KR20220147889A - Adhesive film for organic electronic device encapsulation using melt-extrusion resin composition, organic electronic device encapsulation material and its preparation method using the same - Google Patents

Abstract

Disclosed is a melt-extruded resin layer which is obtained by directly melting and extruding a melt-extruded resin composition including an oxygen absorbent on a metal layer, and specifically, to an adhesive film for an organic electronic device encapsulant including a melt-extruded resin layer including an oxygen absorbent and a moisture absorbent, an organic electronic device encapsulant using the same, and a method for producing the same. According to the present invention, an adhesive film for an organic electronic device encapsulant or an encapsulant can effectively block moisture and/or gas such as oxygen while increasing adhesion. Accordingly, problems such as adhesion deterioration caused by a moisture absorbent of a conventional encapsulant adhesive film, deterioration in interfacial adhesion of an adhesive layer, and deterioration in reliability caused by oxygen and/or moisture penetration can be prevented. In addition, a T-Die device for extrusion coating is utilized to directly melt and extrude a melt-extruded resin composition onto a metal layer, preferably an anchor-coated metal layer so as to reduce the possibility of interfacial separation and increase adhesion while making a manufacturing process easy and fast. Accordingly, even when novel materials that are different from those used in the manufacture of existing organic electronic device encapsulants are utilized, it is possible to achieve process shortening, increase the production speed, and lower manufacturing costs such that products' price competitiveness can be increased.

Description

TECHNICAL FIELD Adhesive film for organic electronic device encapsulation using melt-extrusion resin composition, organic electronic device encapsulation material and its preparation method using the same}

The present specification provides an adhesive film for an organic electronic device encapsulant comprising a melt-extrusion resin layer, in particular, a melt-extrusion resin layer imparted with oxygen absorption and/or moisture barrier properties, an organic electronic device encapsulant using the same, and a method for manufacturing the same, the organic electronic device It relates to a method for encapsulating an organic electronic device using a device encapsulant and an organic electronic device.

Compared to conventional displays such as LCDs, currently commercialized OLEDs have a simple structure due to self-luminescence, which reduces the number of panel components by half, and has various advantages such as colors close to natural colors, high contrast ratio, and reduced power consumption. The market needs are shifting to OLED.

However, OLED has a fatal problem of being vulnerable to moisture and gas, and various encapsulation technologies have been developed to overcome this problem. Thin Film Encapsulation (TFE) is performed on small and medium-sized OLEDs such as smartphones. Thin film encapsulation (TFE) is a multilayer structure in which an inorganic layer and an organic layer on a thin film formed by inkjet are overlapped with each other, and the inorganic layer mainly prevents the inflow of oxygen or moisture to protect the OLED material. As a method of forming an inorganic layer for thin film encapsulation (TFE), there is a method using plasma CVD (PECVD) or Atomic Layer Deposition (ALD). is being used

On the other hand, in large displays such as TVs, a metal thin barrier layer and an OLED panel are attached for thin film encapsulation, but an encapsulation adhesive film for OLED for removing moisture and gas generated in the OLED panel and an encapsulant containing the same are used. Currently being adopted, the encapsulant and encapsulation technology that prevent material deterioration by moisture or oxygen play an important role in greatly affecting the light emitting characteristics and lifespan of OLED panels.

The conventional encapsulation adhesive film for OLED is generally composed of an adhesive layer containing a desiccant for removing moisture.

1A is a schematic diagram showing an example of an adhesive film for a conventional organic electronic device encapsulant, and FIG. 1B is a schematic diagram showing another example of a conventional adhesive film for an organic electronic device sealing material.

As shown in FIG. 1, the conventional adhesive film for an organic electronic device encapsulant includes a single adhesive layer 2 containing a moisture absorbent (FIG. 1a) or an adhesive layer 1 that does not contain a moisture absorbent on the side of the organic electronic device element. ) is located and the adhesive layer 2 containing a moisture absorbent is located on the metal layer.

A large amount of desiccant powder, which is mainly a metal oxide or metal salt, is used as such a desiccant. As a result, the adhesion with the substrate such as the metal layer that meets the adhesive film is deteriorated, which can cause reliability problems such as rapid moisture penetration in the initial stage. have.

Korean Patent No. 1293803

In exemplary embodiments of the present invention, in one aspect, an adhesive film for an organic electronic device encapsulant comprising a melt-extrusion resin layer, particularly a melt-extrusion resin layer imparted with oxygen absorption and/or moisture barrier properties, and an organic electronic device using the same An object of the present invention is to provide an encapsulant and a method for manufacturing the same.

