Method for manufacturing sealing film

Abstract

The present application relates to a method for manufacturing an encapsulating film and a method for manufacturing an organic electronic device using the same, and provides a method for manufacturing an encapsulating film that can form a structure that can block moisture or oxygen from flowing into an organic electronic device from the outside and ensure the long-term reliability of the organic electronic device.

Description

[Technical Field]

[0001] The present application relates to a method for manufacturing a sealing film. [Background technology]

[0002] Organic electronic device (OED) refers to a device containing layers of organic materials that use holes and electrons to generate alternating currents of charge, and examples include photovoltaic devices, rectifiers, transmitters, and organic light emitting diodes (OLEDs).

[0003] Among the organic electronic devices, organic light emitting diodes (OLEDs) consume less power and have a faster response speed than conventional light sources, which is advantageous for making display devices or lighting thinner. OLEDs also have excellent space utilization, and are expected to be applied in various fields such as various portable devices, monitors, laptops, and TVs.

[0004] The biggest problem in the commercialization and expansion of OLED applications is durability. The organic materials and metal electrodes contained in OLEDs are easily oxidized by external factors such as moisture. Therefore, an encapsulation film with maximized moisture blocking properties is required. Summary of the Invention [Problem to be solved by the invention]

[0005] The present application provides a method for manufacturing an encapsulating film that can form a structure that can block moisture or oxygen from entering an organic electronic device from the outside and ensure long-term reliability of the organic electronic device.

[0006] The technical problems of the present application are not limited to those mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art from the following description. [Means for solving the problem]

[0007] Since the present invention can be modified in various ways and can have various embodiments, specific embodiments are illustrated in the drawings and described in detail, but it is not intended to limit the present invention to the specific embodiments, and it should be understood that the present invention includes all modifications, equivalents, and alternatives that fall within the spirit and technical scope of the present invention.

[0008] When an element such as a layer, region, or substrate is referred to as being "on" another component, it will be understood that this may be directly on the other element, or there may be intermediate elements therebetween.

[0009] The terms used in this application are merely used to describe specific embodiments and are not intended to limit the present invention. The singular expressions include the plural expressions unless the context clearly indicates otherwise. In this application, the terms "comprise" or "have" are intended to specify the presence of features, numbers, steps, operations, components, parts, or combinations thereof described in the specification, and should be understood not to preclude the possibility of the presence or addition of one or more other features, numbers, steps, operations, components, parts, or combinations thereof.

[0010] Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. Terms as defined in commonly used dictionaries should be interpreted to have a meaning consistent with the meaning they have in the context of the relevant art, and should not be interpreted as having an ideal or overly formal meaning unless expressly defined in this application.

[0011] The present application relates to a method for manufacturing an encapsulating film, which may be applied to seal or encapsulate an organic electronic device, such as an OLED.

[0012] As used herein, the term "organic electronic device" refers to an article or device having a structure including an organic material layer that generates an alternating current of charge using holes and electrons between a pair of opposing electrodes, examples of which include, but are not limited to, photovoltaic devices, rectifiers, transmitters, and organic light-emitting diodes (OLEDs). In one example of this application, the organic electronic device may be an OLED.

[0013] In an embodiment of the present application, the method for producing the encapsulating film may include mixing the encapsulating resin and the moisture adsorbent in a single step to produce a solventless encapsulating composition.

[0014] Here, the term "solvent-free type" means that the sealing composition does not substantially contain a solvent or contains a solvent in an amount of 0.1 wt% or less or 0.01 wt% or less based on the total amount of the sealing composition. That is, the sealing composition contains a solid content of 99 wt% or more or 100 wt%. The present application provides a sealing film that can be formed using raw materials with a solid content of 99 wt% or more or 100 wt% without the need for a separate solvent.

[0015] Furthermore, mixing the encapsulating resin and the moisture adsorbent in a single step means that the encapsulating resin and the moisture adsorbent are added simultaneously, or added successively immediately after the other is added, or added within at least 5 minutes, 3 minutes, or 100 seconds after the other is added. That is, this is different from a process in which a separate mixture is prepared by dissolving the moisture adsorbent using a solvent, and the mixture with the dissolved moisture adsorbent is then separately mixed with a resin or a solution in which the resin is dissolved to prepare a hermetic sealant composition.

[0016] One of the key challenges for OLED encapsulation films is to maximize moisture barrier properties to ensure long-term reliability. To ensure moisture barrier properties, the encapsulation film must contain a moisture adsorbent that can remove moisture or humidity that has penetrated the encapsulation film. In particular, to maximize moisture barrier properties, the moisture adsorbent must be well dispersed within the composition. Here, "dispersed" refers to a state in which particles are uniformly dispersed and not agglomerated to form clumps. Well-dispersed particles can also be separated from each other.

[0017] Conventionally, to prepare an encapsulating composition, a solvent-based resin solution is prepared by dissolving an encapsulating resin in a solvent, and a moisture adsorbent is dispersed in the solvent using a dispersant. This mixture is then added to the resin solution to form a coating liquid containing a resin and a moisture adsorbent. This requires two or more steps to prepare the coating liquid. To improve the dispersibility of the moisture adsorbent, a separate dispersant, such as an organic acid, must be used. However, the high viscosity of the coating liquid limits the extent to which the dispersant can improve the dispersibility of the moisture adsorbent. Furthermore, when a solvent is used to form the mixture, the solvent remains inside the film even after a subsequent solvent drying process, resulting in problems such as damage to the organic electronic device due to the involatilized solvent. Therefore, the present application provides an organic electronic device that maximizes the dispersibility of the moisture adsorbent and effectively ensures long-term reliability by using a solventless encapsulating composition by mixing an encapsulating resin and a moisture adsorbent in a single step and then preparing an encapsulating layer through extrusion, as described below.

[0018] In one example, the step of preparing the encapsulating composition may be performed under high-temperature conditions, for example, at a temperature of 50°C or higher and a pressure of 5 bar or higher. The temperature may be higher than the melting point of the resin, for example, 60°C or higher, 70°C or higher, 80°C or higher, 90°C or higher, 100°C or higher, 110°C or higher, 120°C or higher, 125°C or higher, 130°C or higher, 135°C or higher, 140°C or higher, 145°C or higher, or 150°C or higher. The upper limit of the temperature may be appropriately adjusted to a temperature at which the components added to the encapsulating composition do not thermally decompose, for example, 200°C or lower or 180°C or lower. The pressure may be 7 bar or higher, 10 bar or higher, 13 bar or higher, 15 bar or higher, 17 bar or higher, or 20 bar or higher. The upper limit of the pressure may be appropriately adjusted depending on the purpose, for example, 30 bar or lower. For example, but not limited thereto, the step of preparing the encapsulating composition may involve kneading the components in a kneader such as a kneader or a Banbury mixer, and the temperature of 50°C or higher and the pressure of 5 bar or higher may be the temperature or pressure in the kneader. In the present application, by performing the step of preparing the encapsulating composition at a specific temperature or higher, the components in the encapsulating composition are melt-kneaded to further improve the dispersibility of the moisture adsorbent, and the compatibility between the components in the composition is excellent, resulting in excellent workability in the extrusion process.

[0019] In one embodiment, the method for producing a seal film according to the present application may include transferring the seal composition prepared above to an extruder, compounding the compound, and extruding the compound at a temperature of 90°C or higher to produce a seal layer.

[0020] The extrusion temperature in the step of preparing the sealing layer refers to the internal temperature or molding temperature of the extruder. Here, the internal temperature of the extruder refers to the temperature in the section where the sealing composition transferred from the kneader to the extruder moves toward the discharge section by the screw in the extruder and is blended. Furthermore, the molding temperature refers to the temperature of the molding section attached to the discharge section of the extruder, for example, the temperature of the T-die. The molding temperature refers to the temperature in the section where the sealing composition is discharged and molded into a film by the molding section.

