Encapsulation film

09698378 ยท 2017-07-04

Assignee

Inventors

Cpc classification

International classification

Abstract

Provided are an encapsulating film, an electronic device and a method of manufacturing the same. An encapsulating film having excellent moisture blocking property, handleability, workability and durability and a structure including a diode encapsulated with the encapsulating film may be provided.

Claims

1. An encapsulating film, comprising: a first layer that includes a component having a contact angle of deionized water of 80 degrees or more and a water vapor transmission rate of 50 g/m.sup.2.Math.day or less; and a second layer including a curable resin composition, wherein the water vapor transmission rate of the component is measured in a thickness direction at 100 F. and a relative humidity of 100% by using a specimen of the component having a film form with a thickness of 100 m.

2. The film according to claim 1, wherein the component for the first layer has a glass transition temperature after curing of less than 0 C.

3. The film according to claim 1, wherein the composition of the second layer has a glass transition temperature after curing of more than 85 C.

4. The film according to claim 1, wherein the second layer is disposed on one or both surfaces of the first layer.

5. The film according to claim 1, wherein the first layer has a lower tensile modulus after curing at 25 C. than that of the second layer.

6. The film according to claim 1, wherein a tensile modulus after curing at 25 C. of the first layer is 0.001 to 300 MPa.

7. The film according to claim 1, wherein a tensile modulus after curing at 25 C. of the second layer is 200 to 1000 MPa.

8. The film according to claim 1, wherein a ratio (M1/M2) of a tensile modulus (M1) after curing at 25 C. of the first layer to a tensile modulus (M2) after curing at 25 C. of the second layer is 110.sup.6 to 0.5.

9. The film according to claim 1, wherein the first layer further includes a moisture scavenger.

10. The film according to claim 9, wherein the first layer includes the moisture scavenger of 5 to 250 parts by weight with respect to 100 parts by weight of the component of the first layer.

11. The film according to claim 1, wherein the second layer includes the moisture scavenger of less than 5 parts by weight with respect to 100 parts by weight of a total solid content of the second layer.

12. The film according to claim 1, wherein the second layer is a solid or semi-solid at room temperature.

13. The film according to claim 12, wherein the second layer is in a non-cured state.

14. The film according to claim 13, wherein the second layer includes the curable resin composition in a film type.

15. An electronic device comprising: an upper substrate; a bottom substrate; and an encapsulating layer which includes the film of claim 1 encapsulating a diode between the upper and bottom substrates.

16. The electronic device according to claim 15, wherein the diode is formed on a surface of the bottom substrate facing the upper substrate, and the second layer of the film is in contact with the bottom substrate.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 is a schematic diagram of a film according to an exemplary embodiment;

(2) FIG. 2 is a schematic diagram of a film according to another exemplary embodiment;

(3) FIG. 3 is a schematic diagram of an organic electronic device according to an exemplary embodiment;

(4) FIG. 4 is a schematic diagram of an organic electronic device according to another exemplary embodiment;

(5) FIG. 5 is a schematic diagram illustrating a method of manufacturing an organic electronic device according to an exemplary embodiment; and

(6) FIG. 6 is a schematic diagram illustrating a method of manufacturing an organic electronic device according to another exemplary embodiment.

DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS

(7) Hereinafter, a film will be described in further detail with reference to Examples and Comparative Examples, but the scope of the film is not limited to the following Examples.

(8) Hereinafter, physical properties shown in Examples and Comparative Examples are evaluated by the following methods.

(9) 1. Measurement of Contact Angle

(10) A contact angle was measured with respect to a coating layer formed by preparing a solution having a solid content of 15 wt % by dissolving a base resin in a dilutable solvent, coating the prepared solution on a glass to have a thickness of 10 m and drying the coated solution. Particularly, the contact angle was measured using DSA100 produced by KRUSS. Deionized water was dropped to the coating layer at approximately 25 C., which was repeated 10 times, and then an average of the measured results was determined as the contact angle.

(11) 2. Measurement of WVTR

(12) A resin composition was prepared by dissolving the component for the first layer used in Example or the resin used in Comparative Example in a solvent. The resin composition was coated on a base film (releasing polyester film, RS-21G, SKC) having a thickness of 38 m. Subsequently, the coated composition was dried at 110 C. for 10 minutes, and thereby a film-type layer having a thickness of 100 m was prepared. Afterward, the base film was detached, the film-type layer was maintained at 100 F. and a relative humidity of 100%, and then a WVTR with respect to a thickness direction of the film-type layer was measured. The WVTR was measured as prescribed in regulations of ASTM F1249.

(13) 3. Measurement of Tensile Modulus

(14) A resin composition was prepared by dissolving a first or second layer prepared in Example or Comparative Example in a solvent. The resin composition was coated on a base film (releasing polyester film, RS-21G, SKC) having a thickness of 38 m. Subsequently, the coated composition was dried at 110 C. for 10 minutes, and thereby a film-type layer having a thickness of 40 m was prepared. The prepared coating layer was designed to be coated in a length direction, and then cut in a size of 50 mm10 mm (lengthwidth), thereby preparing a specimen. Both terminal ends of the specimen were taped to leave 25 mm in a length direction. Subsequently, while the taped part was extended at 25 C. at a rate of 18 mm/min, a tensile modulus was measured.

