WO2015147600A1 - Film d'étanchéification et dispositif électronique organique comprenant ledit film - Google Patents

Film d'étanchéification et dispositif électronique organique comprenant ledit film Download PDF

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Publication number
WO2015147600A1
WO2015147600A1 PCT/KR2015/003067 KR2015003067W WO2015147600A1 WO 2015147600 A1 WO2015147600 A1 WO 2015147600A1 KR 2015003067 W KR2015003067 W KR 2015003067W WO 2015147600 A1 WO2015147600 A1 WO 2015147600A1
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Prior art keywords
resin
film
encapsulation
layer
electronic device
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PCT/KR2015/003067
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English (en)
Korean (ko)
Inventor
조윤경
유현지
배경열
장석기
이정형
최준례
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LG Chem Ltd
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LG Chem Ltd
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Priority to JP2017502552A priority Critical patent/JP6410066B2/ja
Priority to CN201580027885.7A priority patent/CN106415875B/zh
Priority to EP15767907.7A priority patent/EP3125328B1/fr
Priority to US15/129,349 priority patent/US10103353B2/en
Priority claimed from KR1020150043390A external-priority patent/KR101687479B1/ko
Publication of WO2015147600A1 publication Critical patent/WO2015147600A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/80—Constructional details
    • H10K50/84—Passivation; Containers; Encapsulations
    • H10K50/846—Passivation; Containers; Encapsulations comprising getter material or desiccants

Definitions

  • the present application relates to an encapsulation film, an organic electronic device including the same, and a manufacturing method of the organic electronic device using the same.
  • An organic electronic device refers to a device including an organic material layer that generates an exchange of electric charges using holes and electrons, and examples thereof include a photovoltaic device, a rectifier, Transmitters and organic light emitting diodes (OLEDs); and the like.
  • an organic light emitting diode has a low power consumption, a fast response speed, and is advantageous for thinning a display device or lighting, as compared with a conventional light source.
  • OLED has excellent space utilization, and is expected to be applied in various fields including various portable devices, monitors, notebooks, lighting, and TVs.
  • Patent Document 1 In the commercialization of OLEDs and the expansion of their use, the main problem is durability. Organic materials and metal electrodes included in the OLED are very easily oxidized by external factors such as moisture. Therefore, products containing OLEDs are highly sensitive to environmental factors. Accordingly, various methods have been proposed to effectively block the penetration of oxygen or moisture from the outside into organic electronic devices such as OLEDs, for example, Patent Document 1.
  • the backlight unit of the OLED display device includes a diffusion film, and the diffusion film diffuses the light generated from the light source to make the image of the light source invisible and maintains the brightness of the entire screen without damaging the brightness of the light source. Is required.
  • the diffuser film scatters the light emitted from the light guide plate and enters the display screen to uniform the luminance distribution.
  • the diffuser film includes a transparent film in which transparent fillers are dispersed on a transparent polyester film surface and a regular reflection type in which a silver thin film is laminated. There is a milky white diffuse reflective film that diffusely reflects white like film and paper.
  • Patent Document 1 US Patent No. 6,226,890
  • the present application provides an encapsulation film and an organic electronic device including the same, which not only effectively block moisture or oxygen introduced into the organic electronic device from the outside, but also satisfy light diffusion and light extraction effects.
  • the present application relates to an encapsulation film.
  • the encapsulation film may be applied to encapsulation of an organic electronic device.
  • the encapsulation film of the present application may be applied to, for example, a side through which light is transmitted in an organic electronic device such as an OLED.
  • organic electronic device means an article or device having a structure including an organic material layer that generates an exchange of electric charge using holes and electrons between a pair of electrodes facing each other.
  • the photovoltaic device, a rectifier, a transmitter, and an organic light emitting diode (OLED) may be mentioned, but is not limited thereto.
  • the organic electronic device may be an OLED.
  • Exemplary encapsulation film may be composed of a single layer or two or more layers. In one example, when the encapsulation film is composed of two or more layers, it may include a first layer and a second layer to be described later.
  • the encapsulation film may include an encapsulation layer including an encapsulation resin, a hygroscopic filler and a nonhygroscopic filler.
  • the encapsulation layer may include 1 to 40 parts by weight of a hygroscopic filler and 1 to 10 parts by weight of a nonhygroscopic filler.
  • the encapsulation film may exhibit 70% or more light transmittance in the visible light region, or may have a haze of 50% or more.
  • the unit "parts by weight” means a weight ratio between each component.
  • the encapsulation film may include at least one or more first layers and at least one or more second layers, wherein the first layer includes an encapsulating resin and a hygroscopic filler, and a second The layer may comprise an encapsulating resin and a nonhygroscopic filler.
  • the first layer may not include a nonhygroscopic filler and the second layer may not include a hygroscopic filler. 1 and 2, specifically, as shown in FIG. 1, when the encapsulation layer of the present application is formed as a single layer, the single layer itself may constitute the encapsulation layer 3, and is non-hygroscopic filler 4.
  • the encapsulation layer 3 when the encapsulation layer 3 is formed in two or more layers, the encapsulation layer 3 includes the first layer 3a including the hygroscopic filler 4 and the nonhygroscopic filler 5. It may include a second layer (3b) comprising a.
  • the 1st layer 3a and the 2nd layer 3b can comprise the sealing layer 3 together, and the lamination order of the 1st layer 3a and the 2nd layer 3b is not specifically limited.
  • the first layer may be directly attached to the second layer. In the present specification, "direct adhesion" may mean that no other layer exists between the two layers.
  • the composition constituting the first layer 3a and the second layer 3b may be the same or different except for the kind of the filler.