In exemplary embodiments of the present invention, in another aspect, a decrease in adhesion with a substrate such as a metal layer that meets an adhesive film generated by a desiccant, which can prevent a problem of reliability deterioration due to penetration of oxygen and / or moisture, An object of the present invention is to provide an adhesive film for an organic electronic device encapsulant including a melt-extrusion resin layer, an organic electronic device encapsulant using the same, and a manufacturing method thereof.

In exemplary embodiments of the present invention, in another aspect, a melt-extrusion resin layer that can prevent oxygen and/or moisture penetration due to lack of interfacial adhesion between various adhesive layers used in the encapsulant is included. An object of the present invention is to provide an adhesive film for an organic electronic device encapsulant, an organic electronic device encapsulant using the same, and a method for manufacturing the same.

In exemplary embodiments of the present invention, in another aspect, an adhesive film for an organic electronic device encapsulant including a melt-extrusion resin layer, which can prevent material deterioration by gas and/or moisture such as oxygen, An object of the present invention is to provide an organic electronic device encapsulant and a manufacturing method thereof.

In exemplary embodiments of the present invention, in another aspect, by applying a melt extrusion coating process of melt extrusion coating of the melt extrusion resin composition directly on the metal layer, preferably the anchor coating-treated metal layer, the manufacturing process is shortened and the manufacturing process is shortened. An object of the present invention is to provide an adhesive film for an organic electronic device encapsulant including a melt-extruded resin layer, an organic electronic device encapsulant using the same, and a method for manufacturing the same, which can reduce costs.

In exemplary embodiments of the present invention, in the adhesive film for an organic electronic device encapsulant, a melt-extrusion resin layer in which a melt-extrusion composition including an oxygen absorber is directly melt-extruded into a metal layer, preferably an oxygen absorber and a moisture absorbent An organic electronic device comprising a melt-extrusion resin layer in which the melt-extrusion composition is directly melt-extruded, more preferably a melt-extrusion resin layer in which a melt-extrusion composition comprising a melt-extrusion resin, a barrier resin, an oxygen absorber and a desiccant is directly melt-extruded An adhesive film for encapsulants is provided.

Exemplary embodiments of the present invention also provide an organic electronic device encapsulant including the metal layer and the above-described adhesive film for the organic electronic device encapsulant.

Exemplary embodiments of the present invention also provide a method for manufacturing an organic electronic device encapsulant comprising; forming a melt-extrusion resin layer by melt-extruding the above-described resin composition for extrusion on a metal layer.

Exemplary embodiments of the present invention also provide a method of encapsulating an organic electronic device using the above-described organic electronic device encapsulant.

Exemplary embodiments of the present invention also provide an organic electronic device encapsulated with the above-described organic electronic device encapsulant.

In exemplary embodiments of the present invention, in an adhesive film or encapsulant for an organic electronic device encapsulant, the melt-extrusion resin composition is directly melt-extruded on a metal layer, preferably an anchor-coated metal layer, to form a melt-extrusion resin layer. It can reduce the possibility of peeling and increase the adhesion with the metal layer .

In particular, by introducing a melt-extrusion resin layer to which oxygen absorption and/or moisture barrier properties are imparted, it is possible to effectively block gases such as oxygen and/or moisture while enhancing adhesion. Accordingly, it is possible to prevent a decrease in adhesion due to the moisture absorbent of the conventional sealing material adhesive film, a decrease in interfacial adhesion of the adhesive layer, and a decrease in reliability due to penetration of moisture and/or oxygen.

In addition, by using a T-die device for extrusion coating, the molten extrusion resin composition is directly melt-extruded on the metal layer, making the manufacturing process easier and faster compared to thermal bonding of a separate film to the metal layer. Therefore, it is possible to shorten the process and improve the production speed while using a novel material different from the material used for manufacturing the existing organic electronic device encapsulant, and it is possible to increase the price competitiveness of the product by lowering the manufacturing cost.

1A is a schematic diagram illustrating an example of a conventional adhesive film for an organic electronic device.
1B is a schematic view showing another example of a conventional adhesive film for an organic electronic device.
2 is a schematic view showing an adhesive film for an organic electronic device encapsulant according to an embodiment of the present invention.
3 is a schematic diagram showing an example of a melt extrusion coating apparatus used in an exemplary embodiment of the present invention.

In the present specification, the substrate means that an adhesive film such as a metal layer, a release film, and an organic electronic device is in contact.

In the present specification, when a part "includes" a component, it means that other components may be further included, rather than excluding other components, unless otherwise stated.

As used herein, the melt-extrusion resin refers to a resin that can be bonded to the metal layer through melt extrusion.

In the present specification, the barrier resin refers to a resin having gas and/or moisture barrier properties such as oxygen.

