JP2002273793A - Method for manufacturing polymer sheet and polymer sheet by the method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method which can inexpensively manufacture an optical polymer sheet having high gas-steam barrier properties, a substrate for a liquid crystal display element using the polymer sheet obtained by the method, and a liquid crystal display. SOLUTION: In the method for manufacturing the polymer sheet, in the polymer sheet having at least a base material (a) and a gas-steam barrier layer, a transfer film in which a protective layer and the gas-steam barrier layer or only the gas-steam barrier layer are or is formed on a peeling base material (b) 0.1 mm or below in thickness is laminated on the base material (a) in which an adhesion layer containing at least a photo-curable resin and a silane coupling agent is formed for molding.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an optical polymer sheet which can be mainly used for a plastic substrate used for a liquid crystal display device.

[0002]

2. Description of the Related Art In a plastic substrate for a liquid crystal display device,
A method of forming a silicon oxide film or an aluminum oxide film serving as a gas / water vapor barrier layer on a single sheet by a vacuum film forming process such as vapor deposition or sputtering is often used. On the other hand, when the sheet thickness is less than about 0.3 mm, a method of performing similar film formation by vapor deposition or sputtering with a roll-to-roll method is also possible. A roll-to-roll method is common. In general, the roll-to-roll method has higher productivity than the method of forming a film on a single sheet, but the roll diameter increases with respect to the length as the sheet thickness increases, so that the sheet can be put into a vacuum device at one time. The sheet length becomes short, and the superiority of the roll-to-roll method cannot be sufficiently exhibited in terms of productivity and film formation cost. However, due to the assembly process of the liquid crystal display device, the sheet thickness is at least 0.1 m.
Since a thickness of m or more is required, it is important to further increase the productivity in order to reduce the film formation cost.

Japanese Patent Application Laid-Open No. Hei 8-234181 proposes a method in which a gas barrier layer and an adhesive layer are formed on a film and transferred to a sheet as a base material. When the thickness of the transfer film is reduced using the method described in the above publication, the gas / steam barrier layer can be formed on a thin transfer film, so that the productivity of the gas / steam barrier layer can be improved. As a result, the manufacturing cost of the plastic display element substrate can be reduced. However, when the adhesive layer is formed on the transfer film side as described in the above-mentioned publication, when a thermosetting resin or a photocurable resin is applied to the adhesive layer in consideration of the adhesion to the base material, the usable For a limited time, for example, when a large number of transfer films disclosed in the above-mentioned publication are stocked for cost reduction, the adhesion may deteriorate due to the deterioration of the adhesive layer, and the gas / water vapor barrier properties may decrease. . Further, since the adhesive layer is coated on the gas / water vapor barrier layer formed on the thin film, wrinkles may be formed depending on the coating method, and the gas / water vapor barrier layer may be damaged. Further, when silicon oxide or aluminum oxide is used for the gas barrier layer, the gas barrier property is generally improved by leaving the film in the air after forming the film and before coating the upper layer. So do
In the case of stocking in a state where the coating has been performed, this time is unnecessary, and there is a waste in productivity that extra time is required.

[0004]

SUMMARY OF THE INVENTION The present invention provides a method for inexpensively producing an optical polymer sheet having a high gas / water vapor barrier property. It is intended to provide a liquid crystal display element substrate and a liquid crystal display device used.

[0005]

