WO2018163923A1 - グリーンシート形成用剥離フィルム - Google Patents
グリーンシート形成用剥離フィルム Download PDFInfo
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- WO2018163923A1 WO2018163923A1 PCT/JP2018/007389 JP2018007389W WO2018163923A1 WO 2018163923 A1 WO2018163923 A1 WO 2018163923A1 JP 2018007389 W JP2018007389 W JP 2018007389W WO 2018163923 A1 WO2018163923 A1 WO 2018163923A1
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- agent layer
- release agent
- green sheet
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- 238000007607 die coating method Methods 0.000 description 1
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- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical compound CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 1
- 208000028659 discharge Diseases 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 235000019382 gum benzoic Nutrition 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 125000005439 maleimidyl group Chemical group C1(C=CC(N1*)=O)=O 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- RJMRIDVWCWSWFR-UHFFFAOYSA-N methyl(tripropoxy)silane Chemical compound CCCO[Si](C)(OCCC)OCCC RJMRIDVWCWSWFR-UHFFFAOYSA-N 0.000 description 1
- HLXDKGBELJJMHR-UHFFFAOYSA-N methyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](C)(OC(C)C)OC(C)C HLXDKGBELJJMHR-UHFFFAOYSA-N 0.000 description 1
- 125000002816 methylsulfanyl group Chemical group [H]C([H])([H])S[*] 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- GHJOIQFPDMIKHT-UHFFFAOYSA-N propane-1,2,3-triol;prop-2-enoic acid Chemical compound OC(=O)C=C.OCC(O)CO GHJOIQFPDMIKHT-UHFFFAOYSA-N 0.000 description 1
- QMYDVDBERNLWKB-UHFFFAOYSA-N propane-1,2-diol;hydrate Chemical compound O.CC(O)CO QMYDVDBERNLWKB-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical group 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- OQTSOKXAWXRIAC-UHFFFAOYSA-N tetrabutan-2-yl silicate Chemical compound CCC(C)O[Si](OC(C)CC)(OC(C)CC)OC(C)CC OQTSOKXAWXRIAC-UHFFFAOYSA-N 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- BCLLLHFGVQKVKL-UHFFFAOYSA-N tetratert-butyl silicate Chemical compound CC(C)(C)O[Si](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C BCLLLHFGVQKVKL-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- ZOYFEXPFPVDYIS-UHFFFAOYSA-N trichloro(ethyl)silane Chemical compound CC[Si](Cl)(Cl)Cl ZOYFEXPFPVDYIS-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/30—Producing shaped prefabricated articles from the material by applying the material on to a core or other moulding surface to form a layer thereon
-
- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/056—Forming hydrophilic coatings
Definitions
- the present invention relates to a release film for forming a green sheet.
- the release film is generally composed of a substrate and a release agent layer.
- the green sheet is produced by dispersing ceramic particles and a binder resin in an organic solvent on such a release film, coating the dissolved ceramic slurry, and drying the slurry.
- the manufactured green sheet peels from a peeling film, and is used for manufacture of a ceramic capacitor.
- problems such as a pinhole forming on the surface of a green sheet, when the unevenness
- the recent miniaturization and higher density of ceramic capacitors further reduction in the thickness of green sheets has been demanded. And the further improvement of smoothness is calculated
- the smoothness of the release film is improved, there is a problem that blocking tends to occur. That is, in general, the release film is stored and transported in a rolled state, and is used by being unrolled from the rolled state when forming a green sheet. Therefore, when unwinding the peeled release film, there is a problem that blocking (attachment) between the release agent layer on the surface of the release film and the base material on the back surface of the release film is likely to occur.
- the performance (anti-blocking property) which prevents blocking is calculated
- Patent Document 1 describes a release film in which a release layer containing inert fine particles is provided on at least one surface of a polyester film.
- the 10-point average roughness (Rz) of the release layer surface is 20 to 500 nm.
- the release film described in Patent Document 1 cannot provide a release film that can achieve both smoothness and antiblocking properties.
- an object of the present invention is to provide a release film for forming a green sheet having excellent smoothness and sufficient antiblocking properties.
- the release film for forming a green sheet is a release film for forming a green sheet used for forming a green sheet, and includes a base material and a release agent layer provided on one side of the base material.
- the release agent layer comprises a cured product of a release agent forming material containing (A) an energy ray-curable compound, (B) a hydrophobized silica sol, and (C) a release imparting component. It is what.
- the (B) hydrophobized silica sol preferably has an average particle size of 10 nm to 100 nm.
