TW201705580A - Method for manufacturing package - Google Patents

Abstract

The present invention provides a method for manufacturing a package wherein an organic EL element on a substrate is sealed by means of a resin composition layer. This method for manufacturing a package comprises: (1) a step for drying a sheet for sealing, which is obtained by sequentially laminating a supporting body, a resin composition layer and a cover film in this order, by a near infrared or middle infrared dryer without separating the cover film; and (2) a step for sealing an organic EL element by means of the resin composition layer of the sheet for sealing after removing the cover film from the dried sheet for sealing.

Description

Method of manufacturing package

The present invention relates to a method for producing a package (particularly an organic EL device) in which an organic EL (electroluminescence) element on a substrate is packaged with a resin composition layer. Further, the present invention relates to a method of packaging an organic EL element on a substrate.

The organic EL element is a light-emitting element using an organic substance in a light-emitting material, and has been attracting attention in recent years because it can obtain high-luminance light by a low voltage. However, the organic EL element has a problem that the resistance to moisture is extremely weak, the brightness is lowered due to moisture, the light is not emitted, the interface between the electrode and the light-emitting layer is peeled off, and the metal is oxidized to increase the resistance. Therefore, in order to block the moisture in the inside of the element and the outside air, the resin composition layer is formed to cover the entire surface of the light-emitting layer formed on the substrate, for example, and the organic EL element is encapsulated (for example, Patent Documents 1 to 3).

[Previous Technical Literature] [Patent Document]

[Patent Document 1] International Publication No. 2010/084938

[Patent Document 2] International Publication No. 2010/084939

[Patent Document 3] International Publication No. 2011/016408

The amount of moisture present in the sheet for encapsulating the organic EL element (hereinafter sometimes simply referred to as "package sheet") by forming the resin composition layer on the support may adversely affect the organic EL element. Therefore, the sheet for packaging is desirably transported and stored in a dry state. However, in this case, it is also difficult to completely prevent moisture from intruding, and even a small amount of moisture intrusion becomes a problem.

Before encapsulating the organic EL device, it is conceivable to dry the package sheet, but when the package sheet is heated at an excessively high temperature for drying, the package sheet (especially the resin composition) is denatured (for example, hardened). Not good. On the other hand, when vacuum drying at a low temperature, there is a problem that drying takes time.

Further, the resin composition layer used for the encapsulating sheet before encapsulation is generally protected by a protective film. In the sheet for encapsulation, it is considered that moisture is mainly contained in the resin composition layer, and drying of the resin composition layer of the encapsulating sheet is effective after drying the protective film and drying it. However, when drying after peeling off the protective film, dirt or the like may adhere to the surface of the resin composition layer during drying, which may adversely affect the organic EL element.

The present invention has been made in view of the above circumstances, and an object thereof is to provide a support body, a resin composition layer, and a protective film (cover) Film) A method of manufacturing a package of an organic EL element in which the encapsulating sheet is laminated in this order and the protective sheet is not peeled off, and the step of encapsulating the sheet is effectively dried.

As a result of the positive review, the present inventors have found that when a package is produced by encapsulating an organic EL device with a sheet for encapsulation, a trace amount of moisture contained in the package sheet may adversely affect the organic EL element, and the package sheet may be used. When the moisture contained in the medium is reduced to a certain value or less, the life of the organic EL element can be remarkably improved, and the drying step of the near-infrared to medium-infrared dryer can be introduced before the packaging step, and the film can be effectively dried without peeling off the protective film. The package uses a sheet to remove moisture. The present invention based on this finding is as follows.

[1] A manufacturing method for manufacturing a package of an organic EL element on a substrate by a resin composition layer, comprising the steps of: (1) supporting a support, a resin composition layer, and a protective film; The encapsulating sheet which is sequentially laminated, the step of drying the near-infrared to medium-infrared dryer without peeling off the protective film, and (2) peeling off the protective film from the dried packaging sheet, and then encapsulating the resin composition layer of the encapsulating sheet The step of the organic EL element.

[2] The production method according to the above [1], wherein the step (2) is carried out in the same manufacturing line as the step (1).

[3] The manufacturing method of the above [1] or [2], wherein the subsequent step (1) Go to step (2).

[4] The production method according to any one of [1] to [3], wherein the time from the drying of the step (1) to the start of the packaging of the step (2) is from 1 to 60 minutes.

[5] The production method according to any one of [1] to [3], wherein the time from the drying of the step (1) to the start of the packaging of the step (2) is from 1 to 30 minutes.

[6] The production method according to any one of [1] to [3] above, wherein the time from the drying of the step (1) to the start of the packaging of the step (2) is from 1 to 15 minutes.

[7] The production method according to any one of the above [1] to [3] wherein the time from the drying of the step (1) to the start of the packaging of the step (2) is from 1 to 10 minutes.

[8] The production method according to any one of [1] to [7] wherein the peak wavelength of the near infrared ray to the medium infrared ray irradiated from the near infrared ray to the medium infrared ray dryer is in the range of 1.0 to 4.0 μm.

[9] The production method according to any one of [1] to [7], wherein a peak wavelength of near-infrared to mid-infrared rays irradiated from the near-infrared to medium-infrared dryer is in a range of 1.0 to 3.5 μm.

[10] The production method according to any one of [1] to [7], wherein a peak wavelength of the near infrared ray to the medium infrared ray irradiated from the near infrared ray to the medium infrared ray dryer is in a range of 1.25 to 3.5 μm.

[11] The production method according to any one of [1] to [7], wherein the peak of the near infrared to the middle infrared is irradiated from the near infrared to the medium infrared dryer The value wavelength is in the range of 1.5 to 3.5 μm.

[12] The production method according to any one of [1] to [11] wherein the drying temperature of the near-infrared to medium-infrared dryer is 60 to 160 ° C, and the drying time is 0.5 to 60 minutes.

[13] The production method according to [12] above, wherein the drying temperature of the near-infrared to medium-infrared dryer is 60 to 140 °C.

[14] The production method according to the above [12], wherein the drying temperature of the near-infrared to medium-infrared dryer is 60 to 130 °C.

[15] The production method according to [12] above, wherein the drying temperature of the near-infrared to medium-infrared dryer is 80 to 130 °C.

[16] The production method according to [12] above, wherein the drying temperature of the near-infrared to medium-infrared dryer is 90 to 130 °C.

[17] The production method according to any one of [12] to [16] wherein the drying time of the near-infrared to medium-infrared dryer is from 1 to 30 minutes.

[18] The production method according to any one of [12] to [16] wherein the drying time of the near-infrared to medium-infrared dryer is 5 to 30 minutes.

[19] The production method according to any one of [12] to [16] wherein the drying time of the near-infrared to medium-infrared dryer is 5 to 15 minutes.

[20] The production method according to any one of [1] to [19] wherein the sheet for encapsulation after the step (1) has a water content of 500 ppm by weight or less.