(15) 4. Evaluation of Moisture Blocking Property

(16) Calcium (Ca) was deposited on a glass substrate having a size of 12 mm12 mm (lengthwidth) to have a size of 10 mm10 mm (lengthwidth). Separately, a film formed in Example or Comparative Example was cut to a size of 12 mm12 mm (lengthwidth). Subsequently, the first layer or one surface of the film was transferred to a cover glass. Afterward, an opposite surface to that of the film on which the cover glass was disposed was laminated on the calcium of the glass substrate, and thermally pressed using a vacuum press at 80 C. for 2 minutes, and cured at 100 C. for 3 hours, thereby forming an encapsulating layer. Thus, a specimen was manufactured. Then, while the specimen was maintained in a constant temperature and constant humidity chamber at 85 C. and a relative humidity of 85% for approximately 500 hours, a length of the calcium-deposited part which was oxidized and made transparent was measured. Since calcium had a total length in one direction of 10 mm, the length of the oxidized part of the calcium from one terminal end became 5 mm, which meant that all of the calcium was oxidized.

(17) 5. Evaluation of Durability and Reliability

(18) A film formed in Example or Comparative Example was laminated between soda lime glass substrates, thermally pressed using a vacuum press at 80 C. for 2 minutes, and curing the substrates at 100 C. for 3 hours, thereby forming an encapsulating layer. As a result, a specimen was prepared. Afterward, while the specimen was maintained in a constant temperature and constant humidity chamber at 85 C. and a relative humidity of 85% for approximately 500 hours, it was observed whether or not lifting occurred at an interface between the glass substrate and the encapsulating layer.

(19) 6. Evaluation of Adhesive Strength

(20) Two of 0.7 T glass substrates were crossed to be disposed in a T shape, and a film having a size of 5 mm40 mm (widthlength) formed in Example or Comparative Example was disposed on a contact point of the two substrates. The film was thermally pressed using a vacuum press at 80 C. for 2 minutes, and cured at 100 C. for 3 hours. Afterward, while a terminal end of the T-shaped glass specimen was pressed using a tensile tester at a uniform pressure, power when the attached glass specimen was separated was measured, which was defined as an adhesive strength.

(21) 7. Evaluation of Applicability of Panel

(22) A film formed in Example or Comparative Example was cut to a size of 90 mm90 mm (lengthwidth), and a first layer or one surface of the film was transferred to a cover glass. Then, an opposite surface to that of the film on which the cover glass was disposed was thermally pressed on a glass substrate having a size of 100 mm100 mm (lengthwidth) using a vacuum press at 80 C. for 2 minutes, and cured at 100 C. for 3 hours, thereby preparing a specimen. It was observed whether or not bubbles were generated in the specimen.

Example 1

(1) Preparation of First Layer Solution

(23) A moisture scavenger solution was prepared by adding 100 g of calcined dolomite as a moisture scavenger and 0.5 g of stearic acid as a dispersing agent to a toluene to have a solid content of 50 wt %. In addition, separately, 65 g of a polyisobutene resin (weight average molecular weight of 450,000) and 5 g of a maleic acid anhydride-grated styrene-ethylene-butadiene-styrene block copolymer (MA-SEBS, Product Name: FG-1901X, Manufacturer: Kraton) were added as base resins for the first layer to a reaction vessel at room temperature, and 30 g of a hydrogenated dicyclopentadiene-based resin (softening point: 125 C.) was added thereto as a tackifier and diluted with toluene to have a solid content of approximately 20 wt %. The previously prepared moisture scavenger solution was added to the solution to have a content of the calcined dolomite of 30 parts by weight with respect to 100 parts by weight of the base resins for the first layer, and mixed together, thereby preparing a first layer solution.

(2) Preparation of Second Layer Solution

(24) 200 g of a silane-modified epoxy resin (KSR-177, Kukdo Chemical) and 150 g of a phenoxy resin (YP-50, Tohto Kasei) were added to a reaction vessel at room temperature, and then diluted with methylethylketone. 4 g of imidazole (Shikoku Chemical) which was a curing agent was added to the homogenized solution, and stirred at a high speed for 1 hour, thereby preparing a second layer solution.

(3) Formation of Film

(25) A first layer was formed to have a thickness of 40 m by coating the solution of a first layer prepared above on a release surface of releasing PET and drying the coated solution at 110 C. for 10 minutes.

(26) A second layer was formed to have a thickness of 15 m by coating the solution of a second layer prepared above on a release surface of releasing PET and drying the coated solution at 130 C. for 3 minutes.

(27) A multilayer film was formed by laminating the first and second layers.

Example 2

(28) A first layer solution, a second layer solution and a film were prepared as described in Example 1, except that 60 g of polyisobutene and 10 g of MA-SEBS were used instead of 65 g of polyisobutene and 5 g of MA-SEBS as base resins for the first layer.