- the contact angle of water with the coating film is preferably 100 ° or more.
- the average thickness of the release agent layer is preferably 0.2 ⁇ m or more and 2 ⁇ m or less.
- the arithmetic average roughness Ra of the outer surface of the release agent layer is 8 nm or less, and the maximum protrusion height Rp of the outer surface of the release agent layer Is preferably 50 nm or less.
- a green sheet-forming release film 1 (hereinafter, “release film 1”) according to this embodiment includes a base material 11 and a release agent layer provided on the first surface 11 ⁇ / b> A of the base material 11. 12.
- the base material 11 has a first surface 11A and a second surface 11B.
- the material constituting the substrate 11 is not particularly limited.
- polyester resin polybutylene terephthalate resin, polyethylene terephthalate resin, polyethylene naphthalate resin, etc.
- polyolefin resin polypropylene resin, polymethylpentene resin, etc.
- films made of plastics such as polycarbonate.
- the substrate 11 may be a single layer film or a multilayer film of two or more layers of the same type or different types.
- a polyester film is preferable and a biaxially stretched polyethylene terephthalate film is more preferable from the viewpoint that dust or the like hardly occurs during processing or use.
- a green sheet is manufactured using the release film 1 manufactured using a polyester film, poor coating of ceramic slurry due to dust or the like can be effectively prevented.
- the base material 11 may contain a filler in addition to the above materials.
- the filler include silica, titanium oxide, calcium carbonate, kaolin, and aluminum oxide. These may be used individually by 1 type, or may be used in combination of 2 or more type. By including such a filler, the mechanical strength of the base material 11 is imparted, the slipperiness of the front and back surfaces is improved, and blocking can be suppressed.
- both surfaces are general-purpose grades. Or both surfaces may be in a high smoothness grade roughness range. Further, one of the first surface 11A and the second surface 11B may be a high smoothness grade roughness range, and the other surface may be a general purpose grade roughness range.
- the winding of the release film 10 usually causes blocking. The release film 1 hardly causes blocking.
- the arithmetic average roughness Ra (Ra 1 ) of the first surface 11A of the substrate 11 is preferably 1 nm or more and 40 nm or less, and more preferably 2 nm or more and 20 nm or less.
- the maximum protrusion height Rp (Rp 1 ) of the first surface 11A of the substrate 11 is preferably 10 nm or more and 500 nm or less, and more preferably 15 nm or more and 350 nm or less.
- the arithmetic average roughness Ra (Ra 2 ) of the second surface 11B of the substrate 11 is preferably 1 nm or more and 40 nm or less, and more preferably 2 nm or more and 20 nm or less.
- the maximum protrusion height Rp (Rp 2 ) of the second surface 11B of the substrate 11 is preferably 10 nm or more and 500 nm or less, more preferably 15 nm or more and 350 nm or less, It is particularly preferably 20 nm or more and 300 nm or less.
- the peeling film 1 and the ceramic green sheet formed into a film are wound up by using a high smoothness grade base material, the back surface side (2nd of the peeling film 1 which contacts an application surface) Since the surface 11B side is smooth, the ceramic green sheet is not damaged by being pressed, and the quality of the ceramic capacitor is improved.
- the arithmetic average roughness Ra (Ra 1 ) of the first surface 11A of the base material 11 is usually 5 nm or more and 80 nm or less, and the maximum protrusion height of the first surface 11A of the base material 11
- the thickness Rp (Rp 1 ) is usually 100 nm or more and 700 nm or less.
- the arithmetic average roughness Ra (Ra 2 ) of the second surface 11B of the base material 11 is usually 5 nm or more and 80 nm or less, and the maximum protrusion height of the second surface 11B of the base material 11
- the thickness Rp (Rp 2 ) is usually 100 or more and 700 nm or less.
- the arithmetic average roughness Ra and the maximum protrusion height Rp of the first surface 11A and the second surface 11B of the base material 11 are the surfaces manufactured by Mitutoyo Corporation in accordance with JIS B0601-1994. It is a value obtained by measuring with a roughness measuring instrument SV3000S4 (stylus type).
- the “arithmetic average roughness and maximum protrusion height” refer to values obtained by measurement as described above.
- the average film thickness of the substrate 11 is not particularly limited, but is preferably 10 ⁇ m or more and 300 ⁇ m or less, and more preferably 15 ⁇ m or more and 200 ⁇ m or less. Thereby, while making the softness
- the release agent layer 12 is provided on the first surface 11 ⁇ / b> A of the substrate 11.