  • the sealing resin, the dispersing agent, etc. of the first layer 3a and the second layer 3b may be the same or different from each other.
  • the thickness of the first layer and the second layer may be the same or different.
  • the thickness of the first layer may be 10 ⁇ m to 100 ⁇ m, 10 ⁇ m to 80 ⁇ m, 20 ⁇ m to 60 ⁇ m, or 20 ⁇ m to 40 ⁇ m
  • the thickness of the second layer may be 10 ⁇ m to 100 ⁇ m.
  • the thickness of each layer can be 10 micrometers or more, and impact resistance can be ensured.
  • moisture penetration into a side surface can be suppressed by making thickness of each layer into 100 micrometers or less.
  • the thickness of the second layer may be 30 ⁇ m or less in terms of moisture barrier properties.
  • the ratio of the thickness of the second layer to the thickness of the first layer can be at least 1, at least 1.1, at least 1.2, or at least 1.3.
  • the thickness of the single layer is 10 to 100 ⁇ m, 10 to 95 ⁇ m, 10 to 90 ⁇ m, 13 to 85 ⁇ m, 15 to 80 ⁇ m, 20 to 70 ⁇ m or 25 to 65 ⁇ m.
  • the encapsulation film of the present application may control the above-described content range as well as the thickness range as described above, thereby effectively realizing a water barrier effect and light extraction efficiency simultaneously.
  • the encapsulation film may have excellent light transmittance in the visible light region.
  • the encapsulation film of the present application can exhibit a light transmittance of 80% or more in the visible light region.
  • the encapsulation film including the encapsulation layer may maintain transparency.
  • the encapsulation film formed by applying and drying the encapsulation layer containing the hygroscopic filler or the non-hygroscopic filler so as to have a thickness of 50 ⁇ m is 80%, 81%, 82%, or 83% in the visible light region. It may have the above light transmittance.
  • the encapsulation film can adjust haze with excellent light transmittance.
  • the non-hygroscopic filler may provide a haze-controlled encapsulation film while imparting haze characteristics of the encapsulation layer.
  • the encapsulation film formed under the same conditions for measuring light transmittance may exhibit at least 50%, at least 55%, at least 60%, at least 70%, at least 73%, or at least 75% haze. Since the haze value is higher, the light extraction efficiency can be improved, and the upper limit thereof is not particularly limited, and may be, for example, 100%.
  • the light transmittance and haze in the above can be measured, for example, with a light transmittance at 550 nm using a UV-Vis Spectrometer for the encapsulation film, and can be measured with a haze according to JIS K7105 standard test method using a haze meter. have.
  • the total light transmittance of the encapsulation layer is As described above, it may be 70% or more, and the haze may be 50% or more.
  • the present application may include a non-hygroscopic filler in addition to the hygroscopic filler, in order to optimize the light extraction efficiency, it is possible to optimize the scattering while maintaining the transmittance as high as possible.
  • the light transmittance or haze of the encapsulation film may be implemented by controlling the types of hygroscopic fillers or non-hygroscopic fillers described below, content ratios of the fillers, average particle diameters, and refractive index differences.
  • the encapsulation layer of the encapsulation film has a water vapor transmission rate (WVTR) of 50 g / m 2 ⁇ day or less, preferably 30 g / m 2 ⁇ day or less, more preferably 20 g / m 2 ⁇ day or less, more preferably 15 g / m 2 ⁇ day or less.
  • WVTR water vapor transmission rate
  • the moisture permeability is the moisture permeability measured in the thickness direction of the encapsulation layer under 38 ° C. and 100% relative humidity after the encapsulation layer is formed into a film having a thickness of 100 ⁇ m.
  • the moisture permeability is measured according to ASTM F1249.
  • the present application may exhibit light diffusion and extraction effects by controlling light transmittance and haze in the above-described numerical range, and further controlling moisture permeability in the above-mentioned numerical range, thereby simultaneously controlling light diffusion and extraction effects and moisture blocking properties. Can be satisfied at the same time.
  • the encapsulation layer of the encapsulation film may include 1 to 40 parts by weight of the hygroscopic filler and 1 to 10 parts by weight of the nonhygroscopic filler. That is, when formed as a single layer, 1 to 40 parts by weight of the hygroscopic filler and 1 to 10 parts by weight of the non-hygroscopic filler may be included on the encapsulation layer.
  • the first layer may include a hygroscopic filler
  • the second layer may include a non-hygroscopic filler
  • the hygroscopic filler included in the first layer and the non-hygroscopic filler included in the second layer may be 1 to 1.
  • the hygroscopic filler and the non-hygroscopic filler are 1 to 40 parts by weight and 1 to 10 parts by weight; 1 to 35 parts by weight and 1 to 9 parts by weight; 1 to 30 parts by weight and 1 to 8 parts by weight; 1 to 25 parts by weight and 1 to 7 parts by weight; 1 to 20 parts by weight and 1 to 6 parts by weight; 1 to 15 parts by weight and 1 to 6 parts by weight; 2 to 13 parts by weight and 2 to 6 parts by weight; Or it may be included in the encapsulation layer in a weight ratio of 3 to 12 parts by weight and 2 to 5 parts by weight.
  • the encapsulation film of the present application by controlling the content of the hygroscopic filler and the non-hygroscopic filler as described above, not only effectively block the water or oxygen flowing into the organic electronic device, but also satisfy the light diffusion and extraction effect at the same time.
  • the hygroscopic filler of the present application has an average particle diameter of, for example, 10 nm to 5 ⁇ m, 20 nm to 5 ⁇ m, 30 nm to 4 ⁇ m, 40 nm to 4 ⁇ m, 50 nm to 3 ⁇ m, 60 nm to 3 ⁇ m, 70 nm to 2 ⁇ m, and 80 nm. To 2 ⁇ m, 90 nm to 1 ⁇ m, or 100 nm to 1 ⁇ m.
