WO2021095830A1 - 封止用シート - Google Patents
封止用シート Download PDFInfo
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- WO2021095830A1 WO2021095830A1 PCT/JP2020/042364 JP2020042364W WO2021095830A1 WO 2021095830 A1 WO2021095830 A1 WO 2021095830A1 JP 2020042364 W JP2020042364 W JP 2020042364W WO 2021095830 A1 WO2021095830 A1 WO 2021095830A1
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/26—Polymeric coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/28—Multiple coating on one surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/724—Permeability to gases, adsorption
- B32B2307/7242—Non-permeable
- B32B2307/7246—Water vapor barrier
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/726—Permeability to liquids, absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/748—Releasability
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
- H10K50/8445—Encapsulations multilayered coatings having a repetitive structure, e.g. having multiple organic-inorganic bilayers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to a sealing sheet useful for sealing an electronic device.
- Patent Document 1 proposes a sealing sheet having a first moisture-proof film, a resin composition layer, and a second moisture-proof film in order to suppress moisture absorption of the resin composition layer during storage. ..
- the present invention has been made by paying attention to the above circumstances, and an object of the present invention is to be able to efficiently dry the resin composition layer and prevent contamination of the resin composition layer during the drying.
- the purpose is to provide a sealing sheet.
- Water vapor permeability of the first sheet and third sheet are each independently, 5 (g / m 2 / 24hr) or less, Water vapor permeability of the second sheet, 10 (g / m 2 / 24hr) or more, and the sheet for sealing which can be peeled off the third sheet.
- the sealing sheet according to the above [1], wherein the 90-degree peel strength between the second sheet and the third sheet is 0.1 gf / inch or more and 250 gf / inch or less.
- the sealing sheet of the present invention can efficiently dry the resin composition layer, and can prevent the resin composition layer from being contaminated during the drying.
- the sealing sheet of the present invention is a sealing sheet having a laminated structure containing the first sheet, the resin composition layer, the second sheet, and the third sheet in this order.
- water vapor transmission rate of the first sheet and the third sheet are each independently a 5 (g / m 2 / 24hr ) or less That is, one of the features is that the first sheet and the third sheet are moisture-proof sheets. Further, the present invention is the water vapor permeability of the second sheet, 10 (g / m 2 / 24hr) or that it is, namely, the one wherein the second sheet is a non-moisture-proof sheet. Another feature of the present invention is that the third sheet can be peeled off.
- the third sheet which is a moisture-proof sheet
- the resin composition layer is protected by the second sheet, which is a non-moisture-proof sheet.
- the resin composition layer can be dried efficiently. After the resin composition layer is dried, the peeled third sheet or a new third sheet may be laminated on the second sheet.
- the structures of the first sheet, the second sheet, and the third sheet may be a single-layer structure or a laminated structure, preferably a laminated structure.
- the first sheet and the third sheet which are moisture-proof sheets, are both sheets having a laminated structure including a barrier layer and a base material, more preferably.
- the second sheet which is a non-moisture-proof sheet, may be a sheet composed of only a base material, or may be a sheet having a laminated structure including a release layer and a base material.
- WVTR of the first sheet and third sheet are each independently, preferably 4 (g / m 2 / 24hr ) or less.
- the lower limit of the WVTR of the first sheet and the third sheet is not particularly limited, and a lower value is preferable.
- WVTR of the first sheet and third sheet is most preferably are each ideally 0 (g / m 2 / 24hr ). WVTR is a value measured by the method described in Examples described later.
- the sealing sheet of the present invention is used for sealing an electronic device, and at that time, the first sheet is used as a highly moisture-proof layer in an electronic device without peeling off, the first sheet in the present invention.
- the, WVTR is preferably used moisture-proof sheet of less than 0.01 (g / m 2 / 24hr ).
- WVTR of the sheet is more preferably 0.005 (g / m 2 / 24hr ) or less, more preferably 0.001 (g / m 2 / 24hr ) or less, particularly preferably 0.0005 (g / m 2 / 24 hr) or less.
- the lower limit of WVTR of this sheet is not particularly limited, and a lower value is preferable.
