KR20220093333A - Light diffusing thermosetting sheet - Google Patents

Abstract

The light-diffusing thermosetting sheet is made to contain a thermosetting resin composition containing a thermosetting resin and surface-modified silica particles, and the average primary particle diameter of the surface-modified silica particles is 0.1 µm or more and 1.5 µm or less.

Description

Light diffusing thermosetting sheet

The present invention relates to a light diffusing thermosetting sheet.

Conventionally, in order to suppress deterioration of the optical element with which an image display apparatus is equipped with moisture etc. in air|atmosphere, sealing with a sealing material is known.

As such a sealing material, the image display apparatus sealing material containing a biphenyl frame|skeleton containing epoxy resin and an alicyclic frame|skeleton containing epoxy resin is proposed, for example (refer patent document 1, for example.).

And such an image display device sealing material seals an optical element by hardening|curing, after an optical element is embedded.

International Publication No. 2018/235824

By the way, using the image display apparatus sealing material of patent document 1 for various uses is examined, and providing the performance according to each use to the image display apparatus sealing material of patent document 1 is calculated|required.

For example, when the image display device sealing material described in Patent Document 1 is used for window glass for general buildings, window glass for vehicles, signboards, lighting fixtures, lighting covers such as indicator lights, backlight diffusers for liquid crystals, display panels, etc., from a light source The performance of making the image of a light source, such as a lamp, invisible by diffusely transmitting the emitted light with uniform brightness, and reducing the linear transmitted light is calculated|required.

The present invention provides a light-diffusing thermosetting sheet having a good appearance while achieving an improvement in haze, and capable of imparting excellent light diffusivity to various products.

The present invention [1] includes a thermosetting resin composition comprising a thermosetting resin and surface-modified silica particles, wherein the surface-modified silica particles have an average primary particle diameter of 0.1 µm or more and 1.5 µm or less, and the surface-modified silica The particles include a light-diffusing thermosetting sheet, which is a silica particle surface-modified with a silane coupling agent.

In the present invention [2], the thermosetting resin includes the light-diffusing thermosetting sheet according to the above [1], wherein the thermosetting resin contains an epoxy resin.

The present invention [3] includes the light-diffusing thermosetting sheet according to [1] or [2], wherein the silica particles are nonporous.

In the present invention [4], according to any one of [1] to [3], wherein the content of the surface-modified silica particles is 5 parts by mass or more and 50 parts by mass or less with respect to 100 parts by weight of the thermosetting resin. and a light diffusing thermosetting sheet.

In the present invention [5], the thermosetting resin composition has a haze value of 35% or more and a total light transmittance of 80% or more, The light-diffusing thermosetting sheet according to any one of [1] to [4] is included.

In the present invention [6], the thermosetting resin composition further comprises pigment particles, and the average primary particle diameter of the pigment particles is 100 nm or less, the light diffusion according to any one of [1] to [4]. Includes a thermosetting sheet.

According to the light diffusing thermosetting sheet of the present invention, since the thermosetting resin composition contains the thermosetting resin and the surface-modified silica particles, in the cured product of the thermosetting resin composition, the haze value can be improved and the appearance can promote the improvement of As a result, excellent light diffusivity can be imparted to various products containing the cured product of the thermosetting resin composition.

BRIEF DESCRIPTION OF THE DRAWINGS It is a side sectional view of the sealing sheet as one Embodiment of the light-diffusion thermosetting sheet|seat of this invention.
Fig. 2 is a side cross-sectional view of an organic EL display with a touch sensor as an embodiment (mode having an in-cell structure or an on-cell structure) of an image display device provided with a sealing member formed of the sealing layer shown in Fig. 1 .
Fig. 3 is a side cross-sectional view of an organic EL display with a touch sensor as another embodiment (an aspect having an outcell structure) of an image display device.

<Light diffusive thermosetting sheet>

A light-diffusing thermosetting sealing sheet (hereinafter, also referred to as a sealing sheet) as a first embodiment of the light-diffusing thermosetting sheet of the present invention contains a thermosetting resin composition. The thermosetting resin composition contains a thermosetting resin and surface-modified silica particles.

<Thermosetting resin>

As a thermosetting resin, an epoxy resin etc. are mentioned, for example. In other words, the thermosetting resin contains, for example, an epoxy resin, and preferably consists of an epoxy resin.

As the epoxy resin, for example, a bisphenol type epoxy resin (for example, bisphenol A type, bisphenol F type, bisphenol E type, bisphenol S type, bisphenol AD type, a mixture thereof, etc.), diphenyl ether type epoxy resin, furnace Volak type epoxy resins (for example, phenol novolac type, cresol novolak type, biphenyl novolak type, bisphenol novolak type, naphthol novolak type, trisphenol novolak type, dicyclopentadiene novolak type, etc. ), biphenyl type epoxy resin, naphthyl type epoxy resin, triphenol alkane type epoxy resin (for example, triphenol methane type, triphenol ethane type, triphenol propane type, etc.), alicyclic skeleton containing epoxy resin, etc. can be heard

An epoxy resin can be used individually or in combination of 2 or more types.

In the epoxy resin, Preferably, a bisphenol-type epoxy resin, a biphenyl-type epoxy resin, and an alicyclic skeleton containing epoxy resin are mentioned, More preferably, a bisphenol-type epoxy resin, a biphenyl-type epoxy resin, and an alicyclic skeleton containing epoxy Combination of resin is mentioned.

In other words, the epoxy resin preferably contains at least one selected from the group consisting of a bisphenol-type epoxy resin, a biphenyl-type epoxy resin, and an alicyclic skeleton-containing epoxy resin, More preferably, a bisphenol-type epoxy resin; It contains a biphenyl-type epoxy resin and an alicyclic skeleton-containing epoxy resin, More preferably, it consists of a bisphenol-type epoxy resin, a biphenyl-type epoxy resin, and an alicyclic skeleton-containing epoxy resin.

When an epoxy resin contains a bisphenol-type epoxy resin, a biphenyl-type epoxy resin, and an alicyclic skeleton containing epoxy resin, the improvement of the total light transmittance of the sealing member mentioned later can be aimed at reliably.

Although normal temperature solid may be sufficient as a bisphenol-type epoxy resin, and normal temperature liquid may be sufficient as it, Preferably it is normal temperature solid. On the other hand, "normal temperature solid" indicates that it is a solid state without fluidity at normal temperature (23°C), and "normal temperature liquid" indicates that it is a liquid state with fluidity at normal temperature (23°C) (hereinafter referred to as "normal temperature solid"). same here).

In other words, the bisphenol-type epoxy resin preferably contains a bisphenol-type epoxy resin that is solid at room temperature, more preferably a bisphenol-type epoxy resin that is solid at room temperature. When the bisphenol-type epoxy resin contains the bisphenol-type epoxy resin that is solid at room temperature, the sheet formability of the thermosetting resin composition can be improved, and the moisture permeability of the sealing member described later can be reduced.

In such a bisphenol-type epoxy resin, Preferably, a bisphenol F-type epoxy resin is mentioned, More preferably, the bisphenol F-type epoxy resin of normal temperature solid is mentioned.