  • the average particle diameter of the hygroscopic filler By adjusting the average particle diameter of the hygroscopic filler to 5 ⁇ m or less to ensure the transparency of the film, can satisfy the desired light transmittance value in the present application, by adjusting to 10nm or more to control the effect of blocking the absorption of moisture from the outside Can satisfy.
  • the present application by controlling the particle diameter of the hygroscopic filler in the above range, it is possible to effectively implement the water barrier properties and light diffusion and extraction effect of the encapsulation film together with the non-hygroscopic filler.
  • the hygroscopic filler is 0.1 to 40 parts by weight, 0.3 to 35 parts by weight, 0.5 to 30 parts by weight, 0.7 to 25 parts by weight, 1.0 to 20 parts by weight, 1.5 to 15 parts by weight, based on 100 parts by weight of the encapsulating resin To 13 parts by weight or 3.0 to 12 parts by weight.
  • the encapsulation layer when it is two or more layers, it means a weight ratio to the resin of the entire encapsulation layer.
  • the present application by adjusting the content of the hygroscopic filler as described above, the light transmittance and haze of the encapsulation layer can be adjusted to the desired range, thereby providing an encapsulation film excellent in optical properties and moisture barrier properties.
  • the type of hygroscopic filler is not particularly limited as long as the particle size or content range is satisfied.
  • the hygroscopic filler may be at least one selected from the group consisting of metal oxides, metal salts and phosphorus pentoxide.
  • the hygroscopic filler is CaO, MgO, CaCl 2 , CaCO 3 , CaZrO 3 , CaTiO 3 , SiO 2 , Ca 2 SiO 4 , MgCl 2 , P 2 O 5 , Li 2 O, Na 2 O, BaO, Li 2 SO 4 , Na 2 SO 4 , CaSO 4 , MgSO 4 , CoSO 4 , Ga 2 (SO 4) 3, Ti ( SO 4) 2, NiSO 4, SrCl 2, YCl 3, CuCl 2, CsF, TaF 5, NbF 5, LiBr, CaBr 2, CeBr 3, SeBr 4, VBr 3, MgBr 2, It may include one or more selected from the group consisting of BaI 2 , MgI 2 , Ba (ClO 4 ) 2 and Mg (ClO 4 ) 2 .
  • the average particle diameter of the non-hygroscopic filler is 500nm to 10 ⁇ m, 550nm to 8 ⁇ m, 600nm to 6 ⁇ m, 650nm to 5 ⁇ m, 700nm to 4 ⁇ m, 750nm to 3 ⁇ m, 800nm to 2 ⁇ m or 900nm to It may be in the range of 1.5 ⁇ m.
  • the particle size of the non-hygroscopic filler may be larger than the particle size of the hygroscopic filler described above.
  • the ratio of the average particle diameter of the non-hygroscopic filler to the average particle diameter of the hygroscopic filler may be at least 1, at least 1.1, at least 1.2, at least 1.3, at least 1.4, or at least 1.5.
  • the upper limit may be 2 or less, for example.
  • the refractive index difference between the encapsulating resin and the non-hygroscopic filler may be in the range of 0.1 to 1.0, 0.15 to 0.95, 0.2 to 0.9, 0.25 to 0.85, 0.3 to 0.8, 0.35 to 0.75, or 0.4 to 0.7.
  • the refractive index difference between the non-hygroscopic filler and the hygroscopic filler may be in the range of 0.1 to 1.0, 0.15 to 0.95, 0.2 to 0.9, 0.25 to 0.85, 0.3 to 0.8, 0.35 to 0.75 or 0.35 to 0.7.
  • the encapsulation resin when measuring the refractive index, may refer to the refractive index of the resin itself. By specifying the refractive index as described above, it is possible to control the haze, and to effectively control the light diffusion and extraction.
  • non-hygroscopic filler is not particularly limited as long as it satisfies the above average particle diameter and refractive index.
  • titanium dioxide (TiO 2 ), alumina (Al 2 O 3 ), silicon nitride (Si 3 N 4 ), and nitride It may be at least one selected from the group consisting of aluminum (AlN), gallium nitride (GaN), zinc sulfide (ZnS), cadmium sulfide (CdS), silica, talc, zeolite, titania, zirconia, montmorillonite and clay.
  • the non-hygroscopic filler may be included in 0.1 to 10, 0.3 to 9.5 parts by weight, 0.5 to 9.3 parts by weight, 0.8 to 9.0 parts by weight, 1.0 to 8.5 parts by weight, 2.0 to 8.0 parts by weight based on 100 parts by weight of the encapsulating resin. .
  • the encapsulation layer is two or more layers, it means a weight ratio to the resin of the entire encapsulation layer.
  • the encapsulation layer is 1 to 60 parts by weight, 3 to 55 parts by weight, 5 to 50 parts by weight, 10 to 45 parts by weight or 15 to about 100 parts by weight of the hygroscopic filler and the non-hygroscopic filler 40 parts by weight may be included. If a large amount of non-hygroscopic filler is included in the encapsulation layer, it may adversely affect the life of the organic electronic device. Thus, by adjusting the content of the hygroscopic filler and the non-hygroscopic filler, the light transmittance and haze of the encapsulation layer are adjusted to the desired range. Can be.
  • filler may refer to the hygroscopic filler or the non-hygroscopic filler, and may refer to two fillers collectively.
  • encapsulation resin may include an adhesive resin or an adhesive resin, which will be described later, as a main component constituting the encapsulation layer.
