WO2016103720A1 - 電子デバイスおよびその製造方法 - Google Patents
電子デバイスおよびその製造方法 Download PDFInfo
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- WO2016103720A1 WO2016103720A1 PCT/JP2015/006460 JP2015006460W WO2016103720A1 WO 2016103720 A1 WO2016103720 A1 WO 2016103720A1 JP 2015006460 W JP2015006460 W JP 2015006460W WO 2016103720 A1 WO2016103720 A1 WO 2016103720A1
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Definitions
- the present invention relates to an electronic device and a manufacturing method thereof. More specifically, the present invention relates to an electronic device comprising a protective sheet having a multilayer structure including a substrate (X) and a layer (Y) laminated on the substrate (X), and a quantum dot phosphor. And a manufacturing method thereof.
- Patent Document 1 discloses a method in which a coating liquid containing aluminum oxide particles and a phosphorus compound is applied on a plastic film, followed by drying and heat treatment.
- the gas barrier performance of the conventional gas barrier layer may be deteriorated under a high temperature and high humidity condition, and the gas barrier property for a long time may not be sufficient.
- Quantum dots have come to be used as phosphors that emit light by converting the wavelength of incident light in electronic devices such as light emitting diodes (LEDs).
- Quantum dots are luminescent semiconductor nanoparticles, and the diameter range is usually 1 to 20 nm. Then, the electrons are quantum confined in a three-dimensional and nanoscale semiconductor crystal with a clear outline. Such quantum dot phosphors are likely to aggregate and deteriorate due to oxygen or the like, so that they are generally used dispersed in a resin or the like.
- Patent Document 2 discloses a flash in which a plurality of quantum dots are dispersed in a matrix material composed of a sol or gel, PMMA (polymethyl methacrylate), polystyrene, polycarbonate, UV curable resin, and epoxy. -Modules are listed.
- the quantum dot phosphor dispersed in the resin may still be deteriorated by oxygen, water, etc. contained in the atmosphere.
- gas barrier property means the ability to barrier gas other than water vapor unless otherwise specified. Further, in this specification, when “barrier property” is simply described, it means both a gas barrier property and a water vapor barrier property. Further, in this specification, “optical characteristics” means total light transmittance and haze.
- the present inventors have found that the above object can be achieved by an electronic device including a quantum dot phosphor covered with a protective sheet including a multilayer structure including a specific layer, and the present invention has been achieved. .
- the present invention is an electronic device comprising a quantum dot phosphor
- the electronic device comprises a protective sheet;
- the protective sheet includes a multilayer structure (W) including a base material (X) and a layer (Y) laminated on the base material (X),
- the layer (Y) contains a reaction product (D) of a compound (A) containing aluminum and a phosphorus compound (B),
- the average particle size of the reaction product (D) is in the range of 5 to 50 nm.
- An electronic device including a quantum dot phosphor is provided.
- the protective sheet may be disposed on one side or both sides of the layer including the quantum dot phosphor.
- the phosphorus compound (B) may be an inorganic phosphorus compound (BI).
- the compound (A) containing aluminum may be a metal oxide (Aa) containing aluminum.
- the average particle size of the reaction product (D) may be in the range of 20 to 40 nm.
- the protective sheet for an electronic device containing the quantum dot phosphor of the present invention may have a moisture permeability of 1.0 g / (m 2 ⁇ day) or less under the conditions of 40 ° C. and 90% RH.
- the base material (X) may include a thermoplastic resin film.
- the layer (Y) may contain a polymer (F) containing at least one functional group selected from the group consisting of a carbonyl group, a hydroxyl group, a carboxyl group, a carboxylic anhydride group, and a salt of a carboxyl group. .
- the multilayer structure (W) may further include a layer (Z) disposed adjacent to the layer (Y).
- the layer (Z) may include a polymer (BOa) having a functional group containing a phosphorus atom.
- the polymer (BOa) of the layer (Z) may be poly (vinylphosphonic acid) or poly (2-phosphonooxyethyl methacrylate).
- the present invention also provides a multilayer structure (W) in which an electronic device includes a protective sheet, and the protective sheet includes a base material (X) and a layer (Y) laminated on the base material (X).
- the layer (Y) contains a reaction product (D) of a compound (A) containing aluminum and a phosphorus compound (B);
- a coating liquid (S) containing a compound (A) containing aluminum, a phosphorus compound (B), and a solvent is applied onto the substrate (X), and a layer containing a reaction product (D) precursor (Y
- the solvent content of the precursor layer of the layer (Y) in the step (I) is 0.4 wt% or less, and the average particle size of the reaction product (D) precursor is less than 5 nm.
- the phosphorus compound (B) may be an inorganic phosphorus compound (BI).
- the compound (A) containing aluminum may be a metal oxide (Aa) containing aluminum.
- the drying temperature in the drying step may be less than 140 ° C.
- the ratio a R / a P between the maximum value a P in absorbance may be 2.0 or less.
- an electronic device including a quantum dot phosphor that has high barrier performance before and after the dump heat test and also has excellent optical characteristics.
- an electronic device including a quantum dot phosphor in which deterioration due to oxygen, water, or the like contained in the atmosphere is suppressed during long-term use Furthermore, it is possible to obtain an electronic device including a quantum dot phosphor that is less deteriorated and excellent in performance retention even under long-term use in the atmosphere (for example, continuous light emission for 2,000 hours).
- the meaning of “lamination of a specific layer on a specific member (base material, layer, etc.)” means that the specific layer is in contact with the member.
- the case where the specific layer is laminated above the member with another layer interposed therebetween is included.
- a specific layer is formed on a specific member (base material, layer, etc.)” and “a specific layer is arranged on a specific member (base material, layer, etc.)”.
- the meaning of “application of a liquid (coating liquid, etc.) on a specific member (base material, layer, etc.)” means that the liquid is applied directly to the member.
- the case where the liquid is applied to another layer formed on the member is included.
- An electronic device including a quantum dot phosphor using the multilayer structure (W) of the present invention includes an electronic device body and a protective sheet that covers the surface of the electronic device body.
- the protective sheet used for the electronic device of the present invention includes a multilayer structure (W) including a base material (X) and a layer (Y) laminated on the base material (X). Details of the multilayer structure (W) will be described later.
- the protective sheet may be constituted only by the multilayer structure (W), or may include other members or other layers.
- the case where the protective sheet includes the multilayer structure (W) will be described.
- FIG. 1 shows a partial cross-sectional view of an example of the electronic device of the present invention.
- An electronic device 11 in FIG. 1 includes an electronic device body 1, a sealing material 2 for sealing the electronic device body 1, and a protective sheet 3 for protecting the surface of the electronic device body 1.
- the sealing material 2 covers the entire surface of the electronic device body 1.
- the protective sheet 3 only needs to be arranged so as to protect the surface of the electronic device main body 1, and may be arranged directly on the surface of the electronic device main body 1 (not shown), as shown in FIG. You may arrange
- the 2nd protection sheet may be arrange
- the second protective sheet disposed on the opposite surface may be the same as or different from the first protective sheet.
- a suitable protective sheet protects the quantum dot phosphor material from environmental conditions such as high temperature, oxygen, and humidity.
- Suitable protective sheets are hydrophobic, chemically and mechanically compatible with quantum dot phosphor materials, exhibit light and chemical stability, have high temperature heat resistance, and are non-yellowing transparent Optical materials.
- the one or more protective sheets are index matched with the quantum dot phosphor material.
- the matrix material of the quantum dot phosphor material and one or more adjacent protective sheets are matched in refractive index to have a similar refractive index so that the quantum dot phosphor material is passed through the protective sheet. Most of the light transmitted toward the light is transmitted from the protective sheet into the phosphor material. This refractive index matching reduces optical losses at the interface between the protective sheet and the matrix material.
- Examples of the matrix material of the quantum dot phosphor material of the present invention include polymers, organic and inorganic oxides, and the like.
- the polymer is substantially translucent or substantially transparent.
- Suitable matrix materials include, for example, epoxy, acrylate, norbornene, polyethylene, poly (vinyl butyral): poly (vinyl acetate), polyurea, polyurethane; aminosilicone (AMS), poly, in addition to the dispersing resin described later.
- Silicone and silicone derivatives such as phenylmethylsiloxane, polyphenylalkylsiloxane, polydiphenylsiloxane, polydialkylsiloxane, silsesquioxane, fluorinated silicone, and vinyl and hydride substituted silicones; methyl methacrylate, butyl methacrylate, lauryl methacrylate, etc.
- the protective sheet of the present invention is preferably a solid material.
- the solid material include a cured liquid, a gel, or a polymer.
- the protective sheet may include a flexible or inflexible material depending on the particular application.
- the protective sheet is preferably a planar layer and may include any suitable shape and surface area structure depending on the particular lighting application.
- any suitable protective sheet material known in the art can be used other than the material of the multilayer structure (W) described later.
- Examples of a barrier material suitable as a protective sheet other than the multilayer structure (W) include glass, polymer, and oxide.
- the polymer include polyethylene terephthalate (PET).
- the protective sheet of the present invention includes at least two layers (for example, a substrate (X) and a layer (Y)) containing different materials or compositions, so that the multilayer protective sheet is a protective sheet. It eliminates or reduces pinhole defect arrays within and provides an effective barrier against oxygen and moisture ingress into the quantum dot phosphor material.
- the material, thickness, and number of the protective sheet will depend on the specific application, and preferably the quantum dot phosphor barrier while minimizing the thickness of the electronic device containing the quantum dot phosphor. Selected to maximize protection and brightness.
- each protective sheet includes a laminate (laminated film), preferably a double laminate (double laminated film), and the thickness of each protective sheet is the same as that of a roll-to-roll or laminated manufacturing process. Thick enough to eliminate.
- the number or thickness of the protective sheet further depends on legal toxicity guidelines in embodiments where the quantum dot phosphor material includes heavy metals or other toxic materials, which guides more or thicker protection. A sheet may be required. Additional barrier considerations include cost, availability, and mechanical strength.
- an electronic device including a quantum dot phosphor includes two or more protective sheets including a multilayer structure (W), and these protective sheets are adjacent to each side surface of the quantum dot phosphor material.
- One or more protective sheets other than the protective sheet provided with the multilayer structure (W) may be provided on each side surface. That is, two or three layers (protective sheets) may be included on each side surface.
- an electronic device comprising a quantum dot phosphor comprises two protective sheets on each side of the quantum dot phosphor material, at least one of which comprises a protective sheet comprising a multilayer structure (W). Including.
- the layer containing the quantum dot phosphor of the present invention can be of any desired size, shape, structure, and thickness.
- the quantum dot phosphor can be embedded in the matrix material at any filling rate appropriate for the desired function.
- the thickness and width of the layer containing the quantum dot phosphor can be controlled by any method known in the art, such as wet coating, painting, spin coating, screen printing, and the like.
- the quantum dot phosphor material has a thickness of 500 ⁇ m or less, preferably 250 ⁇ m or less, more preferably 200 ⁇ m or less, more preferably 50 to 150 ⁇ m, and most preferably 50 to 100 ⁇ m. Can have.
- the top and bottom protective sheet layers of the electronic device comprising the quantum dot phosphor of the present invention are mechanically sealed.
- the top protective sheet layer and / or the bottom protective sheet layer are constricted together to seal the quantum dot phosphor.
- the edges are constricted immediately after application of the quantum dot phosphor and protective sheet layer to minimize exposure of the quantum dot phosphor material to oxygen and moisture in the environment.
- the barrier end can be sealed by narrow pressure, stamping, melting, rolling, pressurizing and the like.
- any mechanical adhesive may be used to mechanically seal the top and bottom protective sheet layers of the electronic device comprising the quantum dot phosphor of the present invention, but the ease of edge bonding, From the viewpoint of maintaining high optical properties of the quantum dots, it is preferable to use a suitable optical adhesive material such as an epoxy resin.
- the electronic device main body including the quantum dot phosphor of the present invention includes, for example, a display such as a liquid crystal display (LCD), a television, a computer, a mobile phone, a smartphone, a personal digital assistant (PDA), a game machine, an electronic reading device, and a digital camera. It can be used for backlighting units (BLU) for devices, lighting applications for indoor or outdoor lighting (eg stage lighting, decorative lighting, accent lighting, museum lighting, etc.).
- the electronic device body containing the quantum dot phosphor of the present invention can also be used as a quantum dot down conversion layer or film suitable for use in photovoltaic applications.
- the electronic device body including the quantum dot phosphor of the present invention can convert part of sunlight into lower energy light that can be absorbed by the active layer of the solar cell.
- the wavelength of the converted light can be converted into absorption and electric power by the active layer by such down conversion by the electronic device body including the quantum dot phosphor of the present invention. Therefore, the solar cell that employs the electronic device body including the quantum dot phosphor of the present invention may have an increased solar conversion efficiency.
- the electronic device body including the quantum dot phosphor of the present invention includes use as a light source, an optical filter, and / or a primary light down converter.
- the electronic device body including the quantum dot phosphor of the present invention is a primary light source, and the electronic device including the quantum dot phosphor emits a photon upon electrical stimulation.
- An electroluminescent device comprising:
- the electronic device that includes the quantum dot phosphor is an optical filter, and the quantum dot phosphor absorbs light having a certain wavelength or wavelength range.
- Electronic devices that include quantum dot phosphors can allow passage of specific wavelengths or wavelength ranges while absorbing or filtering out others.
- the electronic device comprising a quantum dot phosphor is a downconverter, whereby at least a portion of the primary light from the primary light source is quantum dot fluorescent within the electronic device comprising the quantum dot phosphor. It is absorbed by the body and re-emitted as secondary light having a lower energy or longer wavelength than the primary light.
- the electronic device that includes the quantum dot phosphor is both a filter and a primary light downconverter, whereby the first portion of the primary light is a quantum within the electronic device that includes the quantum dot phosphor.
- the sealing material 2 is an arbitrary member that is appropriately added according to the type and use of the electronic device body 1.
- Examples of the sealing material include ethylene-vinyl acetate copolymer, polyvinyl butyral resin, silicone resin, epoxy resin, urethane resin, cellulose resin, polystyrene resin, styrene butadiene copolymer, and the like.
- the protective sheet for an electronic device including the quantum dot phosphor of the present invention may have flexibility.
- the term “flexible” means that it can be wound around a roll having a diameter of 50 cm. For example, it means that visual damage is not observed even when wound on a roll having a diameter of 50 cm. It is preferable that the diameter can be wound on a roll smaller than 50 cm because the electronic device or the protective sheet is more flexible.
- the protective sheet containing the multilayer structure (W) is excellent in gas barrier properties and water vapor barrier properties, and is excellent in gas barrier properties and water vapor barrier properties even under high temperature and high humidity conditions. Therefore, by using the protective sheet, the quantum dot phosphor can be protected from oxygen, water, and the like, and an electronic device with little deterioration can be obtained even in a harsh environment.
- the multilayer structure (W) can also be used as a film called a substrate film such as a substrate film for LCD, a substrate film for organic EL, and a substrate film for electronic paper.
- the multilayer structure may serve as both the substrate and the protective film.
- the electronic device to be protected by the protective sheet is not limited to the above example, and may be, for example, an IC tag, an optical communication device, a fuel cell, or the like.
- the protective sheet may include a surface protective layer disposed on one surface or both surfaces of the multilayer structure (W).
- the surface protective layer is preferably a layer made of a resin that is not easily damaged.
- the surface protective layer of the device which may be utilized outdoors like a solar cell consists of resin with high weather resistance (for example, light resistance).
- a surface protective layer with high translucency is preferable.
- Examples of the material for the surface protective layer include acrylic resin, polycarbonate, polyethylene terephthalate, polyethylene naphthalate, ethylene-tetrafluoroethylene copolymer, polytetrafluoroethylene, and 4-fluoroethylene-perchloroalkoxy. Copolymers, 4-fluorinated ethylene-6-fluorinated propylene copolymers, 2-ethylene-4-fluorinated ethylene copolymers, poly-3-fluoroethylene chloride, polyvinylidene fluoride, polyvinyl fluoride, etc. It is done.
- An example of the protective sheet includes an acrylic resin layer disposed on one surface.
- various additives for example, ultraviolet absorbers
- a preferable example of the surface protective layer having high weather resistance is an acrylic resin layer to which an ultraviolet absorber is added.
- ultraviolet absorbers include, but are not limited to, benzotriazole-based, benzophenone-based, salicylate-based, cyanoacrylate-based, nickel-based, and triazine-based ultraviolet absorbers.
- other stabilizers, light stabilizers, antioxidants and the like may be used in combination.
- a protective sheet contains the resin layer for joining with high adhesiveness with a sealing material.