- the WVTR is ideally 0 (g / m 2 / 24hr ) are most preferred.
- WVTR of the second sheet is preferably 15 (g / m 2 / 24hr ) or more.
- the upper limit is not particularly limited, WVTR of the second sheet is typically 20,000 (g / m 2 / 24hr ) or less, preferably 15,000 (g / m 2 / 24hr ) or less.
- an opaque moisture-proof sheet such as a sheet with metal leaf is used as both the first sheet and the third sheet, it becomes difficult to inspect the quality of the resin composition layer. Therefore, it is opaque as one of the first sheet and the third sheet.
- a moisture-proof sheet it is desirable to use a transparent moisture-proof sheet as the other. Regardless of the thickness of the transparent moisture-proof sheet, it is desirable that the total light transmittance with D65 light is 85% or more.
- An "opaque moisture-proof sheet” is defined as a "moisture-proof sheet having a total light transmittance of 50% or less with D65 light". The total light transmittance can be measured with D65 light using an air meter HZ-V3 (halogen lamp) manufactured by Suga Test Instruments Co., Ltd. as a reference.
- WVTR described above can 0.01 (g / m 2 / 24hr ) or 1 (g / m 2 / 24hr ) It is preferable to use the following moisture-proof sheet.
- WVTR is 0.01 (g / m 2 / 24hr ) less moisture-proof sheet, especially WVTR is 0.005 (g / m 2 / 24hr ) or less of moisture-proof sheet, for example, silicon oxide (silica to the substrate surface ), Aluminum oxide, magnesium oxide, silicon nitride, silicon nitride, SiCN, amorphous silicon, etc., by chemical vapor deposition (for example, heat, plasma, ultraviolet rays, vacuum heat, vacuum plasma, or chemical vapor deposition by vacuum ultraviolet rays).
- the moisture-proof sheet produced by such a method is a transparent sheet.
- a metal foil such as SUS foil or aluminum foil
- a moisture-proof sheet manufactured by a method such as laminating a base material and a metal foil with an adhesive.
- a metal leaf, or a moisture-proof sheet consisting of a substrate and a metal leaf, is usually opaque.
- the moisture-proof sheet is a method of depositing an inorganic film containing an inorganic substance such as silicon oxide (silica), aluminum oxide, magnesium oxide, silicon nitride, silicon nitride, SiCN, and amorphous silicon on the surface of the base material as a barrier layer, or It can be produced by a method of applying a coating liquid made of a metal oxide and an organic resin having a barrier property to a base material and drying the substrate (see, for example, JP2013-108103A, Patent No. 4028353, etc.). ..
- the moisture-proof sheet produced by such a method is a transparent sheet.
- a commercially available product may be used as the moisture-proof sheet.
- Examples of commercially available products include “Clarista CI” manufactured by Kuraray, “Tech Barrier HX”, “Tech Barrier LX” and “Tech Barrier L” manufactured by Mitsubishi Plastics, and “IB-PET-PXB” manufactured by Dai Nippon Printing Co., Ltd. , "GL, GX series” manufactured by Toppan Printing Co., Ltd., “PET Tsuki AL1N30” manufactured by Toyo Aluminum Co., Ltd., “X-BARRIER” manufactured by Mitsubishi Plastics, etc.
- the first sheet may be a sheet having no release layer. Further, the first sheet may be a sheet having a release layer, and the release layer may be in contact with the resin composition layer.
- the first sheet which is a sheet having a release layer, include a sheet having a laminated structure containing a barrier layer, a base material, and a release layer in this order, and a base material, a barrier layer, and a release layer. Examples thereof include a sheet having a laminated structure containing the above in order, and a sheet having a laminated structure containing a barrier layer, a base material, an adhesive layer, a base material, and a release layer in this order. Examples of the base material and the barrier layer include those described above.
- the adhesive is not particularly limited, and a commercially available adhesive can be used.
- the second sheet is a sheet having a release layer and the release layer is in contact with the resin composition layer.
- the second sheet which is a sheet having a release layer, include a sheet having a laminated structure including a release layer and a base material.