- the release agent layer 12 is made of a cured product of a release agent forming material.
- the release agent layer 12 is formed by irradiating the release agent layer forming material with an active energy ray and curing it.
- the release agent layer 12 can impart smoothness, peelability and antiblocking property to the release film 1.
- the arithmetic average roughness Ra (Ra 0 ) of the outer surface 12A of the release agent layer 12 is preferably 15 nm or less, and more preferably 8 nm or less. Further, the maximum protrusion height Rp (Rp 0 ) on the outer surface of the release agent layer 12 is preferably 50 nm or less, and more preferably 45 nm or less. As a result, when the green sheet is molded on the outer surface 12A side of the release agent layer 12, it is possible to more reliably prevent the green sheet from causing pinholes or partial thickness variations. Higher smoothness can be achieved.
- the outer surface 12A is highly smooth as described above, and the blocking is performed even when the second surface 11B of the substrate 11 is also highly smooth. It will not wake up.
- the release agent layer forming material which will be described later, has appropriate fluidity when applied onto the first surface 11A of the substrate 11. Therefore, if such a release agent layer forming material is used, the unevenness of the first surface 11A of the substrate 11 can be easily embedded, and the embedded state can be maintained. As a result, the unevenness of the base material 11 can be prevented from affecting the outer surface 12A side of the release agent layer 12 opposite to the base material 11, and the outer surface 12A of the release agent layer 12 can be smoothed. .
- the average thickness of the release agent layer 12 is preferably 0.2 ⁇ m or more and 2 ⁇ m or less, and more preferably 0.3 ⁇ m or more and 1.5 ⁇ m or less. If the average thickness of the release agent layer 12 is equal to or greater than the lower limit, the smoothness of the outer surface 12A of the release agent layer 12 can be improved, and pinholes or partial thickness variations can be generated in the green sheet. It can be surely prevented. On the other hand, if the thickness of the release agent layer 12 is equal to or less than the above upper limit, the occurrence of curling of the release film 1 due to curing shrinkage of the release agent layer 12 can be prevented, and the substrate in contact with the release film 1 is wound up. It can suppress that blocking generate
- the elastic modulus of the release agent layer 12 is preferably 3.5 GPa or more and 8.0 GPa or less, and more preferably 4.0 GPa or more and 8.0 GPa or less. If the average elastic modulus of the release agent layer 12 is within the above range, when the outer surface 12A of the release agent layer 12 is sufficiently hard and the release films are in close contact with each other, the segregated hydrophobized silica sinks to the surface. Can be suppressed. Therefore, the effect of imparting anti-blocking properties by the hydrophobized silica can be further enhanced.
- the elastic modulus of the release agent layer 12 is determined by using a nanoindenter (trade name “Nano Indenter SA4” manufactured by MTS), a maximum indenter depth of 100 nm, and a strain rate of 0.05 sec ⁇ 1. A nanoindentation test was performed under the conditions of a displacement amplitude of 2 nm and a vibration frequency of 45 Hz, and the coating modulus of the release film was measured.
- the “elastic modulus” refers to a value obtained by measurement as described above.
- the release agent layer-forming material contains (A) an energy ray-curable compound, (B) a hydrophobized silica sol, and (C) a release imparting component.
- (Energy ray curable compound) there is no restriction
- the energy ray curable compound (A) include energy ray curable monomers, oligomers and resins, and compositions containing these. Specific examples include polyfunctional (meth) acrylate, urethane (meth) acrylate, polyester (meth) acrylate, polyether (meth) acrylate, and silicone (meth) acrylate. These may be used individually by 1 type, and may be used in combination of 2 or more types.
- Polyfunctional (meth) acrylates include 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, ethylene glycol di (meth) acrylate, Propylene glycol di (meth) acrylate, hexanediol di (meth) acrylate, trimethylolethane tri (meth) acrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, dipentaerythritol hexa (meth) acrylate Glycerol tri (meth) acrylate, triallyl (meth) acrylate, and the like.
- the release agent layer 12 can be provided with appropriate hardness.
- the polyfunctional (meth) acrylate the polyfunctional (meth) acrylate containing a functional group may be sufficient.
- the functional group used is preferably a hydroxyl group, and the dispersibility of the hydrophobic silica sol of component (B) in the release agent layer forming material and the ubiquity in the formed release agent layer 12 can be optimized. .