Although the weight average molecular weight ( _Mw ) in particular of a bisphenol-type epoxy resin is not restrict|limited, For example, 100 or more, Preferably, 1,000 or more, More preferably, 5,000 or more, More preferably, 10,000 or more, especially Preferably, it is 20,000 or more, Especially preferably, it is 30,000 or more, for example, 100,000 or less, Preferably, it is 90,000 or less. A weight average molecular weight (M _w ) can be calculated|required by gel permeation chromatography (GPC) which uses polystyrene as a standard substance (the same below).

The barrier property in the hardened|cured material of a thermosetting resin composition as the weight average molecular weight of a bisphenol-type epoxy resin is more than the said minimum, and the improvement of bending resistance can be aimed at.

The epoxy equivalent in a bisphenol-type epoxy resin is 100 g/eq. or more, preferably, 500 g/eq. Above, more preferably, 2,000 g/eq. or more, more preferably, 4,000 g/eq. or more, particularly preferably, 7,000 g/eq. or more, for example, 20,000 g/eq. Hereinafter, preferably, 16,000 g/eq. is below. Epoxy equivalent can be measured based on JISK7236:2001 (the same below).

Thermosetting resin WHEREIN: The content rate of a bisphenol type epoxy resin is 0 mass % or more, for example, Preferably, 5 mass % or more, More preferably, 10 mass % or more, More preferably, 20 mass % or more, for example, 100 mass % or less, Preferably, 70 mass % or less, More preferably, it is 50 mass % or less.

Although normal temperature solid may be sufficient as a biphenyl type epoxy resin, and normal temperature liquid may be sufficient as it, Preferably it is normal temperature solid.

In other words, the biphenyl-type epoxy resin, Preferably, the biphenyl-type epoxy resin of room temperature solid is contained, More preferably, it consists of the biphenyl-type epoxy resin of room temperature solid. When the biphenyl-type epoxy resin contains the biphenyl-type epoxy resin which is solid at room temperature, the sheet formability of the thermosetting resin composition can be reliably improved, and the moisture permeability of the sealing member described later can be reliably reduced.

The weight average molecular weight (M _w ) of the biphenyl-type epoxy resin is not particularly limited, and for example, 100 or more, preferably 1,000 or more, more preferably 5,000 or more, still more preferably 10,000 or more, Especially preferably, it is 20,000 or more, Especially preferably, it is 30,000 or more, for example, 100,000 or less, Preferably, it is 90,000 or less.

The barrier property in the hardened|cured material of a thermosetting resin composition as the weight average molecular weight of a biphenyl type epoxy resin is more than the said minimum, and the improvement of bending resistance can be aimed at.

The epoxy equivalent in a biphenyl type epoxy resin is 100 g/eq. or more, preferably, 500 g/eq. Above, more preferably, 2,000 g/eq. or more, more preferably, 4,000 g/eq. or more, particularly preferably, 7,000 g/eq. or more, for example, 20,000 g/eq. Hereinafter, preferably, 16,000 g/eq. is below.

Thermosetting resin WHEREIN: The content rate of a biphenyl type epoxy resin is 0 mass % or more, for example, Preferably, 5 mass % or more, More preferably, 10 mass % or more, More preferably, 20 Mass % or more, for example, 100 mass % or less, Preferably, it is 70 mass % or less, More preferably, it is 50 mass % or less.

The alicyclic skeleton-containing epoxy resin is an epoxy resin having at least an epoxy group and an aliphatic ring (alicyclic skeleton).

Although normal temperature solid may be sufficient as an alicyclic skeleton containing epoxy resin, and normal temperature liquid may be sufficient as it, Preferably it is normal temperature liquid.

In other words, the alicyclic skeleton-containing epoxy resin preferably contains an alicyclic skeleton-containing epoxy resin that is liquid at room temperature, and more preferably consists of an alicyclic skeleton-containing epoxy resin that is liquid at room temperature. When the alicyclic skeleton-containing epoxy resin contains an alicyclic skeleton-containing epoxy resin that is liquid at room temperature, it is possible to further improve the transparency of the sealing member, which will be described later, and further reduce the moisture permeability of the sealing member more reliably.

Examples of the alicyclic skeleton-containing epoxy resin include an alicyclic epoxy compound having a cycloalkene oxide structure, a dicyclopentadiene-type epoxy resin (hereinafter referred to as a DCPD-type epoxy resin), and a hydrogenated epoxy resin. .

As an alicyclic epoxy compound having a cycloalkene oxide structure, for example, an epoxy compound having an epoxycyclohexane structure represented by the following formula (1) (hereinafter referred to as an ECH structure-containing epoxy compound), a modified product thereof, etc. can be heard

Formula (1)

[Formula 1]

[In formula (1), X represents a single bond or a linking group (a divalent group having one or more atoms). A substituent such as an alkyl group may or may not be bonded to the carbon atom constituting the cyclohexane ring.]

Examples of the linking group represented by X in the formula (1) include a divalent hydrocarbon group, a carbonyl group, an ether group, a thioether group, an ester group, a carbonate group, an amide group, and a group to which they are linked.

As the divalent hydrocarbon group, for example, a linear or branched alkylene group having 1 to 18 carbon atoms (eg, a methylene group, methylmethylene group, dimethylmethylene group, ethylene group, propylene group, trimethylene group, etc.) , cycloalkylene group (eg, 1,2-cyclopentylene group, 1,3-cyclopentylene group, 1,2-cyclohexylene group, 1,3-cyclohexylene group, 1,4-cyclohexylene group group), a cycloalkylidene group (eg, a cyclopentylidene group, a cyclohexylidene group, etc.), etc. are mentioned.

Among the coupling groups represented by X in the formula (1), from the viewpoint of adhesiveness of a sealing member described later, preferably, a coupling group containing an oxygen atom is mentioned, More preferably, a carbonyl group, an ether group, an ester group and a carbonate group, and more preferably, an ester group.

As an ECH structure containing epoxy compound represented by said Formula (1), For example, (3,3',4,4'- diepoxy)bicyclohexyl, bis(3,4-epoxycyclohexylmethyl)ether, 1 ,2-bis(3,4-epoxycyclohexan-1-yl)ethane, 1,2-epoxy-1,2-bis(3,4-epoxycyclohexan-1-yl)ethane, 2,2-bis (3,4-epoxycyclohexan-1-yl)propane, 3,4-epoxycyclohexylmethyl (3,4-epoxy)cyclohexanecarboxylate, ε-caprolactone-modified 3',4'-epoxycyclo Hexylmethyl 3,4-epoxycyclohexanecarboxylate etc. are mentioned.

A commercial item can also be used for the ECH structure containing epoxy compound represented by said Formula (1). As a commercial item, Celoxide 8000 by Daicel Corporation, Celoxide 2021P, Celoxide 2081, etc. are mentioned, for example.

Dicyclopentadiene type epoxy resin (it is hereafter set as DCPD type epoxy resin.) is represented by following formula (2).

[Formula 2]

[In formula (2), a substituent such as an alkyl group may or may not be bonded to the carbon atom constituting the aliphatic ring derived from dicyclopentadiene.]