[21] The production method according to any one of [1] to [19] wherein the sheet for encapsulation after the step (1) has a water content of 400 ppm by weight or less.

[22] The production method according to any one of [1] to [19] wherein the sheet for encapsulation after the step (1) has a water content of 300 ppm by weight or less.

[23] The production method according to any one of [1] to [19] wherein the sheet for encapsulation after the step (1) has a water content of 250 ppm by weight or less.

[24] The production method according to any one of [1] to [19] wherein the sheet for encapsulation after the step (1) has a water content of 200 ppm by weight or less.

[25] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 2000 ppm by weight or less.

[26] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 1800 ppm by weight or less.

[27] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 1600 ppm by weight or less.

[28] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 1400 ppm by weight or less.

[29] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 1200 ppm by weight or less.

[30] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 1000 ppm by weight or less.

[31] The production method according to any one of [1] to [19] wherein the resin composition layer after the step (1) has a water content of 850 ppm by weight or less.

[32] The production method according to any one of [1] to [31] wherein the drying by the near-infrared to medium-infrared dryer is carried out in a dry air or a dry inert gas atmosphere.

[33] The production method according to the above [32], wherein the amount of water vapor contained in the dried air or the dry inert gas is from 0 to 500 ppm.

[34] The production method according to [32] above, wherein the amount of water vapor contained in the dried air or the dry inert gas is from 0 to 250 ppm.

[35] The production method according to the above [32], wherein the amount of water vapor contained in the dried air or the dry inert gas is from 0 to 100 ppm.

[36] The production method according to the above [32], wherein the amount of water vapor contained in the dried air or the dry inert gas is 0 to 50 ppm.

[37] The production method according to the above [32], wherein the amount of water vapor contained in the dried air or the dry inert gas is 0 to 30 ppm.

[38] The production method according to any one of [1] to [37] wherein the infrared ray from the near-infrared to medium-infrared dryer is irradiated to the sheet for encapsulation from the side of the protective film.

[39] The production method according to any one of [1] to [38] wherein the distance between the light source of the near-infrared to medium-infrared dryer and the sheet for packaging is 5 to 100 cm.

[40] The production method according to any one of [1] to [38] wherein the distance between the light source of the near-infrared to medium-infrared dryer and the sheet for packaging is 10 to 50 cm.

[41] The production method according to any one of [1] to [38] wherein the distance between the light source of the near-infrared to medium-infrared dryer and the sheet for packaging is 10 to 30 cm.

[42] The production method according to any one of [1] to [41] wherein the infrared ray has an irradiation angle of 0 to 80 degrees with respect to the sheet for packaging.

[43] The production method according to any one of [1] to [41] wherein the infrared ray is irradiated to the package sheet at an angle of 0 to 70 degrees.

[44] The manufacturing method according to any one of [1] to [41] wherein the infrared ray has an irradiation angle of 0 to 60 degrees with respect to the sheet for packaging.

[45] The production method according to any one of [1] to [44] wherein the protective film is a polyethylene terephthalate film, a polyethylene naphthalate film, a polypropylene film or a cyclic olefin polymerization. Film.

[46] The production method according to any one of [1] to [44] wherein the protective film is a polyethylene terephthalate film, a polyethylene naphthalate film or a cycloolefin polymer film.

[47] The production method according to any one of [1] to [44] wherein the protective film is a polyethylene terephthalate film.

[48] The production method according to any one of [1] to [47] wherein the protective film has a thickness of 10 to 200 μm.

[49] The production method according to any one of [1] to [47] wherein the protective film has a thickness of 20 to 200 μm.

[50] The production method according to any one of [1] to [47] wherein the protective film has a thickness of 10 to 125 μm.

[51] The manufacturing method according to any one of [1] to [47] wherein the protection The film thickness is 20 to 125 μm.

The manufacturing method of any one of the above [1] to [51], wherein the encapsulation of the organic EL element of the step (2) is performed by bringing the resin composition layer into contact with the organic EL element. It is carried out by laminating the substrate.

[53] The production method according to the above [52], wherein the layer of the step (2) is carried out under an inert gas atmosphere or under vacuum.

According to the method of the present invention, the protective sheet for encapsulating sheets in which the support, the resin composition layer and the protective film are laminated in this order can be removed, and the sheet for packaging can be effectively dried. Further, according to the method of the present invention, the sheet for packaging can be effectively dried even at a relatively low temperature.

[step 1)]

The method of the present invention comprises the step (1) of drying the encapsulating sheet without using a near-infrared to medium-infrared dryer without peeling off the protective film.

(1-1) Near-infrared to medium-infrared dryer

In the present specification, the near-infrared to medium-infrared dryer means a dryer that irradiates near-infrared to mid-infrared. A filament (heat source) used in a light source (heater) of a near-infrared to medium-infrared dryer is exemplified by, for example Tungsten, nickel-chromium alloy, carbon, KANTHAL (registered trademark), etc., preferably tungsten, KANTHAL, and particularly preferably tungsten. In order to effectively dry the resin composition layer, it is preferred to use a dryer capable of irradiating near-infrared to mid-infrared rays having a peak wavelength in the range of 1.0 to 4.0 μm. The peak wavelength is preferably from 1.0 to 3.5 μm, more preferably from 1.25 to 3.5 μm, and even more preferably from 1.5 to 3.5 μm. Further, in the present specification, the near-infrared to mid-infrared region means a wavelength in the range of 0.78 to 4.0 μm, the near-infrared region means a wavelength of 0.78 μm or more and less than 2.0 μm, and the mid-infrared region means a wavelength of 2.0 μm or more. The range of 4.0 μm or less. In the present specification, the near-infrared to mid-infrared rays may be simply referred to as infrared rays, and the near-infrared to medium-infrared dryers may be simply referred to as infrared dryers.

Drying in a near-infrared to medium-infrared dryer is preferably carried out in a dry air or a dry inert gas atmosphere. The inert gas is exemplified by, for example, nitrogen, argon, helium, neon or the like. The amount of water vapor contained in the air or the inert gas is preferably from 0 to 500 ppm (that is, from 0 to 500 μmol/mol), more preferably from 0 to 250 ppm, still more preferably from 0 to 100 ppm, and even more preferably from 0 to 50 ppm. Very good is 0~30ppm.

In order to avoid adverse effects on the resin composition layer and to effectively dry, the drying temperature is preferably 60 to 160 ° C, more preferably 60 to 140 ° C, still more preferably 60 to 130 ° C, and even more preferably 80 to 130 ° C. The temperature is preferably 90 to 130 ° C, and the drying time is preferably 0.5 to 60 minutes, more preferably 1 to 30 minutes, more preferably 5 to 30 minutes, and even more preferably 5 to 15 minutes. The term "drying temperature" as used herein means the surface temperature of the protective film on the resin composition, which can be measured by mounting a surface contact type K thermocouple on the protective film. Again, the so-called drying time It means the time when the surface temperature of the protective film is at a specific drying temperature.