- the sealing material is made of an ethylene-vinyl acetate copolymer
- the bonding resin layer include polyethylene terephthalate having improved adhesion to the ethylene-vinyl acetate copolymer.
- Each layer constituting the protective sheet may be bonded using a known adhesive or the above-described adhesive layer.
- the quantum dot phosphor dispersed resin molded body is used.
- the quantum dot phosphor-dispersed resin molded body is obtained by dispersing a quantum dot phosphor in a resin to obtain a dispersion (composition) and molding the dispersion.
- molding method is not specifically limited, A well-known method can be used.
- the dispersing resin a cycloolefin (co) polymer is preferable.
- cycloolefin (co) polymer examples include a cycloolefin polymer (COP) represented by the following formula [Q-1] or a cycloolefin copolymer (COC) represented by the following formula [Q-2]. Is mentioned. A commercial item can be used as such a cycloolefin (co) polymer.
- COP cycloolefin polymer
- COC cycloolefin copolymer
- ZEONEX registered trademark
- APL5014DP manufactured by Mitsui Chemicals, chemical structure;-(C 2 H 4 ) x (C 12 H 16 ) y- ; subscripts x and y are real numbers larger than 0 and smaller than 1, and represent a copolymerization ratio
- R 1 and R 2 are each independently the same or different and represent a hydrogen atom; a linear or branched saturated hydrocarbon group having 1 to 6 carbon atoms (preferably an alkyl group ); A monovalent group selected from the group consisting of a halogen atom of chlorine or fluorine; and a trihalomethyl group in which the halogen atom is a chlorine atom or a fluorine atom.
- the hydrocarbon groups of R 1 and R 2 may be bonded to each other at adjacent substitution sites to form at least one cyclic structure of a 5- to 7-membered saturated hydrocarbon.
- r is a positive integer.
- R 3 represents a hydrogen atom; a linear or branched saturated hydrocarbon group having 1 to 6 carbon atoms (preferably an alkyl group); a halogen atom of chlorine or fluorine; and a halogen atom Represents a monovalent group selected from the group consisting of a trihalomethyl group in which is a chlorine atom or a fluorine atom.
- R 4 and R 5 are each independently the same or different and are each a hydrogen atom; a linear or branched saturated hydrocarbon group having 1 to 6 carbon atoms (preferably an alkyl group); a halogen of chlorine or fluorine And a monovalent group selected from the group consisting of a trihalomethyl group in which the halogen atom is a chlorine atom or a fluorine atom.
- the hydrocarbon groups of R 4 or R 5 may be bonded to each other at adjacent substitution sites to form at least one cyclic structure of a 5- to 7-membered saturated hydrocarbon.
- the cycloolefin polymer (COP) represented by the formula [Q-1] can be obtained, for example, by subjecting norbornenes as raw materials to ring-opening metathesis polymerization using a Grubbs catalyst or the like and then hydrogenating.
- the cycloolefin copolymer (COC) represented by the formula [Q-2] is obtained, for example, by copolymerization with ethylene or the like using a norbornene as a raw material and using a metallocene catalyst or the like.
- the method of dispersing the quantum dot phosphor in the resin is not particularly limited, but the dispersion liquid in which the quantum dot phosphor is dispersed in a dispersion medium is added to a solution obtained by dissolving the resin in a solvent under an inert gas atmosphere. It is preferable to add and knead under.
- the dispersion medium used in that case is preferably a solvent that dissolves the resin, and more preferably, the dispersion medium and the solvent are the same.
- the solvent and the dispersion medium can be used without limitation, but preferably a hydrocarbon solvent such as toluene, xylene (o-, m- or p-), ethylbenzene, tetralin and the like can be used.
- chlorinated hydrocarbon solvents such as chlorobenzene, dichlorobenzene (o-, m- or p-), and trichlorobenzene can also be used.
- chlorinated hydrocarbon solvents such as chlorobenzene, dichlorobenzene (o-, m- or p-), and trichlorobenzene can also be used.
- helium gas, argon gas, and nitrogen gas are mentioned as an inert gas used at the above process, These may be used independently and may be mixed and used for arbitrary ratios.
- the quantum dot phosphor applied to the first embodiment is a phosphor exhibiting a quantum effect when the particle diameter is 1 to 100 nm and is several tens of nm or less.
- the particle size of the quantum dot phosphor is preferably in the range of 2 to 20 nm.
- the structure of the quantum dot phosphor is composed of an inorganic phosphor core and a capping layer (for example, an organic passive layer having an aliphatic hydrocarbon group) coordinated on the surface of the inorganic phosphor.
- the (metal part) is covered with an organic passive layer.
- an organic passivating layer is coordinated to the core surface on the surface of the quantum dot phosphor particles mainly for the purpose of preventing aggregation.
- the organic passivation layer also called shell
- the organic passivation can be selected according to the purpose, and for example, it is a linear or branched organic molecule having an aliphatic hydrocarbon having about 6 to 18 carbon atoms (for example, an alkyl group). May be.
- inorganic phosphors include group II-VI compound semiconductor nanocrystals, group III-V compound semiconductor nanocrystals, and the like.
- the form of these nanocrystals is not particularly limited.
- a crystal having a core-shell structure in which a core part of InP nanocrystal is coated with a shell part made of ZnS / ZnO or the like A crystal having a structure in which the boundary of the shell is not clear and the composition changes in a gradient, or a mixed crystal or two or more types of nanocrystals in which two or more types of compound crystals are partially separated in the same crystal Examples include alloys of crystalline compounds.
- the carbon number is 2 to 30, preferably 4 to 20, and more preferably 6 to 6 carbon atoms.
- Organic molecules having an aliphatic hydrocarbon group having 18 straight-chain structures or branched structures are exemplified.
- a capping agent coordinated on the surface of the inorganic phosphor (a reagent for forming an organic passivation layer) has a functional group for coordination with the inorganic phosphor.
- Examples of such a functional group include a carboxyl group, amino group, amide group, nitrile group, hydroxyl group, ether group, carbonyl group, sulfonyl group, phosphonyl group, and mercapto group.
- a carboxyl group is preferable.
- the composition used for the manufacture of the quantum dot phosphor-dispersed resin molded article for the electronic device including the quantum dot phosphor of Embodiment 1 contains a resin (eg, cycloolefin (co-olefin) in a concentration range of 0.01 to 20% by mass. )
- the polymer is uniformly dispersed with quantum dot phosphors.
- the composition containing the quantum dot phosphor of Embodiment 1 preferably has a cycloolefin (concentration range of more than 0.1% by mass and less than 15% by mass, more preferably more than 1% by mass and less than 10% by mass.
- the quantum dot phosphor should be uniformly dispersed in the (co) polymer.
- the concentration of the quantum dot fluorescent substance is less than 0.01 mass%, sufficient light emission intensity
- the concentration of the quantum dot phosphor exceeds 20% by mass, the quantum dot phosphor may be aggregated, and the quantum dot phosphor dispersed resin molded body in which the quantum dot phosphor is uniformly dispersed is obtained. It cannot be obtained and is not preferable.
- the quantum dot phosphor used in Embodiment 1 is manufactured by using a metal precursor from which a nanocrystal of a desired compound semiconductor is obtained, and then this is further dispersed in an organic solvent.
- the quantum dot fluorescent substance which has the structure where the hydrocarbon group coordinated to the surface of inorganic fluorescent substance can be prepared by processing a nanocrystal with a predetermined reactive compound (compound of a shell part).
- the treatment method is not particularly limited, and examples thereof include a method in which a nanocrystal dispersion is refluxed in the presence of a reactive compound.
- a method for producing the quantum dot phosphor for example, a method disclosed in Japanese Patent Application Laid-Open No. 2006-199963 can be used.
- the amount of the hydrocarbon group constituting the organic passivation layer covering the surface of the inorganic phosphor (core part) is not particularly limited, but one particle of inorganic phosphor (core)
- the hydrocarbon chain of the hydrocarbon group is usually in the range of 2 to 500 mol, preferably in the range of 10 to 400 mol, more preferably in the range of 20 to 300 mol.
- the hydrocarbon chain is less than 2 mol, the function as the organic passive layer cannot be imparted, and for example, the phosphor particles tend to condense.
- the quantum dot phosphor-dispersed resin molded body according to Embodiment 1 may be manufactured by molding a composition containing the quantum dot phosphor into a molded product.
- This molded product works effectively as a molded product that absorbs at least a part of the light emitted from the light source and emits secondary light from the quantum dot phosphor contained in the molded product.
- a method for molding a composition containing a quantum dot phosphor for example, after applying the composition to a substrate or filling a mold, the solvent is removed by heating and drying in the inert gas atmosphere, There is a method of peeling from a material or a mold.
- the composition containing quantum dot fluorescent substance can also be used as a sealing material which seals an LED chip.
- Examples of the method for producing a quantum dot phosphor-dispersed resin molded body include a step of preparing a solution in which a cycloolefin-based (co) polymer is dissolved in a solvent, and a quantum dot phosphor in the molded body obtained in the solution.
- a step of applying the composition containing the composition to a substrate or filling the mold into a mold and drying by heating.
- the solvent and the dispersion medium are as described above.
- Quantum dot phosphor-dispersed resin molded body can be produced by heating and drying, or a resin lens, a resin plate, a resin film, etc. can be produced by pressure molding.
- FIG. 2 shows a cross-sectional view of an example of a light emitting device using a composition containing the quantum dot phosphor according to the first embodiment as at least a part of a sealing material.
- the light emitting device 100 includes an LED chip 10, a lead electrode 12, a cup 14, and sealing materials 16 and 17.
- the resin lens 20 is disposed on the light emitting device 100 as necessary.
- the cup 14 can be formed of a suitable resin or ceramic.
- the LED chip 10 is not limited, the light emitting diode which comprises the light source of a suitable wavelength in cooperation with quantum dot fluorescent substance can be used.
- the sealing material 16 can be formed using the composition containing the quantum dot fluorescent substance in which the quantum dot fluorescent substance 18 was disperse
- a white light source that emits white light from the sealing material 16 using light emitted from the LED chip 10 can be formed.
- the sealing material 17 seals LED, a lead wire, etc.
- the sealing material 16 and the sealing material 17 are prepared by injecting a predetermined amount of resin (for example, epoxy resin, silicone resin) or the like into the cup 14 in an inert gas (for example, argon gas) atmosphere. It can be manufactured by forming a sealing material 17 by solidifying by a method, then injecting a composition containing a quantum dot phosphor onto the sealing material 17 and drying by heating.
- a lens-shaped resin (resin lens 20) formed of the quantum dot phosphor-dispersed resin molded body, or at least a part thereof has a convex portion above the sealing material 16 accommodated in the cup 14. It is good also as a structure which arrange
- the quantum dot phosphor 18 may not be dispersed in the sealing material 16.
- the thickness of the said sealing material 16 is 0.01 mm or more and less than 0.4 mm.
- the sealing material 16 When the thickness of the sealing material 16 exceeds 0.4 mm, the lead electrode 12 is sealed when the sealing material 16 is sealed in the concave portion of the cup 14, although depending on the depth in the concave portion of the cup 14. An excessive load is applied to the wire connected to the wire, which is not preferable.
- the composition containing the quantum dot phosphor is used for at least a part of the LED chip sealing material, the sealing material 16 has a thickness of less than 0.01 mm. Not enough as a material.
- a lens-shaped resin 20 (resin lens 20) formed of a quantum dot phosphor-dispersed resin molded body.
- FIG. 3 is a cross-sectional view of an example of a light emitting device using the quantum dot phosphor-dispersed resin molded body according to the first embodiment.
- FIG. 3 is an example of a light-emitting device that does not use the composition containing the quantum dot phosphor according to the first embodiment as a sealing material.
- the lens-shaped resin (resin lens 20) is a quantum dot formed by molding a composition in which the quantum dot phosphor 18 is dispersed in a cycloolefin (co) polymer in a concentration range of 0.01 to 20% by mass. It is formed of a phosphor-dispersed resin molded body.
- FIG. 4 is a cross-sectional view of an example of a light-emitting device using the composition including the quantum dot phosphor according to the first embodiment and the quantum dot phosphor-dispersed resin molded body.
- FIG. 4 shows a light-emitting device in which the composition containing the quantum dot phosphor according to the first embodiment is used as a part of a sealing material, and a resin lens 20 made of a quantum dot phosphor-dispersed resin molded body is disposed on the composition.
- the quantum dot phosphor 18 is formed in any resin by being dispersed in the cycloolefin (co) polymer in a concentration range of 0.01 to 20% by mass.
- a mobile phone, a television, Electronic devices such as displays and panels, and mechanical devices such as automobiles, computers, and game machines incorporating the electronic devices can be driven stably for a long time.
- FIG. 5 shows a cross-sectional view of an example of a structure including the quantum dot phosphor according to the second embodiment.
- the structure including the quantum dot phosphor includes a quantum dot phosphor-dispersed resin molded body 22 in which the quantum dot phosphor 18 is dispersed in a dispersion resin in a concentration range of 0.01 to 20% by mass.
- a gas barrier layer (protective sheet) 24 that covers the entire surface of the quantum dot phosphor-dispersed resin molded body 22 and reduces permeation of oxygen or the like to the quantum dot phosphor-dispersed resin molded body 22.
- the gas barrier layer 24 may be configured to cover a part of the surface of the quantum dot phosphor-dispersed resin molded body 22 (see FIGS. 6 and 7). Moreover, it is preferable that the gas barrier layer 24 is comprised from a multilayer structure (W) from the point which can reduce permeation
- W multilayer structure
- the gas barrier layer 24 means that the spectral radiant energy of the quantum dot phosphor 18 when the light emitting diode (LED) continuously emits light for 2,000 hours in the vicinity of the structure including the quantum dot phosphor is an initial value of 80.
- the electronic device of the present invention preferably has a spectral radiant energy of 85.0% or more of the initial value when the light is continuously emitted for 2,000 hours, and is 89.0% or more. Some are more preferable, and more preferably 90.0% or more.
- the spectral radiant energy is radiant energy at the fluorescence wavelength of the quantum dot phosphor. Spectral radiant energy can be measured, for example, using a quantum efficiency measuring device QE-1000 manufactured by Otsuka Electronics.
- the cycloolefin (co) polymer described in the first embodiment can be used as the dispersing resin constituting the quantum dot phosphor dispersed resin molded body 22.
- the manufacturing method of the quantum dot fluorescent substance dispersion resin molding demonstrated in Embodiment 1 is applicable.
- the multilayer structure (W) of the present invention constituting the quantum dot phosphor-dispersed resin molded body 22 and the gas barrier layer 24 described above has light transmittance, and the light generated by the light emitting diodes is quantized.
- the light up to the dot phosphor 18 and the light whose wavelength is converted by the quantum dot phosphor 18 can be transmitted to the outside of the quantum dot phosphor-dispersed resin molded body 22.
- FIG. 6 shows a cross-sectional view of an example of a light emitting device to which a structure including a quantum dot phosphor according to the second embodiment is applied.
- the light emitting device 100 includes an LED chip 10, a lead electrode 12, a cup 14, a sealing material 16 in which quantum dot phosphors 18 are dispersed, a sealing material 17 in which quantum dot phosphors 18 are not dispersed, and
- the gas barrier layer 24 is included.
- the gas barrier layer 24 is used as a lid of the cup 14.
- the sealing material 16 is comprised by the said quantum dot fluorescent substance dispersion
- the sealing material 16 and the sealing material 17 can be the same as those in FIG. Among these components, the quantum dot phosphor 18, the quantum dot phosphor dispersed resin molded body 22, and the gas barrier layer 24 are as described above.
- the LED chip 10 is not limited, but a light emitting diode that constitutes a light source of an appropriate wavelength in cooperation with the quantum dot phosphor can be used.
- the cup 14 can be formed with suitable resin or ceramics. Further, the sealing material 17 seals the LED chip 10, the lead electrode 12, and the like.
- FIG. 7 shows a cross-sectional view of another example of the light emitting device to which the structure including the quantum dot phosphor according to the second embodiment is applied, and the same elements as those in FIG. 6 are denoted by the same reference numerals.
- the surface of the cutter 14 including the lid portion of FIG. 6
- the surface of the lead electrode 12 exposed outside the cup 14 are covered with the gas barrier layer 24.
- a part of the surface of the lead electrode 12 is exposed without being covered with the gas barrier layer 24. This is because, for example, electrical connection is established with a power supply path on the mounting board.
- the gas barrier layer 24 covers the upper surface of the sealing material 16 in the figure.