- hydroxyl group-containing acrylic compound examples include pentaerythritol tri (meth) acrylate, dipentaerythritol tri (meth) acrylate, dipentaerythritol tetra (meth) acrylate, dipentaerythritol penta (meth) acrylate, trimethylolpropane di (Meth) acrylate, pentaerythritol di (meth) acrylate, etc. are mentioned. These may be used individually by 1 type, and may be used in combination of 2 or more types. Among these, it is more preferable to use pentaerythritol tri (meth) acrylate because it can impart appropriate rigidity to the release agent layer 12.
- the release agent layer 12 can be cured by two systems of energy rays and heating by crosslinking with a crosslinking agent, and the degree of curing can be set as desired. Can be a level.
- polyfunctional (meth) acrylate contains EO (ethylene oxide) or PO (propylene oxide) addition type polyfunctional (meth) acrylate.
- the EO (ethylene oxide) or PO (propylene oxide) addition type polyfunctional (meth) acrylate is a compound obtained by esterifying an EO or PO addition type polyhydric alcohol with acrylic acid. Specific examples include EO or PO-modified glycerol triacrylate, EO or PO-modified trimethylolpropane acrylate, EO or PO-modified pentaerythritol tetraacrylate, and EO or PO-modified dipentaerythritol hexaacrylate.
- EO or PO-modified dipentaerythritol hexaacrylate EO or PO-modified trimethylolpropane tetraacrylate May be used.
- the content in terms of solid content (content ratio in the total solid content excluding the solvent) of the (A) energy beam curable compound in the release agent layer forming material is preferably 50% by mass or more.
- hydrophobized silica sol examples of the type of (B) hydrophobized silica sol according to this embodiment include sols of silica fine particles such as alkoxysilane compounds and chlorosilane compounds.
- the anti-blocking property can be imparted to the release agent layer 12 by the hydrophobized silica sol.
- an alkoxysilane compound if it is a silicon compound which has a hydrolyzable alkoxyl group, it will not specifically limit, For example, the compound represented by General formula (1) is mentioned.
- R 1 represents a hydrogen atom or a non-hydrolyzable group.
- non-hydrolyzable group examples include an alkyl group, a substituted alkyl group (substituent: halogen atom, epoxy atom, (meth) acryloyloxy group, etc.), alkenyl group, aryl group, and aralkyl group.
- R 2 represents a lower alkyl group (an alkyl group having 1 to 10 carbon atoms (preferably having 1 to 4 carbon atoms)).
- n is an integer of 0 to 2
- plural R 1 may be the same or different
- plural OR 2 may be the same or different.
- alkoxysilane compound represented by the general formula (1) tetramethoxysilane, tetraethoxysilane, tetra-n-propoxysilane, tetraisopropoxysilane, tetra-n-butoxysilane, tetraisobutoxysilane , Tetra-sec-butoxysilane, tetra-tert-butoxysilane, trimethoxysilane hydride, triethoxysilane hydride, tripropoxysilane hydride, methyltrimethoxysilane, methyltriethoxysilane, methyltripropoxysilane, methyltriisopropoxysilane , Ethyltrimethoxysilane, ethyltriethoxysilane, propyltriethoxysilane, butyltrimethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane
- an alkoxysilane compound a compound in which n is 0, or a compound in which n is 1 or 2 and R 1 is a hydrogen atom can be obtained by completely hydrolyzing an inorganic silica-based cured product. By doing so, a polyorganosiloxane-based cured product or a mixed cured product of inorganic silica and polyorganosiloxane can be obtained.
- a compound in which n is 1 or 2 and R 1 is a non-hydrolyzable group has a non-hydrolyzable group, so that a polyorganosiloxane-based cured product is obtained by partial or complete hydrolysis.
- chlorosilane compound examples include ethyldichlorosilane, ethyltrichlorosilane, dimethyldichlorosilane, trichlorosilane, trimethylchlorosilane, dimethyldichlorosilane, and methyltrichlorosilane. These may be used individually by 1 type, and may be used in combination of 2 or more types.
- the silica sol is a dispersion of silica fine particles in a sol state in water or an organic solvent.
- an organic solvent is not particularly limited, and includes methanol, ethanol, isopropanol, ethylene glycol, n-propyl cellosolve, methyl ethyl ketone, methyl isobutyl ketone, dimethylacetamide, propylene glycol monomethyl ether, cyclohexane, benzene, and toluene. These may be used individually by 1 type, and may be used in combination of 2 or more types. Among these, methyl isobutyl ketone and propylene glycol monomethyl ether are more preferable from the viewpoint of relatively high boiling point.