In the present specification, the extrudable barrier resin means a barrier resin that can be directly melt-extruded into the metal layer as described above.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

In one aspect, in exemplary embodiments of the present invention, in the adhesive film for an organic electronic device encapsulant, an adhesive film for an organic electronic device encapsulant comprising a melt-extrusion resin layer in which a melt-extrusion resin composition is directly melt-extruded on a metal layer. to provide.

Here, the melt-extrusion resin composition of the melt-extrusion resin layer preferably contains an oxygen absorber, more preferably an oxygen absorber and a moisture absorbent, in addition to the basic melt-extrusion resin that can be melt-extruded into the metal layer, and most preferably, the barrier property It may further include a resin, an oxygen absorbent and a desiccant.

In another aspect, exemplary embodiments of the present invention provide an encapsulant comprising a metal layer and a melt-extrusion resin layer directly melt-extruded onto the metal layer.

2 is a schematic view showing an adhesive film for an organic electronic device encapsulant according to an embodiment of the present invention.

As shown in FIG. 2, the adhesive film for an organic electronic device encapsulant of an exemplary embodiment is directly melt-extruded on a metal layer, and a melt-extrusion resin layer ( 10) and an oxygen absorbent and/or a moisture absorbent-free adhesive layer 30 positioned on the side of the organic electronic device.

In an exemplary embodiment, the melt-extrusion resin layer may have oxygen absorption.

In an exemplary embodiment, the melt-extrusion resin may have a moisture barrier property.

In an exemplary embodiment, the oxygen absorbent in the total melt-extrusion resin composition in the melt-extrusion resin layer may be included in an amount of 10-50 parts by weight based on 100 parts by weight of the melt-extrusion resin.

When the oxygen absorbent is less than 10 parts by weight, the oxygen absorption performance decreases, and when it exceeds 50 parts by weight, the oxygen absorption performance is similar to 50 parts by weight, while lowering of adhesion and workability (processability) may occur during extrusion processing.

In an exemplary embodiment, the moisture absorbent in the total melt-extrusion resin composition in the melt-extrusion resin layer may be included in an amount of 20-60 parts by weight based on 100 parts by weight of the melt-extrusion resin. When the absorbent is less than 20 parts by weight, the moisture absorption performance is lowered, and when it is more than 60 parts by weight, the moisture absorption performance is at a level similar to that of 60 parts by weight, while the adhesive strength and workability (processability) decrease during extrusion processing may occur.

In an exemplary embodiment, the melt-extrusion resin may be a polyolefin-based resin, and polyethylene is preferable in terms of an adhesive layer with the metal layer during melt-extrusion.

In an exemplary embodiment, the melt-extrusion resin composition may further include a T-die extrudable barrier resin.

Examples of the extrudable barrier resin include a cyclic olefin copolymer (COC) having moisture and/or oxygen barrier properties; and/or a liquid crystal polymer (LCP) having moisture and/or oxygen barrier properties; It is preferable to use at least one of them.

In addition, as a resin having moisture and/or oxygen barrier properties, one or more selected from the group consisting of ethylene vinyl alcohol (EVOH), polyacrylonitrile (PAN), and metaxylenediamine (m-xylenediamine) may be used. .

In an exemplary embodiment, the melt-extrusion resin composition may include polyethylene, a cyclic olefin copolymer (COC), an oxygen absorbent, and a desiccant.

Here, the melt-extrusion resin composition is based on 100 parts by weight of polyethylene, 10 to 30 parts by weight of cyclic olefin copolymer (COC), 10 to 50 parts by weight of an oxygen absorbent, and 20 to 60 parts by weight of a desiccant. have.

When the oxygen absorbent is less than 10 parts by weight, the oxygen absorption performance is deteriorated, and when it exceeds 50 parts by weight, the oxygen absorption performance is similar to 50 parts by weight, while lowering of adhesion and workability (processability) may occur during extrusion processing.

Similarly, when the absorbent is less than 20 parts by weight, the moisture absorption performance is lowered, and when it is more than 60 parts by weight, the moisture absorption performance is similar to 60 parts by weight, whereas the adhesive strength and workability (processability) decrease during extrusion processing may occur.

In addition, when the cyclic olefin copolymer is used in an amount of less than 10 parts by weight, barrier properties may be reduced, and when it exceeds 30 parts by weight, workability (processability) during extrusion processing may be reduced.

In an exemplary embodiment, the melt-extrusion resin may include polyethylene, a liquid crystal polymer (LCP), an oxygen absorbent, and a desiccant. As described above, the liquid crystal polymer is a T-Die extrudable resin having a moisture and oxygen barrier function.