- the base material include those described above.
- the release agent examples include a silicone-based release agent, an alkyd-based release agent, a fluorine-based release agent, an olefin-based release agent, and the like.
- the release layer is preferably formed from a silicone-based release agent or an alkyd-based release agent.
- the thickness of the release layer is preferably 0.05 to 5 ⁇ m, more preferably 0.05 to 3 ⁇ m, and even more preferably 0.05 to 2 ⁇ m.
- the second sheet may have a release layer.
- the configuration in which the third sheet is a sheet having an adhesive layer, the second sheet is a sheet having a release layer, and the adhesive layer is in contact with the release layer is included in the configuration (1).
- the description of the release layer is as described above.
- the second sheet may have release layers on both sides.
- the third sheet is a sheet having an adhesive layer
- the second sheet is a sheet having a release layer on both sides
- the adhesive layer is in contact with one of the release layers
- the other of the release layers is The configuration in contact with the resin composition layer. The description of the release layer is as described above.
- the third sheet may have a release layer.
- the configuration in which the second sheet is a sheet having an adhesive layer, the third sheet is a sheet having a release layer, and the adhesive layer is in contact with the release layer is included in the configuration (2).
- the third sheet may have release layers on both sides.
- the configuration in which the second sheet is a sheet having an adhesive layer, the third sheet is a sheet having a release layer on both sides, and the adhesive layer is in contact with one of the release layers is the configuration (2). Is included in. The description of the release layer is as described above.
- the configuration (1) is preferable.
- the 90-degree peel strength between the second sheet and the third sheet is preferably 0.1 gf / inch or more, more preferably 0.2 gf / inch or more, still more preferably 0.25 gf / inch or more, and is preferable. Is 250 gf / inch or less, more preferably 200 gf / inch or less, still more preferably 150 gf / inch or less.
- This 90-degree peel strength is a value measured by the method described in Examples described later.
- the “90 degree peel strength between the second sheet and the third sheet” is “the adhesive layer of the second sheet and the third sheet”. It means “90 degree peel strength between”.
- the second sheet has a release layer and the release layer is in contact with the adhesive layer of the third sheet, "between the second sheet and the third sheet”.
- “90 degree peel strength” means “90 degree peel strength between the release layer and the adhesive layer”.
- the “90 degree peel strength between the second sheet and the third sheet” is “the adhesive layer of the second sheet and the third sheet. It means “90 degree peel strength between”.
- the third sheet has a release layer and the release layer is in contact with the adhesive layer of the second sheet, "between the second sheet and the third sheet”.
- “90 degree peel strength” means “90 degree peel strength between the release layer and the adhesive layer”.
- the 90-degree peel strength between the resin composition layer and the second sheet is preferably larger than the 90-degree peel strength between the second sheet and the third sheet. With such a configuration, it is possible to prevent the second sheet from being peeled off when the third sheet is peeled off.
- the 90-degree peel strength between the resin composition layer and the second sheet is preferably 0.2 gf / inch or more, more preferably 0.25 gf / inch or more, still more preferably 0.30 gf / inch or more, and is preferable. Is 300 gf / inch or less, more preferably 250 gf / inch or less, still more preferably 200 gf / inch or less.
- the "90 degree peel strength between the resin composition layer and the second sheet” is ". It means "90 degree peel strength between the release layer and the resin composition layer”.
- the thickness of the adhesive layer is preferably 0.5 to 50 ⁇ m, more preferably 1 to 40 ⁇ m, and even more preferably 1 to 30 ⁇ m.
- a resin composition prepared by appropriately adding an alicyclic saturated hydrocarbon resin to various base polymers can also be used for forming an adhesive layer.
- the base polymer include olefin elastomers such as tough selenium X1102, X1104, X1105, and X1107 (all manufactured by Sumitomo Chemical Co., Ltd.), Septon 1020, 2002, 2004, 2005, 2006, 2063, 2104, 4033, 4044, 4055, Examples thereof include styrene-based thermoplastic elastomers such as 4077 and 4099 (both manufactured by Kuraray Co., Ltd.).