- the hydrophobized silica sol is a hydrophobized silica sol in which a part or all of silanol groups on the surface of silica particles is treated with a surface modifier having a hydrophobic group.
- the surface modifier include a silane coupling agent having both a functional group capable of reacting with a silanol group on the surface of the silica particle and a hydrophobic group.
- Examples of commercially available hydrophobized silica sol include SIRPGM15WT% -E26 manufactured by CIK Nanotech.
- (B) The degree of hydrophobicity of the hydrophobized silica sol was determined by applying the silica sol on a PET film, removing the solvent to form a silica sol coating film, and measuring the contact angle of water with the coating film. More specifically, when a coating film of (B) hydrophobized silica sol is formed, the contact angle of water with this coating film is preferably 100 ° or more. That is, if the contact angle of water with the silica sol coating film is 100 ° or more, it can be determined that the surface of the silica sol is hydrophobic.
- FIG. 2 shows a schematic diagram for conceptually explaining the segregation state of (B) the hydrophobized silica sol.
- the hydrophobized silica sol P is applied to the outer surface 12A of the release agent layer 12 in the release agent layer 12, as shown in FIG. It is understood that there are many and the ratio of the substrate 11 near the first surface 11A and in the release agent layer 12 is low. Therefore, an appropriate surface roughness can be imparted to the surface of the release agent layer 12 with the addition of a small amount of hydrophobic silica sol. Therefore, even if it is a case where peeling film 1 mutually overlaps and time passes, it can prevent that the 2nd surface 11B of the base material 11 and the releasing agent layer 12 block.
- a release agent layer having excellent smoothness can be formed because a predetermined anti-blocking effect can be exhibited with a relatively small amount of addition.
- the coating film of (B) hydrophobized silica sol it is more preferable that the contact angle of water with respect to this coating film is 100 ° or more and 130 ° or less.
- the contact angle of water with respect to this coating film is 100 ° or more and 130 ° or less.
- the silica sol coating when a silica sol coating is formed, when the contact angle of water with respect to the coating becomes less than 100 ° and the hydrophilicity of the silica sol increases, the silica sol segregates on the outer surface 12A of the release agent layer 12. It has been confirmed that it exists in a state dispersed throughout the release agent layer 12. Therefore, it is understood that the anti-blocking property cannot be imparted to the release agent layer 12.
- Example 1 the method of measuring the contact angle of water with respect to this coating film when a silica sol coating film is formed will be specifically
- the average particle size of the hydrophobized silica sol is preferably 10 nm or more and 100 nm or less.
- the average particle diameter is 10 nm or more, the antiblocking property of the release agent layer 12 can be further improved.
- the average particle diameter of (B) the hydrophobized silica sol is more preferably 10 nm or more and 50 nm or less, and further preferably 15 nm or more and 40 nm or less.
- the average particle diameter of (B) hydrophobized silica sol is a particle diameter (median diameter D50) in the integrated value 50% in the particle size distribution calculated
- the content of (B) the hydrophobized silica sol is preferably 0.4 parts by mass or more and 100 parts by mass or less with respect to 100 parts by mass of the energy ray-curable compound (A) in terms of solid content. It is more preferably 4 parts by mass or more and 30 parts by mass or less, still more preferably 0.4 parts by mass or more and 10 parts by mass or less, and particularly preferably 0.4 parts by mass or more and 3 parts by mass or less. If content is more than the said minimum, sufficient antiblocking property can be provided to the release agent layer 12. FIG. On the other hand, if content is below the said upper limit, the adhesiveness of the peeling agent layer 12 and the base material 11 is securable.
- Examples of the (C) peeling imparting component according to this embodiment include a silicone compound, a fluorine compound, and a long-chain alkyl-modified compound. These may be used individually by 1 type, and may be used in combination of 2 or more types.
- the (C) peeling imparting component is preferably a silicone compound, and examples thereof include polyorganosiloxane having a linear or branched molecular chain.
- the peelability of the release agent layer 12 can be imparted by the peel imparting component.
- the polyorganosiloxane has a reaction having at least one selected from the group consisting of a (meth) acryloyl group, a vinyl group, a hydroxyl group, a thiol group, and a maleimide group at least at one of the molecular chain terminal and the side chain. It preferably has a functional functional group.
- the polyorganosiloxane is more preferably one in which the reactive functional group is bonded to a silicon atom in the molecular chain directly or via a divalent linking group.
- the reactive functional group should just have at least 1 in 1 molecule.