A commercial item can also be used for DCPD-type epoxy resin represented by said Formula (2). As a commercial item of DCPD-type epoxy resin represented by said Formula (2), For example, EP-4088S (epoxy equivalent 170g/eq.) by ADEKA company, EP-4088L (epoxy equivalent 165g/eq.) by ADEKA company, etc. can be heard

The hydrogenated epoxy resin is an epoxy resin obtained by hydrogenating an epoxy resin having an aromatic ring among the above epoxy resins, and specific examples thereof include a hydrogenated bisphenol-type epoxy resin and a hydrogenated biphenyl-type epoxy resin, preferably For example, a hydrogenated bisphenol type epoxy resin is mentioned.

Specific examples of the hydrogenated bisphenol-type epoxy resin include a hydrogenated bisphenol F-type epoxy resin and a hydrogenated bisphenol-A-type epoxy resin.

A commercial item can also be used for the hydrogenated bisphenol-type epoxy resin.

As a commercial item of hydrogenated bisphenol F-type epoxy resin, the Mitsubishi Chemical Corporation YL-6753 etc. are mentioned, for example. As a commercial item of hydrogenated bisphenol A epoxy resin, For example, YX-8000 and YX-8034 by Mitsubishi Chemical Corporation, EXA-7015 by DIC Corporation, ST-3000 by Shin-Nippon Sumikin Chemical Corporation, Rika resin by Shin-Nippon Rika Corporation, for example. HBE-100, EX-252 by Nagase Chemtex Corporation, etc. are mentioned.

Such an alicyclic skeleton containing epoxy resin can be used individually or in combination of 2 or more types.

In alicyclic skeleton containing epoxy resin, Preferably, a hydrogenated epoxy resin and an ECH structure containing epoxy compound are mentioned.

In other words, the alicyclic skeleton-containing epoxy resin preferably contains a hydrogenated epoxy resin and/or an ECH structure-containing epoxy compound, more preferably a hydrogenated epoxy resin or an ECH structure-containing epoxy compound, further Preferably, it consists of a hydrogenated epoxy resin or an ECH structure containing epoxy compound.

In the hydrogenated epoxy resin, Preferably, a hydrogenated bisphenol A epoxy resin is mentioned. In an ECH structure containing epoxy compound, Preferably, 3,4-epoxycyclohexylmethyl (3,4-epoxy) cyclohexanecarboxylate is mentioned.

The weight average molecular weight of such an alicyclic skeleton containing epoxy resin is, for example, 100 or more, Preferably, it is 180 or more, for example, 1,000 or less, Preferably, it is 790 or less, More preferably, it is 500 or less. .

The epoxy equivalent in an alicyclic skeleton containing epoxy resin is 90 g/eq. or more, preferably, 100 g/eq. above, for example, 300 g/eq. Below, preferably, 200 g/eq. is below.

In the thermosetting resin, the content of the alicyclic skeleton-containing epoxy resin is, for example, 0 mass % or more, preferably 10 mass % or more, more preferably 20 mass % or more, for example, 100 mass % or more. % or less, preferably 50 mass% or less, more preferably 40 mass% or less, still more preferably 35 mass% or less.

The content rate of the thermosetting resin in the thermosetting resin composition is, for example, 60 mass % or more, Preferably, 70 mass % or more, for example, 95 mass % or less, Preferably, 92 mass % or less. , More preferably, it is 90 mass % or less.

<Surface-modified silica particles>

The surface-modified silica particles are silica particles surface-modified with a silane coupling agent.

Silica particles, Preferably, it has a spherical shape. As for the silica particle, it is more preferable that a sphericity degree is high. Silica particles can be prepared, for example, by a dry method (a combustion method or an arc method).

The silica particle may be porous or nonporous may be sufficient as it. Porous silica particles have higher hygroscopicity and gas adsorption properties than non-porous silica particles. Therefore, the porous silica particle and the non-porous silica particle are used separately according to the use of the sealing sheet.

For example, when a sealing sheet is used as a sealing sheet for image display elements, such as organic electroluminescent, a silica particle is from a viewpoint of discharge|release of the component which adsorb|sucked on the silica particle, Preferably, it is nonporous.

On the other hand, as the definition of silica particles herein, the specific surface area of the porous silica particles is 300 m ² /g or more, and the specific surface area of the non-porous silica particles is 30 m ² /g or less.

As the silane coupling agent, for example, an epoxy group-containing silane coupling agent (eg, γ-glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, β-(3, 4-epoxycyclohexyl)ethyltrimethoxysilane), an amino group-containing silane coupling agent (eg, N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane, N-2- (aminoethyl)-3-aminopropylmethyltrimethoxysilane, N-2-(aminoethyl)-3-aminopropylmethyltriethoxysilane, 3-aminopropyltrimethoxysilane, etc.), methacryl and a loyl group-containing silane coupling agent (eg, γ-methacryloxypropylmethyldimethoxysilane, γ-methacryloxypropyltrimethoxysilane, etc.) and the like.

A silane coupling agent can be used individually or in combination of 2 or more types.

In a silane coupling agent, Preferably, an epoxy group containing silane coupling agent is mentioned.

In order to prepare such a surface-modified silica particle, the surface of said silica particle is processed with said silane coupling agent.

As a surface treatment method with a silane coupling agent, for example, after adding a silane coupling agent to water to hydrolyze it, adding a catalyst such as alcohol and acetic acid, dissolving it in water to prepare an aqueous solution, and silica in this aqueous solution The method of surface-treating by immersing particle|grains, etc. are mentioned. In addition, as a method of surface treatment with a silane coupling agent, for example, a method in which the target powder made of silica particles is accommodated in a processing container, and the target powder is reacted with a vaporized silane coupling agent while stirring. have.

The average primary particle diameter of the surface-modified silica particles is 0.1 µm or more, preferably 0.2 µm or more, more preferably 0.4 µm or more, 1.5 µm or less, preferably 1.3 µm or less. The average primary particle size can be measured with a laser diffraction/scattering particle size distribution analyzer (such as HORIBA LA-750) (hereinafter the same). In addition, let the average primary particle diameter in this indication be a particle diameter corresponding to 50% of volume accumulation from the small-diameter side.

If the average primary particle diameter of the surface-modified silica particles is equal to or greater than the above lower limit, a haze value within the range of the present invention can be provided to the sealing member described later. If the average primary particle diameter of the surface-modified silica particles is equal to or less than the upper limit, sedimentation of the surface-modified silica particles in the varnish of the thermosetting resin composition described later can be suppressed.

A commercial item can also be used for surface-modified silica particle. As a commercial item of surface-modified silica particle, SE1050-SEO, SC-2050MB, 10SE-CM1 by Admatex Corporation, etc. are mentioned, for example.

The content of the surface-modified silica particles is, for example, 5 parts by mass or more, preferably 10 parts by mass or more, more preferably 20 parts by mass or more, for example, with respect to 100 parts by weight of the thermosetting resin, 50 mass parts or less, Preferably, it is 40 mass parts or less, More preferably, it is 35 mass parts or less.

The content rate of the surface-modified silica particles in the thermosetting resin composition is, for example, 3 mass% or more, preferably 4 mass% or more, more preferably 8 mass% or more, for example 40 mass% % or less, preferably 30 mass % or less, more preferably 25 mass % or less.

When the content rate of the surface-modified silica particles is equal to or more than the lower limit, the haze value of the sealing member described later can be improved reliably, and the light diffusivity of the sealing member can be improved. When the content of the surface-modified silica particles is equal to or less than the upper limit, it is possible to reliably improve the total light transmittance of the sealing member described later.