- a resin composition containing an olefin-based resin described later can also be used to form an adhesive layer. In order to form the adhesive layer, a resin composition containing no semi-baked hydrotalcite or other inorganic filler described later may be used.
- the adhesive layer can be formed, for example, by applying a liquid adhesive to the second sheet or the third sheet and drying it. Further, a pressure-sensitive adhesive varnish obtained by dissolving a pressure-sensitive adhesive in a solvent may be used for forming the pressure-sensitive adhesive layer.
- the resin composition layer is not particularly limited, and a known resin composition can be used to form the resin composition layer.
- the resin composition layer preferably contains an olefin resin and / or an epoxy resin.
- the olefin resin is not particularly limited as long as it has a skeleton derived from an olefin monomer.
- an ethylene-based resin, a propylene-based resin, a butene-based resin, and an isobutylene-based resin are preferable.
- These olefin-based resins may be homopolymers, or copolymers such as random copolymers and block copolymers.
- copolymer examples include a copolymer of two or more kinds of olefins and a copolymer of an olefin and a monomer other than the olefin such as a non-conjugated diene or styrene.
- preferred copolymers are ethylene-non-conjugated diene copolymer, ethylene-propylene copolymer, ethylene-propylene-non-conjugated diene copolymer, ethylene-butene copolymer, propylene-butene copolymer, propylene.
- olefin-based resin for example, isobutylene-modified resin, styrene-isobutylene-modified resin, modified propylene-butene resin and the like are preferably used.
- the acid anhydride group examples include a group derived from succinic anhydride, a group derived from maleic anhydride, a group derived from glutaric anhydride, and the like.
- the olefin resin having an acid anhydride group is, for example, an unsaturated compound having an acid anhydride group, and is obtained by graft-modifying the olefin resin under radical reaction conditions. Further, an unsaturated compound having an acid anhydride group may be radically copolymerized together with an olefin or the like.
- the olefin resin having an epoxy group is an unsaturated compound having an epoxy group such as glycidyl (meth) acrylate, 4-hydroxybutyl acrylate glycidyl ether, and allyl glycidyl ether, and the olefin resin is subjected to radical reaction conditions. It is obtained by graft modification with. Further, an unsaturated compound having an epoxy group may be radically copolymerized together with an olefin or the like.
- the concentration of the acid anhydride group in the olefin resin having an acid anhydride group is preferably 0.05 to 10 mmol / g, more preferably 0.1 to 5 mmol / g.
- the concentration of the acid anhydride group is obtained from the value of the acid value defined as the number of mg of potassium hydroxide required to neutralize the acid present in 1 g of the resin according to the description of JIS K2501.
- the amount of the olefin resin having an acid anhydride group in the olefin resin is preferably 0 to 70% by mass, more preferably 10 to 50% by mass.
- the ratio of the olefin resin having an acid anhydride group to the olefin resin having an epoxy group is not particularly limited as long as an appropriate crosslinked structure can be formed, but the molar ratio of the epoxy group to the acid anhydride group (epoxide group: acid anhydride).
- the group) is preferably 100:10 to 100: 200, more preferably 100: 50 to 100: 150, and particularly preferably 100: 90 to 100: 110.
- the olefin resin is preferably amorphous from the viewpoint of suppressing a decrease in fluidity due to thickening of the varnish.
- amorphous means that the olefin resin does not have a clear melting point, and for example, when the melting point is measured by DSC (differential scanning calorimetry) of the olefin resin, no clear peak is observed. You can use things.
- the olefin resin includes BASF's "Opanol B100" (viscosity average molecular weight: 1,110,000) and BASF's "B50SF” (viscosity average molecular weight: 400,000).
- butene resin examples include "HV-1900” (polybutene, number average molecular weight: 2,900) manufactured by ENEOS (former company name "JXTG Energy”) and "HV-300M” (maleic anhydride) manufactured by Toho Chemical Industry Co., Ltd. Acid-modified liquid polybutene (modified product of "HV-300” (number average molecular weight: 1,400)), number average molecular weight: 2,100, number of carboxy groups constituting acid anhydride groups: 3.2 / 1 Molecule, acid value: 43.4 mgKOH / g, acid anhydride group concentration: 0.77 mmol / g).