[0021] That is, the sealing composition according to the present invention is first kneaded in a kneader to uniformly disperse the moisture adsorbent, and then transferred to an extruder, where it is secondly kneaded using a screw installed in the extruder, thereby further improving the dispersion of the moisture adsorbent.

[0022] Although the extruder may be a single-screw extruder or a twin-screw extruder, a twin-screw extruder is preferred because of its excellent productivity and uniformity. The type and rotation direction of the screws in the twin-screw extruder may be appropriately selected depending on the components to be fed.

[0023] In one example, the temperature for producing the sealing layer by extrusion may be 100°C or higher, 110°C or higher, 120°C or higher, 125°C or higher, 130°C or higher, 135°C or higher, 140°C or higher, 145°C or higher, 150°C or higher, 155°C or higher, 160°C or higher, 165°C or higher, 170°C or higher, 175°C or higher, or 180°C or higher. The upper limit of the temperature may be appropriately adjusted to a temperature at which the components added to the sealing composition do not thermally decompose, and may be, for example, 200°C or lower or 180°C or lower. For example, the internal temperature of the extruder may be 140°C or higher, and the molding temperature may be 150°C or higher. For example, the difference between the internal temperature of the extruder and the molding temperature may be within 50°C or 30°C. In the present application, by controlling the internal temperature of the extruder within the above range, the moisture adsorbent may be uniformly dispersed in the sealing composition, and by controlling the molding temperature within the above range, the film properties may be improved.

[0024] In one example, the step of producing the encapsulating layer by extrusion is performed at a high pressure of 5 bar or more, thereby controlling the viscosity of the encapsulating composition within the range described below, thereby further improving the dispersibility of the moisture adsorbent. Although not limited thereto, the pressure in the extrusion step may be, for example, 6 bar or more, 7 bar or more, 10 bar or more, 11 bar or more, 12 bar or more, 13 bar or more, 14 bar or more, 15 bar or more, 16 bar or more, 17 bar or more, 18 bar or more, or 20 bar or more. The upper limit of the pressure may be appropriately adjusted depending on the purpose, and may be, for example, 30 bar or less.

[0025] In one example, the rotation speed of the screw in the extruder may be within a range of 100 to 400 rpm, 150 to 350 rpm, 170 to 320 rpm, 200 to 300 rpm, or 230 to 270 rpm. The present application utilizes the strong shear force generated by the rotation of the screw in the extruder to uniformly disperse the moisture adsorbent in the sealing composition, even if it is a solvent-free type.

[0026] In one embodiment, the manufacturing method according to the present application may further include a curing step of extruding the sealing layer by irradiating it with an electron beam or UV light. The irradiation with an electron beam or UV light may be carried out by a known method.

[0027] In one example, the encapsulation layer manufactured by the manufacturing method is a single layer, and in Gaussian curve fitting of the distribution of the moisture adsorbent in the thickness (depth) direction in the encapsulation layer, the positional distribution (σ value) of the moisture adsorbent in the thickness direction may be 2 or less.

[0028] For example, in Gaussian curve fitting to the thickness distribution of the moisture adsorbent, the position distribution (σ value) in the thickness direction of the moisture adsorbent may be 1.9 or less, 1.8 or less, 1.7 or less, 1.6 or less, 1.5 or less, 1.4 or less, 1.3 or less, 1.2 or less, 1.1 or less, 1 or less, 0.9 or less, 0.8 or less, 0.7 or less, 0.6 or less, 0.5 or less, 0.4 or less, 0.3 or less, 0.2 or less, 0.15 or less, or 0.1 or less, and the lower limit is not significantly limited, but may be 0.001 or more.

[0029] Here, the Gaussian curve fitting indicates a function for the thickness of the sealing layer, and is shown in Equation 1 below.

[0030]

number

[0031] In Equation 1, A and b are constants relating to the absolute amount of moisture adsorbent;

number

[0032] When the σ value in Gaussian curve fitting for the thickness distribution of the moisture adsorbent satisfies the specific range as described above, the moisture adsorbent may be contained in a high content in a region corresponding to the center of the sealing film in the thickness direction, thereby achieving excellent moisture adsorption properties and simultaneously improving adhesive properties.

[0033] That is, the encapsulating layer may include a first region, a second region, and a third region having different concentrations of the moisture adsorbent in the thickness direction. The encapsulating layer may not have a multi-layer structure, but may be divided into regions of the single layer according to the concentration of the moisture adsorbent. For example, the first region, the second region, and the third region forming the single encapsulating layer may have different moisture adsorbent contents. In this case, in relation to the division of the regions based on the moisture adsorbent content, the moisture adsorbent content at the interface of each region may vary continuously, and therefore the interface of each region does not necessarily need to be clearly defined.

[0034] In one example, the second region may have a higher moisture adsorbent content than the first and third regions. That is, the second region may have a higher moisture adsorbent content than the first and second regions. In this case, it is sufficient that the first and second regions have a lower moisture adsorbent content than the second region, and the moisture adsorbent contents of the first and second regions may be the same or different.

[0035] 1 illustrates a single-layer encapsulating layer with regions distinguished by moisture adsorbent content, and referring to FIG. 1, second region 22, which is a region with a high moisture adsorbent content, may be interposed between first region 21 and third region 23, which are regions with a low moisture adsorbent concentration. That is, first region 21 and third region 23, which are regions with a low moisture adsorbent content, are located on the upper or lower surface, respectively, forming the uppermost or lowermost portion of encapsulating layer 11, and may be in direct contact with other components that are in contact with the upper or lower portion of the encapsulating layer.

[0036] That is, according to the present invention, the moisture adsorbent contained in the sealing layer may be present in a particulate form that is not uniformly distributed within the sealing layer. Here, "distribution" refers to the manner in which particles fill a space, and is a concept that is distinct from "dispersion." The "uniformly distributed" state means that the moisture adsorbent is present at the same or substantially the same density in every part of the sealing layer or sealing film, and the particles are separated as far as possible from each other and uniformly filled within the space.

[0037] On the other hand, if the encapsulating layer in contact with the organic electronic device contains an excessive amount of moisture adsorbent in a uniformly distributed state, the moisture adsorbent will also be present in excess on the upper and lower surfaces of the uppermost and / or lowermost encapsulating layer. In this case, the adhesive performance of the encapsulating layer may be significantly reduced, which may result in problems such as reduced durability and reliability of the organic electronic device.

[0038] Therefore, conventional encapsulation films have a multilayer structure including at least two encapsulation layers. That is, to ensure excellent moisture barrier properties, an OLED encapsulant must include a moisture barrier layer as an essential component, and the moisture barrier layer must have excellent adhesive properties with the upper and / or lower components. A method of separately preparing a moisture barrier layer and an adhesive layer and then bonding them together to form an integrated structure has been considered. However, this method requires the preparation of multiple layers to ensure the required functionality, which can lead to problems such as increased costs, complicated processes, and reduced thinning efficiency. For example, when a multilayer encapsulation film is applied to an organic electronic device, the first encapsulation layer facing the organic electronic device contains no moisture adsorbent or contains only a small amount of moisture adsorbent, while the second encapsulation layer located on the opposite side from the organic electronic device contains a large amount of moisture adsorbent. This ensures adhesion from the first encapsulation layer in contact with the organic electronic device and moisture barrier properties from the second encapsulation layer.