That is, the present invention provides: (1) a peeling substrate (b) having a thickness of 0.1 mm or less in a polymer sheet having at least a substrate (a) and a gas / water vapor barrier layer. Laminating a transfer film, on which a protective layer and a gas / steam barrier layer or only a gas / steam barrier layer are formed, on a substrate (a) provided with an adhesion layer containing at least a photocurable resin and a silane coupling agent A method for producing a polymer sheet, comprising: (2) The method for producing a polymer sheet according to (1), wherein the substrate (a) comprises a transparent polymer film containing polyether sulfone. (3) The method for producing a polymer sheet according to (1) or (2), wherein the protective layer is a resin composition containing a thermosetting resin or a photocurable resin as a main component. (4) The method for producing a polymer sheet according to any one of (1) to (3), wherein the release substrate (b) can be released after lamination. (5) The total light transmittance is 80% or more (1) to (4).
An optical polymer sheet obtained by the production method of 1. (6) A display element substrate manufactured using the optical polymer sheet according to (5). (7) A display element manufactured using the display element substrate according to (6). It is.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION As the polymer material used for the substrate (a) of the present invention, about 15
Heating is performed at 0 ° C., and when thermocompression bonding is performed with an anisotropic conductive film for connection to an external circuit, heating at about 150 ° C. is necessary. It is necessary to be higher than or equal to ° C. Examples of the heat-resistant thermoplastic resin having a glass transition temperature of 160 ° C. or higher include aromatic polyether sulfone, thermoplastic aromatic polyether ketone, polyetherimide, polyphenylene sulfide, polyarylate, cyclic polyolefin, polyester, and copolymers thereof. Of these, polyether sulfone, which has a good balance of transparency, heat resistance, workability, and impact resistance, is particularly preferable in the production of liquid crystal display elements. If the glass transition temperature is not lower than 160 ° C., resins such as thermoplastic polyesters, polyamides and polycarbonates, lubricants, heat stabilizers, weather stabilizers, pigments, dyes, inorganic fillers and the like may be appropriately blended. .

[0007] The photo-curable resin constituting the adhesion layer of the present invention comprises:
Acrylic resins such as epoxy acrylate, urethane acrylate, polyethylene glycol acrylate, and glycerol methacrylate, and alicyclic epoxy resins can be used, but are not particularly limited. These may be used at the same time.

In the present invention, the photocurable resin must be cured by irradiating light, particularly ultraviolet rays, through the substrate (a) or the peeling substrate (b). For this reason, the amount of ultraviolet rays necessary for curing the resin is insufficient because the base material (a) or the peeling substrate (b) itself absorbs ultraviolet rays, which may cause insufficient curing of the adhesive layer forming resin. As a result, there may be a problem that the adhesion strength between the adhesion layer and the water vapor / gas barrier layer is reduced, and the barrier property is thereby reduced.
Therefore, by adding a silane coupling agent, the adhesion strength between the adhesion layer and the substrate (a) or between the adhesion layer and the water vapor / gas barrier layer is improved. As silane coupling agents, epoxy-based, mercapto-based, amino-based,
Examples thereof include methacryloxy-based compounds, and among them, epoxy-based and mercapto-based silane coupling agents are particularly preferable. The silane coupling agent used in the present invention is present in a catalytically effective amount, such an amount being
Although not limited, it is about 0.01-5 parts by weight, more preferably about 0.025-2 parts by weight.

The transfer film of the present invention is obtained by forming only a protective layer or a gas / water vapor barrier layer on a release substrate (b). That is, since there is no adhesive layer, the usable time is not limited, and by keeping in this state, it is also possible to perform a leaving treatment for sufficiently exhibiting the gas barrier property. The peeling substrate (b) comprises:
In order to increase productivity and film formation cost, it is desirable to be as thin as possible, and the thickness is desirably 0.1 mm or less.
However, if the thickness is significantly reduced to less than 0.01 mm,
It is preferable that the thickness be 0.01 mm or more, because handling becomes difficult such as breakage during peeling. Also,
When a photo-curing resin is used for the adhesive layer, it is desirable that the material be capable of transmitting light of a wavelength necessary for curing as much as possible, such as polyethylene, polypropylene, aliphatic polyamide, polyethylene terephthalate,
Examples thereof include polybutylene terephthalate, polysulfone, polyether sulfone, and polycarbonate. Further, it is desirable that the peeling substrate (b) can be peeled off after lamination, and it is preferable that the adhesiveness with the adjacent gas / steam barrier layer or protective layer is low. In some cases, a release layer such as a release agent may be formed between adjacent layers.