- HV-1900 polybutene, number average molecular weight: 2,900
- ENEOS former company name "JXTG Energy”
- HV-300M maleic anhydride manufactured by Toho Chemical Industry Co., Ltd.
- Acid-modified liquid polybutene modified product of "HV-300” (number average molecular
- styrene-isobutylene copolymer examples include “SIBSTAR T102” manufactured by Kaneka (styrene-isobutylene-styrene block copolymer, number average molecular weight: 100,000, styrene content: 30% by mass), manufactured by Seikou PMC.
- TiBSTAR T102 styrene-isobutylene-styrene block copolymer, number average molecular weight: 100,000, styrene content: 30% by mass
- Seikou PMC Specific examples of the styrene-isobutylene copolymer.
- T-YP757B maleic anhydride-modified styrene-isobutylene-styrene block copolymer, acid anhydride group concentration: 0.464 mmol / g, number average molecular weight: 100,000
- T-YP766 manufactured by Seikou PMC.
- T-YP429 manufactured by Seikou PMC (maleic anhydride-modified ethylene-methylmethacrylate copolymer (methylmethacrylate per 100% by mass in total of ethylene unit and methylmethacrylate unit)).
- propylene-butene copolymer "T-YP341” manufactured by Seikou PMC (glycidyl methacrylate-modified propylene-butene random copolymer (amount of butene units per 100% by mass of propylene units and butene units in total:): 29% by mass, epoxy group concentration: 0.638 mmol / g, number average molecular weight: 155,000) 20% by mass swazole solution), Seikou PMC "T-YP279” (maleic anhydride-modified propylene-butene random copolymer) Amount of butene unit per 100% by mass of total of propylene unit and butene unit: 36% by mass, acid anhydride group concentration: 0.464 mmol / g, number average molecular weight: 35,000), Seikou PMC "T” -YP276 "(glycidyl methacrylate-modified propylene-butene random copolymer
- the olefin resin contains an olefin resin having an epoxy group
- an olefin resin having a functional group other than an acid anhydride group that can react with the epoxy group may be used.
- the functional group include a hydroxyl group, a phenolic hydroxyl group, an amino group, a carboxy group and the like.
- an olefin resin having a functional group other than the epoxy group that can react with the acid anhydride group may be used.
- the functional group include a hydroxyl group, a primary or secondary amino group, a thiol group, an oxetane group and the like.
- the epoxy resin can be used without limitation as long as it has two or more epoxy groups per molecule on average.
- examples of the epoxy resin include bisphenol A type epoxy resin, hydrogenated bisphenol A type epoxy resin, biphenyl type epoxy resin, biphenyl aralkyl type epoxy resin, naphthol type epoxy resin, naphthalene type epoxy resin, bisphenol F type epoxy resin, and phosphorus.
- Epoxy resin bisphenol S type epoxy resin, aromatic glycidyl amine type epoxy resin (for example, tetraglycidyl diaminodiphenylmethane, triglycidyl-p-aminophenol, diglycidyl toluidin, diglycidyl aniline, etc.), alicyclic epoxy resin, aliphatic Chain epoxy resin, phenol novolac type epoxy resin, cresol novolac type epoxy resin, bisphenol A novolac type epoxy resin, epoxy resin with butadiene structure, diglycidyl etherified product of bisphenol, diglycidyl etherified product of naphthalene diol, diglycidyl etherified product of phenols Examples thereof include glycidyl etherified products, diglycidyl etherified products of alcohols, alkyl substituents, halides and hydrogenated products of these epoxy resins. Only one type of epoxy resin may be used, or two or more types may be used.
- the epoxy resin may be either liquid or solid, and both liquid epoxy resin and solid epoxy resin may be used.
- liquid and solid are states of the epoxy resin at normal temperature (25 ° C.) and normal pressure (1 atm).