Here, the melt-extrusion resin composition may include 10 to 30 parts by weight of a liquid crystal polymer, 10 to 50 parts by weight of an oxygen absorbent, and 20 to 60 parts by weight of a desiccant based on 100 parts by weight of polyethylene.

When the oxygen absorbent is less than 10 parts by weight, the oxygen absorption performance is deteriorated, and when it exceeds 50 parts by weight, the oxygen absorption performance is similar to 50 parts by weight, while lowering of adhesion and workability (processability) may occur during extrusion processing.

Similarly, when the absorbent is less than 20 parts by weight, the moisture absorption performance is lowered, and when it is more than 60 parts by weight, the moisture absorption performance is similar to 60 parts by weight, whereas the adhesive strength and workability (processability) decrease during extrusion processing may occur.

In addition, when the liquid crystal polymer is used in an amount of less than 10 parts by weight, barrier properties may be reduced, and when it exceeds 30 parts by weight, workability (processability) may be reduced during extrusion processing.

In an exemplary embodiment, the oxygen absorbing agent is at least one oxygen absorbing component selected from the group consisting of cerium oxide, reduced iron, sodium chloride, sodium sulfite, ascorbic acid and cobalt salt, or the oxygen absorbing component is blended with a polymer resin it may have been In particular, the oxygen absorbent preferably includes cerium oxide.

In a non-limiting example, the oxygen absorbing agent comprises at least one oxygen absorbing component (deoxidizer component) selected from the group consisting of cerium oxide, reduced iron, sodium chloride, sodium sulfite and ascorbic acid and / or the oxygen absorbing component with a polymer resin Blends can be used.

As the polymer resin, for example, a polyolefin-based resin, a polyester-based resin, or a polyamide-based resin can be used. As a specific example, as the polyolefin-based resin, various polypropylene-based resins such as high-density polyethylene, low-density polyethylene, linear low-density polyethylene, polyethylene by a metallocene catalyst, propylene-ethylene block copolymer, and propylene-ethylene random copolymer may be used. As the polyester-based resin, aromatic and aliphatic polyesters may be used. As the polyamide resin, aromatic polyamide and aliphatic polyamide may be used.

Also, in a non-limiting example, the oxygen absorbent may include MXD6 nylon and cobalt salts; double bond polymers and cobalt salts; and a polymer resin blended with a cobalt salt as an oxidation catalyst such as a cyclohexane side chain-containing polymer and a cobalt salt may be used.

The double bond-based polymer includes oleic acid, dimer acid, ricinolic acid, linoleic acid, arichidonic acid, farinaric acid, and the like, and may include triglycerides, esters, and transition metal salts of each polymer.

In an exemplary embodiment, the desiccant may include a metal oxide.

In an exemplary embodiment, the desiccant is selected from the group consisting of lithium oxide (Li2O), sodium oxide (Na2O), potassium oxide (K2O) barium oxide (BaO), calcium oxide (CaO), and magnesium oxide (MgO) It may include one or more, for example, calcium oxide may be included, and in the case of calcium oxide (CaO), it is preferable because the color change can be easily observed with the naked eye when water is contained.

In an exemplary embodiment, the thickness of the melt-extrusion resin layer may be 20 ~ 60㎛. If it is too thin (less than 20 μm), moisture absorption performance and adhesive strength may decrease, and if it is too thick if it exceeds 60 μm, extrusion processability and workability may deteriorate.

In an exemplary embodiment, the adhesive layer may include a main resin, a tackifier, an acrylic monomer or oligomer, and a photoinitiator.

In an exemplary embodiment, the thickness of the adhesive layer may be 5 ~ 35㎛. If it is too thin (less than 5 μm), adhesion may deteriorate, and if it is too thick, exceeding 35 μm, coating workability may deteriorate.

In an exemplary embodiment, a polyolefin-based binder may be used as the main resin, and the polyolefin-based binder may be any general polyolefin-based binder known in the art.

The polyolefin-based binder may be a polyethylene-based resin or a polypropylene-based resin, and may be a modified polyethylene resin, a modified polypropylene-based resin, an ethylene copolymer, or a propylene copolymer, for example, a plastic polyolefin having good moisture resistance and low price. , may be a polyolefin elastomer (POE), and may be EPDM or butyl rubber.