  • the kind of the encapsulating resin is not particularly limited.
  • the encapsulation resin has a water vapor transmission rate (WVTR) in a cured or crosslinked state of 50 g / m 2 ⁇ day or less, preferably 30 g / m 2 ⁇ day or less, more preferably May be 20 g / m 2 ⁇ day or less, more preferably 15 g / m 2 ⁇ day or less.
  • WVTR water vapor transmission rate
  • the term "cured or crosslinked state of the encapsulating resin” refers to the performance as a structural adhesive when the encapsulating resin is cured or crosslinked through reaction with other components such as alone or with a curing agent, a crosslinking agent, or the like, and is applied as an encapsulant. It means a state that has been converted to a possible state.
  • the moisture permeability is the thickness direction of the cured product or the crosslinked product under 38 ° C and 100% relative humidity after curing or crosslinking the encapsulating resin and making the cured product or crosslinked product into a film shape having a thickness of 100 ⁇ m. Moisture permeability measured for. In addition, the moisture permeability is measured according to ASTM F1249. The lower the moisture permeability, the better the moisture barrier property, so the lower limit is not particularly limited, and may be 0 g / m 2 ⁇ day or 0.001 g / m 2 ⁇ day.
  • the encapsulating resin may be acrylic resin, epoxy resin, silicone resin, fluorine resin, styrene resin, polyolefin resin, thermoplastic elastomer, polyoxyalkylene resin, polyester resin, polyvinyl chloride resin, polycarbonate resin, polyphenylene Sulfide resins, polyamide resins or mixtures thereof and the like can be exemplified.
  • styrene resin for example, styrene-ethylene-butadiene-styrene block copolymer (SEBS), styrene-isoprene-styrene block copolymer (SIS), acrylonitrile-butadiene-styrene block copolymer (ABS) , Acrylonitrile-styrene-acrylate block copolymers (ASA), styrene-butadiene-styrene block copolymers (SBS), styrene-based homopolymers or mixtures thereof.
  • SEBS styrene-ethylene-butadiene-styrene block copolymer
  • SIS styrene-isoprene-styrene block copolymer
  • ABS acrylonitrile-butadiene-styrene block copolymer
  • ASA Acrylonitrile-styrene-acrylate block
  • the olefin resin for example, a high density polyethylene resin, a low density polyethylene resin, a polypropylene resin or a mixture thereof can be exemplified.
  • the thermoplastic elastomer for example, an ester thermoplastic elastomer, an olefin thermoplastic elastomer, a mixture thereof, or the like can be used.
  • polybutadiene resin or polyisobutylene resin may be used as the olefinic thermoplastic elastomer.
  • the polyoxyalkylene resins include polyoxymethylene resins, polyoxyethylene resins, mixtures thereof, and the like.
  • polyester resins examples include polyethylene terephthalate resins, polybutylene terephthalate resins, and mixtures thereof.
  • polyvinyl chloride resin polyvinylidene chloride etc. can be illustrated, for example.
  • a mixture of hydrocarbon resins may be included, for example, hexatriacotane or paraffin may be exemplified.
  • polyamide resin nylon etc. can be illustrated, for example.
  • acrylate resin polybutyl (meth) acrylate etc. can be illustrated, for example.
  • silicone resin polydimethylsiloxane etc. can be illustrated, for example.
  • polytrifluoroethylene resin polytetrafluoroethylene resin, polychlorotrifluoroethylene resin, polyhexafluoropropylene resin, polyvinylidene fluoride, polyvinylidene fluoride, polyfluoro Ethylene propylene propylene or mixtures thereof and the like can be exemplified.
  • the above-listed resins may be used, for example, by grafting with maleic anhydride, or the like, or may be used after being copolymerized with other listed resins or monomers for preparing the resins, or may be modified with other compounds.
  • the other compounds include carboxyl-terminated butadiene-acrylonitrile copolymers.
  • the encapsulation resin of the encapsulation composition may include a polyisobutylene resin.
  • Polyisobutylene resins may have hydrophobicity to exhibit low water vapor permeability and low surface energy.
  • polyisobutylene resin For example, homopolymer of isobutylene monomer; Or the copolymer which copolymerized the isobutylene monomer and the other monomer which can superpose
  • the other monomers polymerizable with the isobutylene monomer may include, for example, 1-butene, 2-butene, isoprene or butadiene.
  • the copolymer may be butyl rubber.
  • a base resin having a weight average molecular weight (Mw) that can be molded into a film shape may be used.
  • Mw weight average molecular weight
  • the weight average molecular weight may be about 100,000 to 2 million, 100,000 to 1.5 million, or 100,000 to 1 million.
  • weight average molecular weight means a conversion value with respect to standard polystyrene measured by gel permeation chromatography (GPC).
  • 1 type may be used among the structures mentioned above, and 2 or more types may be used.
  • 2 or more types 2 or more types of resin from a different kind may be used, 2 or more types of resin from which a weight average molecular weight differs, or 2 or more types of resin from a both type and weight average molecular weight may be used.
  • the encapsulation resin according to the invention can be a curable resin.
  • the specific kind of curable resin that can be used in the present invention is not particularly limited, and various thermosetting or photocurable resins known in the art may be used.
  • the term "thermosetting resin” means a resin that can be cured through an appropriate heat application or aging process
  • the term "photocurable resin” means a resin that can be cured by irradiation of electromagnetic waves.
  • the curable resin may be a dual curable resin including both thermosetting and photocuring properties.
  • the curable resin of the present invention constitutes an encapsulation composition together with a light absorbing material described below, the curable resin may be preferably a thermosetting resin, and photocurable resin may be excluded, but is not limited thereto.