- the amount of epoxy resin is not particularly limited. When an epoxy resin is used, the amount thereof is preferably 20 to 80% by mass, more preferably 30 to 70% by mass, and 50 to 50% by mass per whole resin composition layer (that is, per total non-volatile content of the resin composition). 65% by mass is more preferable.
- Unfired hydrotalcite is, for example, a metal hydroxide having a layered crystal structure typified by natural hydrotalcite (Mg 6 Al 2 (OH) 16 CO 3 ⁇ 4H 2 O), for example, It consists of a basic skeleton layer [Mg 1-X Al X (OH) 2 ] X + and an intermediate layer [(CO 3 ) X / 2 ⁇ mH 2 O] X ⁇ .
- the uncalcined hydrotalcite in the present invention is a concept including hydrotalcite-like compounds such as synthetic hydrotalcite. Examples of the hydrotalcite-like compound include those represented by the following formulas (I) and (II).
- M 2+ is Mg 2+, a divalent metal ion such as Zn 2+, M 3+ represents a trivalent metal ion such as Al 3+, Fe 3+, A n- is CO 3 2-, Cl -, NO 3 - represents a n-valent anion, such as a 0 ⁇ x ⁇ 1, a 0 ⁇ m ⁇ 1, n is a positive number).
- M 2+ is preferably Mg 2+
- M 3+ is preferably Al 3+
- a n- is preferably CO 3 2-.
- Semi-calcined hydrotalcite refers to a metal hydroxide having a layered crystal structure in which the amount of interlayer water is reduced or eliminated, which is obtained by calcining uncalcined hydrotalcite.
- interlayer water refers to "H 2 O" described in the above-mentioned composition formulas of uncalcined natural hydrotalcite and hydrotalcite-like compounds, if it is described using a composition formula.
- calcined hydrotalcite refers to a metal oxide having an amorphous structure obtained by calcining uncalcined hydrotalcite or semi-calcined hydrotalcite, in which not only interlayer water but also hydroxyl groups are eliminated by condensation dehydration.
- Unfired hydrotalcite, semi-fired hydrotalcite and fired hydrotalcite can be distinguished by the saturated water absorption rate.
- the saturated water absorption rate of the semi-baked hydrotalcite is 1% by mass or more and less than 20% by mass.
- the saturated water absorption rate of uncalcined hydrotalcite is less than 1% by mass, and the saturated water absorption rate of calcined hydrotalcite is 20% by mass or more.
- the saturated water absorption rate of the semi-baked hydrotalcite is preferably 3% by mass or more and less than 20% by mass, and more preferably 5% by mass or more and less than 20% by mass.
- uncalcined hydrotalcite, semi-calcined hydrotalcite and calcined hydrotalcite can be distinguished by the thermogravimetric reduction rate measured by thermogravimetric analysis.
- the thermogravimetric reduction rate of the semi-baked hydrotalcite at 280 ° C. is less than 15% by mass, and the thermogravimetric reduction rate at 380 ° C. is 12% by mass or more.
- the thermogravimetric reduction rate of uncalcined hydrotalcite at 280 ° C. is 15% by mass or more
- the thermogravimetric reduction rate of calcined hydrotalcite at 380 ° C. is less than 12% by mass.
- thermogravimetric reduction rate 100 ⁇ (mass before heating-mass when a predetermined temperature is reached) / mass before heating (ii) Can be obtained at.
- Powder X-ray diffraction measurement is performed by a powder X-ray diffractometer (PANalytical, Empyrean) with anti-cathode CuK ⁇ (1.5405 ⁇ ), voltage: 45 V, current: 40 mA, sampling width: 0.0260 °, scanning speed: 0.
- the measurement was performed under the conditions of .0657 ° / s and the measurement diffraction angle range (2 ⁇ ): 5.0131 to 79.9711 °.
- the peak search uses the peak search function of the software attached to the diffractometer, and "minimum significance: 0.50, minimum peak tip: 0.01 °, maximum peak tip: 1.00 °, peak base width: 2". It can be performed under the condition of "0.00 °, method: minimum value of second derivative".
- the particle size of the semi-baked hydrotalcite is preferably 1 to 1,000 nm, more preferably 10 to 800 nm.