- the quantum dot phosphor 18 dispersed in the sealing material 16 it is possible to avoid or reduce the penetration of oxygen or the like to the quantum dot phosphor 18 dispersed in the sealing material 16. Further, a part of the light from the LED chip 10 is converted into light of another wavelength by the quantum dot phosphor 18 dispersed in the sealing material 16, and then mixed with the light from the LED chip 10 to form a gas barrier. It passes through the layer 24 and is taken out to the outside.
- the lid of the cup 14 is formed of the gas barrier layer 24 and covers the upper surface of the sealing material 16 in the figure. Thereby, it is possible to avoid or reduce the penetration of oxygen or the like to the quantum dot phosphor 18 dispersed in the sealing material 16.
- the above-described quantum dot phosphor dispersed resin composition or molded body thereof or a structure containing the quantum dot phosphor includes, for example, plant growth illumination, colored illumination, white illumination, LED backlight light source, phosphor-containing liquid crystal
- the present invention can also be applied to filters, phosphor-containing resin plates, hair growth equipment light sources, communication light sources, and the like.
- the multilayer structure (W) used for the electronic device containing the quantum dot phosphor of the present invention includes a substrate (X) and a layer (Y) containing aluminum.
- the layer (Y) contains a reaction product (D) of a compound (A) containing aluminum (hereinafter also simply referred to as “compound (A)”) and a phosphorus compound (B).
- the material of the base material (X) is not particularly limited, and base materials made of various materials can be used.
- Examples of the material of the substrate (X) include resins such as thermoplastic resins and thermosetting resins; wood; glass and the like. Among these, a thermoplastic resin is preferable.
- the form of the substrate (X) is not particularly limited, and may be a layered form such as a film or a sheet.
- a base material (X) what contains a thermoplastic resin film is preferable, and it is more preferable that it is a thermoplastic resin film.
- thermoplastic resin used for the substrate (X) examples include polyolefin resins such as polyethylene and polypropylene; polyethylene terephthalate (PET), polyethylene-2,6-naphthalate, polybutylene terephthalate, and copolymers thereof.
- Polyester resins such as nylon-6, nylon-66, nylon-12, etc .; hydroxyl group-containing polymers such as polyvinyl alcohol and ethylene-vinyl alcohol copolymers; polystyrene; poly (meth) acrylic acid esters; polyacrylonitrile; Polyvinyl acetate; Polycarbonate; Polyarylate; Regenerated cellulose; Polyimide; Polyetherimide; Polysulfone; Polyethersulfone; Polyetheretherketone; Ionomer resin
- the material for the substrate (X) is preferably at least one thermoplastic resin selected from the group consisting of polyethylene, polypropylene, polyethylene terephthalate, nylon-6, and nylon-66.
- the substrate (X) When a film made of a thermoplastic resin is used as the substrate (X), the substrate (X) may be a stretched film or an unstretched film.
- a stretched film, particularly a biaxially stretched film is preferred because the processability (printing, laminating, etc.) of the resulting multilayer structure is excellent.
- the biaxially stretched film may be a biaxially stretched film produced by any one of a simultaneous biaxial stretching method, a sequential biaxial stretching method, and a tubular stretching method.
- the thickness is preferably 1 to 1,000 ⁇ m, more preferably 5 to 500 ⁇ m from the viewpoint of improving the mechanical strength and workability of the resulting multilayer structure. 9 to 200 ⁇ m is more preferable.
- the layer (Y) contains a reaction product (D) of the compound (A) and the phosphorus compound (B).
- Compound (A) is a compound containing aluminum.
- the phosphorus compound (B) has a functional group containing a phosphorus atom.
- the phosphorus compound (B) is an inorganic phosphorus compound (BI) and / or an organic phosphorus compound (BO). The compound (A) and the phosphorus compound (B) will be described below.
- the compound (A) is preferably a metal oxide (Aa) containing aluminum (hereinafter also simply referred to as “metal oxide (Aa)”).
- Metal oxide containing aluminum (Aa) The metal oxide (Aa) containing aluminum is usually reacted with a phosphorus compound (B) (preferably an inorganic phosphorus compound (BI)) in the form of particles.
- a phosphorus compound (B) preferably an inorganic phosphorus compound (BI)
- the metal atoms constituting the metal oxide (Aa) containing aluminum are at least one selected from metal atoms belonging to Groups 2 to 14 of the periodic table. It is a seed metal atom, but it contains at least aluminum.
- the metal atom (M) may be aluminum alone or may contain aluminum and other metal atoms. Two or more metal oxides (Aa) may be used in combination as the metal oxide (Aa).
- the proportion of aluminum in the metal atom (M) is usually 50 mol% or more, 60 to 100 mol%, or 80 to 100 mol%.
- the metal oxide (Aa) include a metal oxide produced by a method such as a liquid phase synthesis method, a gas phase synthesis method, or a solid pulverization method.
- the metal oxide (Aa) may be a hydrolysis condensate of the compound (E) containing a metal atom (M) to which a hydrolyzable characteristic group is bonded.
- Examples of the characteristic group include R 1 of the general formula [I] described later.
- the hydrolysis condensate of compound (E) can be substantially regarded as a metal oxide. Therefore, in this specification, the hydrolysis condensate of compound (E) may be referred to as “metal oxide (Aa)”. That is, in the present specification, “metal oxide (Aa)” can be read as “hydrolysis condensate of compound (E)”, and “hydrolysis condensate of compound (E)” is “metal oxidation condensate”. It can be read as “object (Aa)”.
- the compound (E) is a compound (Ea) represented by the following general formula [I]. It is preferable to include at least one. Al (R 1 ) k (R 2 ) 3-k [I] In the formula, R 1 has a halogen atom (fluorine atom, chlorine atom, bromine atom, iodine atom), NO 3 , an optionally substituted alkoxy group having 1 to 9 carbon atoms, or a substituent.
- R 1 has a halogen atom (fluorine atom, chlorine atom, bromine atom, iodine atom), NO 3 , an optionally substituted alkoxy group having 1 to 9 carbon atoms, or a substituent.
- R 2 represents an optionally substituted alkyl group having 1 to 9 carbon atoms, an optionally substituted aralkyl group having 7 to 10 carbon atoms, and an optionally substituted carbon.
- k is an integer of 1 to 3.
- Compound (E) may contain at least one compound (Eb) represented by the following general formula [II] in addition to compound (Ea).
- M 1 is a metal atom other than aluminum and is at least one metal atom selected from metal atoms belonging to Groups 2 to 14 of the periodic table.
- R 3 may have a halogen atom (fluorine atom, chlorine atom, bromine atom, iodine atom), NO 3 , an optionally substituted alkoxy group having 1 to 9 carbon atoms, or a substituent.
- R 4 represents an optionally substituted alkyl group having 1 to 9 carbon atoms, an optionally substituted aralkyl group having 7 to 10 carbon atoms, and an optionally substituted carbon.
- m is an integer of 1 to n.
- n is equal to the valence of M 1 .
- alkoxy group of R 1 and R 3 examples include methoxy group, ethoxy group, n-propoxy group, isopropoxy group, n-butoxy group, isobutoxy group, sec-butoxy group, tert-butoxy group, benzyloxy group, diphenyl Methoxy group, trityloxy group, 4-methoxybenzyloxy group, methoxymethoxy group, 1-ethoxyethoxy group, benzyloxymethoxy group, 2-trimethylsilylethoxy group, 2-trimethylsilylethoxymethoxy group, phenoxy group, 4-methoxyphenoxy group Etc.
- Examples of the acyloxy group for R 1 and R 3 include an acetoxy group, an ethylcarbonyloxy group, an n-propylcarbonyloxy group, an isopropylcarbonyloxy group, an n-butylcarbonyloxy group, an isobutylcarbonyloxy group, and a sec-butylcarbonyloxy group. Group, tert-butylcarbonyloxy group, n-octylcarbonyloxy group and the like.
- alkenyloxy group for R 1 and R 3 examples include allyloxy group, 2-propenyloxy group, 2-butenyloxy group, 1-methyl-2-propenyloxy group, 3-butenyloxy group, 2-methyl-2-propenyl Oxy group, 2-pentenyloxy group, 3-pentenyloxy group, 4-pentenyloxy group, 1-methyl-3-butenyloxy group, 1,2-dimethyl-2-propenyloxy group, 1,1-dimethyl-2- Propenyloxy group, 2-methyl-2-butenyloxy group, 3-methyl-2-butenyloxy group, 2-methyl-3-butenyloxy group, 3-methyl-3-butenyloxy group, 1-vinyl-2-propenyloxy group, And 5-hexenyloxy group.
- Examples of the ⁇ -diketonato group for R 1 and R 3 include 2,4-pentandionato group, 1,1,1-trifluoro-2,4-pentandionato group, 1,1,1,5, 5,5-hexafluoro-2,4-pentanedionate group, 2,2,6,6-tetramethyl-3,5-heptanedionate group, 1,3-butanedionate group, 2-methyl-1,3-butanedionate Group, 2-methyl-1,3-butanedionato group, benzoylacetonato group and the like.
- Examples of the acyl group of the diacylmethyl group of R 1 and R 3 include carbon numbers such as formyl group, acetyl group, propionyl group (propanoyl group), butyryl group (butanoyl group), valeryl group (pentanoyl group), hexanoyl group and the like. 1-6 aliphatic acyl groups; aromatic acyl groups (aroyl groups) such as benzoyl groups and toluoyl groups.
- Examples of the alkyl group for R 2 and R 4 include a methyl group, an ethyl group, an n-propyl group, an isopropyl group, an n-butyl group, an isobutyl group, a sec-butyl group, a tert-butyl group, an n-pentyl group, Examples include isopentyl group, n-hexyl group, isohexyl group, 3-methylpentyl group, 2-methylpentyl group, 1,2-dimethylbutyl group, cyclopropyl group, cyclopentyl group, cyclohexyl group and the like.
- Examples of the aralkyl group of R 2 and R 4 include a benzyl group and a phenylethyl group (phenethyl group).
- alkenyl group for R 2 and R 4 examples include a vinyl group, 1-propenyl group, 2-propenyl group, isopropenyl group, 3-butenyl group, 2-butenyl group, 1-butenyl group, 1-methyl-2 -Propenyl group, 1-methyl-1-propenyl group, 1-ethyl-1-ethenyl group, 2-methyl-2-propenyl group, 2-methyl-1-propenyl group, 3-methyl-2-butenyl group, 4 -Pentenyl group and the like.
- Examples of the aryl group for R 2 and R 4 include a phenyl group, a 1-naphthyl group, and a 2-naphthyl group.
- Examples of the substituent in R 1 , R 2 , R 3 and R 4 include alkyl groups having 1 to 6 carbon atoms; methoxy group, ethoxy group, n-propoxy group, isopropoxy group, n-butoxy group, isobutoxy group , Sec-butoxy group, tert-butoxy group, n-pentyloxy group, isopentyloxy group, n-hexyloxy group, cyclopropyloxy group, cyclobutyloxy group, cyclopentyloxy group, cyclohexyloxy group, etc.
- R 1 and R 3 include a halogen atom, NO 3 , an optionally substituted alkoxy group having 1 to 6 carbon atoms, an optionally substituted acyloxy group having 2 to 6 carbon atoms, A ⁇ -diketonato group having 5 to 10 carbon atoms which may have a substituent or a diacylmethyl group having an acyl group having 1 to 6 carbon atoms which may have a substituent is preferable.
- An optionally substituted alkoxy group having 1 to 6 carbon atoms is more preferable.
- R 2 and R 4 are preferably an alkyl group having 1 to 6 carbon atoms which may have a substituent.
- K in the formula [I] is preferably 3.
- M 1 is preferably a metal atom belonging to Group 4 of the periodic table, more preferably titanium or zirconium.
- m in Formula [II] is preferably 4.
- boron and silicon may be classified as semi-metals, but in this specification, these are included in the metal.
- Examples of the compound (Ea) include aluminum chloride, aluminum nitrate, aluminum acetate, tris (2,4-pentanedionato) aluminum, trimethoxyaluminum, triethoxyaluminum, tri-n-propoxyaluminum, triisopropoxyaluminum, Tri-n-butoxyaluminum, tri-sec-butoxyaluminum, tri-tert-butoxyaluminum and the like can be mentioned, among which triisopropoxyaluminum and tri-sec-butoxyaluminum are preferable.
- the compound (E) two or more kinds of compounds (Ea) may be used in combination.
- Examples of the compound (Eb) include tetrakis (2,4-pentanedionato) titanium, tetramethoxytitanium, tetraethoxytitanium, tetraisopropoxytitanium, tetra-n-butoxytitanium, tetrakis (2-ethylhexoxy) titanium and the like. Titanium compounds; zirconium compounds such as tetrakis (2,4-pentanedionato) zirconium, tetra-n-propoxyzirconium, tetra-n-butoxyzirconium, and the like. These may be used alone or in combination of two or more compounds (Eb).
- the ratio of the compound (Ea) in the compound (E) is not particularly limited as long as the effect of the present invention is obtained.
- the proportion of the compound other than the compound (Ea) (for example, the compound (Eb)) in the compound (E) is, for example, preferably 20 mol% or less, more preferably 10 mol% or less, further preferably 5 mol% or less, It may be 0 mol%.
- the hydrolyzate condenses to form a compound in which the metal atom (M) is bonded through the oxygen atom (O).
- a compound that can be substantially regarded as a metal oxide is formed.
- a hydroxyl group usually exists on the surface of the metal oxide (Aa) thus formed.
- a compound having a ratio of [number of moles of oxygen atom (O) bonded only to metal atom (M)] / [number of moles of metal atom (M)] of 0.8 or more is metal It shall be included in oxide (Aa).
- the oxygen atom (O) bonded only to the metal atom (M) is the oxygen atom (O) in the structure represented by MOM, and the structure represented by MOH.
- Oxygen atoms bonded to metal atoms (M) and hydrogen atoms (H) such as oxygen atoms (O) in are excluded.
- the ratio in the metal oxide (Aa) is preferably 0.9 or more, more preferably 1.0 or more, and further preferably 1.1 or more. Although the upper limit of this ratio is not particularly limited, it is usually represented by n / 2, where n is the valence of the metal atom (M).
- the compound (E) In order for the hydrolysis condensation to occur, it is important that the compound (E) has a hydrolyzable characteristic group. When these groups are not bonded, the hydrolysis condensation reaction does not occur or becomes extremely slow, making it difficult to prepare the target metal oxide (Aa).
- the hydrolyzed condensate of compound (E) may be produced from a specific raw material by, for example, a method adopted in a known sol-gel method.
- the raw materials include compound (E), partial hydrolyzate of compound (E), complete hydrolyzate of compound (E), compound obtained by partially hydrolytic condensation of compound (E), and compound (E ) Can be used at least one selected from the group consisting of compounds obtained by condensing a part of the complete hydrolyzate.
- the metal oxide (Aa) provided for mixing with an inorganic phosphorus compound (BI) -containing material substantially contains a phosphorus atom. It is preferable not to contain.
- the phosphorus compound (B) has a functional group containing a phosphorus atom.
- the phosphorus compound (B) is an inorganic phosphorus compound (BI) and / or an organic phosphorus compound (BO), and an inorganic phosphorus compound (BI) is preferable.
- the inorganic phosphorus compound (BI) contains a site capable of reacting with the metal oxide (Aa), and typically contains a plurality of such sites.
- the inorganic phosphorus compound (BI) is preferably a compound containing 2 to 20 such sites (atomic groups or functional groups). Examples of such a part include a part capable of performing a condensation reaction with a functional group (for example, a hydroxyl group) present on the surface of the metal oxide (Aa). Examples of such a site include a halogen atom directly bonded to a phosphorus atom, an oxygen atom directly bonded to a phosphorus atom, and the like.
- the functional group (for example, hydroxyl group) present on the surface of the metal oxide (Aa) is usually bonded to the metal atom (M) constituting the metal oxide (Aa).
- Examples of the inorganic phosphorus compound (BI) include phosphoric acid, diphosphoric acid, triphosphoric acid, polyphosphoric acid condensed with 4 or more molecules of phosphoric acid, phosphorous acid, phosphonic acid, phosphonous acid, phosphinic acid, and phosphine.
- Phosphorus oxoacids such as acids, and salts thereof (eg, sodium phosphate), and derivatives thereof (eg, halides (eg, phosphoryl chloride), dehydrates (eg, diphosphorus pentoxide)), and the like It is done.
- inorganic phosphorus compounds (BI) may be used alone or in combination of two or more.
- inorganic phosphorus compounds (BI) it is preferable to use phosphoric acid alone or to use phosphoric acid and other inorganic phosphorus compounds (BI) in combination.
- phosphoric acid By using phosphoric acid, the stability of the coating liquid (S) described later and the gas barrier properties of the resulting multilayer structure (W) are improved.