[0039] However, the sealing layer according to the present application contains a moisture adsorbent at a high concentration in the center in the thickness (depth) direction of the sealing layer and at low concentrations on both surfaces of the sealing layer, thereby showing a specific distribution state of the moisture adsorbent. Therefore, the present application can provide a sealing film that exhibits above-optimal adhesion even without a separate adhesive layer or bonding layer, including a single-layer sealing layer, and also has excellent barrier properties. Therefore, the present application can provide a sealing film that can exhibit excellent moisture blocking properties and adhesion with only a single layer.

[0040] In one example, the encapsulating layer of the present application may be a single layer, but is not limited thereto and may have a multilayer structure including at least two encapsulating layers. When the encapsulating layer includes two or more encapsulating layers, the encapsulating layer may include a first encapsulating layer that faces the organic electronic element when encapsulating the element and a second encapsulating layer located on the opposite side of the first encapsulating layer facing the element. In one specific example, the encapsulating film may include at least two encapsulating layers, and the encapsulating layer may include a first encapsulating layer that faces the organic electronic element when encapsulating and a second encapsulating layer that does not face the organic electronic element. When the encapsulating layer includes two or more layers, the compositions of the layers may be the same or different. In one example, the encapsulating layer may include an encapsulating resin and / or a moisture absorbent, and the encapsulating layer may be a pressure-sensitive adhesive layer or an adhesive layer. For example, when the encapsulating film is applied to an organic electronic element, the first encapsulating layer, which is the encapsulating layer facing the organic electronic element, may contain no moisture adsorbent, or may contain only a small amount of moisture adsorbent of 5 wt % or less based on the total weight of the moisture adsorbent, and a large amount of moisture adsorbent as described below may be contained in the second encapsulating layer.

[0041] In one example, the metal adhesion strength of the encapsulating layer may be 4,000 gf / in or more, 4,200 gf / in or more, 4,400 gf / in or more, 4,600 gf / in or more, 4,800 gf / in or more, 5,000 gf / in or more, 5,100 gf / in or more, 5,200 gf / in or more, 5,300 gf / in or more, 5,400 gf / in or more, or 5,500 gf / in or more. That is, since the encapsulating film according to the present application has a different content of moisture adsorbent in the thickness direction as described above and a first region or a third region, which is a region with a low content of moisture adsorbent, is located on the upper surface or the lower surface of the encapsulating layer, the encapsulating layer according to the present application may have excellent metal adhesion strength. The metal adhesive strength is the adhesive strength to a metal layer that can be added onto the sealing layer, as described below, and may be measured by fixing the sealing film, which has been left in a constant temperature and humidity chamber at 85±5°C and 85±10% for 30 minutes, to a tensile machine (TA, Texture Analyzer) and measuring it in tension mode at 25°C and a tension speed of 5 mm / min.

[0042] In one example, the sealing layer manufactured from the above may have a gel content of 60% or more as measured by the following general formula 1:

[0043] [General Formula 1] Gel content (%) = A / B × 100

[0044] In General Formula 1, B represents the mass of the sealing layer sample, and A represents the dry mass of the insoluble portion of the sealing layer that does not pass through a 200-mesh mesh after immersing the sample in toluene at 60°C for 24 hours and then filtering the sample through a 200-mesh mesh. In this specification, the unit mesh may be an ASTM unit. The mass B of the sealing layer sample may be measured as 1 g. The gel content may be, for example, 63% or more, 65% or more, 67% or more, 70% or more, 72% or more, 75% or more, or 78% or more, and the upper limit may be, for example, 99% or less, 95% or less, 93% or less, 89% or less, 86% or less, 84% or less, 82% or less, or 80% or less. By adjusting the gel content, the present application can provide a sealing film that has excellent moisture barrier properties, stress absorption properties, and cured physical properties.

[0045] The encapsulating layer according to the present application may also have an acid value of 1 or less. The acid value may be, for example, 0.9 or less, 0.8 or less, or 0.7 or less. The lower limit is not particularly limited, but may be 0.1 or more. Unlike the conventional issues of moisture barrier properties and the occurrence of dark spots and bright spots in organic electronic devices, white spots occurring in organic electronic devices have recently become a major cause of panel defects. The present application has confirmed that the mechanism behind the occurrence of white spots is due to the organic acid present in the encapsulating composition. The occurrence of white spots can be effectively suppressed by adjusting the acid value of the encapsulating layer itself and the degree of crosslinking of the encapsulating layer matrix to the gel content. In a specific example, the organic acid reaches the organic electronic device in the form of ions and causes cracks that may form on the device, thereby shifting the threshold voltage and generating white spots. These technical issues can be avoided by adjusting the acid value and gel content of the encapsulating layer that encapsulates the entire surface of the organic electronic device.

[0046] Furthermore, the sealing layer according to the present application may have excellent light transmittance in the visible light region. In one example, the sealing composition according to the present application may exhibit a light transmittance of 80% or more in accordance with JIS K7105 after curing. For example, the sealing composition may have a light transmittance of 85% or more, 90% or more, 92% or more, or 93% or more in the visible light region. The sealing layer according to the present application may exhibit low haze along with excellent light transmittance. In one example, the sealing composition may have a haze of 5% or less, 4% or less, 3% or less, or 1% or less after curing, as measured according to JIS K7105. The optical properties may be measured at 550 nm using a UV-Vis spectrometer.

[0047] In one example, after curing the organic electronic element encapsulating layer, the yellow index (△YI) value measured according to ASTM D1003 standard using a colorimeter may be 1 or less, and the lower limit is not particularly limited, but may be -2 or more.

[0048] In one example, when the encapsulating layer is subjected to purge and trap at 100°C for 60 minutes using a Purge & Trap sampler (JAI JTD-505III-GC / MSD system (Agilent 7890B / 5977A)), and then the total outgassing amount is measured using gas chromatography mass spectrometry, the measured outgassing amount may be less than 400 ppm, specifically 300 ppm or less, 200 ppm or less, 100 ppm or less, 90 ppm or less, 80 ppm or less, 70 ppm or less, 50 ppm or less, 30 ppm or less, 20 ppm or less, or 10 ppm or less. That is, since the encapsulating layer according to the present invention includes the composition described below, the amount of outgassing generated from the encapsulating layer is small, and therefore, an organic electronic device to which the encapsulating layer is applied may have excellent reliability.

[0049] In one specific example, the encapsulating layer may have a thickness of 30 μm or more and 500 μm or less. The encapsulating layer of the present application may have a thickness of 30 μm or more, 33 μm or more, 35 μm or more, 40 μm or more, 43 μm or more, 45 μm or more, 47 μm or more, 50 μm or more, 52 μm or more, 55 μm or more, 57 μm or more, or 60 μm or more, and the upper limit is not particularly limited, and may be 500 μm or less, 400 μm or less, 300 μm or less, 250 μm or less, or 200 μm or less. The present application achieves a desired level of gel content while increasing the thickness of the encapsulating layer compared to conventional methods, thereby maximizing moisture barrier properties and absorbing stress when panel warpage occurs in harsh environments such as high temperatures, thereby providing a highly reliable organic electronic device. In the past, encapsulating films were formed by coating them to a certain thickness or more and then irradiating them with UV light, but this had problems such as the inability of UV light to penetrate deep into the film, resulting in significantly reduced curing properties, and the fact that the solvent remained inside the film, with some of the solvent remaining unvolatilized and uncured material damaging the organic electronic device. In particular, the encapsulating composition of the present application can encapsulate the entire surface of an organic electronic device and come into direct contact with one side of the organic electronic device. By using a solventless encapsulating composition having the composition described below without a separate dispersant, the reliability of the organic electronic device can be further improved. Furthermore, the encapsulating composition exhibits an improved curing rate even at a certain thickness or more, thereby realizing excellent curing properties as well as moisture barrier properties and stress absorption.