The protective layer of the present invention protects the gas / water vapor barrier layer, and is preferably a material having good adhesion to the gas / water vapor barrier layer and having a certain surface height. As an example, a resin composition containing a thermosetting resin or a photocurable resin as a main component is preferable. Examples of the thermosetting resin include orthocresol novolak epoxy, bisphenol A epoxy, bisphenol F epoxy, and bisphenol S epoxy. , Epoxy resins such as biphenyl type epoxy and dicyclopentadiene type epoxy, phenol resins, bismaleimides, unsaturated polyesters and the like, and those containing inorganic fillers such as silica in these. Examples of the resin include acrylic resins such as epoxy acrylate, urethane acrylate, polyethylene glycol acrylate, and glycerol methacrylate, alicyclic epoxy resins, and the like, and those containing inorganic fillers such as silica in these. Constant are not.

The gas / water vapor barrier layer of the present invention is for protecting the liquid crystal or preventing the substrate itself from changing step by step.
Organic materials such as polyvinyl alcohol and poly (ethylene vinyl alcohol), silicon oxide, aluminum oxide,
Inorganic materials such as tin oxide and indium tin oxide may be mentioned, and among these, those obtained by forming a thin film of an inorganic material having no humidity dependence on gas barrier properties are desirable. , Sol-gel method, vacuum deposition, ion plating, sputtering, CVD
However, a vacuum deposition method such as vacuum deposition, ion plating, sputtering, and CVD is preferable because a dense film having excellent gas barrier properties is easily obtained.

The transfer film of the present invention can be laminated on one side or both sides of the base material (a). If it is laminated on one side, it is on the back side, if it is laminated on both sides, it is on one side, and in some cases, it is undercoat. The display element substrate is completed by forming a transparent conductive layer through the layer.

Hereinafter, the present invention will be described based on examples, but the present invention is not limited to these examples.

[0014]

EXAMPLE 1 15 parts by weight of an epoxy acrylate resin as an ultraviolet-curable resin composition, 20 parts by weight of urethane acrylate, and Irgacure 907 (Cibas Co., Ltd.) as a photopolymerization initiator were placed on one side of a 25 μm-thick nylon film. A mixture of 1 part by weight of Charity Chemicals) and 64 parts by weight of butyl acetate was applied by spin coating, heated at 120 ° C. for 5 minutes to remove the solvent, and then irradiated with 350 mJ of ultraviolet light using a high-pressure mercury lamp.
/ Cm ² to form a protective layer having a thickness of 2.5 μm.

On top of this, 500
ＳｉＯThick SiO _x was obtained. The value of x was set to 1.6 to 1.8 by controlling the flow rate of oxygen gas during sputtering. Thus, a transfer film having a gas / water vapor barrier layer was prepared. After the preparation, it was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

A polyether sulfone having a thickness of 200 μm was used as a base material, and 25 parts by weight of an epoxy acrylate resin, 10 parts by weight of a urethane acrylate resin as an ultraviolet-curable resin composition, and Irgacure 9 as a photopolymerization initiator.
07 (manufactured by Ciba-Charity Chemicals), 0.2 parts by weight of γ-mercaptopropyltrimethoxysilane as a silane coupling agent, and 65 parts by weight of butyl acetate are dried to form a film having a thickness of 2.5 μm. The coating was applied by a spin coating method as described above, and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesive layer provided in this way and the gas barrier layer of the transfer film are laminated using a laminating roll set at a temperature of 80 ° C., and ultraviolet rays are irradiated from the transfer film side using a high-pressure mercury lamp at 350 mJ. / Cm
^Two irradiations were performed to cure the ultraviolet curable resin composition. After lamination, the nylon film was peeled off to obtain an optical polymer sheet. The total light transmittance of this sheet was measured according to JIS K710.
It was 88% when measured by the method according to 5. Generally, the total light transmittance required for a liquid crystal display element is considered to be 80% or more.