In an exemplary embodiment, the acrylic monomer may be an acrylate-based monomer or a methacrylate-based monomer, for example, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, dimethylaminoethyl acrylate, t- It may be butylaminoethyl methacrylate, for example, as an acrylic monomer with high moisture resistance and chemical resistance, it may be an acrylic monomer having more than two functional groups, preferably tricyclodecanedimethanol diacrylate (common name TCDDA). ) can be

In an exemplary embodiment, the acrylic oligomer is 1,3-butylene glycol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, 1,8-octanediol di(meth)acrylate, 1,12-dodecanediol di(meth)acrylate, adamantane di(meth)acrylate, trimethylolpropane tri(meth)acrylate, cyclohexane- 1,4-dimethanol di(meth)acrylate, neopentylglycol di(meth)acrylate, dicyclopentanyl di(meth)acrylate, tricyclodecanedimethanol(meth)diacrylate, dimethylol dicyclopentane It may include di(meth)acrylate, neopentylglycol-modified trimethylpropane di(meth)acrylate, or a mixture thereof.

In an exemplary embodiment, the photoinitiator may be a photoinitiator that can be used in a general 300 to 400 nm wavelength band, for example, benzoinmethyl ether, 2,4,6-trimethylbenzoyl diphenylphosphine oxide, bis(2, 4,6-trimethylbenzoyl)phenylphosphine oxide, α,α-methoxy-α-hydroxyacetophenone, 2-benzoyl-2-(dimethylamino)-1-[4-(4-morphonyl)phenyl] It may include one or more selected from the group consisting of -1-butanone, 2,2-dimethoxy-2-phenylacetophenone, oxime ester, and the like. In addition, for example, 1-hydroxy-cyclohexyl-phenyl-ketone (1-Hydroxy-cyclohexyl-phenyl-ketone) or bis (2,4,6-trimethylbenzoyl) -phenylphosphine oxide (Bis (2,4) ,6-trimethylbenzoyl)-phenylphosphineoxide), preferably diphenyl (2,4,6-trimethylbenzoyl)phosphine oxide (Diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide) (common name TPO) have.

In an exemplary embodiment, an anchor coating layer may be further formed on the metal layer. As the anchor coating layer, for example, toluene diisocyanate (TDI) and a polyester two-component anchor coating solution may be used.

Meanwhile, in an exemplary embodiment, the adhesive strength of the metal layer of the melt-extrusion resin layer of the adhesive film may be 1.5 to 3.5 Kgf/25 mm. If the adhesive force between the metal layer and the melt-extrusion resin layer is low, interfacial peeling may occur.

In addition, in an exemplary embodiment, the moisture penetration distance WTV of the adhesive film may be 400 um/100 hrs or more and 1,100 um/1000 hrs as shown in an experimental example to be described later. That is, the moisture penetration distance for 1000 hours may be 1,100um or less.

The water penetration distance WTV varies depending on the moisture absorption capacity of the desiccant and the blocking effect of the barrier resin, and the smaller the WTV, the better. For reference, for an effective encapsulation effect of the organic electronic device, it is preferable to be at least 1,200um/1000hrs, that is, 1,200um or less for 1000 hours.

In an exemplary embodiment, the oxygen absorption capacity may be 20 to 90%. Oxygen absorption capacity is calculated as (absorbed oxygen/initial oxygen) x 100. If the oxygen absorption capacity is less than 20%, the oxygen absorption performance is deteriorated, and if it is more than 90%, the oxygen absorption capacity is similar to 90%, whereas the adhesive strength and workability (processability) decrease during extrusion processing may occur.

Exemplary embodiments of the present invention also provide an organic electronic device encapsulant including the metal layer and the above-described adhesive film for the organic electronic device encapsulant.

Exemplary embodiments of the present invention also provide a method for manufacturing an organic electronic device encapsulant comprising; directly melt-extruding the above-described resin composition for extrusion onto a metal layer to form a melt-extrusion resin layer.

In an exemplary embodiment, the method comprises the steps of compounding the above-described resin composition for melt extrusion; forming a melt extrusion resin layer by extruding the resin composition for melt extrusion onto a metal layer using a T die, particularly a multi manifold die; It may include; coating the adhesive layer on the melt-extrusion resin layer.

3 is a schematic diagram showing an example of a melt extrusion coating apparatus used in an exemplary embodiment of the present invention.

The apparatus of FIG. 3 is a T-die apparatus for coating an extruded resin in the case of a metal layer (eg, aluminum foil). In Figures 3a and 3b, AC (anchor coating) is an anchor coating area for performing anchor coating on the metal layer, EC (extrusion coating) is a melt extrusion area for coating an anchor-coated metal layer with melt-extrusion resin, and PC (adhesive layer coating) ) refers to the adhesive layer coating area that coats the adhesive layer.

If there are many manufacturing processes, the production rate and production yield may be reduced. In exemplary embodiments of the present invention, a T-Die device for extrusion coating is used so that multi-layers can be manufactured at once while directly melt-extruding the melt-extrusion resin composition onto the metal layer. By using it, it is possible to shorten the process and improve the production speed, thereby securing price competitiveness.