[0050] In one specific example, the encapsulating film 1 manufactured by the present application may include an encapsulating layer 11 and a substrate layer 12, as shown in Figure 2. The encapsulating film may seal the entire surface of an organic electronic device formed on a substrate.

[0051] In one example, the encapsulating composition of the present application may include an encapsulating resin, which may be a crosslinkable or curable resin, and in specific examples, may include an olefin-based resin.

[0052] In one example, the sealing resin may have a glass transition temperature of less than 0° C., less than −10° C., less than −30° C., less than −50° C., or less than −60° C. The lower limit is not particularly limited, and may be −150° C. or higher. The glass transition temperature may be the glass transition temperature after curing.

[0053] In one embodiment of the present application, the encapsulating resin may be an olefin-based resin. For example, the olefin-based resin may be a homopolymer of a butylene monomer, a copolymer obtained by copolymerizing a butylene monomer with another monomer polymerizable therewith, a reactive oligomer using a butylene monomer, or a mixture thereof. The butylene monomer may include, for example, 1-butene, 2-butene, or isobutylene. For example, the olefin-based resin may include polymerized units of isobutylene monomer.

[0054] Other monomers polymerizable with the butylene monomer or derivative may include, for example, isoprene, styrene, butadiene, etc. By using the copolymer, physical properties such as processability and degree of crosslinking can be maintained, and the heat resistance of the adhesive itself can be ensured when applied to an organic electronic device.

[0055] The reactive oligomer using a butylene monomer may include a butylene polymer having a reactive functional group. The oligomer may have a weight-average molecular weight in the range of 500 to 5,000 g / mol. The butylene polymer may be bonded to another polymer having a reactive functional group. The other polymer may be, but is not limited to, an alkyl (meth)acrylate. The reactive functional group may be a hydroxyl group, a carboxyl group, an isocyanate group, or a nitrogen-containing group. The reactive oligomer and the other polymer may be crosslinked with a multifunctional crosslinking agent, and the multifunctional crosslinking agent may be at least one selected from the group consisting of an isocyanate crosslinking agent, an epoxy crosslinking agent, an aziridine crosslinking agent, and a metal chelate crosslinking agent.

[0056] In one example, the encapsulating resin of the present application may include a copolymer of a diene and an olefinic compound containing one carbon-carbon double bond. Here, the olefinic compound may include butylene, etc., and the diene may be a monomer polymerizable with the olefinic compound, such as isoprene or butadiene, etc. For example, the copolymer of the olefinic compound containing one carbon-carbon double bond and the diene may be butyl rubber.

[0057] The resin or elastomer component in the sealing layer may have a weight-average molecular weight (Mw) sufficient to allow the PSA composition to be molded into a film. For example, the resin or elastomer may have a weight-average molecular weight of approximately 100,000 to 2,000,000 g / mol, 120,000 to 1,500,000 g / mol, 150,000 to 1,000,000 g / mol, 200,000 to 700,000 g / mol, 230,000 to 600,000 g / mol, 250,000 to 500,000 g / mol, or 300,000 to 470,000 g / mol. The term "weight-average molecular weight" used herein refers to a value measured by gel permeation chromatography (GPC) relative to standard polystyrene, and unless otherwise specified, the unit is g / mol. However, the resin or elastomer component does not necessarily have the weight-average molecular weight described above. For example, if the molecular weight of the resin or elastomer component is not sufficient to form a film, a separate binder resin may be added to the PSA composition.

[0058] In one example, the encapsulating resin may be included in the encapsulating layer at 10 wt % or more, 13 wt % or more, 15 wt % or more, 17 wt % or more, 20 wt % or more, 21 wt % or more, 22 wt % or more, 23 wt % or more, or 24 wt % or more, and the upper limit may be 90 wt % or less, 80 wt % or less, 70 wt % or less, 60 wt % or less, 50 wt % or less, 40 wt % or less, or 30 wt % or less. The encapsulating resin has good moisture barrier properties but a drawback of poor heat resistance durability. Therefore, the present application adjusts the content of the encapsulating resin to fully realize the moisture barrier properties of the resin itself while maintaining heat resistance durability at high temperatures and humidity.

[0059] In one example, the sealing film may include a moisture absorbent. As used herein, the term "moisture absorbent" refers to, for example, a chemically reactive absorbent that can remove moisture or humidity that has permeated the sealing film through a chemical reaction with the moisture or humidity, as described below.

[0060] In one example, the moisture adsorbent may be free of organic acids on its surface. Generally, moisture adsorbents may be surface-treated with a dispersant to ensure good dispersion within the composition, in which case the organic acid is present on the surface of the moisture adsorbent. Such organic acids may penetrate into the encapsulation layer, which is in direct contact with the device, and cause white dot defects in OLED panels. In the present application, the moisture adsorbent does not contain a dispersant or an organic acid, thereby improving the reliability of the entire encapsulation composition and preventing OLED panel defects.

[0061] Examples of the moisture adsorbent that can be used in the above-mentioned process include metal oxides, sulfates, and organic metal oxides. Specific examples of the sulfates include magnesium sulfate, sodium sulfate, and nickel sulfate, and examples of the organic metal oxides include aluminum oxide octylate. Specific examples of the metal oxides include phosphorus pentoxide (PO), lithium oxide (LiO), sodium oxide (NaO), barium oxide (BaO), calcium oxide (CaO), and magnesium oxide (MgO). Examples of the metal salts include sulfates such as lithium sulfate (LiSO), sodium sulfate (NaSO), calcium sulfate (CaSO), magnesium sulfate (MgSO), cobalt sulfate (CoSO), gallium sulfate (Ga(SO)), titanium sulfate (Ti(SO)), and nickel sulfate (NiSO), calcium chloride (CaCl), magnesium chloride (MgCl), and strontium chloride. Examples of suitable moisture adsorbents include, but are not limited to, metal halides such as strontium (SrCl2), yttrium chloride (YCl3), copper chloride (CuCl2), cesium fluoride (CsF), tantalum fluoride (TaF5), niobium fluoride (NbF5), lithium bromide (LiBr), calcium bromide (CaBr2), cerium bromide (CeBr3), selenium bromide (SeBr4), vanadium bromide (VBr3), magnesium bromide (MgBr2), barium iodide (BaI2) or magnesium iodide (MgI2), or metal chlorates such as barium perchlorate (Ba(ClO4)2) or magnesium perchlorate (Mg(ClO4)2). The moisture adsorbent that may be included in the sealing layer may be one or more of the above-mentioned compositions. In one example, when two or more types of moisture adsorbents are used, calcined dolomite may be used.

[0062] Such moisture adsorbents may be controlled to an appropriate size depending on the application. In one example, the average particle size of the moisture adsorbent may be controlled to 100 to 15,000 nm, 500 to 10,000 nm, 800 to 8,000 nm, 1 to 7 μm, 2 to 5 μm, or 2.5 to 4.5 μm. Moisture adsorbents having sizes within these ranges do not react too quickly with moisture, are easy to store, and do not damage the device to be encapsulated. Unless otherwise specified, particle size herein refers to the average particle size, and may be measured using a D50 particle size analyzer by a known method.

