Encapsulation film including metal layer and protective layer with resin component

Abstract

The present application provides an encapsulation film comprising an encapsulation layer, a metal layer, and a protective layer. The encapsulation film provides a structure capable of blocking moisture or oxygen introduced into an organic electronic device from the outside, minimizes the appearance change of the film due to excellent handling properties and processability, and prevents physical and chemical damage during encapsulation process.

Claims

1. An encapsulation film comprising an encapsulation layer, a metal layer and a protective layer, wherein the protective layer has a thickness of more than 5 μm and comprises a resin component, wherein a glass transition temperature of the resin component after curing is 0° C. or higher, the glass transition temperature measured after curing the encapsulation film by heating at a temperature in a range of 50 to 300° C.; by irradiating ultraviolet ray; or by both, and wherein the resin component is a thermosetting resin, a photo-curing resin or a dual curing resin, comprises a curable oligomer and a curable monomer, and comprises an epoxy resin having a cyclic structure in addition to the epoxy group in its molecular structure.

2. The encapsulation film according to claim 1, wherein the encapsulation layer is formed as a single layer or a multilayer of two or more layers.

3. The encapsulation film according to claim 1, wherein the encapsulation layer comprises an encapsulating resin having a glass transition temperature of less than 0° C. after curing.

4. The encapsulation film according to claim 1, wherein the encapsulation layer comprises a moisture adsorbent.

5. The encapsulation film according to claim 4, wherein the moisture adsorbent is a moisture-reactive adsorbent.

6. The encapsulation film according to claim 1, wherein the encapsulation layer comprises a multifunctional active energy ray polymerizable compound.

7. The encapsulation film according to claim 1, wherein the metal layer comprises any one of a metal, a metal oxide, a metal nitride, a metal carbide, a metal oxynitride, a metal oxyboride, and a combination thereof.

8. The encapsulation film according to claim 1, wherein the metal layer comprises any one of iron, aluminum, copper, nickel, silicon oxide, aluminum oxide, titanium oxide, indium oxide, tin oxide, indium tin oxide, tantalum oxide, zirconium oxide, niobium oxide, and a combination thereof.

9. The encapsulation film according to claim 1, wherein the protective layer has a thickness in a range of more than 5 μm and 50 μm or less.

10. The encapsulation film according to claim 1, wherein the protective layer has a tensile elastic modulus in a range of 0.01 MPa to 1000 MPa at 25° C.

11. The encapsulation film according to claim 1, wherein the resin component has a glass transition temperature after curing in a range of 50° C. to 200° C.

12. The encapsulation film according to claim 1, wherein the curable oligomer and the curable monomer are comprised in amounts of 15 to 35 parts by weight and 10 to 40 parts by weight, respectively.

13. The encapsulation film according to claim 1, wherein the curable oligomer has a weight average molecular weight in a range of 400 to 10,000 g/mol, and the curable monomer has a weight average molecular weight of less than 400 g/mol.

14. The encapsulation film according to claim 1, wherein the protective layer comprises an initiator or a curing agent.

15. An organic electronic device comprising a substrate, an organic electronic element formed on the substrate, and the encapsulation film according to claim 1 for encapsulating the entire surface of the organic electronic element.

16. A method for manufacturing an organic electronic device comprising a step of applying the encapsulation film according to claim 1 a substrate, on which an organic electronic element is formed, so as to cover the organic electronic element.

Description

BRIEF DESCRIPTION OF DRAWINGS

(1) FIG. 1 is a cross-sectional view showing an encapsulation film according to one example of the present application.

(2) FIG. 2 is a cross-sectional view showing an organic electronic device according to one example of the present invention.

(3) FIGS. 3 to 6 are endurance reliability experiment photographs of encapsulation films according to Examples and Comparative Examples.

EXPLANATION OF REFERENCE NUMERALS

(4) 10: encapsulation film 11: encapsulation layer 12: metal layer 13: protective layer 21: substrate 22: organic electronic element

BEST MODE

(5) Hereinafter, the above-described details will be described in more detail with reference to Examples and Comparative Examples. However, the scope of the present application is not limited by the following examples.

Example 1

(6) Preparation of Protective Layer Solution

(7) A styrene-isobutylene copolymer (SIBS 103T, Mw: 100,000 g/mol, Kaneka), a hydrogenated bisphenol A epoxy resin (YX8000, Mw: 3,810 g/mol, epoxy equivalent: 201 g/eq, Mitsubishi Chemical) and an alicyclic epoxy resin (Celloxide 2021P, Mw: 250 g/mol, Daicel Corporation) were each introduced into a reaction vessel at a weight ratio of 50:30:20 (SIBS103T: YX8000: Celloxide2021P), and Irgacure 290 as a cationic photoinitiator was added thereto in an amount of 0.1 parts by weight relative to 100 parts by weight of the resin component, and then the mixture was diluted with toluene to a solid content of about 15 wt % or so to prepare a protective layer composition coating solution.

(8) The prepared solution was applied on the release surface of the releasing PET and dried in an oven at 100° C. for 15 minutes to form a protective layer having a thickness of 15 μm.

(9) Production of Encapsulation Layer

(10) A CaO (average particle diameter less than 5 μm) solution (solid content 50%) was prepared as a moisture adsorbent. Separately, a solution (solid content 50%), in which 200 g of a butyl rubber resin (BT-20, Sunwoo Chemtech) and 60 g of a DCPD petroleum resin (SU5270, Sunwoo Chemtech) were diluted with toluene, was prepared and then the solution was homogenized. 10 g of a multifunctional compound (trimethylolpropane triacrylate, TMPTA, Miwon) and 15 g of a photoinitiator (Irgacure 819, Ciba) were introduced to the homogenized solution, homogenized and then 100 g of the CaO solution was introduced thereto, followed by stirring at high speed for 1 hour to prepare a solution of an encapsulation layer.