In an exemplary embodiment, the extrusion temperature during the extrusion may be 200 ~ 350 ℃. When the extrusion temperature is low, the processability that is not extruded from the T-die may be deteriorated, and the adhesion between the extruded resin layer and the metal layer may be deteriorated. If the extrusion temperature is too high, a change in intrinsic physical properties may occur due to thermal deformation of the extrusion resin due to high temperature, and processability may deteriorate due to excessive flowability.

In an exemplary embodiment, the extrusion thickness during the extrusion may be 20 ~ 60㎛.

In an exemplary embodiment, the thickness of the adhesive layer may be 5 ~ 35㎛.

In an exemplary embodiment, in the method, an anchor coating layer for extrusion for improving adhesion to the metal layer may be further formed. The anchor coating layer may be formed using, for example, toluene diisocyanate (TDI) and a polyester two-component anchor coating solution.

In an exemplary embodiment, the amount of the anchor coating layer applied may be 0.2 to 0.5 g/m ² . When the amount of the anchor coating layer applied is less than 0.2 g/m ² , adhesion failure may occur, and if it is greater than 0.5 g/m ² , a problem in that the coating agent does not dry may occur.

On the other hand, exemplary embodiments of the present invention also provide a method of encapsulating an organic electronic device using the above-described organic electronic device encapsulant.

Exemplary embodiments of the present invention also provide an organic electronic device encapsulated using the above-described organic electronic device encapsulant.

As described above, according to the exemplary embodiments of the present invention, by using the melt-extrusion resin, the adhesion decrease due to the use of a desiccant, the gas and/or moisture penetration problem such as oxygen, and the problem of insufficient interfacial adhesion of the adhesive layer are prevented. and can increase reliability and effectively block gases such as moisture and/or oxygen.

In addition, by performing a high-speed melt extrusion process that directly melts and extrudes a metal layer, preferably an anchor-coated metal layer, without thermocompression bonding a separate film to the metal layer, the possibility of interfacial delamination, which is important in organic electronic device encapsulants, is reduced. The manufacturing process can be easily and simplified while increasing the adhesion.

Accordingly, it is possible to shorten the process, improve the production speed, reduce the manufacturing cost, and improve productivity while using a new material different from the material used for manufacturing the existing organic electronic device encapsulant.

Exemplary embodiments of the present invention are described in more detail through the following examples. The embodiments disclosed in this specification are illustrated for the purpose of explanation only, and the embodiments of the present invention may be embodied in various forms and should not be construed as being limited to the embodiments described herein.

[Example 1]

(1-1) Manufacturing of resin for melt extrusion resin

In order to prepare a film using T-die (T-die), compounded to include 100 parts by weight of polyethylene, 35 parts by weight of cerium oxide, 20 parts by weight of cyclic olefin copolymer and 35 parts by weight of calcium oxide (CaO) for extrusion A resin was prepared.

(1-2) Preparation of adhesive layer coating solution

An adhesive layer coating solution was prepared by adding 0.5wt% of acrylic monomer and 10wt% of photoinitiator compared to 100wt% of acrylic monomer to a solution of EPDM, Butyl Rubber, and tackifier in a ratio of 1:2:4.

(1-3) Encapsulation film manufacturing

40 μm of aluminum foil cleaned as a metal layer was put into a T-die device as a first grade (substrate to be melt-extrusion coating), and the resin for melt extrusion resin was extruded at an extrusion temperature of 200 to 300° C. at 40 μm. . The metal layer was coated with an anchor coating agent for extrusion to further improve adhesion. As an anchor coating agent, TDI (Toluene diisocynate) and a polyester two-component anchor coating solution were used.

(1-4) Adhesive layer coating

Then, the pressure-sensitive adhesive layer coating solution was coated on the extruded coating layer in a thickness of 10 μm.

[Example 2]

(1-1) When manufacturing the resin for melt extrusion resin, compounding to include 100 parts by weight of polyethylene, 50 parts by weight of cerium oxide, 20 parts by weight of cyclic olefin copolymer and 50 parts by weight of calcium oxide (CaO) to prepare the resin for extrusion Except for the preparation, the rest of the process was performed in the same manner as in Example 1.

[Example 3]

(1-1) When manufacturing the resin for melt-extrusion resin, compounding to include 100 parts by weight of polyethylene, 35 parts by weight of cerium oxide, 20 parts by weight of liquid crystal polymer and 35 parts by weight of calcium oxide (CaO) to prepare a resin for extrusion Except that, the rest of the procedure was performed in the same manner as in Example 1.