[0063] The content of the moisture adsorbent is not particularly limited and may be appropriately selected in consideration of the desired blocking properties. The moisture adsorbent may be included in an amount of 90 parts by weight or more relative to 100 parts by weight of the sealing resin, for example, 93 to 800 parts by weight, 95 to 770 parts by weight, 97 to 750 parts by weight, 100 to 730 parts by weight, 103 to 700 parts by weight, 105 to 670 parts by weight, 110 to 650 parts by weight, 113 to 630 parts by weight, 115 to 600 parts by weight, 117 to 570 parts by weight, 120 to 530 parts by weight, 123 to 500 parts by weight, or the like. parts by weight, 125 to 480 parts by weight, 127 to 460 parts by weight, 130 to 440 parts by weight, 133 to 420 parts by weight, 135 to 400 parts by weight, 137 to 380 parts by weight, 140 to 360 parts by weight, 143 to 340 parts by weight, 145 to 320 parts by weight, 150 to 300 parts by weight, 153 to 290 parts by weight, 155 to 280 parts by weight, 158 to 270 parts by weight, or 160 to 260 parts by weight. That is, the encapsulating film according to the present application may contain a larger amount of moisture adsorbent than conventional ones, yet exhibit excellent compatibility with other components in the encapsulating layer, and at the same time, exhibit excellent dispersibility for the moisture adsorbent without the need for a separate dispersant, thereby achieving an excellent moisture blocking effect.

[0064] In one example, the sealing film may further contain a tackifier. The tackifier may be, for example, a compound with a softening point of 70°C or higher. Specifically, the softening point may be 75°C or higher, 78°C or higher, 83°C or higher, 85°C or higher, 90°C or higher, or 95°C or higher. The upper limit is not particularly limited, but may be 150°C or lower, 145°C or lower, 140°C or lower, 135°C or lower, 130°C or lower, or 125°C or lower. The tackifier may be a compound having a cyclic structure within its molecular structure, and the cyclic structure may have 5 to 15 carbon atoms. The number of carbon atoms may be, for example, 6 to 14, 7 to 13, or 8 to 12. The cyclic structure may be a monocyclic compound, but is not limited thereto, and may also be a bicyclic or tricyclic compound. The tackifier may further be an olefin-based polymer, and the polymer may be a homopolymer or a copolymer. The tackifier of the present application may also be a hydrogenated compound. The hydrogenated compound may be a partially or fully hydrogenated compound. Such a tackifier may have good compatibility with other components in the sealing film, excellent moisture-blocking properties, and external stress relaxation properties. Specific examples of tackifiers include hydrogenated terpene resins, hydrogenated ester resins, and hydrogenated dicyclopentadiene resins. The weight-average molecular weight of the tackifier may be within the range of approximately 200 to 5,000 g / mol, 300 to 4,000 g / mol, 400 to 3,000 g / mol, or 500 to 2,000 g / mol. The content of the tackifier may be appropriately adjusted as needed. For example, the content of the tackifier may be 15 to 200 parts by weight, 20 to 190 parts by weight, 25 to 180 parts by weight, or 30 to 150 parts by weight per 100 parts by weight of the sealing resin. By using the specific tackifier, the present application can provide a sealing film that has excellent moisture-blocking properties and external stress relaxation properties.

[0065] In the encapsulating film of the present application, the encapsulating layer may contain a bright spot inhibitor. The bright spot inhibitor may have an adsorption energy of 0 eV or less with respect to outgassing, calculated by density functional theory. The lower limit of the adsorption energy is not particularly limited, but may be -20 eV. The type of outgassing is not particularly limited, but may include oxygen, H atoms, H2 molecules, and / or NH3. In the encapsulating film of the present application, the bright spot inhibitor can prevent bright spots caused by outgassing from an organic electronic device.

[0066] In a specific example of the present application, the adsorption energy between the bright spot inhibitor and the bright spot-causing atom or molecule can be calculated through electronic structure calculations based on density functional theory. This calculation may be performed using methods known in the art. For example, the present application creates a two-dimensional slab structure in which the close-packed surfaces of the bright spot inhibitor, which has a crystalline structure, appear on the surface, and then performs structural optimization. Then, structural optimization is performed on the structure in which the bright spot-causing molecule is adsorbed on the vacuum surface. The adsorption energy is defined as the difference in total energy between these two systems minus the total energy of the bright spot-causing molecule. To calculate the total energy for each system, a revised-PBE function, a function of the generalized gradient approximation (GGA) series, is used in exchange correlation, which simulates electron-electron interactions. A cutoff for the electron kinetic energy was set to 500 eV, and calculations were performed including only the gamma point corresponding to the origin of reciprocal space. The conjugate gradient method was used to optimize the atomic structure of each system, and calculations were repeated until the interatomic forces were below 0.01 eV / Å. The series of calculations was performed using the commercial code VASP.

[0067] The material of the bright spot inhibitor is not limited as long as it is a substance that can prevent bright spots on the panel of the organic electronic device when the encapsulating film is applied to the organic electronic device. For example, the bright spot inhibitor is an outgas generated from an inorganic deposition layer of silicon oxide, silicon nitride, or silicon oxynitride deposited on the electrode of the organic electronic device, such as oxygen, H2 gas, ammonia (NH3) gas, H + , N.H. 2+ , NHR2, or NH2R. In the above, R may be an organic group, such as, but not limited to, an alkyl group, an alkenyl group, or an alkynyl group.

[0068] In one example, the material of the bright spot inhibitor is not limited as long as it satisfies the adsorption energy value, and may be a metal or a non-metal. The bright spot inhibitor may include, for example, Li, Ni, Ti, Rb, Be, Mg, Ca, Sr, Ba, Al, Zn, In, Pt, Pd, Fe, Cr, Si, or a combination thereof, or may include an oxide or nitride of the above material, or an alloy of the above material. In one example, the bright spot inhibitor may include nickel particles, nickel oxide particles, titanium nitride, iron-titanium titanium alloy particles, iron-manganese manganese alloy particles, magnesium-nickel magnesium alloy particles, rare earth alloy particles, carbon nanotubes, graphite, aluminophosphate molecular particles, or mesosilica particles. The bright spot inhibitor may be included in an amount of 3 to 150 parts by weight, 6 to 143 parts by weight, 8 to 131 parts by weight, 9 to 123 parts by weight, 10 to 116 parts by weight, 10 to 95 parts by weight, 10 to 50 parts by weight, or 10 to 35 parts by weight, based on 100 parts by weight of the encapsulating resin. This content range allows the present application to realize bright spot prevention in an organic electronic device while improving the adhesive strength and durability of the film. The particle size of the bright spot inhibitor may be within the range of 10 nm to 30 μm, 50 nm to 21 μm, 105 nm to 18 μm, 110 nm to 12 μm, 120 nm to 9 μm, 140 nm to 4 μm, 150 nm to 2 μm, 180 nm to 900 nm, 230 nm to 700 nm, or 270 nm to 400 nm. The particle size may be measured by D50 particle size analysis. By including the bright spot inhibitor, the present application can efficiently absorb hydrogen generated in an organic electronic device while realizing moisture barrier properties and durable reliability of the encapsulation film.

[0069] In one example, the sealing layer of the present application may contain an active energy ray-polymerizable compound that is highly compatible with the sealing resin and can form a specific crosslinked structure together with the sealing resin.

[0070] For example, the encapsulating layer of the present application may include, together with the encapsulating resin, a polyfunctional active energy ray-polymerizable compound that can be polymerized by irradiation with active energy rays. The active energy ray-polymerizable compound refers to, for example, a compound containing two or more functional groups that can participate in a polymerization reaction by irradiation with active energy rays, such as a functional group containing an ethylenically unsaturated double bond, such as an acryloyl group or a methacryloyl group, an epoxy group, or an oxetane group.

[0071] As the multifunctional active energy ray polymerizable compound, for example, multifunctional acrylate (MFA) may be used.

[0072] The active energy ray-polymerizable compound may be contained in an amount of 0.5 to 10 parts by weight, 0.7 to 9 parts by weight, 1 to 8 parts by weight, 1.3 to 7 parts by weight, or 1.5 to 6 parts by weight relative to 100 parts by weight of the encapsulating resin. Within the above range, the present application provides an encapsulating film that has excellent durability and reliability even under harsh conditions such as high temperature and high humidity.