- Organic phosphorus compound (BO) examples include a phosphoric acid group, a phosphorous acid group, a phosphonic acid group, a phosphonous acid group, a phosphinic acid group, and a phosphinic acid group.
- Functional groups for example, salts, (partial) ester compounds, halides (for example, chloride), dehydrates), etc., among which phosphoric acid groups and phosphonic acid groups are preferred, and phosphonic acid groups are more preferred. preferable.
- the organic phosphorus compound (BO) is preferably a polymer (BOa) having a functional group containing the phosphorus atom.
- the polymer (BOa) include 6-[(2-phosphonoacetyl) oxy] hexyl acrylate, 2-phosphonooxyethyl methacrylate, phosphonomethyl methacrylate, 11-phosphonoundecyl methacrylate, and methacrylic acid.
- the polymer (BOa) may be a homopolymer of a monomer having a functional group containing at least one phosphorus atom, or may be a copolymer of two or more monomers.
- a polymer (BOa) which consist of a single monomer as a polymer (BOa).
- a polymer of phosphono (meth) acrylic acid esters and a polymer of vinylphosphonic acids are preferable, and a polymer of vinylphosphonic acids is more preferable. That is, as the polymer (BOa), poly (vinyl phosphonic acid) is preferable.
- the polymer (BOa) can also be obtained by hydrolyzing a vinylphosphonic acid derivative such as vinylphosphonic acid halide or vinylphosphonic acid ester alone or copolymerized.
- the polymer (BOa) may be a copolymer of a monomer having a functional group containing at least one phosphorus atom and another vinyl monomer.
- the proportion of the structural unit derived from the monomer having a functional group containing a phosphorus atom in the total structural unit of the polymer (BOa) is 10 mol%.
- the above is preferable, 20 mol% or more is more preferable, 40 mol% or more is more preferable, 70 mol% or more is particularly preferable, and 100 mol% may be sufficient.
- the molecular weight of the polymer (BOa) is not particularly limited, but the number average molecular weight is preferably in the range of 1,000 to 100,000. When the number average molecular weight is within this range, it is possible to achieve both a high level of improvement in the bending resistance by laminating the layer (Y) and the viscosity stability of the coating liquid (T) described later.
- the layer of the multilayer structure (W) (Y) if it contains inorganic phosphorus compound (BI), a layer of the mass W BO inorganic phosphorus compound in the (Y) Weight W BI and the organic phosphorus compound (BI) (BO) It is preferable that the ratio W BO / W BI satisfies the relationship of 0.01 / 99.99 ⁇ W BO / W BI ⁇ 6.00 / 94.00, and 0.10 / 99.90 from the viewpoint of excellent barrier performance.
- W BO / W BI ⁇ 4.50 / 95.50 is more preferable, and 0.20 / 99.80 ⁇ W BO / W BI ⁇ 4.00 / 96.00 is satisfied More preferably, those satisfying the relationship of 0.50 / 99.50 ⁇ W BO / W BI ⁇ 3.50 / 96.50 are particularly preferable. That is, W BO is a trace amount of 0.01 or more and less than 6.00, whereas W BI is preferably used in a large amount of 94.00 or more and 99.99 or less.
- the inorganic phosphorus compound (BI) and / or the organic phosphorus compound (BO) constituting the reaction product.
- the mass of the inorganic phosphorus compound (BI) and / or the organic phosphorus compound (BO) used for forming the reaction product (the mass of the inorganic phosphorus compound (BI) and / or the organic phosphorus compound (BO) before the reaction).
- reaction product (D) The reaction product (D) is obtained by a reaction between a compound (A) containing aluminum and a phosphorus compound (B).
- the reaction product (D) also includes a compound produced by a reaction between the compound (A) containing aluminum, the phosphorus compound (B), and another compound.
- the reaction product (Dc) obtained by reacting the product (Aa) with the inorganic phosphorus compound (BI) is more preferable.
- the maximum absorption wave number in the region of 800 to 1,400 cm ⁇ 1 is preferably in the range of 1,080 to 1,130 cm ⁇ 1 .
- the metal atom (M) derived from the metal oxide (Aa) and the inorganic phosphorus compound (BI) And a phosphorus atom (P) derived from the above form a bond represented by MOP via an oxygen atom (O).
- a characteristic absorption band derived from the bond is generated in the infrared absorption spectrum of the reaction product (D).
- the obtained multilayer structure has an excellent gas barrier. It was found to express sex. In particular, when the characteristic absorption band is the strongest absorption in the region of 800 to 1,400 cm ⁇ 1 in which absorption derived from bonds between various atoms and oxygen atoms is generally observed, the obtained multilayer structure was found to exhibit even better gas barrier properties.
- the layer (Y) In the infrared absorption spectrum of the layer (Y), 800 half-value width of the maximum absorption band in the region of ⁇ 1,400cm -1, from the gas barrier properties of the viewpoint of the resulting multilayer structure, 200 cm -1 or less is preferable, 150 cm -1 The following is more preferable, 100 cm ⁇ 1 or less is further preferable, and 50 cm ⁇ 1 or less is particularly preferable.
- the infrared absorption spectrum of the layer (Y) can be measured by the method described in Examples. However, when measurement by the method described in Examples is not possible, reflection measurement such as reflection absorption method, external reflection method, attenuated total reflection method, etc., scraping the layer (Y) from the multilayer structure, Nujol method, tablet method, etc. Although it may measure by the method of transmission measurement, it is not limited to these.
- the layer (Y) may partially contain a metal oxide (Aa) and / or an inorganic phosphorus compound (BI) that is not involved in the reaction.
- the molar ratio of the metal atom constituting the metal oxide (Aa) to the phosphorus atom derived from the inorganic phosphorus compound (BI) is [metal atom constituting the metal oxide (Aa)]: [ The phosphorus atom derived from the inorganic phosphorus compound (BI)] is preferably in the range of 1.0: 1.0 to 3.6: 1.0, and 1.1: 1.0 to 3.0: 1. More preferably, it is in the range of 0. Outside this range, the gas barrier performance decreases.
- the molar ratio in the layer (Y) can be adjusted by the mixing ratio of the metal oxide (Aa) and the inorganic phosphorus compound (BI) in the coating liquid for forming the layer (Y).
- the molar ratio in the layer (Y) is usually the same as that in the coating liquid.
- the average particle size of the reaction product (D) is 5 nm or more and 50 nm or less.
- the upper limit of the average particle diameter is preferably 40 nm or less, and more preferably 35 nm or less.
- the lower limit of the average particle diameter is preferably 15 nm or more, and more preferably 20 nm or more.
- the average particle size of the reaction product (D) is more preferably 15 nm or more and 40 nm or less, and further preferably 20 nm or more and 35 nm or less.
- the particle size is less than 5 nm, the barrier performance after dump heat may be deteriorated.
- the particle size is larger than 50 nm, sufficient barrier performance cannot be obtained, and the total light transmittance or haze decreases.
- the measuring method of the average particle diameter of the reaction product (D) is as described in Examples described later.
- the average particle size of the reaction product (D) is the concentration of the solution used for the reaction, the viscosity of the coating solution, the temperature conditions (reaction temperature, drying temperature, heat treatment temperature, etc.), the compound (A) and the phosphorus compound (B). It can be controlled by changing or appropriately combining the mixing ratio (such as the molar ratio of aluminum atom to phosphorus atom).
- the average particle diameter of the reaction product (D) precursor of the precursor layer of the layer (Y) is preferably less than 5 nm, and more preferably less than 4 nm from the viewpoint of exhibiting excellent barrier performance even after stricter retorting. More preferably, it is less than 3 nm.
- the average particle diameter of the reaction product (D) in the layer (Y) obtained by the average particle diameter of the reaction product (D) precursor in the precursor layer of the layer (Y) after the drying treatment being in the above range. And a better barrier performance can be obtained.
- limiting in particular in the minimum of the average particle diameter of a reaction product (D) precursor For example, 0.1 nm or more may be sufficient and 1 nm or more may be sufficient.
- the measuring method of the average particle diameter of a reaction product (D) precursor is as having described in the Example mentioned later.
- the multilayer structure (W) may further include a layer (Z).
- the layer (Z) contains a polymer (BOa) having a functional group containing a phosphorus atom.
- the layer (Z) is preferably disposed adjacent to the layer (Y). That is, the layer (Z) and the layer (Y) are preferably arranged so as to contact each other.
- the layer (Z) is preferably disposed on the opposite side (preferably the surface on the opposite side) of the substrate (X) with the layer (Y) interposed therebetween. In other words, it is preferable to arrange the base (X) / layer (Y) / layer (Z) in this order.
- the layer (Z) is disposed on the side opposite to the substrate (X) (preferably the surface on the opposite side) across the layer (Y), and is disposed adjacent to the layer (Y).
- the layer (Z) may further include a polymer (F) containing at least one functional group selected from the group consisting of a carbonyl group, a hydroxyl group, a carboxyl group, a carboxylic anhydride group, and a salt of a carboxyl group. .
- the kind, amount, etc. of the polymer (BOa) in the layer (Z) can be used as those in the layer (Y).
- the layer (Z) may be composed only of the polymer (BOa), may be composed only of the polymer (BOa) and the polymer (F), or may further include other components.
- examples of other components contained in the layer (Z) include inorganic acid metal salts such as carbonates, hydrochlorides, nitrates, hydrogen carbonates, sulfates, hydrogen sulfates and borates; acetates and stearates.
- Organic acid metal salts such as oxalate and tartrate; metal complexes such as cyclopentadienyl metal complexes (for example, titanocene) and cyano metal complexes (for example, Prussian blue); layered clay compounds; cross-linking agents; Polymer compounds other than BOa) and polymer (F): plasticizers; antioxidants; ultraviolet absorbers; flame retardants and the like.
- the content of the other components in the layer (Z) is preferably 50% by mass or less, more preferably 20% by mass or less, further preferably 10% by mass or less, and more preferably 5% by mass. The following is particularly preferable, and may be 0% by mass (excluding other components).
- the layer (Z) includes at least one of a compound (A) containing aluminum, a phosphorus compound (B), and a reaction product (D) of the compound (A) containing aluminum and the phosphorus compound (B). Absent. Typically, layer (Z) does not contain at least a metal oxide (Aa).
- the multilayer structure (W) may further include an inorganic vapor deposition layer.
- An inorganic vapor deposition layer can be formed by vapor-depositing an inorganic substance.
- the inorganic substance for example, metal (for example, aluminum), metal oxide (for example, silicon oxide, aluminum oxide), metal nitride (for example, silicon nitride), metal nitride oxide (for example, silicon oxynitride), or metal Examples thereof include carbonitrides (for example, silicon carbonitride).
- the layer (Y) in the multilayer structure (W) of the present invention may include an inorganic vapor deposition layer containing aluminum.
- the layer (Y) may include an aluminum deposition layer (Ac) and / or an aluminum oxide deposition layer (Ad).
- the method for forming the inorganic vapor deposition layer is not particularly limited, and physical vapor deposition methods such as vacuum vapor deposition methods (for example, resistance heating vapor deposition, electron beam vapor deposition, molecular beam epitaxy method, etc.), sputtering methods, ion plating methods, heat Chemical vapor deposition (for example, catalytic chemical vapor deposition), photochemical vapor deposition, plasma chemical vapor deposition (for example, capacitively coupled plasma, inductively coupled plasma, surface wave plasma, electron cyclotron resonance, dual magnetron, Chemical vapor deposition methods such as atomic layer deposition and the like, and metal organic chemical vapor deposition.
- vacuum vapor deposition methods for example, resistance heating vapor deposition, electron beam vapor deposition, molecular beam epitaxy method, etc.
- sputtering methods ion plating methods
- heat Chemical vapor deposition for example, catalytic chemical vapor deposition
- photochemical vapor deposition for example, plasma chemical vapor deposition
- the thickness of the inorganic vapor deposition layer varies depending on the types of components constituting the inorganic vapor deposition layer, but is preferably 0.002 to 0.5 ⁇ m, more preferably 0.005 to 0.2 ⁇ m, and 0.01 to 0.1 ⁇ m. Further preferred. Within this range, a thickness that improves the barrier properties or mechanical properties of the multilayer structure may be selected.
- the thickness of the inorganic vapor deposition layer is less than 0.002 ⁇ m, the reproducibility of the barrier property expression of the inorganic vapor deposition layer against oxygen or water vapor tends to decrease, and the inorganic vapor deposition layer does not exhibit sufficient barrier properties There is also.
- the thickness of the inorganic vapor deposition layer exceeds 0.5 ⁇ m, the barrier property of the inorganic vapor deposition layer tends to be lowered when the multilayer structure is pulled or bent.
- the layer (Y) contained in the multilayer structure (W) may be constituted only by the reaction product (D) of the compound (A) containing aluminum and the phosphorus compound (B); metal oxidation containing aluminum
- the product (Aa) and the phosphorus compound (B) may be constituted only by the reaction product (Da); the compound (A) containing aluminum reacts with the inorganic phosphorus compound (BI). It may be comprised only by the reaction product (Db) which becomes; It is comprised only by the reaction product (Dc) which the metal oxide (Aa) containing aluminum and inorganic phosphorus compound (BI) react. Also good.
- the layer (Y) can further contain other components.
- Examples of other components include inorganic acid metal salts such as carbonates, hydrochlorides, nitrates, hydrogen carbonates, sulfates, hydrogen sulfates, borates; oxalates, acetates, tartrate, stearates
- Organic acid metal salts such as: metal complexes such as cyclopentadienyl metal complexes (for example, titanocene) and cyano metal complexes (for example, Prussian blue); layered clay compounds; cross-linking agents; polymers other than organic phosphorus compounds (BO) (F); Plasticizer; Antioxidant; Ultraviolet absorber; Flame retardant and the like.
- the content of the other component in the layer (Y) in the multilayer structure is preferably 50% by mass or less, more preferably 20% by mass or less, and further preferably 10% by mass or less.
- the content is particularly preferably 5% by mass or less, and may be 0% by mass (excluding other components).
- the polymer (F) is, for example, a polymer (Fa) having at least one functional group selected from the group consisting of an ether bond, a carbonyl group, a hydroxyl group, a carboxyl group, a carboxylic acid anhydride group, and a carboxyl group salt. It may be.
- polymer (Fa) examples include polyalkylene glycols having 2 to 4 carbon atoms such as polyethylene glycol, polyethylene oxide, polypropylene glycol, polypropylene oxide, polyoxyethylene polyoxypropylene glycol, polytetramethylene ether glycol and the like.
- the polymer (Fa) may be a homopolymer of a monomer having a polymerizable group (for example, vinyl acetate or acrylic acid), or may be a copolymer of two or more monomers. It may be a copolymer of a monomer having a hydroxyl group and / or a carboxyl group and a monomer having no such group. In addition, as a polymer (Fa), you may use 2 or more types of polymers (Fa) together.
- a polymerizable group for example, vinyl acetate or acrylic acid
- the molecular weight of the polymer (Fa) is not particularly limited, but in order to obtain a multilayer structure having better gas barrier properties and mechanical strength, the weight average molecular weight of the polymer (Fa) should be 5,000 or more. Is preferably 8,000 or more, more preferably 10,000 or more.
- the upper limit of the weight average molecular weight of a polymer (Fa) is not specifically limited, For example, it is 1,500,000 or less.
- the content of the polymer (Fa) in the layer (Y) is preferably 85% by mass or less, based on the mass of the layer (Y) (100% by mass). More preferably, it is more preferably 20% by mass or less, particularly preferably 10% by mass or less.
- the polymer (Fa) may or may not react with the component in the layer (Y).
- the thickness of the layer (Y) (when the multilayer structure (W) has two or more layers (Y), the total thickness of each layer (Y)) is preferably 0.05 to 4.0 ⁇ m, 0.1 to 2.0 ⁇ m is more preferable.
- the thickness per layer (Y) is preferably 0.05 ⁇ m or more from the viewpoint of gas barrier properties.
- the thickness of the layer (Y) can be controlled by the concentration of a coating liquid (S) described later used for forming the layer (Y) or the coating method thereof.
- the thickness of the layer (Y) can be measured by observing the cross section of the multilayer structure (W) with a scanning electron microscope or a transmission electron microscope.
- a coating liquid (S) (first coating liquid) containing a compound (A) containing aluminum, a phosphorus compound (B) and a solvent is used as a base material ( Step (I) for forming the precursor layer of the layer (Y) containing the reaction product (D) precursor by coating on X), and the precursor layer of the layer (Y) at a temperature of 140 ° C. or higher
- the manufacturing method which includes the formation process (II) of the layer (Y) containing the reaction product (D) can be given by performing the heat treatment in step (b).