Subsequently, the liquid crystal display element is processed in the following procedure.
A child was made. First, the transparent polymer sheet was
The initial vacuum degree is 3 × by DC magnetron method
10 ^-FourFrom the state of Pa, a mixed gas of oxygen / argon gas 4%
1 × 10^-1Sputtering under Pa conditions
When the ring is performed and the atomic ratio of In / (In + Sn) is 0.98,
A transparent conductive film made of certain indium tin oxide (ITO)
Obtained. As a result of the measurement, the film thickness was 1600 ° and the specific resistance was 4 × 1.
0^-FourΩ-cm. After forming ITO, apply resist
Cloth and development, 10vol% HC as etchant
1, pattern etching at a liquid temperature of 40 ° C, diagonal length 3
Inch, L / S = 150 / 50μm display pattern
Done. After pattern formation, an alignment film for STN is applied and
After firing at 50 ° C for 2 hours, twist 240 °
A rubbing treatment was performed so as to obtain the orientation. Rubbing treatment
After that, a spacer is sprayed, a sealant is applied, and 130 ° C.
The cell is hardened by sealing and poured into the liquid crystal composition for STN.
Entered. Paste the polarizing plate at the position where the contrast is maximum
In addition, a liquid crystal display device was manufactured. This liquid crystal display element
There are no bubbles due to insufficient gas barrier properties and no display defects
I wasn't.

Example 2 In the same manner as in Example 1, a protective film and a gas / water vapor barrier layer were provided on one side of a nylon film having a thickness of 25 μm to prepare a transfer film. After creation, temperature 30 ℃, humidity 60%
Was stored for one month in the environment described above.

A polyether sulfone having a thickness of 200 μm was used as a base material, 25 parts by weight of an epoxy acrylate resin and 10 parts by weight of a urethane acrylate resin as an ultraviolet-curable resin composition, and Irgacure 9 as a photopolymerization initiator.
07 (manufactured by Ciba-Charity Chemicals), 0.2 parts by weight of γ-glycidoxypropyltrimethoxysilane as a silane coupling agent, and 65 parts by weight of butyl acetate are dried to form a film having a thickness of 2.5 μm. Was applied by a spin coating method, and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesive layer provided in this manner and the gas barrier layer of the transfer film are laminated using a laminating roll set at a temperature of 80 ° C., and ultraviolet rays are irradiated from the transfer film side using a high-pressure mercury lamp at 350 mJ. / Cm
^Two irradiations were performed to cure the ultraviolet curable resin composition. After lamination, the nylon film was peeled off to obtain an optical polymer sheet. The total light transmittance of this sheet was measured according to JIS K710.
It was 86% when measured by the method according to 5. Subsequently, a liquid crystal display device was manufactured in the same manner as in Example 1. In this liquid crystal display element, no bubbles were generated due to insufficient gas barrier properties, and no display defect was observed.

Example 3 In the same manner as in Example 1, a protective film and a gas / water vapor barrier layer were provided on one side of a 25 μm-thick nylon film to prepare a transfer film. After the preparation, it was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

A polyether sulfone having a thickness of 200 μm as a base material, 25 parts by weight of an epoxy acrylate resin, 10 parts by weight of a urethane acrylate resin as an ultraviolet curable resin composition, and Irgacure 90 as a photopolymerization initiator.
7 (manufactured by Ciba-Charity Chemicals), a mixture of 0.5 parts by weight of β- (3,4 epoxycyclohexyl) ethyltrimethoxysilane as a silane coupling agent and 64 parts by weight of butyl acetate was dried, and the film was dried. The solution was applied by spin coating so as to have a thickness of 2.5 μm, and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesion layer thus provided and the gas barrier layer of the transfer film were laminated in the same manner as in Example 1, and 350 mJ / cm ^{2 of} ultraviolet light was irradiated from the transfer film surface using a high-pressure mercury lamp. Then, the ultraviolet curable resin composition was cured. After lamination, the nylon film was peeled off to obtain an optical polymer sheet. The total light transmittance of this sheet was measured by a method according to JIS K7105 and found to be 84%. Subsequently, a liquid crystal display device was manufactured in the same manner as in Example 1. In this liquid crystal display element, no bubbles were generated due to insufficient gas barrier properties, and no display defect was observed.