[0073] The polyfunctional active energy ray-polymerizable compound that can be polymerized by irradiation with active energy rays may be used without any limitation. For example, the compound may include 1,4-butanediol di(meth)acrylate, 1,3-butylene glycol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate (HDDA), 1,8-octanediol di(meth)acrylate, 1,12-dodecanediol di(meth)acrylate, neopentyl glycol di(meth)acrylate, dicyclopentanyl di(meth)acrylate, cyclohexane-1,4-dimethanol di(meth)acrylate, tricyclodecane dimethanol (meth)diacrylate, dimethyloldicyclopentane di(meth)acrylate, neopentyl glycol modified trimethylpropane di(meth)acrylate, adamantane di(meth)acrylate, trimethylolpropane tri(meth)acrylate (TMPTA), or mixtures thereof.

[0074] The polyfunctional active energy ray-polymerizable compound may be, for example, a compound having a molecular weight of 100 or more and less than 1,000 g / mol and containing two or more functional groups. The cyclic structure contained in the polyfunctional active energy ray-polymerizable compound may be a carbocyclic structure, a heterocyclic structure, or a monocyclic or polycyclic structure.

[0075] In the specific example of the present application, the sealing layer may further include a radical initiator. The radical initiator may be a photoinitiator or a thermal initiator. The specific type of photoinitiator may be appropriately selected taking into consideration the curing speed, the possibility of yellowing, and the like. For example, a benzoin-based, hydroxyketone-based, aminoketone-based, or phosphine oxide-based photoinitiator may be used. Specific examples include benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin n-butyl ether, benzoin isobutyl ether, acetophenone, dimethylaminoacetophenone, 2,2-dimethoxy-2-phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexylphenyl ketone, 2-methyl-1-[4-(methylthio)phenyl]-2-morpholino-propan-1-one, 4-(2-hydroxyethoxy)phenyl-2-(hydroxy-2-propan-1-one, 4 ... Phenyl ketone, benzophenone, p-phenylbenzophenone, 4,4'-diethylaminobenzophenone, dichlorobenzophenone, 2-methylanthraquinone, 2-ethylanthraquinone, 2-t-butylanthraquinone, 2-aminoanthraquinone, 2-methylthioxanthone, 2-ethylthioxanthone, 2-chlorothioxanthone, 2,4-dimethylthioxanthone, 2,4-diethylthioxanthone, benzyl dimethyl ketal, acetophenone dimethyl ketal, p-dimethylaminobenzoic acid ester, oligo[2-hydroxy-2-methyl-1-[4-(1-methylvinyl)phenyl]propanone], and 2,4,6-trimethylbenzoyl-diphenyl-phosphine oxide may also be used.

[0076] The radical initiator may be contained in an amount of 0.2 to 20 parts by weight, 0.5 to 18 parts by weight, 1 to 15 parts by weight, or 2 to 13 parts by weight relative to 100 parts by weight of the active energy ray-polymerizable compound, which can effectively induce the reaction of the active energy ray-polymerizable compound and prevent the physical properties of the sealing layer composition from being deteriorated by remaining components after curing.

[0077] In addition to the above-described components, the sealing layer may contain various additives depending on the intended use and the manufacturing process of the sealing film described below. For example, the sealing layer may contain a curable material, a crosslinking agent, a filler, or the like in an appropriate range of content depending on the desired physical properties.

[0078] In one example, the sealing composition is heated at 170° C. and 50 s -1 The viscosity measured at shear rate may be within a range of 1,000 to 2,000 Pa·s. For example, the lower limit of the viscosity may be 1,100 Pa·s or more, 1,200 Pa·s or more, 1,300 Pa·s or more, 1,400 Pa·s or more, or 1,500 Pa·s or more. Without being limited thereto, the viscosity may be measured using an Advanced Rheometric Expansion System (ARES). Although the encapsulating composition is a highly viscous liquid, the present application allows the moisture adsorbent to be uniformly dispersed within the encapsulating composition through the extrusion process, as described above.

[0079] In a specific example of the present application, the method for manufacturing a seal film according to the present application may further include a step of forming a metal layer on the seal layer. That is, the seal film may have a structure in which the seal layer and the metal layer are laminated together. The metal layer of the present application may have a thermal conductivity of 20 W / m·K or more, 50 W / m·K or more, 60 W / m·K or more, 70 W / m·K or more, 80 W / m·K or more, 90 W / m·K or more, 100 W / m·K or more, 110 W / m·K or more, 120 W / m·K or more, 130 W / m·K or more, 140 W / m·K or more, 150 W / m·K or more, 200 W / m·K or more, or 210 W / m·K or more. The upper limit of the thermal conductivity is not particularly limited and may be 800 W / m·K or less. Such high thermal conductivity allows for faster dissipation of heat generated at the bonding interface during the metal layer bonding process. In addition, high thermal conductivity allows heat accumulated during operation of the organic electronic device to be quickly released to the outside, thereby keeping the temperature of the organic electronic device itself lower and reducing the occurrence of cracks and defects. The thermal conductivity may be measured at any temperature in the range of 15 to 30°C.

[0080] The term "thermal conductivity" as used herein refers to the degree to which a material can transfer heat by conduction, and can be expressed in units of W / m K. This unit indicates the degree to which a material transfers heat at the same temperature and distance, and refers to the unit of heat (watts) relative to the unit of distance (meters) and the unit of temperature (Kelvin).

[0081] In a specific example of the present application, the metal layer of the sealing film may be transparent or opaque. The thickness of the metal layer may be within a range of 3 μm to 200 μm, 10 μm to 100 μm, 20 μm to 90 μm, 30 μm to 80 μm, or 40 μm to 75 μm. The present application provides a thin sealing film with sufficient heat dissipation effect by controlling the thickness of the metal layer. The metal layer may be a thin metal foil or a polymer substrate layer onto which a metal is vapor-deposited. The metal layer is not particularly limited as long as it satisfies the above-mentioned thermal conductivity and contains a metal. The metal layer may include any of metal, metal oxide, metal nitride, metal carbide, metal oxynitride, metal oxyboride, and combinations thereof. For example, the metal layer may include an alloy in which one metal is added with one or more metallic or non-metallic elements, such as stainless steel (SUS). Also, in one example, the metal layer may include iron, chromium, copper, aluminum nickel, iron oxide, chromium oxide, silicon oxide, aluminum oxide, titanium oxide, indium oxide, tin oxide, indium tin oxide, tantalum oxide, zirconium oxide, niobium oxide, and combinations thereof. The metal layer may be deposited by electrolysis, rolling, thermal evaporation, electron beam evaporation, sputtering, reactive sputtering, chemical vapor deposition, plasma enhanced chemical vapor deposition, or electron cyclotron resonance plasma enhanced chemical vapor deposition means. In one embodiment of the present application, the metal layer may be deposited by reactive sputtering.

[0082] The sealing film may have a structure in which the sealing layer is formed on a substrate film or a release film (hereinafter, sometimes referred to as a "first film"), and the structure may further include a substrate film, a protective film, or a release film (hereinafter, sometimes referred to as a "second film") formed on the metal layer.