Example 3

(29) A first layer solution, a second layer solution and a film were prepared as described in Example 1, except that 55 g of polyisobutene and 15 g of MA-SEBS were used instead of 65 g of polyisobutene and 5 g of MA-SEBS as base resins of a first layer.

Example 4

(30) A first layer solution, a second layer solution and a film were prepared as described in Example 2, except that a styrene-butadiene-styrene block copolymer (SBS, Product Name: D-1101, Manufacturer: Kraton) was used instead of MA-SEBS of the base resins for the first layer.

Example 5

(31) A first layer solution, a second layer solution and a film were prepared as described in Example 2, except that a styrene-isoprene-styrene block copolymer (SIS, Product Name: D-1107, Manufacturer: Kraton) was used instead of MA-SEBS of the base resins for the first layer.

Example 6

(32) A first layer solution, a second layer solution and a film were prepared as described in Example 2, except that 70 g of a polyisobutene resin was used instead of 60 g of a polyisobutene resin and 10 g of MA-SEBS as base resins for the first layer.

Comparative Example 1

(33) A second layer solution and a film were prepared as described in Example 1, except that the second layer solution in Example 1 was used as a first layer solution.

Comparative Example 2

(1) Preparation of First Layer Solution

(34) An acrylic resin solution was prepared by reacting 15 g of n-butyl acrylate (n-BA), 40 g of methylethyl acrylate (MEA), 20 g of isobornyl acrylate (IBoA), 15 g of methylacrylate (MA) and 10 g of 2-hydroxyethyl acrylate (HEA) in a 1 L reaction vessel refluxing a nitrogen gas and equipped with a cooling device to facilitate temperature control. A first layer solution was prepared by mixing the moisture scavenger solution previously prepared in Example 1 with the solution to have a content of calcined dolomite of 30 parts by weight with respect to 100 parts by weight of the solid content of the acrylic resin solution.

(2) Preparation of Second Layer Solution

(35) A second layer solution was prepared as described in Example 1.

(3) Formation of Film

(36) A film was formed as described in Example 1, except that the solution prepared in Comparative Example 2 was used as a first layer solution.

Comparative Example 3

(37) A first layer solution, a second layer solution and a film were prepared as described in Comparative Example 2, except that a trimethylolpropane-type epoxy resin (SR-TMP, SAKAMOTO) was added to an acrylic resin solution as an epoxy crosslinking agent at 5 parts by weight with respect to 100 parts by weight of a solid content of an acrylic resin solution, and a triarylsulfonium salt-type with SbF6 as anions (CPI-110A, SAN APRO Ltd.) was further added as a cationic initiator at 5 parts by weight with respect to 100 parts by weight of the epoxy crosslinking agent.

Comparative Example 4

(38) A film was formed as described in Example 1, except that no second layer was included.

(39) TABLE-US-00001 TABLE 1 Contact Angle.sup.a WVTR.sup.b M1.sup.c M2.sup.d Tg 1.sup.e Tg 2.sup.f EXAMPLE 1 108 7.8 0.5 680 60 101 2 103 7.8 0.71 680 57 101 3 101 41.0 0.76 680 55 101 4 110 10.0 0.6 680 62 101 5 109 9.3 0.69 680 59 101 6 111 3.2 0.5 680 65 101 C. EXAMPLE 1 76 11 680 680 101 101 2 110 More 0.2 680 42 101 than 500 3 72 85 0.45 680 10 101 4 108 7.8 0.5 60 .sup.aContact Angle (Unit: ) of Base Resin of First Layer .sup.bWVTR (Unit: g/m.sup.2 .Math. day) of Base Resin of First Layer .sup.cTensile Modulus (Unit: MPa) of First Layer .sup.dTensile Modulus (Unit: MPa) of Second Layer .sup.eGlass Transition Temperature (Unit: C.) of Base Resin of First Layer After Curing .sup.fGlass Transition Temperature (Unit: C.) of Base Resin of Second Layer After Curing *C. EXAMPLE: Comparative Example

(40) TABLE-US-00002 TABLE 2 Moisture Durability Possibility Blocking and Adhesive to Apply Property.sup.g Reliability Strength.sup.h Panel EXAM- 1 2.7 Good 1650 No Bubbles PLE 2 3.1 Good 1799 No Bubbles 3 3.3 Good 2001 No Bubbles 4 2.8 Good 1242 No Bubbles 5 2.8 Good 1277 No Bubbles 6 2.5 Good 1547 No Bubbles C. 1 More Destroyed Impossible No Bubbles EXAM- than 5 to PLE Measure 2 More Good 2498 No Bubbles than 5 3 More Good 1542 No Bubbles than 5 4 2.2 Good 1650 Great Amount of Bubbles .sup.gLength of calcium oxidized in one direction from one surface (Unit: mm) .sup.hImpossible to measure refers that the specimen was destroyed without separation, (unit: gf/25 mm) *C. EXAMPLE: Comparative Example