(11) The above-prepared encapsulation layer solution was applied to the release surface of a releasing PET using a comma coater and dried in a dryer at 130° C. for 3 minutes to form an encapsulation layer having a thickness of 60 μm.

(12) Production of Encapsulation Film

(13) The release-treated PET attached to the outside of the above-produced protective layer was peeled off, the protective layer was laminated on one side of the metal layer (copper, 18 μm) prepared in advance, and the above-produced encapsulation layer was laminated on the other side of the metal layer to produce an encapsulation film.

Example 2

(14) An encapsulation film was produced in the same manner as in Example 1, except that a bisphenol A epoxy resin (YP-50, Mw: 65,000 g/mol, Kukdo Chemical), a hydrogenated bisphenol A epoxy resin (YX8000, Mw: 3,810 g/mol, epoxy equivalent: 201 g/eq, Mitsubishi Chemical) and an alicyclic epoxy compound (Celloxide 2021P, Mw: 250 g/mol, Daicel Corporation) were each introduced into the reaction vessel at a weight ratio of 50:30:20 (YP-50: YX8000: Celloxide2021P) at the time of producing the protective layer.

Comparative Example 1

(15) An encapsulation film was produced in the same manner as in Example 1, except that PET (polyethylene terephthalate) having a urethane-based adhesive (glass transition temperature: −20° C.) on one side was used as the protective layer and formed on the metal layer (in the order of PET/urethane-based adhesive/metal layer).

Comparative Example 2

(16) An encapsulation film was produced in the same manner as in Example 1, except that the protective layer was not used.

Comparative Example 3

(17) An encapsulation film was produced in the same manner as in Example 1, except that the protective layer was formed to have a thickness of 3 μm.

Comparative Example 4

(18) An encapsulation film was produced in the same manner as in Example 1, except that to prepare a protective layer composition coating solution, 200 g of a butyl rubber resin (BT-20, Sunwoo Chemtech), 60 g of a DCPD-based petroleum resin (SU5270, Sunwoo Chemtech) and 15 g of a multifunctional compound (TMPTA, Miwon) were introduced into a vessel, and then toluene was added so as to have a solid content of 20 wt %. The Tg of the resin component is −50° C.

Comparative Example 5

(19) An encapsulation film was produced in the same manner as in Example 1, except that the base and the curing agent of Sylgard 184 (polydimethylsiloxane, Tg: −100° C.) from Dow Corning were mixed in a weight ratio of 5:1 to prepare a protective layer composition coating solution.

Experimental Example 1—Confirmation of Endurance Reliability of Metal Layer

(20) The encapsulation films prepared in Examples and Comparative Examples were each bonded to glass and the encapsulation films were each irradiated with light having a wavelength range of UV-A region band at a light quantity of 3 J/cm.sup.2, and then heat-treated in an oven at 100° C. for 3 hours to prepare a specimen. Thereafter, the specimen was maintained in a constant temperature and humidity chamber at 85° C. and 85% relative humidity for 30 days, and then the color change of the metal layer was confirmed. FIGS. 3 to 6 are photographs of the encapsulation films of Examples 1 and 2 and Comparative Examples 1 and 2 in this order, respectively, after the above experiment. In Comparative Examples 1 and 2, it can be confirmed that the color change of the metal layer occurs.

Experimental Example 2—Endurance Reliability of Organic Electronic Device at High Temperature

(21) After the organic electronic elements were each deposited on a glass substrate, the encapsulation films prepared in Examples and Comparative Examples above were each bonded on the element under conditions of 50° C., a vacuum level of 50 mtorr and 0.4 MPa using a vacuum bonding machine, and irradiated with light having a wavelength range of UV-A region band at a light quantity of 3 J/cm.sup.2, and then heat was applied thereto in an oven at 100° C. for 3 hours to prepare an organic electronic panel.

(22) Thereafter, while the prepared organic electronic panel was held in a constant temperature and humidity chamber at 85° C. and 85% relative humidity for 500 hours, lifting between the film and the element was confirmed, and when the lifting occurred, it was classified as X.

Experimental Example 3—Surface Property

(23) After the encapsulation films prepared in Examples and Comparative Examples were each irradiated with UV rays having an intensity of 1000 mW/cm.sup.2 at 3 J/cm.sup.2, tack free time of the protective layer at room temperature was measured. The time until the tacky feeling disappears and there is no sticking out when touching the surface of the protective layer immediately after curing is defined as tack free time and measured. When the tack free time was less than 1 minute, it was classified as O; when it was 5 minutes or more, it was classified as Δ; and when it was 30 minutes or more, it was classified as X.

(24) TABLE-US-00001 TABLE 1 Endurance reliability Surface of Organic Property of Endurance Reliability Electronic Protective of Metal Layer Device Layer Example 1 Good (FIG. 3) Good ◯ Example 2 Good (FIG. 4) Good ◯ Comparative 1 Color change X ◯ Example occurrence (FIG. 5) 2 Color change Good — occurrence (FIG. 6) 3 Color change X ◯ occurrence 4 Good Good X 5 Color change Good X occurrence

(25) As a result of the surface property of the protective layer, in the case of Comparative Examples 4 and 5 in which the tacky property was high, the multiple sheets of the encapsulation films to be laminated adhered to each other, so that the encapsulation process of the organic electronic element was substantially impossible.