  • curable resin in this invention will not be restrict
  • it may be cured to exhibit adhesive properties, and may include one or more thermosetting functional groups such as glycidyl group, isocyanate group, hydroxy group, carboxyl group or amide group, or may be an epoxide group or a cyclic ether. and resins containing at least one functional group curable by irradiation of electromagnetic waves such as a (cyclic ether) group, a sulfide group, an acetal group, or a lactone group.
  • specific types of the resin may include an acrylic resin, a polyester resin, an isocyanate resin, an epoxy resin, and the like, but is not limited thereto.
  • the curable resin aromatic or aliphatic; Or an epoxy resin of linear or branched chain type can be used.
  • an epoxy resin having an epoxy equivalent of 180 g / eq to 1,000 g / eq may be used as containing two or more functional groups.
  • an epoxy resin having an epoxy equivalent in the above range it is possible to effectively maintain properties such as adhesion performance and glass transition temperature of the cured product.
  • examples of such epoxy resins include cresol novolac epoxy resins, bisphenol A epoxy resins, bisphenol A novolac epoxy resins, phenol novolac epoxy resins, tetrafunctional epoxy resins, biphenyl epoxy resins, and triphenol methane types.
  • a kind or mixture of an epoxy resin, an alkyl modified triphenol methane epoxy resin, a naphthalene type epoxy resin, a dicyclopentadiene type epoxy resin, or a dicyclopentadiene modified phenol type epoxy resin is mentioned.
  • an epoxy resin containing a cyclic structure in a molecular structure can be used as the curable resin, and an epoxy resin containing an aromatic group (for example, a phenyl group) can be used.
  • an epoxy resin containing an aromatic group for example, a phenyl group
  • the cured product may have excellent thermal and chemical stability while exhibiting low moisture absorption, thereby improving reliability of the organic electronic device encapsulation structure.
  • aromatic group-containing epoxy resin examples include biphenyl type epoxy resin, dicyclopentadiene type epoxy resin, naphthalene type epoxy resin, dicyclopentadiene modified phenol type epoxy resin, cresol type epoxy resin, Bisphenol-based epoxy resins, xylox-based epoxy resins, polyfunctional epoxy resins, phenol novolac epoxy resins, triphenol methane-type epoxy resins and alkyl-modified triphenol methane epoxy resins, such as one or a mixture of two or more, but is not limited thereto. no.
  • the epoxy resin a silane-modified epoxy resin or a silane-modified epoxy resin having an aromatic group can be used.
  • an epoxy resin modified with silane and structurally having a silane group is used, the adhesion of the organic electronic device to the glass substrate or the substrate inorganic material can be maximized, and the moisture barrier property, durability and reliability can be improved.
  • the specific kind of the above epoxy resin that can be used in the present invention is not particularly limited, and such a resin can be easily obtained from a place of purchase such as, for example, National Chemical.
  • the encapsulation layer may further include a dispersant so that the encapsulating resin, the hygroscopic filler or the nonhygroscopic filler can be uniformly dispersed.
  • a dispersing agent which can be used here, the nonionic surfactant which has affinity with the surface of a hygroscopic filler and a nonhygroscopic filler, and is compatible with sealing resin etc. can be used, for example.
  • selection of an appropriate dispersant may be necessary.
  • the dispersant may comprise at least one selected from the group consisting of stearic acid, palmitic acid, oleic acid, linoleic acid, cetyl alcohol, stearyl alcohol, cetostearyl alcohol, oleyl alcohol, octylglucoside, decylglucoside or lauryl glucoside. It may include.
  • the content of such a dispersant may be controlled according to the type and / or size of the hygroscopic filler and the nonhygroscopic filler. Specifically, the smaller the size of the hygroscopic filler and the non-hygroscopic filler, the wider the surface area of the hygroscopic filler and the non-hygroscopic filler, so that a large amount of dispersant may be used to uniformly disperse.
  • hygroscopic fillers and non-hygroscopic fillers 0.1 to 5 parts by weight, 0.2 to 4.5 parts by weight, 0.3 to 4.3 parts by weight, or 0.5 to 0.5 based on 100 parts by weight of the hygroscopic filler and the nonhygroscopic filler
  • a dispersant of about 4.0 can be used.
  • the hygroscopic filler or the nonhygroscopic filler can be uniformly dispersed without affecting the overall physical properties such as the adhesive force of the encapsulation film.
  • the encapsulation layer may include various additives depending on the use and the manufacturing process of the encapsulation film in addition to the above-described configuration.
  • the encapsulation layer may include a curable material, a crosslinking agent, a crosslinking compound, a polyfunctional active energy ray polymerizable compound, an initiator, a tackifier or a coupling agent in an appropriate range of contents depending on the desired physical properties. .
  • the structure of the encapsulation film 1 of the present application is not particularly limited, as long as it includes the encapsulation layer 3.
  • the base film 2 or the release film 2 hereinafter, it may be called “1st film.”
  • the sealing film of this application may further contain the base film or release film (henceforth a "second film” may be called.) Formed on the said sealing layer.
  • the specific kind of the said 1st film which can be used by this application is not specifically limited.
  • a general polymer film of this field may be used as the first film.
  • 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 , Ethylene-vinyl acetate film, ethylene-propylene copolymer film, ethylene-ethyl acrylate copolymer film, ethylene-methyl acrylate copolymer film, polyimide film and the like can be used.
  • an appropriate release treatment may be performed on one side or both sides of the base film or the release film of the present application.
  • Alkyd-based, silicone-based, fluorine-based, unsaturated ester-based, polyolefin-based, or wax-based may be used as an example of the release agent used in the release treatment of the base film, and among these, it is preferable to use an alkyd-based, silicone-based, or fluorine-based release agent in terms of heat resistance. Preferred, but not limited to.