- the said manufacturing method may contain the organophosphorus compound (BO) in the coating liquid (S) used for process (I), and the organophosphorus compound (BO) in the coating liquid (S) used for process (I).
- the organic phosphorus compound (BO) -containing coating liquid (T) is not contained, a step (I ′) of coating the surface of the layer (Y) obtained in the step (II) may be included.
- the compound (A), the inorganic phosphorus compound (BI), the organic phosphorus compound (BO), and the mass ratio thereof have been described above, redundant descriptions are omitted in the manufacturing method.
- step (I) the base material is coated with a coating liquid (S) (first coating liquid) containing a compound (A) containing aluminum, a phosphorus compound (B), and a solvent on the base material (X).
- the precursor layer of the layer (Y) containing the reaction product (D) precursor is formed on (X).
- the coating liquid (S) is obtained by mixing a compound (A) containing aluminum, a phosphorus compound (B), and a solvent.
- the layer (Y) includes an aluminum vapor deposition layer (Ac) or an aluminum oxide vapor deposition layer (Ad)
- these layers can be formed by the general vapor deposition method described above.
- a preferred embodiment will be described using an embodiment using a metal oxide (Aa), an inorganic phosphorus compound (BI), and a solvent.
- the coating liquid (S) can be prepared by mixing and reacting a metal oxide (Aa), an inorganic phosphorus compound (BI), and a solvent in a solvent.
- the coating liquid (S) is a method of mixing a dispersion of a metal oxide (Aa) and a solution containing an inorganic phosphorus compound (BI); an inorganic phosphorus compound in a dispersion of a metal oxide (Aa) It can be prepared by adding (BI) and mixing.
- the temperature at the time of mixing is preferably 50 ° C. or less, more preferably 30 ° C. or less, and further preferably 20 ° C. or less.
- the coating liquid (S) may contain other compounds (for example, polymer (F) (preferably excluding polyvinyl alcohol polymer)), and acetic acid, hydrochloric acid, nitric acid, trifluoro as necessary. It may contain at least one acid compound (Q) selected from the group consisting of acetic acid and trichloroacetic acid.
- the dispersion of the metal oxide (Aa) is prepared, for example, by mixing a compound (E), water, and an acid catalyst or an organic solvent as necessary in accordance with a method adopted in a known sol-gel method.
- E) can be prepared by condensation or hydrolysis condensation.
- a dispersion of the metal oxide (Aa) is obtained by condensing or hydrolytically condensing the compound (E)
- a specific treatment is applied to the obtained dispersion as necessary.
- the solvent to be used is not particularly limited, but alcohols such as methanol, ethanol and isopropanol; water; or a mixed solvent thereof is preferable.
- the solution containing the inorganic phosphorus compound (BI) can be prepared by dissolving the inorganic phosphorus compound (BI) in a solvent.
- the solvent may be appropriately selected according to the type of inorganic phosphorus compound (BI), but preferably contains water.
- the solvent may contain an organic solvent (for example, alcohols such as methanol) as long as it does not hinder the dissolution of the inorganic phosphorus compound (BI).
- the solid content concentration of the coating liquid (S) is preferably 1 to 20% by mass, more preferably 2 to 15% by mass, from the viewpoint of storage stability of the coating liquid and coating properties with respect to the substrate (X). More preferred is 10% by mass.
- the solid content concentration can be calculated, for example, by dividing the mass of the solid content remaining after the solvent of the coating liquid (S) is distilled off by the mass of the coating liquid (S) subjected to the treatment.
- the coating solution (S) has a viscosity measured with a Brookfield rotational viscometer (SB type viscometer: rotor No. 3, rotation speed 60 rpm) of 3,000 mPa ⁇ s or less at the coating temperature. Is preferably 2,500 mPa ⁇ s or less, and more preferably 2,000 mPa ⁇ s or less. When the viscosity is 3,000 mPa ⁇ s or less, the leveling property of the coating liquid (S) is improved, and a multilayer structure having a better appearance can be obtained. Further, the viscosity of the coating liquid (S) is preferably 50 mPa ⁇ s or more, more preferably 100 mPa ⁇ s or more, and further preferably 200 mPa ⁇ s or more.
- the molar ratio of aluminum atoms to phosphorus atoms can be calculated by performing a fluorescent X-ray analysis of the dried solid of the coating liquid (S).
- the coating liquid (S) may be applied directly on at least one surface of the substrate (X), or may be applied on the substrate (X) through another layer (J). Good. Further, before coating the coating liquid (S), the surface of the substrate (X) is treated with a known anchor coating agent, or a known adhesive is applied to the surface of the substrate (X). As a result, the adhesive layer (G) may be formed on the surface of the substrate (X).
- Coating of the coating liquid (S) is not particularly limited, and a known method can be adopted. Coating methods include, for example, casting method, dipping method, roll coating method, gravure coating method, screen printing method, reverse coating method, spray coating method, kiss coating method, die coating method, metalling bar coating method, chamber doctor combined coating Method, curtain coating method, bar coating method and the like.
- the precursor layer of the layer (Y) is formed by removing the solvent in the coating liquid (S).
- a well-known drying method is applicable. Examples of the drying method include a hot air drying method, a hot roll contact method, an infrared heating method, and a microwave heating method. It is important that the solvent content after drying and the average particle size of the reaction product (D) precursor are in a specific range because the resulting multilayer structure has excellent gas barrier properties even after dump heat treatment. .
- the solvent content of the precursor layer of the layer (Y) after the drying treatment is 0.4 wt% or less, and 0.3 wt% or less is preferable from the viewpoint of excellent barrier performance even under more severe dump heat treatment conditions. .
- the solvent content after the drying treatment is larger than the above range, the particle size of the reaction product (D) precursor tends to increase in the subsequent heat treatment step (II), and therefore the reaction product ( In some cases, the average particle diameter of D) becomes large and sufficient barrier performance cannot be obtained.
- the method for measuring the solvent content the method for measuring the content of methanol and water in Examples described later can be used.
- the average particle size of the reaction product (D) precursor after the drying treatment is less than 5 nm, and is preferably less than 4 nm, more preferably less than 3 nm in view of excellent barrier performance even under more severe dump heat treatment conditions. . If the average particle size of the reaction product (D) precursor after the drying treatment is larger than the above range, the average particle size of the reaction product (D) in the resulting layer (Y) becomes large, and sufficient barrier performance is obtained. It may not be possible. Although the minimum of the average particle diameter of a reaction product (D) precursor is not specifically limited, For example, 0.1 nm may be sufficient and 1 nm may be sufficient. In addition, the measuring method of the average particle diameter of a reaction product (D) precursor is as having described in the Example mentioned later.
- the ratio A R / A P can be thought of as an index representing the reaction of the metal oxide containing aluminum reaction product of (Aa) to (D).
- the reaction of the metal oxide (Aa) to the reaction product (D) is suppressed to a certain amount or less, thereby having good barrier performance. It is considered effective for obtaining a multilayer structure. Therefore, when the ratio A R / AP is larger than the above range, the barrier performance of the resulting multilayer structure may be insufficient.
- the drying temperature after coating of the coating liquid (S) is preferably less than 140 ° C., for example, 60 ° C. or more and 140 ° C. Is preferably less than 70 ° C., more preferably less than 130 ° C., and even more preferably less than 80 ° C. and less than 120 ° C.
- drying time is not specifically limited, For example, 1 second or more and less than 1 hour are preferable, 5 seconds or more and less than 15 minutes are more preferable, and 5 seconds or more and less than 300 seconds are more preferable. In particular, when the drying temperature is 100 ° C.
- the drying time is preferably 1 second to less than 4 minutes, more preferably 5 seconds to less than 4 minutes, and further preferably 5 seconds to less than 3 minutes. preferable.
- the drying temperature is lower than 100 ° C. (eg, 60 to 99 ° C.)
- the drying time is preferably 3 minutes or more and less than 1 hour, more preferably 6 minutes or more and less than 30 minutes, and further preferably 8 minutes or more and less than 25 minutes.
- the layer (Y) is formed by heat-treating the precursor layer of the layer (Y) formed in the step (I) at a temperature of 140 ° C. or higher.
- the heat treatment temperature in step (II) is preferably higher than the drying temperature in step (I).
- a reaction for generating a reaction product (D) proceeds.
- the temperature of the heat treatment is 140 ° C. or higher, preferably 170 ° C. or higher, more preferably 180 ° C. or higher, and further preferably 190 ° C. or higher. If the heat treatment temperature is low, it takes a long time to obtain a sufficient reaction rate, which causes a decrease in productivity.
- the temperature of the heat treatment is not particularly limited because it varies depending on the type of the base material (X), but may be 270 ° C. or less. For example, when a thermoplastic resin film made of a polyamide-based resin is used as the base material (X), the heat treatment temperature is preferably 270 ° C. or lower.
- the temperature of heat processing is 240 degrees C or less.
- the heat treatment may be performed in an air atmosphere, a nitrogen atmosphere, an argon atmosphere, or the like.
- the heat treatment time is preferably 1 second to 1 hour, more preferably 1 second to 15 minutes, and further preferably 5 to 300 seconds.
- the heat treatment is preferably performed in two or more stages by changing the treatment temperature. That is, the step (II) preferably includes a first heat treatment step (II-1) and a second heat treatment step (II-2).
- the temperature of the second stage heat treatment (hereinafter referred to as the second heat treatment) is preferably higher than the temperature of the first stage heat treatment (hereinafter referred to as the first heat treatment). It is more preferably higher by 15 ° C., more preferably higher by 25 ° C., and particularly preferably higher by 35 ° C.
- the heat treatment temperature in step (II) (first heat treatment temperature in the case of two or more heat treatments) is 30 ° C. higher than the drying temperature in step (I) because a multilayer structure having good characteristics can be obtained. It is preferably higher, more preferably 50 ° C. or higher, more preferably 55 ° C. or higher, particularly preferably 60 ° C. or higher.
- the temperature of the second heat treatment is higher than the temperature of the first heat treatment, the temperature of the first heat treatment is 140 ° C. or more and less than 200 ° C., and the temperature of the second heat treatment is It is preferable that it is 180 degreeC or more and 270 degrees C or less, the temperature of 2nd heat processing is 15 degreeC or more higher than the temperature of 1st heat processing, the temperature of 1st heat processing is 140 degreeC or more and less than 200 degreeC, and the temperature of 2nd heat processing Is more preferably 180 ° C. or more and 270 ° C. or less, the temperature of the second heat treatment is 25 ° C.
- the temperature of the first heat treatment is 140 ° C. or more and less than 200 ° C. More preferably, the temperature is 180 ° C. or higher and 270 ° C. or lower.
- each heat treatment time is preferably from 0.1 second to 10 minutes, more preferably from 0.5 second to 15 minutes, and further preferably from 1 second to 3 minutes.
- each heat treatment time is preferably 1 second to 15 minutes, more preferably 5 seconds to 10 minutes, and further preferably 10 seconds to 5 minutes.
- Step (I ′) In the case where an organic phosphorus compound (BO) is used in the production method, as the step (I ′), a coating liquid (T) (second coating liquid) obtained by mixing the organic phosphorus compound (BO) and a solvent is used as a step ( It may be coated on the layer (Y) obtained in II). In the step (I ′), the coating liquid (T) (second coating liquid) obtained by mixing the organic phosphorus compound (BO) and the solvent is used after the first heat treatment step (II-1) in the step (II). After coating on the layer (Y), it is preferable to use the second heat treatment step (II-2) in the step (II).
- the solvent used in the coating liquid (T) may be appropriately selected according to the type of the organic phosphorus compound (BO), but may be alcohols such as methanol, ethanol, isopropanol, water, or a mixed solvent thereof. preferable.
- the solvent is an ether such as tetrahydrofuran, dioxane, trioxane, dimethoxyethane; a ketone such as acetone or methyl ethyl ketone; a glycol such as ethylene glycol or propylene glycol; a methyl cellosolve or an ethyl cellosolve.
- Glycol derivatives such as n-butyl cellosolve; glycerin; acetonitrile; amides such as dimethylformamide; dimethyl sulfoxide; sulfolane and the like.
- the concentration of the solid content in the coating liquid (T) is preferably from 0.01 to 60% by mass, more preferably from 0.1 to 50% by mass, and from 0.2 to 0.2% from the viewpoint of storage stability or coating property of the solution. More preferred is 40% by mass.
- the solid content concentration can be determined by a method similar to the method described for the coating liquid (S).
- coating liquid (T) may also contain the other component (for example, polymer (F)) contained in the layer (Y) mentioned above.
- the method for applying the coating liquid (T) is not particularly limited, and a known method can be employed.
- the solvent is removed.
- the method for removing the solvent of the coating liquid (T) is not particularly limited, and a known drying method can be applied.
- the drying method include a hot air drying method, a hot roll contact method, an infrared heating method, and a microwave heating method. It is preferable that a drying temperature is below the flow start temperature of a base material (X).
- the drying temperature after coating of the coating liquid (T) may be, for example, about 90 to 240 ° C., and preferably 100 to 200 ° C.
- Step (II) can use the same heating equipment that is continuous with step (I) or whose heating temperature can be changed stepwise. Furthermore, step (II) can precede step (I ').
- a drying treatment is performed to form a precursor layer of the layer (Y), Further, the heat treatment of step (II) is performed.
- the temperature of the heat treatment is preferably 30 ° C. or more higher than the temperature of the drying treatment, and more preferably 50 ° C. or more.
- the coating liquid (S) of the step (I) is applied and dried.
- the first heat treatment step (II-1) of step (II) is performed.
- the coating liquid (T) in the step (I ′) is applied and dried, and then the second heat treatment step (II-2) in the step (II) is further performed.
- the temperature of the first heat treatment is preferably 30 ° C. or more, more preferably 50 ° C. or more higher than the temperature of the drying treatment in step (I).
- the temperature of 2nd heat processing is higher than the temperature of 1st heat processing.
- the layer (Y) may be laminated so as to be in direct contact with the substrate (X), and the layer (Y) is bonded to another member (for example, an adhesive). It may be laminated on the substrate (X) via the layer (G) or another layer (J).
- extruded coat laminate In the multilayer structure (W), for example, after the layer (Y) is laminated on the substrate (X) directly or via the adhesive layer (G), another layer (J) is directly or directly adhered to the adhesive layer (G ) Through an extrusion coat laminating method, it can further have a layer formed by extrusion coat lamination.
- the extrusion coat laminating method There is no particular limitation on the extrusion coat laminating method that can be used in the present invention, and a known method may be used.
- a typical extrusion coat laminating method a laminated film is produced by sending a molten thermoplastic resin to a T-die and cooling the thermoplastic resin taken out from the flat slit of the T-die.
- extrusion coat laminating method examples include a single laminating method, a sandwich laminating method, and a tandem laminating method.
- laminate including the multilayer structure (W) of the present invention it is possible to maintain high barrier performance even after extrusion coating lamination and to reduce the decrease in light transmittance.
- the adhesion between the base material (X) and the layer (Y) may be improved by using the adhesive layer (G).
- the adhesive layer (G) may be made of an adhesive resin.
- the adhesive layer (G) composed of an adhesive resin is obtained by treating the surface of the substrate (X) with a known anchor coating agent or by applying a known adhesive to the surface of the substrate (X). Can be formed.
- the adhesive is preferably a two-component reactive polyurethane adhesive in which a polyisocyanate component and a polyol component are mixed and reacted.
- the adhesion may be further improved by adding a small amount of an additive such as a known silane coupling agent to the anchor coating agent or adhesive.
- silane coupling agent examples include, but are not limited to, a silane coupling agent having a reactive group such as an isocyanate group, an epoxy group, an amino group, a ureido group, or a mercapto group.
- a silane coupling agent having a reactive group such as an isocyanate group, an epoxy group, an amino group, a ureido group, or a mercapto group.
- the multilayer structure (W) may include other layers (J) in order to improve various properties (for example, heat sealability, barrier properties, and mechanical properties).
- the other layer (J) is further directly or It can be produced by bonding or forming via an adhesive layer (G).
- the other layer (J) include, but are not limited to, an ink layer; a thermoplastic resin layer such as a polyolefin layer and an ethylene-vinyl alcohol copolymer resin layer.
- the multilayer structure (W) may include an ink layer for printing a trade name or a pattern.
- Such a multilayer structure (W) is manufactured, for example, by directly forming the ink layer after laminating the layer (Y) directly on the base material (X) or via the adhesive layer (G). it can.
- the ink layer for example, a film obtained by drying a liquid in which a polyurethane resin containing a pigment (for example, titanium dioxide) in a solvent is dispersed may be used.
- a film obtained by drying a resist for forming an electronic circuit wiring may be used.