[Comparative example]

Calcium oxide (CaO) was prepared in a ratio of 1:1 with the coating solution in the adhesive coating solution used in Example 1 as a moisture absorption layer, and coated on a metal layer, and the adhesive coating solution of Example 1 (without moisture absorbent and oxygen absorber) was re-coated thereon. An encapsulation film was prepared.

[Experiment 1: Evaluation of Oxygen Absorption]

The oxygen absorption amount of the encapsulation films prepared according to Examples 1, 2, 3 and Comparative Examples was evaluated. The film was placed in a pouch made of high-barrier nylon/aluminum material having a volume of 500 cc, filled with a gas containing 0.5% oxygen and 99.5% nitrogen, and then the bag was sealed.

Then, the pouch was placed in a thermostat at 25-27°C.

Since it is difficult to vacuum the air outside the pouch, the oxygen content inside the pouch was measured using Iijima Electronics Co., Ltd.'s Packmaster RO-105 oxygen concentration meter after leaving the pouch for one day. After obtaining about 15 cc of initial oxygen amount data, the amount of oxygen absorption was measured over time.

Table 1 below shows the evaluation results.

division initial amount of oxygen
(CC) Oxygen Absorption (CC) 24 hours 72 hours 168 hours 240 hours 360 hours 480 hours Example 1 15.0 1.2 3.8 6.5 8.1 10.2 11.5 Example 2 1.9 4.8 8.5 10.3 12.7 13.1 Example 3 15.2 1.3 3.9 6.6 8.2 10.4 11.8 Comparative Example 1 15.3 0 0.1 0.3 0.5 0.6 0.8

As can be seen from the above results, it can be seen that the oxygen absorption amount is significantly improved compared to the comparative example in all time zones.

[Experiment 2: Water Through Velocity (WTV) evaluation]

Water Through Velocity (WTV) of the encapsulation films prepared according to Examples 1, 2, and 3 and Comparative Examples was evaluated.

Specifically, after laminating alkali-free glass on both outer surfaces of each film, put it in a reliability chamber with a temperature of 85'C and a humidity of 85%, and measure the penetration length of moisture through a microscope for up to 1000 hours in units of 100 hours did.

[Experiment 3: Evaluation of thermal bonding strength (peel strength) of metal layer and melt-extrusion resin layer]

On the other hand, the adhesive force with the metal layer was measured as follows.

(1) A sample was prepared in which each specimen was cut horizontally (25mm)*lengthwise (25mm) using a cutter bar.

(2) The adhesive surface (between the metal layer and the extruded resin layer) at the end of each specimen was peeled off between layers for only a certain length.

(3) For the above sample, the adhesive strength (peel strength) was measured at a peel angle of 180 degrees using a universal tensile tester (SHIMADZU, model AGS-X).

Table 2 below shows the evaluation results.

division metal layer
adhesion
(Kgf/25mm) WTV (㎛) 100
hour 200
hour 300
hour 400
hour 500
hour 600
hour 700
hour 800
hour 900
hour 1000
hour Example 1 531 658 719 858 925 990 1042 1094 Example 2 509 562 611 663 728 797 862 930 992 1048 Example 3 1.7 486 552 607 679 741 797 865 924 973 1004 comparative example 1.1 882 995 1042 1127 1172 1273 1398 1450 1485 1554

As can be seen from the above results, it can be seen that the WTV results of up to 1000 hours show a tendency to improve the hygroscopicity. In particular, it was confirmed that the WTV values of the Examples were relaxed compared with the Comparative Examples.

In addition, the adhesion to the metal layer was evaluated in the order of Example 1 = Example 2 > Example 3 > Comparative Example.

That is, according to the exemplary embodiments of the present invention, it is confirmed that the reliability can be improved by improving the adhesion by melt-extruding the melt-extrusion resin composition directly on the metal layer and alleviating the problem of oxygen and/or moisture absorption in the initial stage. could

Although non-limiting exemplary embodiments of the present invention have been described above, the technical spirit of the present invention is not limited to the accompanying drawings or the above description. It is apparent to those skilled in the art that various types of modifications are possible within the scope of the present invention without departing from the spirit of the present invention, and also, such modifications will fall within the scope of the claims of the present invention.