  • the kind of 2nd film (Hereinafter, a "cover film” may be called.) Which can be used by this application is not specifically limited, either.
  • the second film the same or different kind as the first film can be used within the range illustrated in the above-described first film.
  • an appropriate release treatment may also be performed on the second film.
  • the thickness of the base film or the release film (first film) as described above is not particularly limited and may be appropriately selected depending on the application to be applied.
  • the thickness of the first film may be about 10 ⁇ m to 500 ⁇ m, preferably about 20 ⁇ m to 200 ⁇ m. If the thickness is less than 10 ⁇ m, deformation of the base film may occur easily during the manufacturing process. If the thickness is more than 500 ⁇ m, the economy is inferior.
  • the thickness of the second film in the present application is also not particularly limited. In this application, you may set the thickness of the said 2nd film similarly to a 1st film, for example. In the present application, the thickness of the second film may also be set relatively thinner than the first film in consideration of processability and the like.
  • the present application also relates to a method for producing an encapsulation film.
  • Exemplary encapsulation film may include molding the encapsulation composition into a film or sheet shape.
  • the encapsulation composition may mean a main component constituting the encapsulation layer, and for example, an encapsulation resin, a dispersant, a hygroscopic filler or a nonhygroscopic filler, and the like.
  • the method may include applying the coating liquid including the encapsulation composition in a sheet or film form on a substrate or a release film, and drying the applied coating liquid.
  • the manufacturing method may also include attaching an additional substrate or release film on the dried coating solution.
  • the coating liquid containing the sealing composition can be prepared, for example, by dissolving or dispersing the components of each of the sealing compositions described above in a suitable solvent.
  • the encapsulation composition can be prepared in a manner that includes dissolving or dispersing the filler in a solvent, if necessary, and then mixing the pulverized filler with the encapsulating resin after grinding.
  • the kind of solvent used for coating liquid manufacture is not specifically limited. However, when the drying time of the solvent is too long or when drying at a high temperature is required, problems may occur in terms of workability or durability of the encapsulation film, and thus a solvent having a volatilization temperature of 150 ° C. or less may be used. In consideration of film formability, a small amount of a solvent having a volatilization temperature of the above range or more can be mixed and used.
  • the solvent include methyl ethyl ketone (MEK), acetone, toluene, dimethylformamide (DMF), methyl cellosolve (MCS), tetrahydrofuran (THF), xylene or N-methylpyrrolidone (NMP).
  • MEK methyl ethyl ketone
  • DMF dimethylformamide
  • MCS methyl cellosolve
  • THF tetrahydrofuran
  • xylene xylene
  • NMP N-methylpyrrol
  • the method of applying the coating solution to the substrate or the release film is not particularly limited, and for example, a known coating method such as a knife coat, roll coat, spray coat, gravure coat, curtain coat, comma coat, or lip coat may be applied. Can be.
  • the applied coating liquid may be dried to volatilize the solvent and form an encapsulation layer.
  • the drying may be performed, for example, for 1 minute to 10 minutes at a temperature of 70 °C to 150 °C.
  • the conditions of the drying may be changed in consideration of the type or proportion of the solvent used or the possibility of curing the curable pressure-sensitive adhesive resin.
  • Drying may then form additional substrates or release films on the encapsulation layer.
  • formation of such a base material or a release film can be performed by crimping
  • Hot roll lamination can be used in view of the possibility and efficiency of the continuous process.
  • the temperature may be about 10 ° C. to 100 ° C.
  • the pressure may be about 0.1 kgf / cm 2 to 10 kgf / cm 2 , but is not limited thereto.
  • the present application also shows a substrate 21, as shown in FIG. An organic electronic device 23 formed on one surface of the substrate 21; And it relates to an organic electronic device comprising the above-mentioned encapsulation film (3) formed on the other side of the substrate.
  • the organic electronic device may include a transparent electrode layer on the substrate, an organic layer on the transparent electrode layer and including at least a light emitting layer, and a reflective electrode layer on the organic layer.
  • the organic electronic device may further include a moisture barrier layer 6 formed on the organic electronic device 23 and encapsulating the entire surface of the device.
  • a cover substrate 22 formed on the moisture barrier layer 6 may be further included.
  • the material constituting the moisture barrier layer 6 is not particularly limited, and may include the encapsulation resin described above, and may further include the hygroscopic filler described above.
  • the encapsulating resin may be acrylic resin, epoxy resin, silicone resin, fluorine resin, styrene resin, polyolefin resin, thermoplastic elastomer, polyoxyalkylene resin, polyester resin, polyvinyl chloride resin, polycarbonate resin, polyphenylene Sulfide resins, polyamide resins or mixtures thereof and the like can be exemplified.
  • the present application may implement moisture blocking properties and light diffusion and extraction effects through the encapsulation film 3 described above on one surface of the substrate, and the organic electronic device through the moisture blocking layer 6 on the other surface of the substrate. It can effectively block the incoming water or oxygen on both sides.
  • the organic electronic device may be, for example, an organic light emitting device, and in one example, may be an organic light emitting device having a top emission type or an organic light emitting device having a bottom emission type.
  • the above-mentioned encapsulation film may be positioned on the side through which light is transmitted. That is, for example, in the case of the top emission type, an encapsulation film may be provided in the form of encapsulating the entire surface of the device on the organic light emitting device.
  • the encapsulation film may be located on the other side of the substrate on which the device is formed on one side.
  • the present application also relates to a method for manufacturing an organic electronic device.
  • the organic electronic device may be manufactured by, for example, applying the aforementioned encapsulation film.