<thermal curing agent>

The thermosetting resin composition preferably further contains a thermosetting agent.

As a thermosetting agent, a thermal cationic hardening|curing agent, a thermal anionic hardening|curing agent, etc. which start the hardening reaction of a thermosetting resin by heat are mentioned, for example.

A thermal cationic hardening|curing agent is a thermal acid generator which generate|occur|produces an acid (cation) by heating.

As a thermal cationic hardening|curing agent, a well-known thermal cationic polymerization initiator can be used. As a thermal cationic polymerization initiator, for example, a sulfonium salt using AsF ₆ ^- , SbF ₆ ^- , PF ₆ ^- , BF ₄ ^- , B(C ₆ F ₅ ) ₄ ^- , CF ₃ SO ₃ ^- or the like as a counter anion. , a phosphonium salt, a quaternary ammonium salt, a diazonium salt, an iodonium salt, etc. are mentioned.

A thermal anionic hardening|curing agent is a basic compound which melt|dissolves by heat|fever, or the compound used as a basic compound by a bond dissociated by heat|fever.

As the thermal anionic curing agent, for example, a solid imidazole compound at room temperature, an amine-epoxy adduct compound (a reaction product of an amine compound and an epoxy compound), an amine-isocyanate compound (an amine compound and an isocyanate) a reaction product of a nate compound) and the like.

A thermosetting agent can be used individually or in combination of 2 or more types.

In a thermosetting agent, Preferably, a thermal cationic hardening|curing agent is mentioned, More preferably, a quaternary ammonium salt is mentioned.

The content of the thermosetting agent is, for example, 0.3 parts by mass or more, preferably 0.5 parts by mass or more, for example, 10 parts by mass or less, preferably 5 parts by mass with respect to 100 parts by mass of the thermosetting resin. is below.

The content rate of the thermosetting agent in the thermosetting resin composition is, for example, 1 mass % or more, Preferably, 2 mass % or more, for example, 10 mass % or less, Preferably, it is 5 mass % or less. .

<Pigment>

Moreover, depending on the use of the sealing member mentioned later, it may be desired to provide a desired color to a sealing member. In this case, the thermosetting resin composition preferably contains pigment particles.

When the thermosetting resin composition contains the surface-modified silica particles and the pigment particles, a desired color can be imparted to the sealing member described later, and the haze value and the total light transmittance can be adjusted in a well-balanced manner.

A pigment particle is a solvent-dispersible pigment dispersible in a solvent, and has a particulate form.

The average primary particle diameter of the pigment particles is, for example, 10 nm or more, preferably 30 nm or more, for example, 100 nm or less, preferably 70 nm or less.

If the average primary particle diameter of a pigment particle is more than the said minimum, reduction of the content rate of the pigment particle mentioned later can be aimed at. Transparency can be ensured in the sealing member mentioned later as the average primary particle diameter of a pigment particle is below the said upper limit.

As a pigment particle, an inorganic pigment particle is mentioned, for example, More specifically, black pigment particles, such as carbon black, an oxide type pigment, a hydroxide type pigment, etc. are mentioned. A pigment particle can be used individually or in combination of 2 or more types.

In the pigment particle, Preferably, an inorganic pigment particle is mentioned, More preferably, a black pigment particle is mentioned, More preferably, carbon black is mentioned.

The content rate of the pigment particle is, for example, 0.01 parts by mass or more, preferably 0.1 parts by mass or more, for example, 10 parts by mass or less, preferably 5 parts by mass with respect to 100 parts by mass of the thermosetting resin. Hereinafter, more preferably, it is 2 mass parts or less.

The content rate of the pigment particles in the thermosetting resin composition is, for example, 0.1 mass% or more, preferably 0.2 mass% or more, for example, 15 mass% or less, preferably 10 mass% or less, More preferably, it is 5 mass % or less.

A desired color can be provided to the sealing member mentioned later as the content rate of a pigment particle is more than the said minimum. The sealing member mentioned later as the content rate of a pigment particle is below the said upper limit. WHEREIN: A total light transmittance can fully be ensured, while being able to provide a desired color.

<Other ingredients>

The thermosetting resin composition may contain other components other than the above in an appropriate ratio as needed. As other components, a thermoplastic resin, a coupling agent, a leveling agent, a polymerization initiation adjuvant, an antioxidant, a wettability improving agent, surfactant, a plasticizer, a ultraviolet absorber, a preservative, an antibacterial agent, etc. are mentioned.

<Light diffusive thermosetting sheet>

Next, with reference to FIG. 1, the sealing sheet 1 as one Embodiment of the light-diffusion thermosetting sheet|seat of this invention is demonstrated.

As shown in FIG. 1, the sealing sheet 1 is equipped with the sealing layer 2 which consists of said thermosetting resin composition, the base film 3, and the release film 4.

In order to prevent foreign matter from adhering to the sealing layer 2 , it is preferable that the sealing layer 2 is protected by the base film 3 and the release film 4 when the sealing sheet 1 is stored. do. On the other hand, at the time of use of the sealing sheet 1, the base film 3 and the release film 4 peel.

The sealing layer 2 is a dried product of the above-described thermosetting resin composition, and has a sheet shape (plate shape). Specifically, the sealing layer 2 has a predetermined thickness, extends in a predetermined direction orthogonal to the thickness direction, and has a flat surface and a flat back surface.

In the sealing layer 2, said thermosetting resin is not reacting (hardening), but the sealing layer 2 contains these thermosetting resin in the non-hardened state.

The thickness of the sealing layer 2 is, for example, 1 micrometer or more, Preferably, it is 5 micrometers or more, for example, 100 micrometers or less, Preferably, it is 30 micrometers or less.

In addition, in the case where the sealing layer 2 having a thickness of 15 μm is cured (that is, when the thermosetting resin composition is formed into a sheet shape having a thickness of 15 μm and is thermoset), the haze value of the cured product of the sealing layer 2 is , for example at least 30%, preferably at least 35%, more preferably at least 40%, particularly preferably at least 50%, particularly preferably at least 80%, for example 100% or less, preferably 95% or less. In addition, a haze value can be measured based on the method as described in the Example mentioned later.

If the haze value of the hardened|cured material of the sealing layer 2 is more than the said minimum, the sealing layer can be thickened, without raising a haze value large. If the haze value of the hardened|cured material of the sealing layer 2 is below the said upper limit, a sealing layer can be made thin, without reducing a haze value large.

Further, when the sealing layer 2 having a thickness of 15 μm is cured, the total light transmittance of the cured product of the sealing layer 2 is, for example, 10% or more, preferably 20% or more, more preferably , 50% or more, more preferably 70% or more, particularly preferably 80% or more, particularly preferably 85% or more, most preferably 90% or more, for example 100% or less, preferably Usually, it is 98% or less. In addition, total light transmittance can be measured based on the method described in the Example mentioned later.

The extraction loss of a light source can be decreased as the total light transmittance of the hardened|cured material of the sealing layer 2 is more than the said minimum. If the total light transmittance of the hardened|cured material of the sealing layer 2 is below the said upper limit, the extraction loss of a light source can be eliminated.

