the glue film, and the specific evaluation method is as follows:
sandwiching the adhesive film between two release films, and applying 200N/m on the upper release film2The force of (1) was kept in an oven at 40 ℃ for 7 days, after which the aging was observedIf the change distance of the marginal positions of the front and rear adhesive films is more than 0.15mm, the storage stability is marked as poor, otherwise, the storage stability is marked as passing.
(IV) evaluation of reliability
The reliability refers to the capability of a finished product after the adhesive film is pasted to resist bubbles, floating and peeling under different environmental conditions, and the specific evaluation method comprises the following steps:
the (glass-adhesive film-display module) assembly was set at 3000mJ/cm2The cured product was allowed to stand at 85 ℃ and 85% RH for 500 hours, and then cooled to room temperature to see whether or not bubbles were formed. If the bubble is present, the bubble is considered to be bad, otherwise, the bubble is recorded as passing.
Adhesive sheets were obtained in the same manner as in example 1, except that the compounding amounts were as shown in tables 1, 2 and 3. The results of the evaluation in the same manner as in example 1 are shown in tables 1, 2 and 3.
The effect of varying amounts of alkaline monomer on the performance of the adhesive sheets is shown in Table 1.
TABLE 1
In Table 1, examples 1 to 4 and comparative examples 1 to 2, the content of the basic monomer in the acrylic derivative polymer material was 0.5%, 7.5%, 15%, 14%, 0%, 24%, respectively, and the coating curing intensity was 1mW/cm in the same photoinitiator2Under the condition, the performance of the obtained product is detected, and the glass transition temperature of the product is lower than-23 ℃ when the content of the basic monomer in the acrylic derivative polymer is lower than 0.5 percent, so that the storage stability and the reliability of the product are poor; when the content of the basic monomer in the acrylic derivative polymer is more than 15%, or when the glass transition temperature of the product is more than 0 ℃, the filling property of the product is affected.
Second, the effect of different types and amounts of hydrogen abstraction-type UV initiators on the performance of the adhesive sheets is shown in Table 2.
TABLE 2
As can be seen from Table 2, under otherwise comparable conditions, the absence of the hydrogen abstraction-type UV initiator such as 4ABP or 4MBP leads to poor reliability of the adhesive sheet, and if the amount of 4ABP or 4MBP added exceeds 1% of the amount of acrylic derivative polymer, the filling properties of the adhesive sheet are poor.
Third, the effect of different Tan δ on the performance of the adhesive sheets is shown in Table 3.
TABLE 3
From table 3, it can be seen that under the condition that other components are not changed, the addition of HDDA causes the tan δ value to be reduced, and further causes the reliability of the product to be lengthened, and the more the addition amount is, the more the tan δ value between 25 ℃ and 55 ℃ is reduced, and further causes the influence on the filling property of the product, and from table 3 in combination with tables 1 and 2, it can be seen that the tan δ value between 25 ℃ and 100 ℃ of the product needs to be controlled to be 0.42 to 0.84 while the glass transition temperature of the product is controlled to be-23 ℃ to 0 ℃, otherwise, the reliability, the storage stability and the filling property of the adhesive sheet are influenced.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (9)
1. An adhesive film for an image display device, characterized in that the adhesive film has a glass transition temperature of-23 to 0 ℃ and a tan δ of 0.42 to 0.84 at 25 to 100 ℃, the glass transition temperature being a temperature at which tan δ shows a peak within-40 to 80 ℃, the tan δ being a value obtained by dividing a loss modulus by a storage modulus, the adhesive film comprising the following components:
1) an acrylic derivative polymer comprising the following raw materials: C4-C18 acrylate monomer, hydrophilic monomer and basic monomer;
2) a photoinitiator which comprises a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator,
wherein the adding amount of the alkaline monomer is 0.5-15% of the mass of the acrylic derivative polymer raw material.
2. The adhesive film for image display device according to claim 1, wherein the C4-C18 acrylate monomer comprises one or more selected from but not limited to butyl (meth) acrylate, isooctyl (meth) acrylate, isobornyl (meth) acrylate, isobutyl (meth) acrylate, t-butyl (meth) acrylate, cyclohexyl (meth) acrylate, n-octyl (meth) acrylate, dodecyl (meth) acrylate, stearyl (meth) acrylate and isostearyl (meth) acrylate, and the amount of the C4-C18 acrylate monomer is 50-95% by mass of the raw material of the acrylic derivative polymer.
3. The adhesive film for image display device according to claim 1, wherein the hydrophilic monomer comprises one or more of hydroxyethyl acrylate, 2-hydroxypropyl acrylate, and 4-hydroxybutyl acrylate, and the amount of the hydrophilic monomer added is 5-30% by mass of the acrylic derivative polymer material.
4. The adhesive film for image display device according to claim 1, wherein the basic monomer is one or more selected from the group consisting of (meth) acrylamide, (meth) acryloylmorpholine, and N, N-dimethylacrylamide.
5. The adhesive film for image display device according to claim 1, wherein the hydrogen abstraction-type ultraviolet light initiator includes but is not limited to one or more of 4-methylbenzophenone, benzophenone, and 4-acrylyl oxybenzoic acid benzophenone, and the amount of the hydrogen abstraction-type ultraviolet light initiator is 0.1-1% of the amount of the acrylic derivative polymer.
6. The adhesive film for image display device according to claim 1, wherein the cleavage type UV initiator comprises one or more of but not limited to benzoin derivatives, benzil ketal derivatives, dialkoxyacetophenones, α -hydroxyalkylphenylketones, α -aminoalkylphenones, acylphosphine hydrides, esterified oxime ketone compounds, aryl peroxy ester compounds, halogenated methyl aryl ketones, organic sulfur compounds, and benzoyl esters, and is used in an amount of 0.1 to 2% by weight based on the amount of the acrylic derivative polymer.
7. The adhesive film for image display device according to claim 1, wherein the adhesive film comprises the following components:
1) the acrylic acid derivative polymer comprises the following raw materials in percentage by mass: 75-89.5% of C4-C18 acrylate monomer, 10% of hydrophilic monomer and the balance of alkaline monomer;
2) the photoinitiator adopts a hydrogen abstraction type ultraviolet initiator and a cracking type ultraviolet initiator, wherein the cracking type ultraviolet initiator adopts benzil dimethyl ether, the hydrogen abstraction type ultraviolet initiator adopts 4-acrylyl oxybenzoic acid benzophenone or 4-methyl benzophenone, and the adding amount of the hydrogen abstraction type ultraviolet initiator is 0.1-1% of the mass of the acrylic derivative polymer;
and the adhesive film has a glass transition temperature of-23 to 0 ℃ and a tan delta of 0.42 to 0.84 at 25 to 100 ℃, the glass transition temperature being a temperature at which tan delta shows a peak value within-40 to 80 ℃, the tan delta being a value obtained by dividing a loss modulus by a storage modulus.
8. An image display device, wherein a layer to which the image display device according to claim 1 is adhered with an adhesive film is provided on a visible side.
9. The image display device according to claim 8, which has the adhesive film for an image display device according to claim 1 between a transparent protective plate and a touch panel or between a transparent protective plate and an image display unit.
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