Example 4 In exactly the same manner as in Example 1, a protective film and a gas / water vapor barrier layer were provided on a 25 μm-thick nylon film to obtain a transfer film. After the preparation, it was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

A polyethersulfone having a thickness of 200 μm as a base material, 35 parts by weight of an epoxy acrylate resin as an ultraviolet-curable resin composition, and Irgacure 907 (manufactured by Ciba Charity Chemicals) 1 as a photopolymerization initiator.
Parts by weight, 0.2 part by weight of γ-mercaptopropyltrimethoxysilane as a silane coupling agent, butyl acetate 6
After drying, 5 parts by weight of the mixed solution was applied by spin coating so that the film thickness became 2.5 μm, and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesive layer thus provided and the gas barrier layer of the transfer film are laminated using a laminating roll set at a temperature of 80 ° C., and ultraviolet rays are irradiated from the transfer film side using a high-pressure mercury lamp at 350 mJ. / Cm
^Two irradiations were performed to cure the ultraviolet curable resin composition. After lamination, the nylon film was peeled off to obtain an optical polymer sheet. The total light transmittance of this sheet was measured according to JIS K710.
It was 84% when measured by the method according to 5. Subsequently, a liquid crystal display device was manufactured in the same manner as in Example 1. In this liquid crystal display element, no bubbles were generated due to insufficient gas barrier properties, and no display defect was observed.

Example 5 In the same manner as in Example 1, a protective layer and a gas / steam barrier layer were provided on one surface of a 38 μm thick polypropylene film in the same manner as in Example 1, to obtain a transfer film. After the preparation, it was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

A polyether sulfone having a thickness of 200 μm was used as a base material, 25 parts by weight of an epoxy acrylate resin, 10 parts by weight of a urethane acrylate resin as an ultraviolet curable resin composition, and Irgacure 90 as a photopolymerization initiator.
7 (manufactured by Ciba Charity Chemicals), a mixture of 0.2 parts by weight of γ-mercaptopropyltrimethoxysilane and 65 parts by weight of butyl acetate as a silane coupling agent was dried to a film thickness of 2.5 μm. The solution was applied by a spin coating method and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesive layer thus provided and the gas barrier layer of the above-mentioned transfer film are laminated using a laminating roll set at a temperature of 80 ° C., and 350 mJ / cm from the transfer film surface side using a high-pressure mercury lamp. ^Two irradiations were performed to cure the ultraviolet curable resin composition. After lamination, the polypropylene film was peeled off to obtain an optical polymer sheet. The total light transmittance of this sheet was measured according to JIS K71.
It was 82% when measured by the method according to No. 05. Subsequently, a liquid crystal display device was manufactured in the same manner as in Example 1. In this liquid crystal display element, no bubbles were generated due to insufficient gas barrier properties, and no display defect was observed. The total light transmittance measured by a method according to JIS K7105 was 82%.

Example 6 A protective layer and a gas layer were formed on one surface of a polyethylene terephthalate film having a thickness of 50 μm in the same manner as in Example 1.
A water vapor barrier layer was provided to obtain a transfer film. After creation,
It was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

A polyether sulfone having a thickness of 200 μm was used as a base material, 25 parts by weight of an epoxy acrylate resin, 10 parts by weight of a urethane acrylate resin as an ultraviolet curable resin composition, and Irgacure 90 as a photopolymerization initiator.
7 (manufactured by Ciba Charity Chemicals), a mixture of 0.2 parts by weight of γ-mercaptopropyltrimethoxysilane and 65 parts by weight of butyl acetate as a silane coupling agent was dried to a film thickness of 2.5 μm. The solution was applied by a spin coating method and heated at 120 ° C. for 5 minutes to remove the solvent, thereby forming an adhesion layer.

The adhesion layer thus provided and the gas barrier layer of the transfer film were laminated in the same manner as in Example 1, and 350 mJ / cm ^{2 of} ultraviolet light was irradiated from the transfer film surface using a high-pressure mercury lamp. Then, the ultraviolet curable resin composition was cured. After lamination, the polyethylene terephthalate film was peeled off to obtain an optical polymer sheet.
The total light transmittance of this sheet was measured by a method according to JIS K7105 and found to be 80%. Then, Example 1
A liquid crystal display device was produced in the same manner as in Example 1. In this liquid crystal display element, no bubbles were generated due to insufficient gas barrier properties, and no display defect was observed. The total light transmittance measured by a method according to JIS K7105 was 80%.