- Examples of the coating method of the ink layer on the layer (Y) include various coating methods such as a wire bar, a spin coater, and a die coater in addition to the gravure printing method.
- the thickness of the ink layer is preferably 0.5 to 10.0 ⁇ m, more preferably 1.0 to 4.0 ⁇ m.
- the multilayer structure (W) when the polymer (Fa) is contained in the layer (Y), an ether bond having a high affinity with the adhesive layer (G) or another layer (J) (for example, an ink layer) , Having at least one functional group selected from the group consisting of a carbonyl group, a hydroxyl group, and a carboxyl group, the adhesion between the layer (Y) and the other layer (J) is improved. For this reason, interlayer adhesive force can be maintained even after dump heat treatment, and it becomes possible to suppress appearance defects such as delamination.
- the polyolefin layer as the outermost surface layer of the multilayer structure of the present invention, heat sealability can be imparted to the multilayer structure or the mechanical properties of the multilayer structure can be improved.
- the polyolefin is preferably polypropylene or polyethylene from the viewpoint of improving heat sealability and mechanical properties.
- the polyester is preferably polyethylene terephthalate
- the polyamide is preferably nylon-6
- the hydroxyl group-containing polymer is preferably an ethylene-vinyl alcohol copolymer.
- the multilayer structure (W) may have a member (for example, an adhesive layer (G) or another layer (J)) other than the base material (X) and the layer (Y). In the example, description of other members is omitted. In addition, a plurality of specific examples may be laminated or combined.
- the multilayer structure (W) and the electronic device used as the protective sheet for the electronic device of the present invention preferably have a total light transmittance of 86.5% or more from the viewpoint of application to a display, a solar cell, etc. More preferably, it is 0.0% or more.
- the multilayer structure (W) and the electronic device preferably have a haze of 3.0 or less.
- the light transmittance and haze measurement methods and measurement conditions are as described in the examples described later.
- the oxygen permeability under the conditions of 20 ° C. and 85% RH before and after the dump heat treatment is 0.7 mL / (m 2 ⁇ day ⁇ atm) or less, preferably 0.5 mL / (m 2 ⁇ day ⁇ atm) or less, more preferably 0.3 mL / (m 2 ⁇ day ⁇ atm) or less, 0.1 mL / ( m 2 ⁇ day ⁇ atm) or less is more preferable.
- An electronic device containing a quantum dot phosphor can be provided.
- the conditions for the dump heat treatment, the method for measuring the oxygen permeability, and the measurement conditions are as described in the examples described later.
- the moisture permeability under the conditions of 40 ° C. and 90% RH is 1.0 g / (m 2 ⁇ day) or less before and after the dump heat test. It is preferably 0.5 g / (m 2 ⁇ day) or less, more preferably 0.3 g / (m 2 ⁇ day) or less, and 0.2 g / (m 2 ⁇ day) or less. Some are more preferred.
- the quantum efficiency of the quantum dot phosphor is prevented from lowering during actual use, and the quantum has a high performance retention even during long-term use in the atmosphere.
- An electronic device containing a dot phosphor can be provided.
- the conditions for the dump heat test, the method for measuring moisture permeability, and the measurement conditions are as described in the examples described later.
- the multilayer structure was cut using the focused ion beam (FIB), and the slice for cross-sectional observation was produced.
- the prepared section was fixed to the sample base with carbon tape, and platinum ion sputtering was performed at an acceleration voltage of 30 kV for 30 seconds.
- the cross section of the multilayer structure was observed using a field emission type transmission electron microscope, and the thickness of each layer was calculated.
- the measurement conditions were as follows. Apparatus: JEM-2100F manufactured by JEOL Ltd. Accelerating voltage: 200kV Magnification: 250,000 times
- Measurement of average particle diameter Measurement is performed using an ultra-high resolution field emission scanning electron microscope, a photograph of particles of the reaction product (D) is taken, and particles observed in the unit field of view (100 The average particle size was calculated using image analysis type particle size distribution measurement software (Mac-View Ver. 4 manufactured by Mountec Co., Ltd.). At this time, the particle diameter of the particles is obtained as an arithmetic average value of the longest length and the shortest length of the particles, and the average primary particle diameter is calculated from the number of particles and the particle diameter.
- the measurement conditions were as follows. Apparatus: SU8010 manufactured by Hitachi High-Technologies Corporation Acceleration voltage: 0.5 kV Magnification: 100,000 times
- a dispersion was obtained by adding 54.29 parts by mass of distilled water and 18.80 parts by mass of methanol to 22.50 parts by mass of the solution thus obtained and stirring the mixture uniformly. Subsequently, 4.41 parts by mass of an 85% by mass phosphoric acid aqueous solution was added dropwise while stirring the dispersion while maintaining the liquid temperature at 15 ° C., and the viscosity was maintained at 15 ° C. until the viscosity reached 1,500 mPa ⁇ s. Stirring was continued to obtain the desired coating solution (S-1).
- PVA124 polyvinyl alcohol
- Example 1-1 “Lumirror (registered trademark) P60” (thickness: 12 ⁇ m) manufactured by Toray Industries, Inc., which is a stretched polyethylene terephthalate film, is prepared as the base material (X) (hereinafter sometimes abbreviated as “X-1”). did. On this substrate, the coating liquid (S-1) was applied using a bar coater so that the thickness after drying was 0.30 ⁇ m. The coated film was dried at 80 ° C. for 10 minutes to form a layer (Y-1) precursor on the substrate. In this way, a structure having a structure of base material (X-1) / layer (Y-1) precursor was obtained.
- the infrared absorption spectrum of the layer (Y) precursor of the obtained structure, the average particle diameter of the reaction product (D) precursor, and the solvent (total amount of methanol and moisture) content were measured by the above methods. Subsequently, a heat treatment was performed at 180 ° C. for 3 minutes, and then a heat treatment was performed at 220 ° C. for 10 seconds to form a layer (Y-1). In this way, a multilayer structure (W1-1) having a structure of base material (X-1) / layer (Y-1) was obtained.
- Average particle size of reaction product (D) precursor, solvent content and A R / A P in layer (Y-1) precursor, and average particle size of reaction product (D) in layer (Y-1) Is shown in Table 1. Further, an SEM photograph of the layer (Y-1) precursor of the multilayer structure (W1-1) is shown in FIG. 8, and an SEM photograph of the layer (Y-1) is shown in FIG. The results are shown in FIG.
- An adhesive layer is formed on the obtained multilayer structure (W1-1), and an acrylic resin film (thickness 50 ⁇ m, “Technoloy” (registered trademark) manufactured by Sumitomo Chemical Co., Ltd.) is laminated on the adhesive layer. To obtain a laminate. Subsequently, an adhesive layer was formed on the multilayer structure (W1-1) of the laminate, and then laminated with a polyethylene terephthalate film. In this way, a protective sheet (1-1) having a configuration of polyethylene terephthalate film / adhesive layer / base material (X-1) / layer (Y-1) / adhesive layer / acrylic resin film was obtained.
- Each of the two adhesive layers was formed by applying a two-component adhesive so that the thickness after drying was 3 ⁇ m and drying.
- the two-component adhesive consists of “Takelac” (registered trademark) “A-1102” manufactured by Mitsui Chemicals, Inc. and “Takenate” (registered trademark) “A-3070” manufactured by Mitsui Chemicals, Inc.
- a two-component reactive polyurethane adhesive was used.
- the obtained protective sheet (1-1) was measured for oxygen permeability, moisture permeability, total light transmittance, and haze. The results are shown in Table 1.
- Example 1-2 Except that the drying condition after coating of the coating liquid (S-1) was changed from 80 ° C. for 10 minutes to 120 ° C. for 3 minutes, it was the same as the production of the multilayer structure (W1-1) of Example 1-1.
- Example 1-3 The drying condition after coating of the coating liquid (S-1) was changed from 80 ° C. for 10 minutes to 120 ° C. for 1 minute, and the thickness of the layer (Y) after drying was changed from 0.30 ⁇ m to 0.45 ⁇ m.
- the multilayer structure (W3-1) having the structure of base material (X-1) / layer (Y-3) is the same as the production of the multilayer structure (W1-1) of Example 1-1 except that Was made. Further, except that the multilayer structure (W1-1) was changed to the multilayer structure (W3-1), the same as in the production of the protection sheet (1-1) of Example 1-1, the protection sheet (3- 1) was produced.
- a multilayer structure (W4-1) having a structure of base material (X-1) / layer (Y-4) was produced in the same manner as in the production of the above. Further, except that the multilayer structure (W1-1) was changed to the multilayer structure (W4-1), the protective sheet (4- 1) was produced.
- Examples 1-5 and 1-6 A multilayer structure was produced in the same manner as in the production of the multilayer structure (W4-1) of Example 1-4 except that the coating liquid (T-1) was changed to the coating liquids (T-2) and (T-3). (W5-1) and (W6-1) were produced. Further, except that the multilayer structure (W1-1) was changed to the multilayer structures (W5-1) and (W6-1), in the same manner as in the production of the protective sheet (1-1) of Example 1-1, Protection sheets (5-1) and (6-1) were produced.
- Example 1-1 Except that the drying condition after coating of the coating liquid (S-1) was changed from 80 ° C. for 10 minutes to 160 ° C. for 1 minute, it was the same as the production of the multilayer structure (W1-1) of Example 1-1. A multilayer structure (CW1-1) having a structure of base material (X-1) / layer (CY-1) was produced. Further, the protective sheet (C1-1-1) was prepared in the same manner as in the production of the protective sheet (1-1) of Example 1-1 except that the multilayer structure (W1-1) was changed to the multilayer structure (CW1-1). 1) was produced.
- Example 1-2 Except that the drying condition after coating of the coating liquid (S-1) was changed from 80 ° C. for 10 minutes to 80 ° C. for 1 minute, it was the same as the production of the multilayer structure (W1-1) of Example 1-1.
- the quantum efficiency and spectral radiant energy were measured by a quantum efficiency measuring device QE-1000 manufactured by Otsuka Electronics.
- the spectral radiant energy is radiant energy at the fluorescence wavelength of the quantum dot phosphor used in this example.
- the molecular structure of the quantum dot phosphor is a nanoparticle having a core / shell structure, a core of InP, a shell of ZnS, and myristic acid as a capping agent, and having a core diameter of 2.1 nm. A thing was used. Thereafter, the dispersion was sufficiently mixed using a rotation / revolution stirrer ARV310-LED manufactured by Sinky Co., Ltd.
- the dispersion was poured into a silicone ring (outer diameter 55 mm ⁇ inner diameter 50 mm ⁇ thickness 1 mm) placed on a petri dish made of polymethylpentene. After air-drying in an argon gas atmosphere as it is to obtain a plate-shaped molded product, the solvent is completely removed by drying at 40 ° C. for 5 hours in an inert oven in which nitrogen gas is circulated, and quantum dot fluorescence A body-dispersed resin molded body was obtained.
- the protective sheet (1-1) of Example 1-1 was bonded to the surface of the quantum dot phosphor-dispersed resin molded body using an adhesive resin, and the gas barrier A layer was formed to obtain a structure (u1) containing a quantum dot phosphor.
- the thickness of the gas barrier layer was 12.5 ⁇ m.
- the quantum efficiency of the structure (u1) containing this quantum dot phosphor was measured by using a quantum efficiency measuring device QE-1000 manufactured by Otsuka Electronics Co., Ltd. and found to be 74%. This value is inferior to the quantum efficiency of 80%, which is obtained when the same measurement is performed with the original quantum dot phosphor toluene dispersion.
- the structure (u1) containing the quantum dot phosphor was placed on a blue LED package of 22 mW and 450 nm and continuously emitted for 2,000 hours in the atmosphere.
- the spectral radiant energy of the quantum dot phosphor at the initial light emission of the LED was 0.42 (mW / nm), whereas the spectral radiant energy after 2,000 hours elapsed was 0.41 (mW / nm). It was. Therefore, the spectral radiant energy after 2,000 hours had kept a high value of 97.6% with respect to the initial value.
- Example 2-2 Resin film containing a quantum dot phosphor having a thickness of 100 ⁇ m, processed at a press pressure of 20 MPa using a press machine heated to 180 ° C. with the quantum dot phosphor dispersed resin molding obtained in Example 2-1 Got.
- the protective sheet (1-1) of Example 1-1 is bonded to the surface of the resin film containing the quantum dot phosphor using an adhesive resin, and a gas barrier is formed. A layer was formed to obtain a structure (u2) containing a quantum dot phosphor. The thickness of the gas barrier layer was 12.5 ⁇ m.
- the quantum efficiency, the spectral radiant energy in the early stage of light emission, and the spectral radiant energy after 2,000 hours were measured in the same manner as in Example 2-1.
- the results are shown in Table 2.
- the quantum efficiency was as good as 76%, and the spectral radiant energy after 2,000 hours had maintained a high value of 97.4% with respect to the initial value.
- Example 2 In order to protect the quantum dot phosphor from the atmosphere, the same as Example 2-1 except that the protective sheet (C1-1) of Comparative Example 1-1 was used on the surface of the quantum dot phosphor-dispersed resin molded body.
- the structure (u3) containing a quantum dot fluorescent substance was obtained by the method of.
- the quantum efficiency of the structure (u3) containing the quantum dot phosphor was measured by using a quantum efficiency measuring device QE-1000 manufactured by Otsuka Electronics Co., Ltd. and found to be 76%. This value is inferior to the quantum efficiency of 82% obtained when the same measurement is performed with the original quantum dot phosphor toluene dispersion.
- a structure (u3) containing a quantum dot phosphor was placed on a blue LED package of 22 mW and 450 nm, and light was emitted continuously for 2,000 hours in the atmosphere.
- Table 2 shows the results of measuring the spectral radiant energy at the initial stage of light emission and the spectral radiant energy after 2,000 hours had elapsed. The spectral radiant energy after 2,000 hours had decreased to 78.5% with respect to the initial value.
- the quantum efficiency of the structure (u4) containing the quantum dot phosphor was measured by using a quantum efficiency measuring device QE-1000 manufactured by Otsuka Electronics Co., Ltd. and found to be 76%. This value is inferior to the quantum efficiency of 82% obtained when the same measurement is performed with the original quantum dot phosphor toluene dispersion.
- a structure (u4) containing a quantum dot phosphor was placed on a blue LED package of 22 mW and 450 nm, and light was emitted continuously for 2,000 hours in the atmosphere.
- Table 2 shows the results of measuring the spectral radiant energy at the initial stage of light emission and the spectral radiant energy after 2,000 hours had elapsed. After 2000 hours, the spectral radiant energy decreased to 71.4% of the initial value.
- an electronic device including a quantum dot phosphor using a protective sheet that is excellent in gas barrier property and water vapor barrier property both before and after the dump heat test and also excellent in optical properties. Therefore, according to the present invention, in addition to the manufacturing stage and the distribution stage, an electronic device that can maintain high characteristics can be obtained even in a use stage that often takes a long time. Furthermore, according to the present invention, a quantum dot phosphor containing a high performance retention even when long-term use in the atmosphere (for example, continuous light emission for 2,000 hours) is suppressed. An electronic device can be provided.