[0083] The specific type of the first film that can be used in the present application is not particularly limited. In the present application, for example, a polymer film commonly used in this field may be used as the first film. In the present application, for example, a polyethylene terephthalate film, a polytetrafluoroethylene film, a polyethylene film, a polypropylene film, a polybutene film, a polybutadiene film, a vinyl chloride copolymer film, a polyurethane film, an ethylene-vinyl acetate film, an ethylene-propylene copolymer film, an ethylene-ethyl acrylate copolymer film, an ethylene-methyl acrylate copolymer film, or a polyimide film may be used as the base film or release film. Furthermore, one or both sides of the base film or release film of the present application may be subjected to an appropriate release treatment. Examples of release agents used in the release treatment of the base film include alkyd-based, silicone-based, fluorine-based, unsaturated ester-based, polyolefin-based, and wax-based release agents. Among these, alkyd-based, silicone-based, and fluorine-based release agents are preferred in terms of heat resistance, but the present application is not limited thereto.

[0084] In the present application, the thickness of the base film or release film (first film) as described above is not particularly limited and may be appropriately selected depending on the application. For example, in the present application, the thickness of the first film may be about 10 μm to 500 μm, preferably about 20 μm to 200 μm. If the thickness is less than 10 μm, deformation of the base film may easily occur during the manufacturing process, and if it exceeds 500 μm, economic efficiency decreases.

[0085] The present application further relates to organic electronic devices.

[0086] 2, the organic electronic device may include a substrate 31, an organic electronic element 32 formed on the substrate 31, and an encapsulation film manufactured by the above-described manufacturing method to encapsulate the organic electronic element 32. The encapsulation film may include an encapsulation layer 33 and may further include a metal layer 34. In this case, the encapsulation film, which integrally includes the encapsulation layer 33 and the metal layer 34, may encapsulate the organic electronic element 32. When the encapsulation film includes a metal layer, the organic electronic device may include the substrate 31, the organic electronic element 32, the encapsulation layer 33, and the metal layer 34, in that order.

[0087] In one example, the encapsulating film may encapsulate the entire surface, for example, both the top and side surfaces, of an organic electronic element formed on a substrate. The encapsulating film may include an encapsulating layer containing a pressure-sensitive adhesive composition or an adhesive composition in a crosslinked or cured state. Furthermore, an organic electronic device may be formed by sealing the entire surface of the organic electronic element formed on a substrate with the encapsulating layer in contact with the surface.

[0088] In a specific example of the present application, the organic electronic device may include a pair of electrodes, an organic layer including at least an emitting layer, and a passivation film. Specifically, the organic electronic device may include a first electrode layer, an organic layer formed on the first electrode layer and including at least an emitting layer, and a second electrode layer formed on the organic layer, and a passivation film including an electrode and an organic layer on the second electrode layer. The first electrode layer may be a transparent electrode layer or a reflective electrode layer, and the second electrode layer may also be a transparent electrode layer or a reflective electrode layer. More specifically, the organic electronic device may include a transparent electrode layer formed on a substrate, an organic layer formed on the transparent electrode layer and including at least an emitting layer, and a reflective electrode layer formed on the organic layer.

[0089] The organic electronic device may be, for example, an organic light emitting device.

[0090] The passivation film may include an inorganic film and an organic film. In one specific example, the inorganic film may be an oxide or nitride of at least one metal selected from the group consisting of Al, Zr, Ti, Hf, Ta, In, Sn, Zn, and Si. The thickness of the inorganic film may be 0.01 μm to 50 μm, 0.1 μm to 20 μm, or 1 μm to 10 μm. In one example, the inorganic film of the present application may be an inorganic material containing no dopant or a dopant. The dopant may be at least one element selected from the group consisting of Ga, Si, Ge, Al, Sn, Ge, B, In, Tl, Sc, V, Cr, Mn, Fe, Co, and Ni, or an oxide of the element, but is not limited thereto. The organic film is distinguished from the aforementioned organic layer containing at least a light-emitting layer in that it does not contain a light-emitting layer, and may be an organic vapor-deposited layer containing an epoxy compound.

[0091] The inorganic or organic film may be formed by chemical vapor deposition (CVD). For example, the inorganic film may be silicon nitride (SiNx). In one example, silicon nitride (SiNx) used as the inorganic film may be deposited to a thickness of 0.01 μm to 50 μm. In another example, the thickness of the organic film may be within a range of 2 μm to 20 μm, 2.5 μm to 15 μm, or 2.8 μm to 9 μm.

[0092] The present application further provides a method for manufacturing an organic electronic device. The method may include applying an encapsulation film obtained by the method to a substrate having an organic electronic device formed thereon so as to cover the organic electronic device. The method may also include curing the encapsulation film. The curing of the encapsulation film refers to the curing of an encapsulation layer, and may be performed before or after the encapsulation film covers the organic electronic device.

[0093] As used herein, the term "curing" means that the pressure-sensitive adhesive composition of the present invention forms a crosslinked structure through a heating or UV irradiation process, etc., to prepare the pressure-sensitive adhesive, or that the adhesive composition is solidified and adhered as an adhesive.

[0094] Specifically, an electrode may be formed on a glass or polymer film substrate by vacuum deposition or sputtering, a layer of a light-emitting organic material, such as a hole transport layer, a light-emitting layer, and an electron transport layer, may be formed on the electrode, and an electrode layer may be further formed thereon to form an organic electronic device. Next, the entire surface of the organic electronic device on the substrate that has undergone the above process may be covered with the encapsulating layer of the encapsulating film. [Effects of the Invention]

[0095] The present application provides a method for manufacturing an encapsulating film that can form a structure that can block moisture or oxygen from entering an organic electronic device from the outside and ensure long-term reliability of the organic electronic device.

[0096] However, the effects of the present invention are not limited to those mentioned above, and other effects not mentioned will be clearly understood by those skilled in the art from the following description. [Brief explanation of the drawings]

[0097] [Figure 1] FIG. 1 is a cross-sectional view illustrating an encapsulation layer according to an example of the present application. [Figure 2] FIG. 2 is a cross-sectional view showing a sealing film according to an example of the present application. [Figure 3] FIG. 3 is a cross-sectional view of an organic electronic device according to an example of the present application. DETAILED DESCRIPTION OF THE INVENTION

[0098] The present invention will be described in more detail below through examples according to the present invention and comparative examples not according to the present invention, but the scope of the present invention is not limited to the following examples.

[0099] Example 1 100 parts by weight of butyl rubber resin (Mw: 410,000 g / mol, glass transition temperature: -65°C), 100 parts by weight of tackifier resin (SU525, softening point: 125°C, Kolon), 3 parts by weight of multifunctional acrylate (tricyclodecane dimethanol diacrylate, Miwon), 1 part by weight of photoinitiator (Irgacure 651, Ciba), and 200 parts by weight of CaO were charged into a pressure kneader set at 150°C and 20 bar, and then kneaded for about 30 minutes, followed by heating at 170°C and 50 seconds. -1 A sealing composition with a viscosity of 1500 Pa·s at shear rate was produced.

[0100] The sealing composition was transferred to a twin-screw extruder (TEK30, manufactured by SM Platek) set at a temperature of 180°C and a screw rotation speed of 250 rpm, and compounded. The compound was then extruded at a temperature of 160°C and a pressure of 20 bar using a T-die attached to the twin-screw extruder to produce a film-like sealing layer having a thickness of 50 μm. The sealing layer was subjected to a load of 1.5 J / cm. 2 The film was irradiated with ultraviolet light to produce a sealing film.

[0101] Example 2 A sealing layer was produced in the same manner as in Example 1, except that the temperature of the T-die was set to 170°C.

[0102] Example 3 A sealing layer was produced in the same manner as in Example 1, except that the temperature of the T-die was set to 180°C.

[0103] Comparative Example 1 100 parts by weight of butyl rubber resin (Mw: 410,000 g / mol), 100 parts by weight of tackifier resin (SU525, Melting point: 125°C, Kolon), 3 parts by weight of multifunctional acrylate (tricyclodecane dimethanol diacrylate, Miwon), 1 part by weight of photoinitiator (Irgacure 651, Ciba), and 200 parts by weight of CaO were blended with 600 parts by weight of toluene, and 0.5 parts by weight of dispersant (oleic acid) per 100 parts by weight of CaO was further added and mixed thoroughly to prepare a solution with a solid content of 40 wt%.