The infrared rays are preferably irradiated from the side of the protective film to the sheet for packaging. In order to effectively dry the package sheet, the distance between the light source (heater) of the near-infrared to medium-infrared dryer and the package sheet is preferably from 5 to 100 cm, more preferably from 10 to 50 cm, even more preferably from 10 to 30 cm. The infrared radiation angle is preferably 0 to 80 degrees, more preferably 0 to 70 degrees, and more preferably 0 to 60 degrees.

When it is conveyed to the infrared dryer, in order to prevent the sheet for packaging, the sheet for packaging is fixed to a glass substrate or the like and conveyed to the infrared dryer and dried.

For drying, a commercially available near infrared to medium infrared dryer can be used. A commercially available near-infrared to mid-infrared dryer is exemplified by, for example, a near-infrared wavelength control system manufactured by NGK INSULATORS, Japan.

(1-2) Package sheets

In the step (1), the sheet for encapsulation in which the support, the resin composition layer, and the protective film are laminated in this order is dried without peeling off the protective film. A conventional packaging sheet can be used as the sheet for packaging.

(1-2-1) Support

The support for the sheet for encapsulation is exemplified by a polyolefin such as polyethylene or polypropylene (PP), a polyester such as polyethylene terephthalate (PET) or polyethylene naphthalate (PEN), or the like. A plastic film of polycarbonate (PC), polyimine (PI), cycloolefin polymer (COP), polyvinyl chloride or the like. The plastic film may be used alone or in combination of two or more. Support body It is preferably a PET film, a PEN film or a COP film, more preferably a PET film.

In order to improve the moisture resistance of the sheet for packaging, a plastic film having a barrier layer may be used as the support. In the sheet for encapsulation, the barrier layer may be brought into contact with the resin composition layer, or the barrier layer may not be in contact with the resin composition layer (that is, on the surface of the support opposite to the surface of the support in contact with the resin composition layer). Form a barrier layer). Examples of the barrier layer include nitrides such as tantalum nitride, oxides such as alumina, and metal foils such as stainless steel foil and aluminum foil. The barrier layer may have a multilayer structure of two or more layers. As the plastic film of the plastic film having the barrier layer, for example, a film of polyethylene terephthalate, polyethylene naphthalate, polycarbonate, cycloolefin polymer or the like is exemplified. The plastic film may have a multilayer structure of two or more layers. Commercially available products can also be used as the plastic film having the barrier layer. A commercially available product of a polyethylene terephthalate film with an aluminum foil is exemplified by "Al (1N30) with PET, manufactured by Tokai Toyo Aluminum Co., Ltd." and "AL3025 with PET" manufactured by Fukuda Metal Co., Ltd., and the like.

For example, when the package obtained by the production method of the present invention is used for a display, a polarizing plate can also be used as a support. Further, the support may be composed of a plurality of layers having different functions such as a plastic film having a barrier layer and a polarizing plate. For example, a plastic film having a barrier layer and a polarizing plate bonded to an adhesive such as an optical adhesive sheet (OCA) can be used as a support. In this case, the sheet for encapsulation is configured such that the plastic film having the barrier layer is in contact with the resin composition layer.

The support may be subjected to mold release treatment or matting by a polyoxymethylene resin release agent, an alkyd resin release agent, a fluororesin release agent, or the like. Management, corona treatment, etc. The thickness of the support is not particularly limited. From the viewpoint of handleability, the lower limit of the thickness of the support is preferably 10 μm, more preferably 20 μm, and the upper limit is preferably 200 μm, more preferably 125 μm. The preferred range of support thickness (i.e., preferred upper and lower limit combinations) is (i) 10 to 200 μm, (ii) 20 to 200 μm, (iii) 10 to 125 μm, and (iv) 20 to 125 μm.

(1-2-2) Protective film

The protective film for the sheet for encapsulation is exemplified as the plastic film of the support. The protective film is preferably a PET film, a PEN film, a PP film or a COP film, more preferably a PET film, a PEN film or a COP film, and more preferably a PET film. The protective film may be subjected to a mold release treatment, a matting treatment, a corona treatment, or the like by a polyoxymethylene resin release agent, an alkyd resin release agent, a fluororesin release agent, or the like. The protective film may have a multilayer structure of two or more layers. The thickness of the protective film is not particularly limited. The lower limit of the thickness of the protective film is preferably 10 μm, more preferably 20 μm, and the upper limit thereof is preferably 200 μm, more preferably 125 μm, from the viewpoints of handleability and drying of the sheet for packaging. The preferred range of the thickness of the protective film (i.e., the preferred upper and lower limit combinations) is (i) 10 to 200 μm, (ii) 20 to 200 μm, (iii) 10 to 125 μm, and (iv) 20 to 125 μm.

(1-2-3) Resin composition layer

The sheet for encapsulation used in the present invention may be a sheet for thermosetting type encapsulation or a sheet for pressure-sensitive adhesive type encapsulation. Here, the sheet for thermosetting type packaging means a sheet for packaging having a thermosetting resin composition layer, After the sheet for encapsulation is laminated with the substrate, it is heated to form a sheet of the cured resin composition layer (encapsulation layer). The pressure-sensitive adhesive-type package sheet means a sheet for encapsulation in which an encapsulating layer has been formed, and a sheet which is not heated after the sheet for encapsulation is laminated with the substrate. The thermosetting resin composition for forming the resin composition layer of the thermosetting type packaging sheet is not particularly limited, and conventional ones such as those described in WO2010/084938 can be used. The resin composition (hereinafter, simply referred to as "the composition of the pressure-sensitive adhesive type") for forming the resin composition layer of the pressure-sensitive adhesive sheet is not particularly limited, and WO2013/108731, WO2011/062167 can be used. Those who have been recorded in the past. The resin composition layer may have a multilayer structure of two or more resin composition layers described in WO2011/016408.

The thermosetting resin composition preferably contains an epoxy resin and a hardener. The epoxy resin and the curing agent are not particularly limited, and those conventionally used can be used. The thermosetting resin composition may also contain a thermoplastic resin.

The composition of the pressure-sensitive adhesive type preferably contains an α-olefin resin and an adhesion-imparting agent. The α-olefin-based resin and the adhesion-imparting agent are not particularly limited, and conventional ones can be used. The α-olefin-based resin is exemplified by a polymer of an α-olefin such as polyethylene or polyisobutylene. The α-olefin resin may also be a copolymer. The copolymer is exemplified by a copolymer of a different α-olefin, a copolymer of an α-olefin and a monomer other than the α-olefin (for example, styrene, a non-conjugated diene, or the like).