  • the encapsulation layer may be formed as a structural encapsulation layer for efficiently fixing and supporting a barrier film applied to the substrate and the organic electronic device while exhibiting excellent moisture barrier properties and optical properties in the organic electronic device.
  • the encapsulation layer exhibits excellent transparency, and may be formed as a stable encapsulation layer regardless of the shape of the organic electronic device such as top emission or bottom emission.
  • the present application for the production of the organic electronic device, for example, forming an organic electronic device on one surface of the substrate; And forming the aforementioned encapsulation film on the other surface of the substrate.
  • the method may further include forming a moisture barrier layer on the organic electronic device.
  • the method may further include curing the encapsulation film.
  • the applying of the encapsulation film to the organic electronic device may be performed by hot roll lamination, hot pressing, or vacuum compression of the encapsulation film, and is not particularly limited.
  • the applying of the encapsulation film to the organic electronic device may be performed at a temperature of 50 ° C. to 90 ° C., followed by a curing step, which may be heated to a temperature range of 70 ° C. to 110 ° C. or irradiated with UV. Can be done.
  • a transparent electrode is formed on a substrate 21 such as glass or a film by vacuum deposition or sputtering, and an organic material layer is formed on the transparent electrode.
  • the organic material layer may include a hole injection layer, a hole transport layer, a light emitting layer, an electron injection layer and / or an electron transport layer.
  • a second electrode is further formed on the organic material layer.
  • the above-described moisture barrier layer 6 is applied to cover all of the organic electronic devices 23 on the organic electronic device 23 on the substrate 21.
  • the encapsulation layer 3 described above is formed on the other surface on which the organic electronic device 23 is not formed on the substrate 21.
  • an additional curing process may be performed on the moisture barrier layer or encapsulation layer on which the organic electronic device is compressed.
  • Such curing process (main curing) may be performed in, for example, a heating chamber or a UV chamber. Preferably it can proceed in a heating chamber. Conditions in the present curing may be appropriately selected in consideration of the stability of the organic electronic device.
  • the present application provides an encapsulation film and an organic electronic device that not only effectively block moisture or oxygen introduced into the organic electronic device from the outside, but also satisfy light diffusion and extraction effects.
  • FIG. 1 and 2 are cross-sectional views showing an encapsulation film according to one example of the present application.
  • FIG 3 is a cross-sectional view illustrating an organic electronic device according to one example of the present application.
  • Silica (refractive index 1.46) having an average particle diameter of about 1 ⁇ m as a non-hygroscopic filler was added to methyl ethyl ketone MEK as a solvent at a concentration of 20% by weight of solid to prepare a non-hygroscopic filler dispersion.
  • 100 g of CaO (Aldrich, average particle diameter: about 1 ⁇ m, refractive index: 1.83) as the hygroscopic filler and methyl ethyl ketone MEK as a solvent were charged at a concentration of 50% by weight of solid content to prepare a hygroscopic filler solution.
  • silane-modified epoxy resin KSR-177, Kukdo Chemical
  • phenoxy resin YP-50, Kyodo Chemical
  • 4 g of imidazole Shikoku Chemical, which is a curing agent, was added to the homogenized solution, followed by high-speed stirring for 1 hour to prepare an encapsulation layer solution.
  • a hygroscopic filler solution and a nonhygroscopic filler solution prepared in advance were added to the solution so that CaO and silica were in a weight ratio of 5: 5 (CaO: silica), and mixed to prepare an encapsulation layer solution.
  • the solution of the said sealing layer was apply
  • a hygroscopic filler solution was prepared by adding CaO (Aldrich, particle size: about 1 ⁇ m, refractive index: 1.83) as a hygroscopic filler and methyl ethyl ketone MEK at a concentration of 50% by weight of solid content as a solvent.
  • CaO Aldrich, particle size: about 1 ⁇ m, refractive index: 1.83
  • a hygroscopic filler and methyl ethyl ketone MEK at a concentration of 50% by weight of solid content as a solvent.
  • 200 g of silane-modified epoxy resin (KSR-177, Kukdo Chemical) and 150 g of phenoxy resin (YP-50, Kyodo Chemical) were added to the reactor at room temperature, and diluted with methyl ethyl ketone.
  • the first layer solution was prepared by adding and mixing a hygroscopic filler solution prepared in advance to the encapsulation layer solution, but the first non-hygroscopic filler and the hygroscopic filler to be described later have a weight ratio of 5: 5 (CaO: silica).
  • Layer solution was prepared.
  • Silica (refractive index 1.46) having a particle size of about 1 ⁇ m as a non-hygroscopic filler was added to methyl ethyl ketone MEK as a solvent at a concentration of 20% by weight of solid to prepare a non-hygroscopic filler dispersion.
  • 200 g of silane-modified epoxy resin (KSR-177, Kukdo Chemical) and 150 g of phenoxy resin (YP-50, Kyodo Chemical) were added to the reactor at room temperature, and diluted with methyl ethyl ketone.
  • the non-hygroscopic filler solution prepared in advance is added to the encapsulation layer solution, and a second layer solution is prepared by mixing, so that the weight ratio of the nonhygroscopic filler and the hygroscopic filler described above is 5: 5 (CaO: silica).
  • a two layer solution was prepared.
  • the solution of the first layer prepared above was applied to the release surface of the release PET using a comma coater and dried at 130 ° C. for 3 minutes in a dryer to form a first layer having a thickness of 20 ⁇ m.
  • the second layer solution prepared above was applied to the release surface of the release PET using a comma coater and dried at 130 ° C. for 3 minutes in a dryer to form a second layer having a thickness of 20 ⁇ m.
  • the first layer and the second layer were plywood to prepare an encapsulation film.