Claims (24)

In the adhesive film for an organic electronic device encapsulant,
An adhesive film for an organic electronic device encapsulant, comprising a melt-extrusion resin layer in which a melt-extrusion resin composition containing an oxygen absorber is melt-extruded on a metal layer.
According to claim 1,
The melt-extrusion resin composition is an adhesive film for an organic electronic device encapsulant, characterized in that it further comprises a moisture absorbent.
3. The method of claim 2,
The melt-extrusion resin composition is an adhesive film for an organic electronic device encapsulant, characterized in that it comprises a melt-extrusion resin and a barrier resin.
4. The method of claim 3,
The adhesive film for the organic electronic device encapsulant,
the melt-extrusion resin layer melt-extruded on the metal layer; and
An adhesive film for an organic electronic device encapsulant comprising a; an adhesive layer that is located on the side of the organic electronic device and does not contain a desiccant.
According to claim 1,
An adhesive film for an organic electronic device encapsulant, characterized in that 10 to 50 parts by weight of an oxygen absorbent is included with respect to 100 parts by weight of the melt-extrusion resin in the melt-extrusion resin composition.
3. The method of claim 2,
An adhesive film for an organic electronic device encapsulant, characterized in that 20 to 60 parts by weight of a desiccant is included with respect to 100 parts by weight of the melt-extrusion resin in the melt-extrusion resin composition.
4. The method of claim 3,
The melt-extrusion resin is polyethylene,
The barrier resin is an adhesive film for an organic electronic device encapsulant, characterized in that at least one selected from a cyclic olefin copolymer (COC) and a liquid crystal polymer.
8. The method of claim 7,
The melt-extrusion resin composition contains 10 to 30 parts by weight of a cyclic olefin copolymer (COC), 10 to 50 parts by weight of an oxygen absorbent, and 20 to 60 parts by weight of a desiccant with respect to 100 parts by weight of polyethylene. Adhesive film for electronic device encapsulants.
8. The method of claim 7,
The melt-extruded resin composition is an adhesive film for an organic electronic device encapsulant, characterized in that it contains 10 to 30 parts by weight of a liquid crystal polymer, 10 to 50 parts by weight of an oxygen absorbent, and 20 to 60 parts by weight of a desiccant, based on 100 parts by weight of polyethylene.
The method of claim 1,
The oxygen absorbing agent is at least one oxygen absorbing component selected from the group consisting of cerium oxide, reduced iron, sodium chloride, sodium sulfite, ascorbic acid and cobalt salt, or the oxygen absorbing component is blended with a polymer resin. Adhesive film for device encapsulants.
3. The method of claim 2,
The adhesive film for an organic electronic device encapsulant, characterized in that the absorbent is calcium oxide (CaO).
5. The method of claim 4,
An adhesive film for an organic electronic device encapsulant, characterized in that the melt-extrusion resin layer has a thickness of 20 to 60 μm.
5. The method of claim 4,
The adhesive film for an organic electronic device encapsulant, characterized in that the thickness of the adhesive layer is 5 ~ 35㎛.
5. The method of claim 4,
The adhesive layer may include a polyolefin-based binder; tackifiers; acrylic monomers or acrylic oligomers; and a photoinitiator; an adhesive film for an organic electronic device encapsulant comprising a.
According to claim 1,
The melt-extrusion resin layer is an adhesive film for an organic electronic device encapsulant, characterized in that the melt-extrusion to the metal layer on which the anchor coating layer is formed.
5. The method of claim 4,
The adhesive film for an organic electronic device encapsulant, characterized in that the oxygen absorption property of the organic electronic device encapsulant is 20 to 90%.
5. The method of claim 4,
The adhesive film for an organic electronic device encapsulant, characterized in that the adhesive strength of the metal layer of the melt-extruded resin layer of the adhesive film for the organic electronic device encapsulant is 1.5 to 3.5 Kgf/25mm.
5. The method of claim 4,
The moisture penetration distance WTV of the adhesive film for an organic electronic device encapsulant is 1,100 μm or less for 1000 hours.
An organic electronic device encapsulant comprising the adhesive film for an organic electronic device encapsulant of any one of claims 1 to 18.
The method for manufacturing the organic electronic device encapsulant of any one of claims 1 to 18,
A method for manufacturing an organic electronic device encapsulant, comprising: melt-extruding a resin composition for extrusion including an oxygen absorber on a metal layer to form a melt-extrusion resin layer.
21. The method of claim 20,
The method comprises the steps of compounding a resin composition for melt extrusion comprising a melt extrusion resin, a barrier resin, an oxygen absorbent and a moisture absorbent;
extruding the resin composition for melt extrusion onto the metal layer using a T die to form a melt extrusion resin layer; and
and coating an adhesive layer on the melt-extrusion resin layer.
22. The method of claim 21,
The method of manufacturing an organic electronic device encapsulant, characterized in that the extrusion temperature when extruding to the metal layer is 200 ~ 350 ℃.
An organic electronic device encapsulation method, characterized in that the organic electronic device is encapsulated with the organic electronic device encapsulant of claim 19.
An organic electronic device, characterized in that it is packaged with the organic electronic device encapsulant of claim 19.

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