The thermosetting resin composition and the composition of the pressure-sensitive adhesive type may each contain an additive. As an additive, for example, hygroscopic metal oxidation An inorganic filler (for example, cerium oxide, mica, talc, etc.) other than a moisture-absorbing metal oxide (for example, calcium oxide or aluminum aluminocarbonate).

[Step (2)]

The method of the present invention comprises the step (2) of encapsulating the organic EL element with a resin composition layer of the encapsulating sheet after peeling off the protective film from the dried package sheet. In order to utilize the effect of the step (1), the step (2) is preferably carried out in the same manufacturing line as the step (1). Further, for the same reason, the step (1) to the step (2) are preferably within 60 minutes. For the same reason, it is preferable to carry out the step (2) following the step (1) (in detail, after the step (1), the step (2) is performed without performing other steps.

(2-1) Substrate

The substrate used in the present invention is not particularly limited, and a conventional one can be used. The substrate is preferably glass, indium tin oxide (ITO)-containing glass, polyimine (PI), polyethylene terephthalate (PET), polyethylene naphthalate (PEN), polycarbonate. At least one selected from the group consisting of an ester (PC) and a cyclic olefin polymer (COP). The thickness of the substrate is preferably from 0.1 to 1.0 mm, more preferably from 0.1 to 0.7 mm. The thickness of the organic EL element is preferably from 0.01 to 1 μm, more preferably from 0.05 to 0.5 μm.

The organic EL element may have another structure for suppressing deterioration due to moisture. For example, a passivation film can also be formed on the organic EL element. In this case, the sheet for encapsulation starts to be laminated from the passivation film. The passivation film is not particularly limited, and for example, an inorganic film of SiN, SiON, SiO ₂ , Al ₂ O ₃ or TiO ₂ formed by sputtering, CVD or the like; an acrylic resin, a polyamidene-based PARYLENE or the like can be used. A polymer film, a laminated film having a multilayer structure in which an inorganic film is laminated, and the like, and a conventional passivation film. The thickness of the passivation film is not particularly limited, and is preferably 1 to 3 μm.

In order to extract light from the organic EL element, any of the support of the substrate and the sheet for packaging must be transparent. For example, when an opaque support (for example, a plastic film having an opaque barrier layer) is used for a sheet for packaging, a transparent substrate must be used in order to extract light from the substrate side.

(2-2) package

The package is formed by laminating the package sheet and the substrate so that the resin composition layer is in contact with the organic EL element. Moreover, the organic EL element as described above also includes an organic EL element having another structure for suppressing deterioration. For example, when the organic EL device has a passivation film, the "resin composition layer is in contact with the organic EL device" means "the resin composition layer is in contact with the passivation film of the organic EL device".

In order to prevent the dried package sheet from adsorbing moisture again, it is preferred to quickly package the substrate having the organic EL element with the resin composition layer of the package sheet after drying in the step (1). The time from the drying of the step (1) to the start of the packaging of the step (2) is preferably from 1 to 60 minutes, more preferably from 1 to 30 minutes, more preferably from 1 to 15 minutes, if it is in an atmosphere. Good for 1~10 minutes. Here, the "start of the package of the step (2)" means the resin composition of the sheet for packaging after the protective film is peeled off from the sheet for packaging. The point at which the layer is in contact with the organic EL element.

In order to prevent moisture from being adsorbed to the resin composition layer of the dried packaging sheet, the encapsulation is preferably carried out under an inert gas atmosphere or under vacuum. As the inert gas, for example, nitrogen, argon, helium, neon or the like is exemplified. The ambient pressure (inert gas pressure) at the time of encapsulation in an inert gas atmosphere is preferably about 1 × 10 ⁵ Pa. The surrounding pressure (decompression degree) at the time of encapsulation under vacuum is preferably from 1 to 1 × 10 ³ Pa, more preferably from 1 to 1 × 10 ² Pa.

The apparatus used for the lamination is not particularly limited, and a conventional one such as a roll laminator, a press machine or the like can be used. It is also possible to use a plurality of devices such as a roll laminator and a press machine in combination.

(2-2-1) Roller laminating machine

When the roll laminator is used, the speed of the roll is preferably from 10 to 1,500 mm/min, more preferably from 100 to 500 mm/min, in order to achieve good adhesion of the resin composition layer to the support.

The roll pressure of the roll laminator is preferably from 0 to 0.5 MPa, more preferably from 0 to 0.3 MPa, in order to avoid damage to the organic EL element. The term "rolling pressure" as used herein means the pressing force of the air cylinder, which is expressed by gauge pressure (original pressure). The so-called roll pressure of 0 means that the pressing force is zero. When the roll pressure is 0, after laminating by a roll laminator, it is preferred to pressurize the laminated body with a press machine described later.

The roll temperature of the roll laminator is preferably 30 to 120 ° C, more preferably 40 to 110 ° C, and even more preferably 50 to 100 ° C in order to soften the resin composition layer and improve the followability to the substrate. Here, the roll temperature means that the heater is built in the roll, and the temperature of the surface of the digitally controlled roll can be surface contact type. K thermocouple measurement.

A commercially available roll laminator can be used for lamination. The commercially available roll laminating machine is exemplified by, for example, "LPD2325" manufactured by FUJIPLA Co., Ltd., "roller laminator VA770H" manufactured by Daewoo LAMINATOR Co., Ltd., "roller laminator VA700", "roller laminator VAII-700", and "Bodong Co., Ltd." Mach630up" and so on. The material of the roll as the roll laminator is, for example, stainless steel, rubber or the like, and is preferably ruthenium rubber.

(2-2-2) Pressing machine

When the press machine is used, the pressurization is preferably 0.01 to 0.5 MPa, more preferably 0.01 to 0.3 MPa, in order to prevent cracking of the EL element due to pressure. The pressurization of the press machine herein means the pressure applied to the body to be pressed (that is, the pressure applied to the surface of the sheet for packaging) controlled by a vacuum hydraulic cylinder or a load.

The pressurizing temperature of the press machine is preferably 30 to 120 ° C, more preferably 40 to 120 ° C, more preferably 50 to 110 ° C, and even more preferably 60 to 100 ° C, and the pressurization time is preferably 20~ 450 seconds, preferably 60 to 300 seconds. Here, the pressurization temperature of the press means that the surface of the pressurizing portion of the press machine (for example, a flat plate such as a metal plate) has a built-in helium heater, and the temperature of the surface of the pressurization portion of the digital position can be controlled by surface contact type K thermoelectricity. Even measured.

For lamination, a commercially available press machine can be used. The commercially available press machine is, for example, a "plate type vacuum pressure laminator CVP-300" manufactured by MOTON Corporation, and a flat press machine such as a vacuum pressurizing machine "VHI-2051" manufactured by Kitagawa Seiki Co., Ltd. The material of the flat plate for pressurization is exemplified by, for example An alloy of stainless steel or iron, preferably stainless steel.