Moreover, if the haze value of the hardened|cured material of the sealing layer 2 is more than the said lower limit, and the total light transmittance is more than the said minimum, the improvement of the light diffusivity of the hardened|cured material of the sealing layer 2 can be aimed at reliably.

The base film 3 is peelably adhered to the back surface of the sealing layer 2 in order to support and protect the sealing layer 2 until the sealing sheet 1 is used for formation of a sealing member (貼着) is done. That is, the base film 3 is laminated|stacked on the back surface of the sealing layer 2 so that the back surface of the sealing layer 2 may be covered at the time of shipment, conveyance, and storage of the sealing sheet 1, and the sealing sheet 1 ) immediately before use. WHEREIN: It is a flexible film which can be pulled off so that it may curve from the back surface of the sealing layer 2 in a substantially U-shape.

The base film 3 has a flat plate shape, specifically, has a predetermined thickness, extends in a predetermined direction orthogonal to the thickness direction, and has a flat surface and a flat back surface. The adhesion surface (surface) of the base film 3 is peeling-processed as needed.

As a material of the base film 3, resin materials, such as polyester (for example, polyethylene terephthalate (PET) etc.) and polyolefin (for example, polyethylene, polypropylene, etc.), are mentioned, for example.

In the base film 3, Preferably, the film which has water-barrier property or gas-barrier property is mentioned, More preferably, the film which consists of polyethylene terephthalate is mentioned. Although the thickness of the base film 3 is suitably selected according to the material of a film, it can be 25 micrometers or more and 150 micrometers or less, for example, from the point which has followability|trackability with respect to to-be-sealed material, such as a display element.

The release film 4 is affixed so that peeling is possible on the surface of the sealing layer 2 in order to protect the sealing layer 2 until the sealing sheet 1 is used for formation of a sealing member. That is, at the time of shipment, conveyance, and storage of the sealing sheet 1, the release film 4 is laminated|stacked on the surface of the sealing layer 2 so that the surface of the sealing layer 2 may be covered, and the sealing sheet 1 ) immediately before use. WHEREIN: It is a flexible film which can be peeled off so that it may curve substantially U-shape from the surface of the sealing layer 2 .

The release film 4 has a flat plate shape, specifically, has a predetermined thickness, extends in a predetermined direction orthogonal to the thickness direction, and has a flat surface and a flat back surface. In addition, the bonding surface (back surface) of the release film 4 is peeling-processed as needed. As a material of the release film 4, the resin material similar to the base film 3 is mentioned, for example. Although the thickness of the release film 4 is suitably selected also according to the material of a film, It can be set as 25 micrometers or more and 150 micrometers or less from the point which has followability with respect to to-be-sealed materials, such as a display element, for example.

<Manufacturing method of encapsulation sheet>

Next, the manufacturing method of the sealing sheet 1 is demonstrated.

In order to manufacture the sealing sheet 1, first, the above-mentioned thermosetting resin composition is prepared.

The thermosetting resin composition is prepared by mixing the above-described thermosetting resin, the above-mentioned surface-modified silica particles, and, if necessary, the above-described thermosetting agent, the above-mentioned pigment particles, and the above-mentioned other components. Moreover, manufacture of the sealing sheet 1 WHEREIN: Preferably, a thermosetting resin composition is diluted with an organic solvent, and the varnish of a thermosetting resin composition is prepared.

The organic solvent is not particularly limited as long as it can uniformly disperse or dissolve the thermosetting resin and the surface-modified silica particles. As the organic solvent, for example, aromatic hydrocarbons (eg, benzene, toluene, xylene, etc.), ketones (eg, acetone, methyl ethyl ketone, methyl isobutyl ketone, etc.), ethers (eg, , dibutyl ether, tetrahydrofuran, dioxane, ethylene glycol monoalkyl ether, ethylene glycol dialkyl ether, 1-methoxy-2-propanol, etc.), esters (eg, ethyl acetate, acetic acid) butyl, 2-methoxymethylethyl acetate, etc.), nitrogen-containing compounds (for example, N-methylpyrrolidone, dimethylimidazolidinone, dimethylformaldehyde, etc.), etc. are mentioned. An organic solvent can be used individually or in combination of 2 or more types.

In the organic solvent, Preferably, ketones are mentioned, More preferably, methyl ethyl ketone is mentioned.

The content rate of the organic solvent is, for example, 50 parts by mass or more, preferably 80 parts by mass or more, for example, 200 parts by mass or less, preferably 150 parts by mass with respect to 100 parts by mass of the thermosetting resin composition. less than wealth

In addition, as a mixing method of the above-mentioned components (thermosetting resin, surface-modified silica particles, thermosetting agent, pigment particles, other components and organic solvent), for example, dispersion mixing by a ball mill, stirring in a flask, 3 Kneading by this roll, etc. are mentioned.

In addition, the above-mentioned components may be mixed collectively, and a part of the above-mentioned components may be previously dispersed or dissolved in the above-described organic solvent, and the dispersion or dissolved solution may be mixed with the remaining components. For example, after uniformly dispersing the surface-modified silica particles in an organic solvent in advance by ultrasonic waves or the like, the dispersion and the remaining components (thermosetting resin, etc.) may be mixed. In addition, after uniformly dispersing the pigment particles in an organic solvent (preferably esters) beforehand, the dispersion and the remaining components (thermosetting resin, etc.) may be mixed.

Next, the thermosetting resin composition is coated on the surface of the base film 3 by a well-known method.

As a coating method of a thermosetting resin composition, screen printing, a dispenser, an application roll, etc. are mentioned, for example.

Then, a coating film is formed by drying a thermosetting resin composition and volatilizing an organic solvent as needed.

The heating temperature is a temperature at which the thermosetting resin is dried without curing, for example, 20°C or higher, preferably 90°C or higher, for example, 120°C or lower, preferably less than 100°C. Heating time is, for example, 1 minute or more, Preferably, it is 2 minutes or more, for example, 30 minutes or less, Preferably, it is 15 minutes or less.

Thereby, the coating film is dried, and the sealing layer 2 formed from the thermosetting resin composition is prepared. Next, the release film 4 is affixed on the surface of the sealing layer 2 .

By the above, the sealing sheet 1 is manufactured.

Such a sealing sheet 1 is applicable to the use by which light diffusivity, such as an image display apparatus, a lighting cover, and a window glass, is calculated|required, for example. When the sealing sheet 1 is applied to various uses, after embedding the to-be-sealed material (for example, a light source etc.) in the sealing layer 2, the sealing layer 2 is 80 degreeC or more 120, for example. ℃ or less, 0.5 hours or more and 3 hours or less Heat to harden.

<Manufacture of image display device>

The sealing sheet 1 is suitably used for sealing of the light source (display element, optical element) of an image display apparatus, for example. With reference to FIG. 2, the organic electroluminescent display with a touch sensor (it is set as the organic electroluminescent display 10 hereafter) as one Embodiment of an image display apparatus is demonstrated.

In addition, in this embodiment, although an organic electroluminescent display with a touch sensor is mentioned as an image display apparatus, the image display apparatus in particular is not restrict|limited. As an image display apparatus, a liquid crystal display (a liquid crystal display with a touch sensor is included), organic electroluminescent display (the organic electroluminescent display with a touch sensor is included), a micro LED display etc. are mentioned, for example.