Comparative Example On one side of a stretched polyester film having a thickness of 30 μm,
100 parts by weight of an epoxy acrylate prepolymer having a melting point of 70 ° C. as a UV-curable resin composition, and butyl acetate 30
0 parts by weight, 100 parts by weight of propylene glycol monomethyl ether acetate, and 2 parts by weight of benzoin ethyl ether were stirred at 50 ° C. and dissolved to form a uniform solution, and after drying, applied by spin coating to a thickness of 2 μm. Then, the mixture was heated at 100 ° C. for 5 minutes to remove the solvent. Subsequently, ultraviolet rays were applied from the application side using a high-pressure mercury lamp at 500 mJ /
cm ^{2 was} irradiated to cure the ultraviolet curable resin composition.

On top of this, 500
ＳｉＯThick SiO _x was obtained. The value of x was set to 1.6 to 1.8 by controlling the flow rate of oxygen gas during sputtering.

Subsequently, 25 parts by weight of an epoxy acrylate resin, 10 parts by weight of a urethane acrylate resin, and Irgacure 907 (1 part by weight, manufactured by Ciba Charity Chemicals, 65 parts by weight of butyl acetate) were used as a photopolymerization initiator on SiO _x.
A part by weight of the mixed solution was dried and applied by spin coating so as to have a film thickness of 1 μm, and heated at 80 ° C. for 3 minutes to remove the solvent. Thus, a transfer film having a gas barrier layer and an adhesive layer was prepared. After the preparation, it was stored for one month in an environment at a temperature of 30 ° C. and a humidity of 60%.

Using a 200 μm-thick polyether sulfone as a base material, lamination was performed using a laminating roll whose temperature was set to 120 ° C. with the bonding surface of the transfer film. After lamination, ultraviolet rays were irradiated from the transfer film surface using a high-pressure mercury lamp at 350 mJ / cm ² to cure the ultraviolet curable resin composition. Thereafter, when the stretched polypropylene film was peeled off, sufficient adhesiveness was not obtained, and the gas barrier layer could only be partially transferred to the substrate side. The total light transmittance of this sheet was measured according to JIS K71.
It was 77% when measured by the method according to 05. Subsequently, a liquid crystal display device was manufactured in the same manner as in Example 1. In this liquid crystal display element, bubbles were generated due to insufficient gas barrier properties, and display defects were observed.

[0038]

According to the present invention, an optical polymer sheet optimal for a substrate for a plastic display element having good gas / water vapor barrier properties can be produced at low cost and with good productivity, and the plastic display produced by this method can be produced. The display element using the element substrate showed good display performance not inferior to the display element using the glass substrate. INDUSTRIAL APPLICABILITY The present invention is extremely effective for reducing the cost of a substrate for a plastic display element, which is lighter and harder to break than a glass substrate.

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Claims (7)

[Claims] 1. A polymer sheet having at least a substrate (a) and a gas / water vapor barrier layer, having a thickness of 0.1 mm
A transfer film in which a protective layer and a gas / steam barrier layer or only a gas / steam barrier layer were formed on the following peeling substrate (b) was provided with an adhesion layer containing at least a photocurable resin and a silane coupling agent. A method for producing a polymer sheet, which is formed by laminating a base material (a). 2. The method for producing a polymer sheet according to claim 1, wherein the substrate (a) comprises a transparent polymer film containing polyether sulfone. 3. The method for producing a polymer sheet according to claim 1, wherein the protective layer is a resin composition containing a thermosetting resin or a photocurable resin as a main component. 4. The peelable substrate (b) can be peeled after lamination.
The method for producing a polymer sheet according to any one of the above items. 5. An optical polymer sheet obtained by the production method according to claim 1, which has a total light transmittance of 80% or more. 6. A display element substrate manufactured using the optical polymer sheet according to claim 5. 7. A display element manufactured using the display element substrate according to claim 6.