(2-3) Hardening of the resin composition layer

When a thermosetting type packaging sheet is used, the laminated body of the packaging sheet and the substrate is heated and cured to form a resin composition layer (that is, an encapsulating layer). The hardening can be carried out using, for example, a hot air circulating oven, an infrared heater, a heat gun, a high frequency induction heating device, a heating plate, or the like. In order to laminate and heat-pressurize using a press machine, the hardening of the laminate and the resin composition layer can be simultaneously performed. The curing temperature varies depending on the resin composition layer and the support used, but is preferably 80 to 120 ° C, more preferably 80 to 110 ° C, and the hardening time is preferably 10 to 120 minutes, more preferably 10 to 60 minutes. . The thickness of the hardened resin composition layer formed is preferably from 3 to 200 μm, more preferably from 5 to 150 μm, still more preferably from 10 to 100 μm.

When a pressure-sensitive adhesive sheet for packaging is used, the resin composition layer can be cured by heating the packaging sheet before laminating the packaging sheet and the substrate. However, after the lamination of the package sheet and the substrate, the film may be further heated. When the laminated sheet for pressure-sensitive bonding is heated after lamination, the heating temperature is preferably from 50 to 150 ° C, more preferably from 60 to 100 ° C, and still more preferably from 60 to 90 ° C in order to avoid thermal deterioration of the organic EL element.

The moisture of the sheet for encapsulation can be measured by a Karl Fischer moisture measuring device under the conditions described in Test Example 1 described later. The moisture content of the sheet for encapsulation can be calculated from the moisture (weight) measured and the weight of the sheet for packaging based on the following formula.

Water content (weight ppm) of the sheet for packaging = (measured moisture) / (weight of package sheet) × 10 ⁶

The moisture content of the sheet for encapsulation after the step (1) is preferably 500 ppm by weight or less, more preferably 400 ppm by weight or less, still more preferably 300 ppm by weight or less, particularly preferably 250 ppm by weight or less, more preferably 200% by weight. Below ppm.

Further, since the moisture contained in the sheet for encapsulation is considered to be contained only in the resin composition, the evaluation of the water content is preferably based on the assumption that the water is contained only in the resin composition layer, and is included in the resin composition layer. The value of the moisture content is carried out. The water content of the resin composition layer can be calculated from the following formula by the water content (weight) of the packaging sheet, the weight of the packaging sheet, and the weight ratio of the resin composition layer.

Water content (weight ppm) of the resin composition layer = (measured moisture) / (weight of package sheet × weight ratio of resin composition layer) × 10 ⁶

The weight ratio of the resin composition layer used in the above formula can be calculated, for example, by measuring the weight of the other layers such as the support and the protective film in the sheet for packaging.

Weight ratio of resin composition layer = (weight of package sheet - other layer weight) / weight of package sheet

The water content of the resin composition layer after the step (1) is preferably 2,000 ppm by weight or less, more preferably 1800 ppm by weight or less, still more preferably 1600 ppm by weight or less, still more preferably 1400 ppm by weight or less, and further preferably. It is 1200 ppm by weight or less, particularly preferably 1000 ppm by weight or less, and most preferably 850 ppm by weight or less.

[Examples]

The present invention will be more specifically described by the following production examples, test examples and examples, but the invention is not limited thereto.

Production Example 1: Manufacturing of Sheet 1 for Thermosetting Type Packaging

56 parts by weight of a liquid bisphenol A type epoxy resin ("jER828EL" manufactured by Mitsubishi Chemical Corporation, epoxy equivalent: about 185 g/eq), and 1.2 parts by weight of decane coupling agent ("KBM403" manufactured by Shin-Etsu Chemical Co., Ltd.), talc 2 parts by weight of powder ("FG-15" manufactured by Japan TALC Co., Ltd.) and 15 parts by weight of calcined aluminum magnesium carbonate ("Ki 2200" manufactured by Kyowa Chemical Co., Ltd.) were kneaded, and then dispersed in a 3-roll mixer to obtain a mixture.

1.5 parts by weight of a hardening accelerator ("U-3512T" manufactured by SUN APRO Co., Ltd.) was dissolved in a methyl ethyl ketone (MEK) solution of phenoxy resin ("YL7213B35" manufactured by Mitsubishi Chemical Corporation, concentration: 35 wt%) 81 In the mixture of parts by weight (phenoxy resin: 28.4 parts by weight), the mixture prepared by dispersing in a 3-roll mixer, solid bisphenol A type epoxy resin ("JER1001" manufactured by Mitsubishi Chemical Corporation, epoxy equivalent) was prepared. : about 475 g/eq) MEK solution (concentration: 80% by weight) 30 parts by weight, organic solvent-dispersed colloidal cerium oxide (particle size of cerium oxide: 10 to 15 nm, solid content: 30% by weight, MEK solvent, Nissan Chemical Industry Co., Ltd. 20 parts by weight of "MEK-EC-2130Y") and 3 parts by weight of an ionic liquid hardener (tetrabutylphosphonium N-acetamidoglycolate) were uniformly dispersed in a high-speed rotary mixer to obtain a resin composition paint.

Plastic film with barrier layer (Al (1N30) with PET made by Tokai Toyo Aluminum Co., Ltd.), plastic film: 25μm thick A polyethylene terephthalate (PET) film, a barrier layer: an aluminum foil having a thickness of 30 μm) was used as a support, and the obtained resin composition paint was applied to a mold by drying the resin composition to a thickness of 20 μm. The cloth machine was uniformly coated on the barrier layer of the support, and dried at 80 to 100 ° C (average 90 ° C) for 5 minutes (the amount of residual solvent in the resin composition layer: 2% by weight).

A PET film having a thickness of 38 μm treated with an alkyd-based release agent was used as a protective film, and it was wound into a roll shape while being bonded to the surface of the resin composition layer. The sheet-like package sheet was cut into a width of 507 mm to obtain a sheet 1 for packaging (horizontal: 507 mm, vertical: 336 mm).

Production Example 2: Manufacturing of the sheet 2 for pressure-sensitive adhesive type packaging

20 parts by weight of a hydrogenated alicyclic petroleum resin ("Escorez 5340" manufactured by EXXON MOBIL Co., Ltd.) and liquid polyisobutylene (41 parts by weight of a polyisobutylene ("Oppanol B100" manufactured by BASF Corporation, 33% by weight of IPSOL 150 solution). 9 parts by weight of a maleic anhydride-modified isobutylene ("HV-300M" manufactured by Nippon Oil Co., Ltd.) of 5 parts by weight of "Tetrax 3T" manufactured by Nippon Oil Co., Ltd.) was uniformly dispersed in a high-speed rotary mixer to obtain a mixed solution. In the mixed solution, 5.3 parts by weight of an epoxy resin ("HP7200H" manufactured by DIC Corporation, 50% by weight of IPSOL 150 solution) and an anionic polymerization type hardener (2,4,6-cis (dicyanomethyl)phenol) were mixed. 0.6 parts by weight, uniformly obtained by a high-speed rotary mixer to obtain a paint.