The organic EL display 10 includes an element mounting unit 11 , a sealing member 14 , and a cover glass or barrier film 15 .

The element mounting unit 11 includes a substrate 13 , an organic EL element 12 , a barrier layer 16 , and an electrode (not shown).

The substrate 13 supports the organic EL element 12 . The substrate 13 preferably has flexibility.

The organic EL element 12 is a known organic EL element, and is mounted on the substrate 13 . Although not illustrated, the organic EL element 12 includes a cathode reflective electrode, an organic EL layer, and an anode transparent electrode.

The barrier layer 16 covers the organic EL element 12 , and suppresses moisture in the air from contacting the organic EL element 12 . The barrier layer 16 includes a first inorganic barrier layer 17 , a planarization layer 19 , and a second inorganic barrier layer 18 .

The first inorganic barrier layer 17 is disposed on the upper surface and the side surface of the organic EL element 12 so as to surround the organic EL element 12 . As a material of the first inorganic barrier layer 17, for example, a metal oxide (eg, aluminum oxide, silicon oxide, copper oxide, etc.), a metal nitride (eg, aluminum nitride, silicon nitride, etc.), etc. can be heard The material of the 1st inorganic barrier layer 17 can be used individually or in combination of 2 or more types. In the material of the 1st inorganic barrier layer 17, Preferably, a metal nitride, More preferably, a silicon nitride is mentioned.

The planarization layer 19 is disposed on the upper surface of the first inorganic barrier layer 17 . As a material of the planarization layer 19, a well-known resin material is mentioned.

The second inorganic barrier layer 18 is disposed on the upper surface and the side surface of the planarization layer 19 so as to surround the planarization layer 19 . As a material of the 2nd inorganic barrier layer 18, the same material as the 1st inorganic barrier layer 17 is mentioned, for example.

An electrode (not shown) comprises the sensor of organic electroluminescent display with a touch sensor. An electrode (not shown) is positioned between the substrate 13 and the sealing member 14 . For example, the electrode (not shown) may be located in the substrate 13 or on the organic EL element 12 .

The sealing member 14 is a hardened|cured material of the sealing layer 2 (sealing sheet), and is sealing the organic electroluminescent element 12 coat|covered by the barrier layer 16. As shown in FIG. The sealing member 14 is formed of the sealing layer 2 from which the base film 3 and the release film 4 were peeled. Specifically, after the base film 3 and the release film 4 are peeled off, the sealing layer 2 is pasted on the substrate 13 so as to embed the organic EL element 12 coated on the barrier layer 16 . , a cover glass or barrier film 15 is affixed on the upper surface of the sealing layer 2 , and then the sealing layer 2 is cured. Thereby, the sealing member 14 is formed.

The water vapor transmission rate of the sealing member 14 is, for example, 20 g/m ² ·24 h or more, for example, less than 45 g/m ² ·24 h. In addition, the water vapor transmission rate can be measured based on the method described in the Example mentioned later.

When the water vapor transmission rate of the sealing member 14 is below the said upper limit, deterioration of the optical element sealed by the sealing member 14 can be suppressed.

The cover glass or barrier film 15 is disposed on the upper surface of the sealing member 14 . Although not shown in figure, the cover glass or the barrier film 15 is provided in the lower surface of a glass plate and is provided with the electrode which comprises the sensor of organic electroluminescent display with a touch sensor.

Such an organic EL display 10 has an in-cell structure in which the organic EL element 12 is disposed between two electrodes constituting the sensor, or one of the two electrodes constituting the sensor is disposed on the organic EL element 12 . It has an on-cell structure that is arranged.

<action effect>

In the above-described light-diffusing thermosetting sheet, the thermosetting resin composition contains the thermosetting resin. Therefore, a to-be-sealed resin composition can seal a to-be-sealed material by hardening, after embedding a to-be-sealed material (for example, a light source etc.).

However, when a large amount of filler is added to thermosetting resins, such as an epoxy resin, generally, the improvement of a haze value can be aimed at, and although light diffusivity is improved, there exists a tendency for total light transmittance to fall. Therefore, it is difficult to make the improvement of a haze value and the outstanding total light transmittance compatible.

In addition, the filler generally tends to aggregate in an organic solvent and has poor dispersibility with a thermosetting resin such as an epoxy resin. Therefore, when the varnish of the thermosetting resin composition added with a large amount of fillers is coated, it originates in the aggregated filler, the case where the surface of a coating film becomes rough, the case where a nonuniformity arises in filler density|concentration, etc. exist.

In contrast to this, in the light diffusing thermosetting sheet described above, the thermosetting resin composition contains surface-modified silica particles. Therefore, the hardened|cured material of a thermosetting resin composition WHEREIN: While the improvement of a haze value can be aimed at, the outstanding total light transmittance is securable. As a result, the hardened|cured material of a thermosetting resin composition can make compatible a sufficient haze value and the outstanding total light transmittance, and can ensure the outstanding light diffusivity.

In addition, in the surface-modified silica particles, since the surface of the silica particles is modified with a silane coupling agent, the adhesion of the surface-modified silica particles to the thermosetting resin can be improved, and the thermosetting resin composition (especially the thermosetting type) In long-term storage of the varnish of the resin composition), sedimentation of the surface-modified silica particles can be suppressed, and the storage characteristics of the thermosetting resin composition can be improved. It is thought that this reason is based on the aggregation of surface-modified silica particles being disturbed by the presence of a silane coupling agent on the surface of a silica particle.

Moreover, depending on the use of a sealing member, it may be desired to provide a desired color and light diffusivity to a sealing member. In this case, the thermosetting resin composition preferably contains pigment particles in addition to the surface-modified silica particles. When the thermosetting resin composition contains surface-modified silica particles and pigment particles, a desired color can be imparted to the sealing member, and the haze value and total light transmittance in the sealing member can be adjusted in a well-balanced manner to ensure light diffusivity. can

<Modified example>

In a modification, about the member and process similar to the said embodiment, the same reference numeral is attached|subjected, and the detailed description is abbreviate|omitted.

As shown in FIG. 1, although the sealing sheet 1 is equipped with the sealing layer 2, the base film 3, and the release film 4, the sealing sheet is not limited to this. The sealing sheet does not need to be equipped with the base film 3 and/or the release film 4, as long as the sealing layer 2 is provided. That is, the sealing sheet may be comprised only with the sealing layer 2, and may be provided with the sealing layer 2, and either the base film 3 and the release film 4 .

As shown in FIG. 2, although the organic electroluminescent display 10 is equipped with the barrier layer 16, it is not limited to this. The organic EL display 10 does not need to include the barrier layer 16 .

Further, the organic EL display 10 has an in-cell structure in which the organic EL element 12 is arranged between two electrodes constituting the sensor, or one of the two electrodes is arranged on the organic EL element 12 . It has an on-cell structure, but is not limited thereto.

For example, as shown in FIG. 3 , the organic EL display 20 may have an outcell structure in which two electrodes constituting the sensor are arranged above the sealing member 14 . The organic EL display 20 includes the element mounting unit 11 described above, the sealing member 14 described above, and a sensor unit 25 .