[0104] The solution was coated onto release PET, dried in an oven at 120°C, and then subjected to a 1.5 J / m 2 The film was irradiated with ultraviolet light to produce a sealing film.

[0105] Comparative Example 2 A sealing layer was produced in the same manner as in Example 1, except that the temperature of the twin-screw extruder was set to 120°C.

[0106] Comparative Example 3 A sealing layer was produced in the same manner as in Example 1, except that the temperature of the T-die was set to 120°C.

[0107] Comparative Example 4 The sealing layer was produced in the same manner as in Example 1, except that the pressure in the T-die was set to 10 bar.

[0108] Comparative Example 5 The sealing layer was prepared in the same manner as in Example 1, except that the moisture adsorbent was added in an amount of 80 parts by weight.

[0109] Experimental Example 1 - Measurement of gel content The sealing films of the Examples and Comparative Examples were prepared into 50 mm x 50 mm test pieces, and 0.3 to 0.4 g of the sealing film (initial weight: A) was taken from each sealing film test piece. The sealing film was then immersed in 70 g of toluene at 60°C for 3 hours. The gel portion was then filtered through a 200-mesh wire mesh (weight of wire mesh: M) and dried in an oven at 125°C for 1 hour. The combined weight (G) of the gel and wire mesh was measured, and the dry mass (B = GM) of the insoluble portion of the sealing film that did not pass through the mesh was used to calculate the gel content (unit: %) using the following general formula 1.

[0110] [General Formula 1] Gel content (unit: %) = (B / A) × 100

[0111] In the general formula 1, A represents the initial mass of the seal film specimen, and B represents the dry mass of the insoluble portion of the seal film that does not pass through a 200 mesh (pore size 200 μm) mesh after immersing the seal film specimen in 70 g of toluene at 60°C for 3 hours and then filtering the seal film specimen through the 200 mesh (pore size 200 μm) mesh.

[0112] Experimental Example 2 - Measurement of swelling index A certain amount of the sealing film according to the Examples or Comparative Examples was placed in a bottle, filled with toluene, and stored for 24 hours to obtain a sol-gel solution. The gel sample was then separated from the sol-gel solution using a 200 mesh (pore size 200 μm) and immediately weighed (X). The resulting gel sample was dried in an oven at 80°C for 12 hours, and immediately after drying, the weight (Y) of the gel sample was measured. The swelling index was calculated using the above values ​​according to the following general formula 2.

[0113] [General Formula 2] Swelling index = weight of gel sample immediately after separation from sol-gel solution (X) / weight of gel sample immediately after drying (Y)

[0114] Experimental Example 3: Measurement of storage modulus The sealing films according to the Examples and Comparative Examples were laminated to a thickness of 600 μm to obtain specimens, and the specimens were measured using parallel plates in the Temp Sweep mode of an ARES (Advanced Rheometric Expansion System, ARES-G2, TA Corporation). Specifically, the specimens were subjected to a deformation of 15.0 rad / s at a strain of 0.1% in the temperature range of 30 to 100°C, and the storage modulus was measured, and the value at a temperature of 50°C was shown.

[0115] Experimental Example 4 - Measurement of moisture permeability distance The sealing films of the examples and comparative examples, each 30 mm x 60 mm, were left in a constant temperature and humidity chamber at 85°C and 85% relative humidity for 895 hours, and the distance that moisture had penetrated was measured using a microscope.

[0116] Experimental Example 5 - Metal Adhesion The sealing films according to the examples and comparative examples were heat-laminated at 75°C onto a 200mm x 220mm Cu surface, cut into 25mm pieces, and then further laminated onto the Cu surface using a 2kg roller to prepare test specimens. The test specimens were left in a constant temperature and humidity chamber at 85°C and 85% for 30 minutes, and then fixed to a tensile tester to measure the metal adhesion strength under the following conditions.

[0117] <Measurement conditions> Measuring equipment: Texture Analyzer Mode: Tension Mode Measurement temperature: 25℃ Tensile speed: 5 mm / min

[0118] Table 1 below summarizes the results of the above-mentioned experimental examples for the sealing films produced in the examples and comparative examples.

[0119] [Table 1] [Explanation of symbols]

[0120] 1: Sealing film 11: Sealing layer 12: Base material layer 3:Organic electronic devices 31: Circuit board 32: Organic electronic devices 33: Sealing layer 34: Metal layer

Claims

1. Mixing the encapsulating resin and the moisture absorbent in a single step to prepare a solventless encapsulating composition; and extruding the sealing composition at a temperature of 90°C or higher to form a sealing layer; The method for producing a sealing film, wherein the sealing composition has a viscosity measured at 170° C. and a shear rate of 50 s −1 in the range of 1,000 to 2,000 Pa·s.

2. The method of claim 1 , wherein the step of preparing the sealing composition is performed at a temperature of 50° C. or more and a pressure of 5 bar or more.

3. The method of claim 1 , wherein the extrusion step of forming the sealing layer is performed at a pressure of 5 bar or more.

4. The method for producing a seal film according to claim 1 , wherein the step of extruding the seal composition is performed using a twin-screw extruder.

5. The method for producing a seal film according to claim 4, wherein the screw rotation speed of the twin-screw extruder is within a range of 100 to 400 rpm.

6. The method for producing a seal film according to claim 1 , wherein the seal layer is a single layer or a multi-layer structure including two or more seal layers.

7. 2. The method for producing a seal film according to claim 1, wherein the seal layer has a gel content of 60% or more as measured by the following general formula 1: [General formula 1] Gel content (%) = A / B x 100 In General Formula 1, B represents the mass of a 50 mm x 50 mm specimen prepared from the sealing layer, and A represents the dry mass of the insoluble portion of the sealing layer that did not pass through a 200-mesh screen after immersing the specimen in toluene at 60°C for 24 hours and then filtering the specimen through the screen.

8. The method for producing a sealing film according to claim 1 , wherein the sealing resin contains an olefin-based resin.

9. The method for producing a sealing film according to claim 1 , wherein the sealing resin is contained in the sealing material in an amount of 10% by weight or more.

10. The method for producing a sealing film according to claim 1 , wherein the moisture adsorbent is a chemically reactive adsorbent.

11. The method for producing a sealing film according to claim 1 , wherein the moisture adsorbent is contained in an amount of 90 parts by weight or more with respect to 100 parts by weight of the sealing resin.

12. The method for producing a sealing film according to claim 1 , wherein the sealing composition further comprises a tackifier.

13. The method for producing a sealing film according to claim 12, wherein the tackifier is contained in a range of 15 to 200 parts by weight with respect to 100 parts by weight of the sealing resin.

14. The method for producing a sealing film according to claim 1 , wherein the sealing composition further contains an active energy ray-polymerizable compound.

15. The method for producing a sealing film according to claim 14, wherein the active energy ray polymerizable compound is contained in a range of 0.5 to 10 parts by weight based on 100 parts by weight of the sealing resin.

16. The method for producing a sealing film according to claim 1 , wherein the sealing composition further comprises a radical initiator.

17. The method for producing an encapsulating film according to claim 1 , wherein the encapsulating layer is in direct contact with an organic electronic element.

18. The method of claim 1 , further comprising forming a metal layer on the encapsulation layer.

19. 10. A method for manufacturing an organic electronic device, comprising: applying the encapsulation film of claim 1 to a substrate having an organic electronic device formed thereon so as to cover the organic electronic device.

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