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Abstract
Description
前記電子デバイスが保護シートを備え、
前記保護シートは、基材(X)と前記基材(X)上に積層された層(Y)とを含む多層構造体(W)を含み、
前記層(Y)がアルミニウムを含む化合物(A)とリン化合物(B)との反応生成物(D)を含み、
前記反応生成物(D)の平均粒子径が5~50nmの範囲内である、
量子ドット蛍光体を含む電子デバイスを提供する。
アルミニウムを含む化合物(A)、リン化合物(B)、および溶媒を含むコーティング液(S)を前記基材(X)上に塗工して、反応生成物(D)前駆体を含む層(Y)前駆体を形成する工程(I)と、 前記層(Y)前駆体を140℃以上の温度で熱処理することで前記層(Y)を形成する工程(II)とを含み、
前記工程(I)における層(Y)の前駆体層の溶媒含有率が0.4wt%以下であり、かつ、反応生成物(D)前駆体の平均粒子径が5nm未満である、
前記量子ドット蛍光体を含む電子デバイスの製造方法を提供する。
本発明の多層構造体(W)を用いた量子ドット蛍光体を含む電子デバイスは、電子デバイス本体と、電子デバイス本体の表面を被覆する保護シートを備える。本発明の電子デバイスに用いる保護シートは、基材(X)と、基材(X)上に積層された層(Y)とを含む多層構造体(W)を備える。多層構造体(W)の詳細については後述する。保護シートは、多層構造体(W)のみによって構成されていてもよいし、他の部材もしくは他の層を含んでもよい。以下では、特に注釈がない限り、保護シートが多層構造体(W)を備える場合について説明する。
本発明の実施形態1にかかる量子ドット蛍光体を含む電子デバイスでは、量子ドット蛍光体分散樹脂成形体を使用する。量子ドット蛍光体分散樹脂成形体は、樹脂中に量子ドット蛍光体を分散させて分散液(組成物)を得て、該分散液を用いて成形することで得られる。成形方法は、特に限定されず、公知の方法を使用できる。分散用樹脂としては、シクロオレフィン(共)重合体が好ましい。シクロオレフィン(共)重合体としては、例えば、下記式[Q-1]で表されるシクロオレフィン重合体(COP)または下記式[Q-2]で表されるシクロオレフィン共重合体(COC)が挙げられる。このようなシクロオレフィン(共)重合体として、市販品を使用できる。市販品としては、例えば、COPタイプとして、ZEONEX(登録商標)シリーズ(日本ゼオン株式会社製)、COCタイプとして、APL5014DP(三井化学株式会社製、化学構造;―(C2H4)x(C12H16)y―;添字x、yは0より大きく1より小さい実数であり、共重合比を表す)等が挙げられる。
式[Q-2]中、R3は、水素原子;炭素数1~6の直鎖状もしくは分岐状の飽和炭化水素基(好適にはアルキル基);塩素もしくはフッ素のハロゲン原子;およびハロゲン原子が塩素原子もしくはフッ素原子であるトリハロメチル基からなる群から選ばれる一価基を表わす。R4、R5は、それぞれ独立に、同一または異なって、水素原子;炭素数1~6の直鎖状もしくは分岐状の飽和の炭化水素基(好適にはアルキル基);塩素もしくはフッ素のハロゲン原子;およびハロゲン原子が塩素原子もしくはフッ素原子であるトリハロメチル基からなる群から選ばれる一価基を表わす。また、R4またはR5の炭化水素基は、隣り合う置換部位で互いに結合して5~7員環の飽和炭化水素の環状構造を少なくとも1つ形成してもよい。x、yは0より大きく1より小さい実数であり、x+y=1の関係式を満たす。
無機蛍光体としては、例えば、II族-VI族化合物半導体のナノ結晶、III族-V族化合物半導体のナノ結晶等が挙げられる。これらのナノ結晶の形態は特に限定されず、例えば、InPナノ結晶のコア部分に、ZnS/ZnO等からなるシェル部分が被覆されたコア・シェル(core-shell)構造を有する結晶、またはコア・シェルの境が明確でなくグラジエント(gradient)に組成が変化する構造を有する結晶、あるいは同一の結晶内に2種以上の化合物結晶が部分的に分けられて存在する混合結晶または2種以上のナノ結晶化合物の合金等が挙げられる。
次に、無機蛍光体の表面に配位するキャッピング剤(有機不動態層を形成するための試剤)としては、炭素数2~30、好ましくは炭素数4~20、より好ましくは炭素数6~18の直鎖構造または分岐構造を有する脂肪族炭化水素基を有する有機分子が挙げられる。無機蛍光体の表面に配位するキャッピング剤(有機不動態層を形成するための試剤)は、無機蛍光体に配位するための官能基を有する。このような官能基としては、例えば、カルボキシル基、アミノ基、アミド基、ニトリル基、水酸基、エーテル基、カルボニル基、スルフォニル基、ホスフォニル基またはメルカプト基等が挙げられる。これらの中でも、カルボキシル基が好ましい。
実施形態1で使用する量子ドット蛍光体は、所望の化合物半導体のナノ結晶が得られる金属前駆体を用いてナノ結晶を製造した後、次いで、これをさらに有機溶媒に分散する。そして、ナノ結晶を所定の反応性化合物(シェル部分の化合物)により処理することにより、無機蛍光体の表面に炭化水素基が配位した構造を有する量子ドット蛍光体を調製することができる。処理方法は、特に制限されず、例えば、ナノ結晶の分散液を反応性化合物の存在下に還流させる方法が挙げられる。また、量子ドット蛍光体の製造方法としては、例えば、特開2006-199963号公報に開示された方法を用いることができる。
図5には、実施形態2にかかる量子ドット蛍光体を含む構造物の一例の断面図が示される。図5において、量子ドット蛍光体を含む構造物は、量子ドット蛍光体18が分散用樹脂中に濃度0.01~20質量%の範囲で分散されている量子ドット蛍光体分散樹脂成形体22と、量子ドット蛍光体分散樹脂成形体22の全面を被覆し、量子ドット蛍光体分散樹脂成形体22への酸素等の透過を低減するガスバリア層(保護シート)24とを含んで構成されている。なお、他の実施形態において、ガスバリア層24は、量子ドット蛍光体分散樹脂成形体22の表面の一部を被覆する構成であってもよい(図6、7参照)。また、ガスバリア層24は、酸素の他、水蒸気の透過を低減できる点から、多層構造体(W)より構成されることが好ましい。
本発明の量子ドット蛍光体を含む電子デバイスに用いる多層構造体(W)は、基材(X)とアルミニウムを含む層(Y)とを含む。層(Y)は、アルミニウムを含む化合物(A)(以下、単に「化合物(A)」ともいう)とリン化合物(B)との反応生成物(D)を含む。
基材(X)の材質は、特に制限されず、様々な材質からなる基材を用いることができる。基材(X)の材質としては、例えば、熱可塑性樹脂、熱硬化性樹脂等の樹脂;木材;ガラス等が挙げられる。これらの中でも、熱可塑性樹脂が好ましい。基材(X)の形態は、特に制限されず、フィルムまたはシート等の層状であってもよい。基材(X)としては、熱可塑性樹脂フィルムを含むものが好ましく、熱可塑性樹脂フィルムであることがより好ましい。
層(Y)は、化合物(A)とリン化合物(B)との反応生成物(D)を含む。化合物(A)はアルミニウムを含有する化合物である。リン化合物(B)は、リン原子を含有する官能基を有する。リン化合物(B)は、無機リン化合物(BI)および/または有機リン化合物(BO)である。化合物(A)、リン化合物(B)について以下に説明する。
化合物(A)は、アルミニウムを含む金属酸化物(Aa)(以下、単に「金属酸化物(Aa)」ともいう)が好ましい。
アルミニウムを含む金属酸化物(Aa)は、通常、粒子の形態でリン化合物(B)(好ましくは、無機リン化合物(BI))と反応させる。
無機リン化合物(BI)との反応の制御が容易になり、得られる多層構造体のガスバリア性が優れることから、化合物(E)は、下記一般式〔I〕で表される化合物(Ea)を少なくとも1種含むことが好ましい。
Al(R1)k(R2)3-k 〔I〕
式中、R1は、ハロゲン原子(フッ素原子、塩素原子、臭素原子、ヨウ素原子)、NO3、置換基を有していてもよい炭素数1~9のアルコキシ基、置換基を有していてもよい炭素数2~9のアシロキシ基、置換基を有していてもよい炭素数3~9のアルケニルオキシ基、置換基を有していてもよい炭素数5~15のβ-ジケトナト基、または置換基を有していてもよい炭素数1~9のアシル基を有するジアシルメチル基である。R2は、置換基を有していてもよい炭素数1~9のアルキル基、置換基を有していてもよい炭素数7~10のアラルキル基、置換基を有していてもよい炭素数2~9のアルケニル基、または置換基を有していてもよい炭素数6~10のアリール基である。kは1~3の整数である。R1が複数存在する場合、R1は互いに同一であってもよいし異なっていてもよい。R2が複数存在する場合、R2は互いに同一であってもよいし異なっていてもよい。
M1(R3)m(R4)n-m 〔II〕
式中、M1は、アルミニウム以外の金属原子であって周期表の2~14族に属する金属原子から選ばれる少なくとも1種の金属原子である。R3は、ハロゲン原子(フッ素原子、塩素原子、臭素原子、ヨウ素原子)、NO3、置換基を有していてもよい炭素数1~9のアルコキシ基、置換基を有していてもよい炭素数2~9のアシロキシ基、置換基を有していてもよい炭素数3~9のアルケニルオキシ基、置換基を有していてもよい炭素数5~15のβ-ジケトナト基、または置換基を有していてもよい炭素数1~9のアシル基を有するジアシルメチル基である。R4は、置換基を有していてもよい炭素数1~9のアルキル基、置換基を有していてもよい炭素数7~10のアラルキル基、置換基を有していてもよい炭素数2~9のアルケニル基、または置換基を有していてもよい炭素数6~10のアリール基である。mは1~nの整数である。nはM1の原子価に等しい。R3が複数存在する場合、R3は互いに同一であってもよいし異なっていてもよい。R4が複数存在する場合、R4は互いに同一であってもよいし異なっていてもよい。
リン化合物(B)は、リン原子を含有する官能基を有する。リン化合物(B)は、無機リン化合物(BI)および/または有機リン化合物(BO)であり、無機リン化合物(BI)が好ましい。
無機リン化合物(BI)は、金属酸化物(Aa)と反応可能な部位を含有し、典型的には、そのような部位を複数含有する。無機リン化合物(BI)としては、そのような部位(原子団または官能基)を2~20個含有する化合物が好ましい。そのような部位の例には、金属酸化物(Aa)の表面に存在する官能基(例えば、水酸基)と縮合反応可能な部位が含まれる。そのような部位としては、例えば、リン原子に直接結合したハロゲン原子、リン原子に直接結合した酸素原子等が挙げられる。金属酸化物(Aa)の表面に存在する官能基(例えば、水酸基)は、通常、金属酸化物(Aa)を構成する金属原子(M)に結合している。
有機リン化合物(BO)が有するリン原子を含む官能基としては、例えば、リン酸基、亜リン酸基、ホスホン酸基、亜ホスホン酸基、ホスフィン酸基、亜ホスフィン酸基、およびこれらから誘導される官能基(例えば、塩、(部分)エステル化合物、ハロゲン化物(例えば、塩化物)、脱水物)等を挙げることができ、中でもリン酸基およびホスホン酸基が好ましく、ホスホン酸基がより好ましい。
反応生成物(D)は、アルミニウムを含む化合物(A)とリン化合物(B)との反応で得られる。アルミニウムを含む化合物(A)とリン化合物(B)とさらに他の化合物とが反応することで生成する化合物も反応生成物(D)に含まれる。反応生成物(D)としては、アルミニウムを含む金属酸化物(Aa)とリン化合物(B)とが反応してなる反応生成物(Da)、アルミニウムを含む化合物(A)と無機リン化合物(BI)とが反応してなる反応生成物(Db)、アルミニウムを含む金属酸化物(Aa)と無機リン化合物(BI)とが反応してなる反応生成物(Dc)が好ましく、アルミニウムを含む金属酸化物(Aa)と無機リン化合物(BI)とが反応してなる反応生成物(Dc)がより好ましい。
多層構造体(W)は、層(Z)をさらに含んでもよい。層(Z)は、リン原子を含む官能基を有する重合体(BOa)を含む。層(Z)は、層(Y)に隣接して配置されることが好ましい。すなわち、層(Z)と層(Y)は、互いに接触するように配置されることが好ましい。また、層(Z)は、層(Y)を挟んで基材(X)と反対側(好ましくは反対側の表面)に配置されることが好ましい。換言すれば、基材(X)/層(Y)/層(Z)の順に配置されることが好ましい。好ましい一例では、層(Z)が、層(Y)を挟んで基材(X)と反対側(好ましくは反対側の表面)に配置され、かつ、層(Y)に隣接して配置される。層(Z)は、カルボニル基、水酸基、カルボキシル基、カルボン酸無水物基、およびカルボキシル基の塩からなる群より選ばれる少なくとも1種の官能基を含有する重合体(F)をさらに含んでもよい。層(Z)における重合体(BOa)の種類、量等は、層(Y)のにおけるものと使用できる。
多層構造体(W)は、さらに無機蒸着層を含んでもよい。無機蒸着層は、無機物を蒸着することによって形成することができる。無機物としては、例えば、金属(例えば、アルミニウム)、金属酸化物(例えば、酸化ケイ素、酸化アルミニウム)、金属窒化物(例えば、窒化ケイ素)、金属窒化酸化物(例えば、酸窒化ケイ素)、または金属炭化窒化物(例えば、炭窒化ケイ素)等が挙げられる。これらの中でも、酸化アルミニウム、酸化ケイ素、酸化マグネシウム、または窒化ケイ素で形成される無機蒸着層は、酸素あるいは水蒸気に対するバリア性が優れる観点から好ましい。本発明の多層構造体(W)中の層(Y)は、アルミニウムを含有する無機蒸着層を含んでいてもよい。例えば、層(Y)は、アルミニウムの蒸着層(Ac)および/または酸化アルミニウムの蒸着層(Ad)を含んでいてもよい。
重合体(F)は、例えば、エーテル結合、カルボニル基、水酸基、カルボキシル基、カルボン酸無水物基、およびカルボキシル基の塩からなる群より選ばれる少なくとも1種の官能基を有する重合体(Fa)であってもよい。
多層構造体(W)について説明した事項は多層構造体(W)の製造方法に適用できるため、重複する説明を省略する場合がある。また、多層構造体(W)の製造方法について説明した事項は、多層構造体(W)に適用できる。
工程(I)では、アルミニウムを含む化合物(A)とリン化合物(B)と溶媒とを含むコーティング液(S)(第1コーティング液)を基材(X)上に塗工することによって基材(X)上に反応生成物(D)前駆体を含む層(Y)の前駆体層を形成する。コーティング液(S)は、アルミニウムを含む化合物(A)、リン化合物(B)および溶媒を混合することによって得られる。層(Y)が、アルミニウムの蒸着層(Ac)または酸化アルミニウムの蒸着層(Ad)を含む場合には、それらの層は上述した一般的な蒸着法によって形成できる。以下、好適な実施態様として、金属酸化物(Aa)、無機リン化合物(BI)、および溶媒を用いる態様を用いて説明する。
工程(II)では、工程(I)で形成された層(Y)の前駆体層を、140℃以上の温度で熱処理することによって層(Y)を形成する。本発明では、上述した特定の溶媒含有率および平均粒子径を有する層(Y)前駆体を140℃以上の温度で熱処理することが、より優れたバリア性能を得るために重要である。工程(II)の熱処理温度は、工程(I)の乾燥温度よりも高いことが好ましい。
前記製造方法において有機リン化合物(BO)を用いる場合、工程(I’)として、有機リン化合物(BO)および溶媒を混合することによって得たコーティング液(T)(第2コーティング液)を工程(II)で得た層(Y)上に塗工してもよい。工程(I’)では、有機リン化合物(BO)および溶媒を混合することによって得たコーティング液(T)(第2コーティング液)を工程(II)の第1熱処理工程(II-1)後の層(Y)上に塗工した後に続いて工程(II)の第2熱処理工程(II-2)に供することが好ましい。
多層構造体(W)は、例えば、基材(X)に直接または接着層(G)を介して層(Y)を積層させた後に、さらに他の層(J)を直接または接着層(G)を介して押出しコートラミネート法により形成することによって、押出しコートラミネートにより形成された層をさらに有することができる。本発明で用いることができる押出しコートラミネート法に特に限定はなく、公知の方法を用いてもよい。典型的な押出しコートラミネート法では、溶融した熱可塑性樹脂をTダイに送り、Tダイのフラットスリットから取り出した熱可塑性樹脂を冷却することによって、ラミネートフィルムが製造される。
多層構造体(W)において、接着層(G)を用いて、基材(X)と層(Y)との接着性を高めることができる場合がある。接着層(G)は、接着性樹脂から構成されていてもよい。接着性樹脂から構成される接着層(G)は、基材(X)の表面を公知のアンカーコーティング剤で処理するか、基材(X)の表面に公知の接着剤を塗工することによって形成できる。該接着剤としては、ポリイソシアネート成分とポリオール成分とを混合し反応させる2液反応型ポリウレタン系接着剤が好ましい。また、アンカーコーティング剤または接着剤に、公知のシランカップリング剤等の少量の添加剤を加えることによって、さらに接着性を高めることができる場合がある。シランカップリング剤としては、例えば、イソシアネート基、エポキシ基、アミノ基、ウレイド基、メルカプト基等の反応性基を有するシランカップリング剤が挙げられるが、これらに限定されるものではない。基材(X)と層(Y)とを接着層(G)を介して強く接着することによって、多層構造体(W)に対して印刷あるいはラミネート等の加工を施す際に、ガスバリア性または外観の悪化をより効果的に抑制することができる。接着層(G)の厚さは0.01~10.0μmが好ましく、0.03~5.0μmがより好ましい。