The sensor unit 25 is disposed on the sealing member 14 . The sensor unit 25 is provided with the electrode which comprises the sensor of the organic electroluminescent display with a touch sensor. On the other hand, in the organic electroluminescent display 20, the board|substrate 13 is not equipped with an electrode.

In addition, in FIG.2 and FIG.3, although the sealing member 14 seals the organic electroluminescent element 12 coat|covered with the barrier layer 16, you may provide the sealing member 14 in another position.

Further, in the above embodiment, the sealing sheet 1 is thermosetted upon or after contact with the sealing material to seal the sealing material. However, the light diffusing thermosetting sheet of the present invention is limited to the sealing material. doesn't happen For example, after heat-curing a light-diffusion thermosetting sheet in advance, using another adhesive and/or another pressure-sensitive adhesive pressure-sensitive adhesive, the cured product of the light-diffusion thermosetting sheet is bonded to an object to which light diffusivity is imparted. (貼合) may be.

Also about each said modification, the effect similar to the above-mentioned embodiment is exhibited. The above-described embodiment and modification can be appropriately combined.

Example

Examples and comparative examples are shown below to explain the present invention more specifically, but the present invention is not limited thereto. Specific numerical values such as the blending ratio (content ratio), physical property values, and parameters used in the description below are described in the above "Specific contents for carrying out the invention" and corresponding blending ratios (content ratio) , physical properties, parameters, etc. may be replaced with upper limits (numeric values defined as “less than” or “less than”) or lower limits (numeric values defined as “greater than” or “exceed”) of the description. In addition, unless otherwise indicated, "part" and "%" are based on mass.

<Raw material>

The raw materials used by the Example and the comparative example are shown below.

Epoxy resin A containing alicyclic skeleton: 3,4-epoxycyclohexylmethyl (3,4-epoxy)cyclohexanecarboxylate, molecular weight 252.3, epoxy equivalent 128 to 145 g/eq., trade name Celoxide 2021P (CEL2021P), Daicel priest,

Alicyclic skeleton-containing epoxy resin B: Hydrogenated bisphenol A epoxy resin, weight average molecular weight 352, epoxy equivalent 205 g/eq., trade name YX8000, manufactured by Mitsubishi Chemical Corporation;

Alicyclic skeleton-containing epoxy resin C: DCPD-type epoxy resin, weight average molecular weight 340, epoxy equivalent 165 g/eq., trade name EP-4088L, manufactured by ADEKA,

Bisphenol F-type liquid epoxy resin A: bisphenol F-type epoxy resin liquid at room temperature, weight average molecular weight 398, epoxy equivalent 165 g/eq., trade name YL983U, manufactured by Mitsubishi Chemical Corporation;

Bisphenol F-type solid epoxy resin B: bisphenol F-type epoxy resin solid at room temperature, weight average molecular weight 7582, epoxy equivalent 10,000 g/eq., trade name jER4005P, manufactured by Mitsubishi Chemical Corporation;

Bisphenol mixed solid epoxy resin C: bisphenol A/bisphenol F solid epoxy resin of room temperature solid, weight average molecular weight 58,287, epoxy equivalent 8,400 g/eq., trade name jER4275, manufactured by Mitsubishi Chemical Corporation;

Biphenyl type epoxy resin A: biphenyl type epoxy resin solid at room temperature, weight average molecular weight 36,691, epoxy equivalent 10,000 g/eq., trade name XY-6954B35, manufactured by Mitsubishi Chemical Corporation;

Methyl ethyl ketone (MEK) solution of biphenyl type epoxy resin A: Prepared by dissolving biphenyl type epoxy resin A in MEK. 35 mass % of the density|concentration of biphenyl type epoxy resin A,

Non-porous surface-modified spherical silica particles A: average primary particle diameter of 0.3 µm, treated with an epoxy group-containing silane coupling agent, trade name SE1050-SEO, manufactured by Admatex,

Non-porous surface-modified spherical silica particles B: average primary particle diameter of 0.5 µm, treated with an epoxy group-containing silane coupling agent, trade name SC-2050MB, manufactured by Admatex, slurry product (containing MEK 30% by mass);

Non-porous surface-modified spherical silica particles C: average primary particle diameter of 1.3 µm, treated with an epoxy group-containing silane coupling agent, trade name 10SE-CM1, manufactured by Admatex, slurry product (containing 25 mass % of MEK);

MEK dispersion of non-porous surface-modified spherical silica particles A: Prepared by dispersing non-porous surface-modified spherical silica particles A in MEK by ultrasonication for 30 minutes. Concentration of non-porous surface-modified spherical silica particles 60% by mass,

Porous spherical silica particles D: average primary particle diameter of 1.0 µm, no surface modification, trade name High Freshica FQ, manufactured by Ube Eximo,

MEK dispersion of porous spherical silica particles D: Prepared by dispersing porous spherical silica particles D in MEK by ultrasonic waves for 30 minutes. Concentration of porous spherical silica particles 60% by mass,

Silicone resin powder spherical particle A: average primary particle diameter of 2.0 µm, trade name KMP-590, manufactured by Shin-Etsu Silicone Co., Ltd.

MEK dispersion of silicone resin powder spherical particle A: Prepared by dispersing silicone resin powder spherical particle A in MEK by ultrasonic wave for 30 minutes. Concentration of silicone resin powder spherical particles 60% by mass,

Silicone rubber composite powder spherical particle B: average primary particle diameter of 2.0 µm, trade name KMP-605, manufactured by Shin-Etsu Silicone Co., Ltd.

MEK dispersion of silicone rubber composite powder spherical particles B: Prepared by dispersing silicone rubber composite powder spherical particles B in MEK by ultrasonication for 30 minutes. Concentration of silicone rubber composite powder spherical particles 60% by mass,

Dispersion of pigment particles: a solvent-based carbon black dispersion in which pigment particles (carbon black, average primary particle diameter of 50 nm) are dispersed in a mixed solvent of 2-methoxymethylethyl acetate/ethyl acetate/butyl acetate, pigment concentration 12% by mass, trade name TSBK-105, made by Daisei Chemicals,

Thermal cationic curing agent: trade name CXC-1612, manufactured by King Industries,

Thermal anionic curing agent: 2-ethyl-4-methylimidazole, trade name 2E4MZ, manufactured by Shikoku Chemical Industry Co., Ltd.

Coupling agent: trade name KBM-403, manufactured by Shin-Etsu Chemical Co., Ltd.

Organic solvent: methyl ethyl ketone (MEK)

<Example 1>

Alicyclic skeleton-containing epoxy resin B, bisphenol F-type solid epoxy resin B, MEK solution of biphenyl-type epoxy resin A, non-porous surface-modified spherical silica particles A, thermal cationic curing agent, coupling agent, and organic solvent , was mixed by the prescription shown in Table 1, and the varnish of the thermosetting resin composition was prepared.

Then, after coating the varnish on the PET film (releasable PET film (trade name: Purex A53, manufactured by Teijin DuPont Film Co., Ltd., thickness: 38 μm, base film)) with a coater, a nitrogen purge oven at 90° C. It dried for 3 minutes and formed the sealing layer with a thickness of 15 micrometers.