  • the hygroscopic filler solution and the non-hygroscopic filler solution were added in a weight ratio of CaO and silica at a weight ratio of 5:15 (CaO: silica), and mixed in the same manner as in Example 1 except that the sealing layer solution was prepared.
  • An encapsulation film was prepared.
  • An organic electronic device is manufactured by applying an encapsulation film prepared according to an example and a comparative example to one surface of a glass on which an organic electronic device is formed.
  • the encapsulation film is laminated so as to be positioned in a direction in which light is emitted from the organic electronic device. After lamination, the panel was completed through an autoclave process, and luminance was measured by a display color analyzer. The relative luminance calculated the relative value of the luminance of the organic electronic devices of Examples and Comparative Examples when the luminance of the reference sample was 100.
  • a testable device is deposited on a glass substrate. After encapsulating the encapsulation layer according to the Examples and Comparative Examples on a glass substrate for encaps, it is vacuum pressed for 3 minutes while pressing at a pressure of 5kg / cm 2 while heating at 80 °C on the substrate. The dark spots were observed in 85 degreeC 85% RH constant temperature and humidity conditions of the vacuum compressed sample. Check if there is no dark spot (good) and if there is (bad) produced by observing for 300 hours.
  • the light transmittance at 550 nm was measured with the UV-Vis Spectrometer about the sealing film prepared above, and haze was measured using the haze meter according to JISK7105 standard test method.
  • the reference sample is data on the encapsulation film prepared in the same manner as in Example 1, except that the hygroscopic filler and the nonhygroscopic filler were not added.
  • the optical properties were obtained at the desired level in the present application, but the moisture permeability was considerably lowered.
  • Comparative Example 2 the moisture barrier property was obtained at the desired level in the present application, but the relative luminance was lowered. Indicated.

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  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

La présente invention concerne un film d'étanchéification et un dispositif électronique organique comprenant ledit film. Ce film d'étanchéification bloque efficacement l'humidité ou l'oxygène introduits de l'extérieur dans un dispositif électronique organique et présente des effets satisfaisants de diffusion et d'extraction de lumière. La présente invention concerne en outre le dispositif électronique organique décrit.
PCT/KR2015/003067 2014-03-27 2015-03-27 Film d'étanchéification et dispositif électronique organique comprenant ledit film Ceased WO2015147600A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2017502552A JP6410066B2 (ja) 2014-03-27 2015-03-27 封止フィルム及びこれを含む有機電子装置
CN201580027885.7A CN106415875B (zh) 2014-03-27 2015-03-27 封装膜及包括该封装膜的有机电子装置
EP15767907.7A EP3125328B1 (fr) 2014-03-27 2015-03-27 Film d'étanchéification et dispositif électronique organique comprenant ledit film
US15/129,349 US10103353B2 (en) 2014-03-27 2015-03-27 Encapsulation film and organic electronic device comprising the same

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2014-0035825 2014-03-27
KR20140035825 2014-03-27
KR10-2015-0043390 2015-03-27
KR1020150043390A KR101687479B1 (ko) 2014-03-27 2015-03-27 봉지 필름 및 이를 포함하는 유기전자장치

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Cited By (3)

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JP2017117761A (ja) * 2015-12-25 2017-06-29 共同印刷株式会社 有機ｅｌデバイス用吸湿性光散乱シート
WO2018052006A1 (fr) * 2016-09-16 2018-03-22 積水化学工業株式会社 Agent d'encapsulation pour élément d'affichage électroluminescent organique
CN108778715A (zh) * 2016-03-11 2018-11-09 株式会社Lg化学 封装膜

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JP2002194066A (ja) * 2000-12-27 2002-07-10 Hitachi Chem Co Ltd 液状封止用エポキシ樹脂組成物及び電子部品装置
KR20060070166A (ko) * 2004-12-20 2006-06-23 삼성에스디아이 주식회사 유기 전계 발광 소자 및 그 제조방법
JP2012097282A (ja) * 2004-04-30 2012-05-24 Kureha Corp 封止用樹脂組成物及び樹脂封止された半導体装置
WO2013103281A1 (fr) * 2012-01-06 2013-07-11 주식회사 엘지화학 Film d'encapsulation
KR20140024040A (ko) * 2012-05-31 2014-02-27 주식회사 엘지화학 유기전자장치의 제조방법

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JP2002194066A (ja) * 2000-12-27 2002-07-10 Hitachi Chem Co Ltd 液状封止用エポキシ樹脂組成物及び電子部品装置
JP2012097282A (ja) * 2004-04-30 2012-05-24 Kureha Corp 封止用樹脂組成物及び樹脂封止された半導体装置
KR20060070166A (ko) * 2004-12-20 2006-06-23 삼성에스디아이 주식회사 유기 전계 발광 소자 및 그 제조방법
WO2013103281A1 (fr) * 2012-01-06 2013-07-11 주식회사 엘지화학 Film d'encapsulation
KR20140024040A (ko) * 2012-05-31 2014-02-27 주식회사 엘지화학 유기전자장치의 제조방법

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017117761A (ja) * 2015-12-25 2017-06-29 共同印刷株式会社 有機ｅｌデバイス用吸湿性光散乱シート
CN108778715A (zh) * 2016-03-11 2018-11-09 株式会社Lg化学 封装膜
US10864706B2 (en) 2016-03-11 2020-12-15 Lg Chem, Ltd. Encapsulation film
CN108778715B (zh) * 2016-03-11 2021-01-08 株式会社Lg化学 封装膜
WO2018052006A1 (fr) * 2016-09-16 2018-03-22 積水化学工業株式会社 Agent d'encapsulation pour élément d'affichage électroluminescent organique

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