Plastic film with barrier layer (Al (1N30) with PET from Tokai Toyo Aluminum Co., Ltd.), plastic film: polyethylene terephthalate (PET) film with a thickness of 25 μm, barrier layer: aluminum foil with a thickness of 30 μm As a support, the obtained paint is dried to a resin composition layer thickness In the form of 20 μm, it was uniformly applied by a die coater, dried at 80 ° C for 30 minutes, and heat-cured at 130 ° C for 30 minutes to obtain a resin composition sheet. A PET film having a thickness of 30 μm which was treated with a polyfluorene-based release agent was used as a protective film, and was bonded to the surface of the resin composition layer to be wound into a roll shape. The sheet-like package sheet was cut into a width of 507 mm to obtain a sheet 2 for packaging (horizontal: 507 mm, vertical: 336 mm).

Production Example 3: Manufacture of pressure-sensitive adhesive type package sheet 3

Polypropylene/polybutylene copolymer modified by maleic anhydride ("T-YP279" manufactured by Starlight PMC Co., Ltd., propylene unit/butene unit = 64% by weight/36% by weight, maleic anhydride group concentration: 0.464 mmol/g , a number average molecular weight of 35,000, a random copolymer, 40% by weight of a SWASOL solution), 20 parts by weight, and 14 parts by weight of calcined aluminum magnesium carbonate ("DHT-4C" manufactured by Kyowa Chemical Industry Co., Ltd.) were mixed and mixed by a 3-roll mixer. 50 parts by weight of a purified hydrocarbon resin ("TFS13-030", manufactured by Arakawa Chemical Co., Ltd., 60% by weight toluene solution) containing a cyclohexyl ring was mixed with a high-speed rotary mixer to obtain a homogeneous mixed solution. A propylene/polybutylene copolymer modified with glycidyl methacrylate obtained from the obtained mixed solution (T-YP276 manufactured by Starlight PMC Co., Ltd., propylene/polybutylene copolymer modified with glycidyl methacrylate, propylene) Unit / butene unit = 64% by weight / 36% by weight, glycidyl group concentration 0.638mmol / g, number average molecular weight 57000, inorganic copolymer, 40% by weight SWASOL solution) 14 parts by weight with anionic polymerization type hardener (2, 0.5 parts by weight of 4,6-gin(dicyanomethyl)phenol) was uniformly dispersed in a high speed rotary mixer to obtain a paint.

Use plastic film with barrier layer (Tokai Toyo Aluminum Sales The company's "Al (1N30) with PET", plastic film: polyethylene terephthalate (PET) film with a thickness of 25μm, barrier layer: aluminum foil with a thickness of 30μm) as a support, the resulting paint is dried. The resin composition had a layer thickness of 30 μm, was uniformly applied by a die coater, dried at 80 ° C for 30 minutes, and heat-cured at 130 ° C for 60 minutes to obtain a resin composition sheet. A 38 μm-thick PET film treated with a polyoxymethylene-based release agent was used as a protective film, and it was wound into a roll shape while being bonded to the surface of the resin composition layer. The sheet-like package sheet was cut into a width of 507 mm to obtain a sheet 3 for packaging (horizontal: 507 mm, vertical: 336 mm).

Test Example 1: Calculation of moisture content of dried package sheet and resin composition layer

Infrared dryer ("Near Infrared Wavelength Control System" manufactured by NGK INSULATORS, Japan, filament: KANTHAL or Tungsten), hot air dryer ("Precision Thermostat" manufactured by YAMATO Scientific Co., Ltd.) or vacuum dryer (manufactured by YAMATO Scientific Co., Ltd.) The square vacuum dryer", the degree of pressure reduction: 100 Pa), and the temperature and time shown in the following Tables 1 to 3, the package sheets 1 to 3 obtained as described above were dried by peeling off the protective film or not peeling off the protective film.

The drying by the infrared dryer was carried out by irradiating the infrared rays from the protective film side to the encapsulating sheet in a nitrogen atmosphere (water vapor amount: 20 ppm or less). The peak wavelength of the infrared ray irradiated from the infrared ray dryer is about 3 μm when the filament is KANTHAL, and is about 1.5 μm when the filament is tungsten. Further, the infrared rays used for drying the packaging sheets 1 and 3 The filament of the dryer is KANTHAL. The filament of the infrared dryer used for drying the encapsulating sheet 2 is tungsten. Further, the distance between the light source (heater) of the infrared dryer and the sheet for packaging is adjusted to 15 cm, and the irradiation angle of the infrared ray is adjusted to 0 to 60 degrees.

After drying, the packaged sheets 1 to 3 were cut out (cross: about 100 mm, vertical: about 100 mm, weight: 100 to 300 mg), and the protective film was peeled off. The Karl Fischer moisture measuring device using the electric quantity titration method (Mitsubishi Chemical Analysis) The company's "micro moisture measuring device CA-200") measures the moisture content of the sheet for packaging. The apparatus is composed of a glass container provided with a heatable sample and a titration device filled with a reaction liquid for titrating vaporized water while heating the sample. The vaporized moisture is moved from the glass container to the reaction liquid side of the titration device by a flow rate of 250 ± 25 ml/min of nitrogen. The measurement was carried out by placing a sample in a glass container replaced with a nitrogen atmosphere (water vapor amount < 0.1 ppm), measuring the moisture vaporized at 130 ° C, and calculating the water content of the package sheet and the moisture content of the resin composition layer. . The results are shown in Tables 1 to 3 below.

Test Example 2: Encapsulation evaluation test of Ca film for dried package sheets

A glass substrate in which a Ca film was formed instead of the organic EL element was subjected to a simulation test of the organic EL element package, and the packageability of the package sheet for drying was evaluated.

In detail, first, a Ca film is formed on a glass substrate (thickness: 700 μm, horizontal: 50 mm, vertical: 50 mm) to form a Ca film (thickness: about 300nm, horizontal: 40mm, vertical: 40mm). The obtained glass substrate had a package width of 5 mm around the Ca film (that is, a width in which the glass substrate in which the Ca film was not formed was in contact with the sheet for packaging).

Next, the package sheets 1 to 3 (horizontal: 50 mm, vertical: 50 mm) described in Test Example 1 were dried at the temperatures and times shown in Tables 1 to 3 below, and dried for 180 seconds to form a resin composition layer and Ca. In a film contact manner, a sheet for encapsulation and a glass substrate are laminated, and a Ca film is encapsulated. This laminate was produced under the conditions of a nitrogen atmosphere using a roll laminator ("LPD2325" manufactured by FUJIPLA Co., Ltd., roll material: rubber) at a roll temperature of 90 ° C, a roll speed of 360 mm/min, and a roll pressure of 0.2 MPa. In addition, when the thermosetting type packaging sheet 1 is used, a laminate (available from AS-2 ONE "HP-2SA") is used, and the laminate of the packaging sheet and the glass substrate is heated at 110 ° C for 30 minutes in an atmosphere to form a resin. The layer is thermally hardened.