Next, the PET film (PET film (trade name: Purex A31, the Teijin DuPont film company make, thickness: 38 micrometers, release film)) by which the release process was carried out was pasted together to the sealing layer by a thermal laminator at 80 degreeC.

By the above, the sealing sheet provided with a sealing layer, a base film, and a release film was prepared.

<Examples 2 to 10, Comparative Examples 1 to 6>

Except having changed the prescription of each raw material into the prescription shown in each of Table 1 and Table 2, it carried out similarly to Example 1, and prepared the varnish and sealing sheet of a thermosetting resin composition.

<Example 11>

An alicyclic skeleton-containing epoxy resin B, a bisphenol F-type solid epoxy resin B, a MEK solution of a biphenyl-type epoxy resin A, a dispersion of pigment particles, a non-porous surface-modified spherical silica particle B, a thermal cationic curing agent, and a couple The ring agent was mixed by the prescription shown in Table 3, and the varnish of the thermosetting resin composition was prepared.

Next, on PET film (PET film (trade name: Purex A53, manufactured by Teijin DuPont Film Co., Ltd., thickness: 38 µm, base film)) subjected to a release treatment by a coater, a varnish is coated to the coating film thickness shown in Table 3 After that, it was dried in a nitrogen purge oven at 90° C. for 3 minutes to form a sealing layer.

Next, the PET film (PET film (trade name: Purex A31, the Teijin DuPont film company make, thickness: 38 micrometers, release film)) by which the release process was carried out was pasted together to the sealing layer by a thermal laminator at 80 degreeC.

By the above, the sealing sheet provided with a sealing layer, a base film, and a release film was prepared.

<Examples 12 to 18, Comparative Examples 7 and 8>

Except having changed the prescription of each raw material into the prescription shown in Table 3, it carried out similarly to Example 11, and prepared the varnish and sealing sheet of a thermosetting resin composition.

<Evaluation>

[Particle Settlement]

30 g of the varnish prepared in each Example and each comparative example shown in Tables 1 and 2 was put into a 50 ml screw tube (35 mm in diameter), and after standing at room temperature (23 ° C.) for 24 hours, the presence or absence of sediment was visually confirmed. And the particle settling property was evaluated by the following reference|standard. The results are shown in Tables 1 and 2.

No sediment: ○

With sediment: ×

[90° Peel Strength]

An aluminum-PET composite film (aluminum surface)/resin/alkali glass spring-type balance (for weighing 1 kg) was prepared. After peeling the release film of the sealing sheet of each Example and each comparative example shown in Table 1 and Table 2 from the sealing layer, the sealing layer was affixed on the aluminum surface of the aluminum-PET composite film. Then, the sealing layer was hardened at 100 degreeC for 1 hour. (In Examples 9 and 10 and Comparative Example 3, curing was performed at 100° C. for 2 hours.)

Next, the 90 degree|times peeling strength of the hardened|cured material of an aluminum surface and a sealing layer was measured. In Examples 1-10 and Comparative Examples 1-6, this 90 degree peeling strength was made into adhesive strength. The results are shown in Tables 1 and 2.

[Water vapor permeability]

After peeling the release film of the sealing sheet of each Example and each comparative example shown in Table 1 and Table 2 from the sealing layer, the sealing layer was hardened at 100 degreeC for 1 hour. (In Examples 9 and 10 and Comparative Example 3, curing was performed at 100° C. for 2 hours.)

Next, the base film was peeled from the sealing layer after hardening, and the sample for a measurement was obtained. Based on JIS Z0208, the water vapor transmission rate (water vapor transmission amount) of the obtained sample was measured on 60 degreeC 90 %RH conditions. Then, from the film thickness of the sample used for a measurement, it converted into the value in case the thickness of a sample is 100 micrometers. The results are shown in Tables 1 and 2.

[Haze value, total light transmittance (TT)]

After peeling the release film of the sealing sheet of each Example and each comparative example shown in Tables 1-3 from the sealing layer, the sealing layer was hardened at 100 degreeC for 1 hour. (In Examples 9 and 10 and Comparative Example 3, curing was performed at 100° C. for 2 hours.)

Next, the base film was peeled from the sealing layer after hardening, and the sample for a measurement was obtained. The haze value and the total light transmittance of the obtained sample were measured using the haze meter NDH2000 by the Nippon Denshoku Kogyo Co., Ltd. product. The results are shown in Tables 1-3. In particular, it was confirmed that the outstanding light diffusivity was exhibited by making the haze value of 80 % or more and 90 % or more of total light transmittance compatible. In addition, it was confirmed that, by adding pigment particles to the thermosetting resin composition, a desired color can be imparted to the cured product of the encapsulation layer, and the haze value and the total light transmittance can be adjusted in a well-balanced manner in the cured product of the encapsulation layer. .

[Appearance of the encapsulation layer]

After peeling the release film of the sealing sheet of each Example and each comparative example shown in Tables 1-3 from the sealing layer, the sealing layer was hardened at 100 degreeC for 1 hour. (In Examples 9 and 10 and Comparative Example 3, curing was performed at 100° C. for 2 hours.)

The sealing layer after hardening was observed visually, and the thing with a smooth surface was evaluated as (circle), and the thing with a rough surface was evaluated as x. The results are shown in Tables 1-3.

[L ^* value (blackness)]

After peeling the release film of the sealing sheet of each Example and each comparative example shown in Table 3 from the sealing layer, the sealing layer was hardened at 100 degreeC for 1 hour.

Next, the base film was peeled from the sealing layer after hardening, and the sample for a measurement was obtained. The L ^* value (blackness) of the obtained sample was measured using the KONICA MINOLTA colorimeter CR-200. The results are shown in Table 3.

In addition, although the said invention was provided as embodiment of the illustration of this invention, this is only a mere illustration and should not be interpreted limitedly. Modifications of the present invention that are obvious to those skilled in the art are included in the following claims.

The light-diffusion thermosetting sheet|seat of this invention is, for example, window glass of a general building; windshields for vehicles; glazing material; protective covers for signs, lighting fixtures, indicator lights, etc.; It is applicable to image display devices (organic EL display, liquid crystal display, micro LED display, etc.).

Claims (6)

A thermosetting resin and a thermosetting resin composition comprising surface-modified silica particles,
The average primary particle diameter of the surface-modified silica particles is 0.1 µm or more and 1.5 µm or less, and the surface-modified silica particles are silica particles surface-modified with a silane coupling agent, A light diffusible thermosetting sheet. The method of claim 1,
The thermosetting resin, light diffusing thermosetting sheet, characterized in that it contains an epoxy resin. The method of claim 1,
The silica particles, characterized in that the non-porous, light diffusible thermosetting sheet. The method of claim 1,
The content rate of the said surface-modified silica particle is 5 mass parts or more and 50 mass parts or less with respect to 100 weight part of said thermosetting resins, The light-diffusion thermosetting sheet|seat characterized by the above-mentioned. The method of claim 1,
The thermosetting resin composition has a haze value of 35% or more and a total light transmittance of 80% or more when the thermosetting resin composition is formed into a sheet shape having a thickness of 15 µm and thermosetted. thermosetting sheet. The method of claim 1,
The thermosetting resin composition further comprises a pigment particle,
The average primary particle diameter of the pigment particles is 100 nm or less, Light diffusible thermosetting sheet, characterized in that.

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