多層構造体(W)は、様々な特性(例えば、ヒートシール性、バリア性、力学物性)を向上させるために、他の層(J)を含んでもよい。このような多層構造体(W)は、例えば、基材(X)に直接または接着層(G)を介して層(Y)を積層させた後に、さらに該他の層(J)を直接または接着層(G)を介して接着または形成することによって製造できる。他の層(J)としては、例えば、インク層;ポリオレフィン層、エチレン-ビニルアルコール共重合体樹脂層等の熱可塑性樹脂層等が挙げられるが、これらに限定されない。
多層構造体(W)の構成の具体例を以下に示す。多層構造体(W)は基材(X)、層(Y)以外の他の部材(例えば、接着層(G)、他の層(J))を有していてもよいが、以下の具体例において、他の部材の記載は省略している。また、以下具体例を複数層積層したり組み合わせたりしてもよい。
(1)層(Y)/ポリエステル層、
(2)層(Y)/ポリエステル層/層(Y)、
(3)層(Y)/ポリアミド層、
(4)層(Y)/ポリアミド層/層(Y)、
(5)層(Y)/ポリオレフィン層、
(6)層(Y)/ポリオレフィン層/層(Y)、
(7)層(Y)/水酸基含有ポリマー層、
(8)層(Y)/水酸基含有ポリマー層/層(Y)、
(9)層(Y)/無機蒸着層/ポリエステル層、
(10)層(Y)/無機蒸着層/ポリアミド層、
(11)層(Y)/無機蒸着層/ポリオレフィン層、
(12)層(Y)/無機蒸着層/水酸基含有ポリマー層
フーリエ変換赤外分光光度計を用い、減衰全反射法で測定した。測定条件は以下の通りとした。
装置:パーキンエルマー株式会社製Spectrum One
測定モード:減衰全反射法
測定領域:800~1,400cm-1
収束イオンビーム(FIB)を用いて多層構造体を切削し、断面観察用の切片を作製した。作製した切片を試料台座にカーボンテープで固定し、加速電圧30kVで30秒間白金イオンスパッタを行った。電界放出形透過型電子顕微鏡を用いて多層構造体の断面を観察し、各層の厚さを算出した。測定条件は以下の通りとした。
装置:日本電子株式会社製JEM-2100F
加速電圧:200kV
倍率:250,000倍
超高分解能電界放出形走査電子顕微鏡を用いて測定を行い、反応生成物(D)の粒子の写真を撮り、その写真の単位視野内に観察される粒子(100個以上)の平均粒子径を、画像解析式粒度分布測定ソフトウェア(株式会社マウンテック製Mac-View Ver.4)を用いて算出した。このとき、粒子の粒子径は、粒子の最長の長さと最短の長さの算術平均値として求められ、粒子の数とその粒子径より、平均一次粒子径が算出される。測定条件は以下の通りとした。
装置:株式会社日立ハイテクノロジーズ製SU8010
加速電圧:0.5kV
倍率:100,000倍
コーティング液(S-1)の塗工、乾燥後の多層構造体を短冊状に切り、ヘッドスペースGC-MSを測定した結果、水のみが検出されメタノールは検出されなかった(検出下限5ppm)。測定条件は以下の通りとした。
装置:サーモフィッシャーサイエンティフィック株式会社製COMBI PAL PolarisQ TraceGC
ヘッドスペース温度:100℃
カラム温度:40℃で5分間保持した後、5℃/分で140℃まで昇温して10分間保持
キャリアガス:ヘリウム
キャリアガス流量:1.0mL/分
コーティング液(S-1)の塗工、乾燥後の多層構造体を短冊状に切り、カールフィッシャー水分率計にて含水率を測定した。同加熱条件(温度、時間)で処理した基材の水分率を同様に測定し、差し引くことによって層(Y)前駆体の水分率を求めた。測定条件は以下の通りとした。
装置:三菱化成株式会社製CA-06型
温度:100℃
キャリアガス:窒素
キャリアガス流量:0.2L/分
滴定法:電量滴定法
酸素透過量測定装置にキャリアガス側に基材の層が向くようにサンプルを取り付け、等圧法により酸素透過度を測定した。測定条件は以下の通りとした。
装置:モダンコントロールズ社製MOCON OX-TRAN2/20
温度:20℃
酸素供給側の湿度:85%RH
キャリアガス側の湿度:85%RH
酸素圧:1.0atm
キャリアガス圧力:1.0atm
水蒸気透過量測定装置にキャリアガス側に基材の層が向くようにサンプルを取り付け、等圧法により透湿度(水蒸気透過度)を測定した。測定条件は以下の通りとした。
装置:モダンコントロールズ社製MOCON PERMATRAN W3/33
温度:40℃
水蒸気供給側の湿度:90%RH
キャリアガス側の湿度:0%RH
全光線透過率およびヘイズの測定は、ヘイズメーターを用いて測定した。
装置:村上色彩技術研究所社製 HR-100
条件:ISO13468-1に準拠
蒸留水230質量部を撹拌しながら70℃に昇温した。その蒸留水に、トリイソプロポキシアルミニウム88質量部を1時間かけて滴下し、液温を徐々に95℃まで上昇させ、発生するイソプロパノールを留出させることによって加水分解縮合を行った。得られた液体に、60質量%の硝酸水溶液4.0質量部を添加し、95℃で3時間撹拌することによって加水分解縮合物の粒子の凝集体を解膠させた。その後、その液体を、固形分濃度が酸化アルミニウム換算で10質量%になるように濃縮し、溶液を得た。こうして得られた溶液22.50質量部に対して、蒸留水54.29質量部およびメタノール18.80質量部を加え、均一になるように撹拌することによって、分散液を得た。続いて、液温を15℃に維持した状態で分散液を攪拌しながら85質量%のリン酸水溶液4.41質量部を滴下して加え、粘度が1,500mPa・sになるまで15℃で攪拌を続け、目的のコーティング液(S-1)を得た。該コーティング液(S-1)における、アルミニウム原子とリン原子とのモル比は、アルミニウム原子:リン原子=1.15:1.00であった。
窒素雰囲気下、ビニルホスホン酸10gおよび2,2’-アゾビス(2-アミジノプロパン)2塩酸塩0.025gを水5gに溶解させ、80℃で3時間攪拌した。冷却後、重合溶液に水15gを加えて希釈し、セルロース膜であるスペクトラムラボラトリーズ社製の「Spectra/Por」(登録商標)を用いてろ過した。ろ液中の水を留去した後、50℃で24時間真空乾燥することによって、重合体(BO-1)を得た。重合体(BO-1)は、ポリ(ビニルホスホン酸)である。GPC分析の結果、該重合体の数平均分子量はポリエチレングリコール換算で10,000であった。
前記合成例で得た有機リン化合物(BO-1)を、水とメタノールの混合溶媒(質量比で水:メタノール=7:3)に溶解させ、固形分濃度が1質量%のコーティング液(T-1)を得た。
前記合成例で得た有機リン化合物(BO-1)を91質量%、重合体(F)として重量平均分子量100,000のポリビニルアルコール(株式会社クラレ製PVA124)を9質量%含む混合物を準備した。この混合物を、水とメタノールの混合溶媒(質量比で水:メタノール=7:3)に溶解させ、固形分濃度が1質量%のコーティング液(T-2)を得た。
前記合成例で得た有機リン化合物(BO-1)を91質量%、重合体(F)として重量平均分子量60,000のポリエチレンオキサイド(明成化学工業株式会社製「アルコックス(登録商標)L-6」)を9質量%含む混合物を準備した。この混合物を、水とメタノールの混合溶媒(質量比で水:メタノール=7:3)に溶解させ、固形分濃度が1質量%のコーティング液(T-3)を得た。
まず、基材(X)として、延伸ポリエチレンテレフタレートフィルムである東レ株式会社製の「ルミラー(登録商標) P60」(厚さ12μm)(以下、「X-1」と略称することがある)を準備した。この基材上に、乾燥後の厚さが0.30μmとなるようにバーコーターを用いてコーティング液(S-1)を塗工した。塗工後のフィルムを、80℃で10分間乾燥することによって、基材上に層(Y-1)の前駆体を形成した。このようにして、基材(X-1)/層(Y-1)前駆体という構造を有する構造体を得た。得られた構造体の層(Y)前駆体の赤外線吸収スペクトル、反応生成物(D)前駆体の平均粒子径、および溶媒(メタノールおよび水分の合計量)含有率を前記の方法で測定した。続いて、180℃で3分間熱処理した後、220℃で10秒間熱処理することによって層(Y-1)を形成した。このようにして、基材(X-1)/層(Y-1)という構造を有する多層構造体(W1-1)を得た。
コーティング液(S-1)の塗工後の乾燥条件を80℃10分間から120℃3分間に変更したこと以外は実施例1-1の多層構造体(W1-1)の作製と同様にして、基材(X-1)/層(Y-2)という構造を有する多層構造体(W2-1)を作製した。また、多層構造体(W1-1)を多層構造体(W2-1)に変更したこと以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(2-1)を作製した。
コーティング液(S-1)の塗工後の乾燥条件を80℃10分間から120℃1分間に変更したこと、および乾燥後の層(Y)の厚みを0.30μmから0.45μmに変更したこと以外は実施例1-1の多層構造体(W1-1)の作製と同様にして、基材(X-1)/層(Y-3)という構造を有する多層構造体(W3-1)を作製した。また、多層構造体(W1-1)を多層構造体(W3-1)に変更したこと以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(3-1)を作製した。
180℃3分間の熱処理後、無機リン化合物(BI)の質量WBIと有機リン化合物(BO)の質量WBOの比WBO/WBI=1.10/98.90となるようにバーコーターを用いてコーティング液(T-1)を塗工し、110℃で3分間乾燥させ、続いて、220℃で1分間熱処理すること以外は実施例1-1の多層構造体(W1-1)の作製と同様にして、基材(X-1)/層(Y-4)という構造を有する多層構造体(W4-1)を作製した。また、多層構造体(W1-1)を多層構造体(W4-1)に変更したこと以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(4-1)を作製した。
コーティング液(T-1)をコーティング液(T-2)および(T-3)に変更した以外は実施例1-4の多層構造体(W4-1)の作製と同様にして、多層構造体(W5-1)および(W6-1)を作製した。また、多層構造体(W1-1)を多層構造体(W5-1)および(W6-1)に変更した以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(5-1)および(6-1)を作製した。
コーティング液(S-1)の塗工後の乾燥条件を80℃10分間から160℃1分間に変更したこと以外は実施例1-1の多層構造体(W1-1)の作製と同様にして、基材(X-1)/層(CY-1)という構造を有する多層構造体(CW1-1)を作製した。また、多層構造体(W1-1)を多層構造体(CW1-1)に変更したこと以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(C1-1)を作製した。
コーティング液(S-1)の塗工後の乾燥条件を80℃10分間から80℃1分間に変更したこと以外は実施例1-1の多層構造体(W1-1)の作製と同様にして、基材(X-1)/層(CY-2)という構造を有する多層構造体(CW2-1)を作製した。また、多層構造体(W1-1)を多層構造体(CW2-1)に変更したこと以外は実施例1-1の保護シート(1-1)の作製と同様にして、保護シート(C2-1)を作製した。
<実施例2-1>
50mLガラス製スクリューボトルに、アルゴンガス雰囲気下、シクロオレフィンポリマー(日本ゼオン株式会社製、ZEONEX(登録商標)480R;構造式[Q-1]を含む非晶質樹脂)5gと、真空凍結脱気した後にアルゴンガス雰囲気下で保存した脱水トルエン(和光純薬工業株式会社製)5gとを仕込み、室温下ローラー式攪拌機上で撹拌することで溶解させ、樹脂溶液(r1)を得た。
実施例2-1で得た量子ドット蛍光体分散樹脂成形体を180℃に加熱したプレス機を用いて、20MPaのプレス圧で加工し、100μmの厚みを持った量子ドット蛍光体を含む樹脂フィルムを得た。
量子ドット蛍光体を大気から保護するために、前記量子ドット蛍光体分散樹脂成形体の表面に比較例1-1の保護シート(C1-1)を用いた以外は、実施例2-1と同様の方法で量子ドット蛍光体を含む構造物(u3)を得た。この量子ドット蛍光体を含む構造物(u3)の量子効率を大塚電子(株)製量子効率測定装置QE-1000を用いて測定したところ76%であった。この値は、元になった量子ドット蛍光体トルエン分散液で同様の測定をした場合に得られる量子効率82%と遜色のない結果である。
量子ドット蛍光体を大気から保護するために、前記量子ドット蛍光体分散樹脂成形体の表面にEVOHフィルム(日本合成製、ソアノールD2908を共押出法により作製した厚さ15μmのフィルム、酸素透過度0.5mL/(m2・day)、透湿度130g/m2・24hrs)を用いた以外は、実施例2-1と同様の方法で量子ドット蛍光体を含む構造物(u4)を得た。この量子ドット蛍光体を含む構造物(u4)の量子効率を大塚電子(株)製量子効率測定装置QE-1000を用いて測定したところ76%であった。この値は、元になった量子ドット蛍光体トルエン分散液で同様の測定をした場合に得られる量子効率82%と遜色のない結果である。
Claims (15)
- 量子ドット蛍光体を含む電子デバイスであって、
前記電子デバイスが保護シートを備え、
前記保護シートが、基材(X)と前記基材(X)に積層された層(Y)とを含む多層構造体(W)を含み、
前記層(Y)がアルミニウムを含む化合物(A)とリン化合物(B)との反応生成物(D)を含み、
前記反応生成物(D)の平均粒子径が5~50nmの範囲内である、電子デバイス。 - 量子ドット蛍光体を含む層の片側または両側に前記保護シートが配置された、請求項1に記載の電子デバイス。
- 前記リン化合物(B)が、無機リン化合物(BI)である、請求項1または2に記載の電子デバイス。
- 前記アルミニウムを含む化合物(A)が、アルミニウムを含む金属酸化物(Aa)である、請求項1~3のいずれか1項に記載の電子デバイス。
- 前記反応生成物(D)の平均粒子径が、20~40nmの範囲内にある、請求項1~4のいずれか1項に記載の電子デバイス。
- 40℃、90%RHの条件下における透湿度が1.0g/(m2・day)以下である、請求項1~5のいずれか1項に記載の電子デバイス。
- 前記基材(X)が、熱可塑性樹脂フィルムを含む、請求項1~6のいずれか1項に記載の電子デバイス。
- 前記層(Y)が、カルボニル基、水酸基、カルボキシル基、カルボン酸無水物基、およびカルボキシル基の塩からなる群より選ばれる少なくとも1種の官能基を含有する重合体(F)を含む、請求項1~7のいずれか1項に記載の電子デバイス。
- 前記多層構造体(W)が、前記層(Y)に隣接して配置された層(Z)をさらに含み、前記層(Z)は、リン原子を含有する官能基を有する重合体(BOa)を含む、請求項1~8のいずれか1項に記載の電子デバイス。
- 前記層(Z)の重合体(BOa)が、ポリ(ビニルホスホン酸)またはポリ(2-ホスホノオキシエチルメタクリレート)である、請求項9に記載の電子デバイス。
- 電子デバイスが保護シートを備え、
前記保護シートが、基材(X)と、前記基材(X)に積層された層(Y)とを含む多層構造体(W)を含み、
前記層(Y)はアルミニウムを含む化合物(A)とリン化合物(B)との反応生成物(D)を含み、
アルミニウムを含む化合物(A)、リン化合物(B)、および溶媒を含むコーティング液(S)を前記基材(X)上に塗工して、反応生成物(D)前駆体を含む層(Y)前駆体を形成する工程(I)と、 前記層(Y)前駆体を140℃以上の温度で熱処理することで前記層(Y)を形成する工程(II)とを含み、
前記工程(I)における層(Y)の前駆体層の溶媒含有率が0.4wt%以下であり、かつ、反応生成物(D)前駆体の平均粒子径が5nm未満である、
請求項1に記載の量子ドット蛍光体を含む電子デバイスの製造方法。 - 前記リン化合物(B)が、無機リン化合物(BI)である、請求項11に記載の製造方法。
- 前記アルミニウムを含む化合物(A)が、アルミニウムを含む金属酸化物(Aa)である、請求項11または12に記載の製造方法。
- 前記工程(I)において、コーティング液(S)を前記基材(X)上に塗工した後、前記コーティング液(S)中の溶媒を除去する乾燥工程とを有し、前記乾燥工程における乾燥温度が140℃未満である、請求項11~13のいずれか1項に記載の製造方法。
- 前記層(Y)前駆体の赤外線吸収スペクトルにおいて、1,080~1,130cm-1の範囲における吸光度の極大値ARと850~950cm-1の範囲における吸光度の極大値APとの比AR/APが2.0以下である、請求項11~14のいずれか1項に記載の製造方法。
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