The laminate of the package sheet and the glass substrate obtained as described above was placed in an accelerated tester ("Small Environmental Tester SH-222" manufactured by ESPEC Co., Ltd., temperature: 60 ° C, humidity: 90% RH), by Ca (opaque) In the reaction of +2H ₂ O→Ca(OH) ₂ (transparent), the time for which the opaque Ca film was reduced by 5 mm (starting reduction time) was measured as a packageability index of the sheet for encapsulation, and the following criteria were evaluated. The longer the shrinking time is started, the more excellent the encapsulation property of the package sheet is. The results are shown in Tables 1 to 3 below.

○: The reduction time is 600 hours or more.

△: The start reduction time was 300 hours or more and less than 600 hours.

×: The reduction time was less than 300 hours.

Moreover, when the sheet 1 for thermosetting type packaging is used, the resin group After the layer of the layer was thermally hardened, the surface of the Ca film was visually observed and evaluated by the following criteria. Moreover, the surface of the Ca film when the package sheet 3 of the pressure-sensitive adhesive type was used was visually observed, and evaluated by the following criteria. The results are shown in Tables 1 and 3 below.

○: The surface of the Ca film did not change before and after the encapsulation, and the silvery luster of the mirror surface was observed.

△: The silvery luster on the surface of the Ca film became dull, and the discoloration was gray.

×: The Ca film disappeared, and many irregularities were observed when viewed from the substrate side.

As shown in Table 1, the unsealed packaging sheet 1 (No. 1-5, moisture content of the sheet for packaging: 1290 ppm by weight) or the encapsulating sheet 1 which was dried by a vacuum dryer without peeling off the protective film (No) In the package evaluation test of .1-4, the moisture content of the sheet for packaging: 768 ppm by weight), the surface of the Ca film on the glass substrate was deteriorated after the resin composition layer was cured. In the encapsulation evaluation test of the package sheet 1 (No. 1-3, moisture content of the package sheet: 511 ppm by weight) which was dried by a hot air dryer (100 ° C, 5 minutes) without peeling off the protective film, the resin was used. The surface of the Ca film on the glass substrate is slightly deteriorated after the composition layer is hardened. It is taught from these results that the packaging sheet having a water content of more than 500 ppm by weight is not suitable for packaging.

In addition, as shown in Table 1, the encapsulating sheet 1 (No. 1-2) which was dried by using a hot air dryer (100 ° C, 5 minutes) and dried, had a water content of 153 ppm by weight and started to shrink over 600 times. Hours, water content and encapsulation are good. However, when the protective film is peeled off, the resin composition layer is contaminated during drying, and as a result, the organic EL element is adversely affected.

Moreover, as shown in Table 1, the moisture content of the package sheet 1 (No. 1-1) can be reduced to 75 by using a near-infrared to medium-infrared dryer (100 ° C, 5 minutes) without peeling off the protective film. Weight ppm. This presumption is that the moisture of the protective film and the resin composition layer is excited by the near-infrared irradiation, and is evaporated by the protective film.

As shown in Table 2, the undried packaging sheet 2 (No. 2-5) had a high water content of 2,900 ppm by weight, which was suggested to be unsuitable for packaging. Moreover, the moisture content (No. 2-4) of the encapsulating sheet 2 which was dried by using a hot air dryer (100 ° C, 5 minutes) without peeling off the protective film was 1131 ppm by weight, and the shrinking time was short. Less than 300 hours.

Further, as shown in Table 2, by using a hot air dryer to dry at a high temperature (No. 2-2, 130 ° C) or a long time (No. 2-3, 840 minutes = 14 hours), even if the protective film is not peeled off, The moisture content of the encapsulating sheet can also be reduced, and the encapsulation property can be improved. However, high-temperature drying has an adverse effect on the resin composition layer, and the drying efficiency is poor for a long period of time.

Moreover, as shown in Table 2, by using a near-infrared to medium-infrared dryer (110 ° C, 5 minutes), even if the protective film is not peeled off, The moisture content of the sheet 2 (No. 2-1) can also be reduced to 31 ppm by weight. From this result, it is understood that drying using a near-infrared to medium-infrared dryer is useful not only for a sheet for thermosetting type packaging but also for a sheet for packaging of a pressure-sensitive adhesive type.

As shown in Table 3, the undried packaging sheet 3 (No. 3-6, moisture content of the sheet for packaging: 3890 ppm by weight, moisture content of the resin composition layer: 18507 ppm by weight) or the non-peeling protective film was used. Encapsulation evaluation test of the packaged sheet 3 (No. 3-3, moisture content of the package sheet: 1114 ppm by weight, resin composition layer moisture content: 5433 ppm by weight) of a hot air dryer (130 ° C, 30 minutes) In the middle, the surface of the Ca film on the glass substrate is deteriorated. From these results, it is taught that the packaging sheet having a water content of the resin composition layer of more than 2000 ppm by weight is not suitable for packaging.

Further, as shown in Table 3, by using a hot air dryer to dry for a long period of time (No. 3-4, 130 ° C, 60 minutes), the moisture content of the sheet for packaging can be reduced to some extent without peeling off the protective film. The drying efficiency is deteriorated, and there is a tendency that the package performance is not easily improved.

In addition, as shown in Table 3, the package sheet 3 (No. 3-1 and No. 3-2) was applied in a short time (10 to 30 minutes) by using a near-infrared to medium-infrared dryer without peeling off the protective film. The water content can also be reduced to 57-64 ppm by weight, and the moisture content of the resin composition layer can be reduced to 272-307 ppm by weight, which can improve the packaging performance.

Test Example 3: Evaluation of Packaging Performance of Organic EL for Dry Packaging Sheets Price test

The encapsulation properties of the dried package sheets were evaluated using an organic EL device.

Specifically, an organic EL device (organic film thickness: 110 nm, Al cathode thickness: 100 nm) was formed on a glass substrate (manufactured by GEOMATEC Co., Ltd.) containing indium tin oxide (ITO) so as to have a light-emitting area of 4 mm ² .