- the particle size of the semi-baked hydrotalcite is the median size of the particle size distribution when the particle size distribution is prepared on a volume basis by laser diffraction scattering type particle size distribution measurement (JIS Z8825).
- alkylsilanes include methyltrimethoxysilane, ethyltrimethoxysilane, hexyltrimethoxysilane, octyltrimethoxysilane, decyltrimethoxysilane, octadecyltrimethoxysilane, dimethyldimethoxysilane, octyltrimethoxysilane, and n-octadecyl. Examples thereof include dimethyl (3- (trimethoxysilyl) propyl) ammonium chloride. One or more of these can be used.
- Examples of the semi-baked hydrotalcite include “DHT-4C” (manufactured by Kyowa Chemical Industry Co., Ltd., particle size: 400 nm), “DHT-4A-2” (manufactured by Kyowa Chemical Industry Co., Ltd., particle size: 400 nm) and the like. ..
- examples of the fired hydrotalsite include “KW-2200” (manufactured by Kyowa Chemical Industry Co., Ltd., particle size: 400 nm)
- examples of the unfired hydrotalsite include “DHT-4A” (Kyowa Chemical Industry).
- STABIACE HT-1, HT-7, HT-P manufactured by Sakai Chemical Industry Co., Ltd.
- the resin composition layer may contain another inorganic filler different from the semi-calcined hydrotalcite.
- inorganic fillers include, for example, unfired hydrotalcite, fired hydrotalcite, talcite, silica, alumina, barium sulfate, clay, mica, aluminum hydroxide, magnesium hydroxide, calcium carbonate, magnesium carbonate, boron nitride. , Aluminum borate, barium titanate, strontium titanate, calcium titanate, magnesium titanate, bismuth titanate, titanium oxide, barium zirconate, calcium zirconate and the like.
- the sealing sheet of the present invention is useful as a sheet used for sealing an electronic device that is sensitive to moisture.
- the electronic device is preferably an organic EL device, a quantum dot device or a solar cell.
- Comparative Example 2 A sealing sheet was produced in the same manner as in Comparative Example 1 except that the sheet C was used as the second sheet.
- Table 3 below lists the first to third sheets used in Examples 1 and 2 and Comparative Examples 1 and 2.
- the sealing sheet of Comparative Example 1 having a laminated structure with the moisture-proof sheet (first sheet) / resin composition layer / moisture-proof sheet (second sheet) is stored. Although it is possible to suppress an increase in the water content in the resin composition layer at that time, the resin composition layer cannot be dried efficiently. Further, the sealing sheet of Comparative Example 2 having a laminated structure with the moisture-proof sheet (first sheet) / resin composition layer / non-moisture-proof sheet (second sheet) is contained in the resin composition layer at the time of storage. The increase in water content cannot be suppressed, and the water content after drying also increases.
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WO2023280598A1 (en) * | 2021-07-08 | 2023-01-12 | Agfa-Gevaert Nv | A separator for alkaline water electrolysis |
WO2023182493A1 (ja) * | 2022-03-25 | 2023-09-28 | 味の素株式会社 | 樹脂シートおよびその製造方法 |
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JP2017043060A (ja) * | 2015-08-28 | 2017-03-02 | 富士フイルム株式会社 | ガスバリアフィルムおよびガスバリアフィルムの転写方法 |
JP2018065328A (ja) * | 2016-10-21 | 2018-04-26 | コニカミノルタ株式会社 | 水蒸気バリア積層体及び有機エレクトロルミネッセンス素子 |
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WO2023280598A1 (en) * | 2021-07-08 | 2023-01-12 | Agfa-Gevaert Nv | A separator for alkaline water electrolysis |
WO2023182493A1 (ja) * | 2022-03-25 | 2023-09-28 | 味の素株式会社 | 樹脂シートおよびその製造方法 |
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JPWO2021095830A1 (zh) | 2021-05-20 |
DE112020005543T5 (de) | 2022-09-01 |
CN114731744A (zh) | 2022-07-08 |
KR20220100902A (ko) | 2022-07-18 |
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