Next, the encapsulating sheet 1 or 3 (horizontal: 15 mm, vertical: 25 mm) described in Test Example 1 was dried at a temperature and time shown in the following Tables 4 and 5, and dried for 180 seconds to form a resin composition and organic. The EL element is contacted in such a manner that the package sheet is laminated with the ITO-attached glass substrate and the organic EL element is packaged. This laminate was produced under the conditions of a nitrogen atmosphere using a roll laminator ("LPD2325" manufactured by FUJIPLA Co., Ltd., roll material: rubber) at a roll temperature of 90 ° C, a roll speed of 360 mm/min, and a roll pressure of 0.2 MPa. In the case of using the thermosetting type packaging sheet 1, a heating sheet ("HP-2SA" manufactured by AS ONE Co., Ltd.) was used, and the resin sheet and the glass substrate were heated at 110 ° C for 30 minutes in a nitrogen atmosphere to heat the resin composition. hardening.

The light-emitting surface of the organic EL element packaged in the package sheet 1 thus obtained was observed at a magnification of 100 times with a CCD camera (manufactured by KYENCE Co., Ltd.), and the ratio of the dark spots immediately after the package in the entire volume of the light-emitting surface was measured and evaluated. Here, the dark spot means a non-light-emitting portion which is generated when the element comes into contact with moisture. The smaller the ratio of the dark spots, the more excellent the packaging performance of the package sheet. The results are shown in Table 4.

○: The ratio of dark spots is less than 1.0%

△: The ratio of dark spots is 1.0% or more and less than 5.0%

×: The ratio of dark spots is 5.0% or more

When the sheet 3 for the pressure-sensitive adhesive type is used, first, the light-emitting surface of the organic EL element packaged by the package sheet obtained as described above is observed at a magnification of 100 times by a CCD camera before the acceleration test described later, and the measurement is performed. Its light-emitting area (initial light-emitting area). Next, the sheet for encapsulation was heated at 85 ° C for 100 hours in a nitrogen atmosphere to carry out a deterioration acceleration test. The light-emitting surface of the organic EL element after the accelerated test was observed at a magnification of 100 times by a CCD camera, and the light-emitting surface area (light-emitting residual area) of the light emission was also measured after the acceleration test. The ratio of the remaining light-emitting area is calculated based on the following formula from the initial light-emitting area and the remaining light-emitting area measured as described above.

Ratio of residual area of light emission (%) = initial light-emitting area / residual light-emitting area × 100

The results are shown in Table 5 below.

○: The ratio of the remaining area of light emission is 70% or more

△: the ratio of the remaining area of the luminescence is 50% or more and less than 70%

×: the proportion of the remaining area of the luminescence is less than 50%

As shown in Table 4, the uncured package sheet 1 (No. 1-10, moisture content of the package sheet: 1290 ppm by weight) or the package sheet 1 dried by the hot air dryer without peeling off the protective film (No) In the package evaluation test of .1-9, moisture content of the package sheet: 511 ppm by weight, the light-emitting surface of the organic EL element immediately after the package had a large number of dark spots. In the same manner as in the test example 2 in which the Ca film was used, the package sheet having a water content of more than 500 ppm by weight was not suitable for packaging, but this test example using an organic EL element was also used.

Further, as shown in Table 4, the sealing sheet 1 (No. 1-8) which was dried by using a hot air dryer (100 ° C, 10 minutes) and dried, and the moisture content of the sheet for encapsulation was 107 ppm by weight. The dark spots existing on the light-emitting surface of the organic EL element after encapsulation are small. However, when the protective film is peeled off and dried, the resin composition is contaminated during drying, and as a result, there is a possibility that the organic EL element is adversely affected.

Further, as shown in Table 4, by using a near-infrared to medium-infrared dryer (90 ° C, 5 minutes to 10 minutes), the package sheet 1 (No. 1-6 and No. 1) was not peeled off even if the protective film was not peeled off. 7) The water content can also be reduced to 150 ppm by weight. When these organic EL elements are packaged, the ratio of dark spots is small, and the package can be well packaged.

As shown in Table 5, the uncured package sheet 3 (No. 3-12, moisture content of the package sheet: 2900 ppm by weight) or the package sheet 3 which was dried for a short time without using a hot air dryer without peeling off the protective film was used. (No. 3-10, moisture content of the sheet for packaging: 710 ppm by weight) In the package performance evaluation test, the ratio of the remaining area of the light emission was greatly lowered. the result It is considered that the drying is insufficient, and therefore, the sealing sheet 3 has moisture remaining, and the organic EL element is deteriorated.

Further, as shown in Table 5, the package sheet 3 (No. 3-7 and No. 3) was used without using a protective film by using a near-infrared to medium-infrared dryer (130 ° C, 5 minutes to 10 minutes). 8) The water content can also be reduced to about 100 ppm by weight. From the results, it is understood that the drying using the near-infrared to medium-infrared dryer is useful not only for the sheet for thermosetting type packaging but also for the sheet for packaging of the pressure-sensitive adhesive type.

[Industrial Applicability]

According to the method of the present invention, the protective sheet can be effectively dried without peeling off the protective film of the sheet for encapsulation in which the support, the resin composition layer and the protective film are laminated in this order. Therefore, the method of the present invention can be used for producing a package (particularly an organic EL device) of an organic EL element on a substrate packaged with a resin composition layer.

The present application is based on Japanese Patent Application No. 2015-058486, the entire contents of which is incorporated herein by reference.

Claims (10)

A manufacturing method for manufacturing a package of an organic EL element on a substrate by a resin composition layer, comprising the steps of: (1) providing a support, a resin composition layer, and a cover film; The encapsulating sheet laminated in this order, the step of drying the near-infrared to medium-infrared dryer without peeling off the protective film, and (2) peeling off the protective film from the dried packaging sheet, and then forming the resin composition for the encapsulating sheet The step of encapsulating the organic EL element. The manufacturing method of claim 1, wherein the step (2) is carried out in the same manufacturing line as the step (1). The manufacturing method of claim 1 or 2, wherein the step (1) is carried out in the following step (1). The manufacturing method according to any one of claims 1 to 3, wherein the time from the drying of the step (1) to the start of the packaging of the step (2) is from 1 to 60 minutes. The manufacturing method according to any one of claims 1 to 4, wherein a peak wavelength of the near infrared ray to the middle infrared ray irradiated from the near infrared ray to the medium infrared ray dryer is in a range of 1.0 to 3.5 μm. The manufacturing method according to any one of claims 1 to 5, wherein the drying temperature of the near-infrared to medium-infrared dryer is 60 to 160 ° C, and the drying time is 0.5 to 60 minutes. The manufacturing method of claim 6, wherein the drying temperature of the near-infrared to medium-infrared dryer is 60 to 130 °C. The manufacturing method of any one of claims 1 to 6, wherein the step (1) The water content of the sheet for encapsulation is 500 ppm by weight or less. The production method according to any one of claims 1 to 6, wherein the resin composition layer after the step (1) has a water content of 2000 ppm by weight or less. The manufacturing method according to any one of claims 1 to 9, wherein the encapsulation of the organic EL device of the step (2) is carried out by laminating the encapsulating sheet and the substrate such that the resin composition layer is in contact with the organic EL element.