- divalent linking group examples include an alkylene group, an alkyleneoxy group, an oxy group, an imino group, a carbonyl group, and a divalent linking group obtained by combining them.
- the divalent linking group preferably has 1 to 30 carbon atoms, and more preferably 1 to 10 carbon atoms.
- polyorganosiloxane can be used in combination of 2 or more type as needed.
- the modified polyorganosiloxane substituted with such a reactive functional group is incorporated and fixed in a crosslinked structure when the (A) energy ray-curable compound is cured by irradiation with active energy rays.
- the transfer transfer of the polyorganosiloxane which is a component of the release agent layer 12 to the green sheet formed on the outer surface 12A side of the release agent layer 12 can be suppressed.
- Examples of the organic group other than the reactive functional group constituting the peeling imparting component include the same or different monovalent hydrocarbon groups having no aliphatic unsaturated bond.
- the monovalent hydrocarbon group preferably has 1 to 12 carbon atoms, and more preferably has 1 to 10 carbon atoms.
- Examples of monovalent hydrocarbon groups include alkyl groups (such as methyl, ethyl and propyl groups) and aryl groups (such as phenyl and tolyl groups).
- (C) Content of peeling provision component is preferably 0.01 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of the (A) energy beam curable compound in terms of solid content. It is more preferably 02 parts by mass or more and 15 parts by mass or less, and particularly preferably 0.05 parts by mass or more and 10 parts by mass or less. If content is more than the said minimum, the peelability of the release agent layer 12 can be improved. On the other hand, if content is below the said upper limit, when a ceramic slurry is apply
- the release agent layer forming material may contain (D) a photopolymerization initiator.
- D By including a photopolymerization initiator, the release agent layer 12 can be efficiently formed when the release agent layer forming material is irradiated with active energy rays.
- the photopolymerization initiator refers to a compound that generates radical species upon irradiation with active energy rays such as ultraviolet rays.
- the photopolymerization initiator for example, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin-n-butyl ether, benzoin isobutyl ether, acetophenone, dimethylaminoacetophenone, 2,2-dimethoxy-2- Phenylacetophenone, 2,2-diethoxy-2-phenylacetophenone, 2-hydroxy-2-methyl-1-phenylpropan-1-one, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-1- [4- (methylthio) Phenyl] -2-morpholinopropanone-1-one, 4- (2-hydroxyethoxy) phenyl-2- (hydroxy-2-propyl) ketone, benzophenone, p-phenylbenzophenone, 4,4-diethi Aminobenzophenone, dichlorobenzophenone, 2-methylanthraquinone, 2-
- the content is 0.5 mass part or more and 20 mass parts or less with respect to 100 mass parts of said (A) energy-beam curable compounds in conversion of solid content. Is more preferably 0.2 parts by mass or more and 20 parts by mass or less, and particularly preferably 0.5 parts by mass or more and 15 parts by mass or less. If the content is within the above range, particularly excellent curability can be obtained even if the thickness of the release agent layer 12 is in a range where it is difficult to obtain curability due to oxygen inhibition.
- the release agent layer forming material according to this embodiment may contain other components in addition to the component (A), the component (B), the component (C), and the component (D).
- other components include a crosslinking agent, an antioxidant, an ultraviolet absorber, an antistatic agent, a polymerization accelerator, a polymerization inhibitor, an infrared absorber, and a plasticizer.
- a crosslinking agent when a hydroxyl group is used as the functional group of the component (A), a polyvalent isocyanate compound, a polyvalent epoxy compound, a polyvalent aziridine compound, a polyvalent metal chelate compound, and the like can be used.
- the content thereof is preferably 0.01 parts by mass or more and 5 parts by mass or less with respect to 100 parts by mass of the (A) energy beam curable compound in terms of solid content. It is more preferably 0.02 parts by mass or more and 3 parts by mass or less, and particularly preferably 0.05 parts by mass or more and 2 parts by mass or less.
- the release agent layer forming material according to the present embodiment can be produced by mixing and dispersing the component (A1) and the component (B).
- the solvent according to this embodiment include methyl alcohol, ethyl alcohol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, pentyl alcohol, ethyl cellosolve, benzene, toluene, xylene, ethylbenzene, cyclohexane, and ethyl.
- Examples include cyclohexane, ethyl acetate, butyl acetate, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, tetrahydrofuran, propylene glycol monomethyl ether, and water. These may be used individually by 1 type, and may be used in combination of 2 or more types.
- the release film 1 of the present embodiment includes a base material preparation step for preparing the base material 11, a coating layer forming step for forming a coating layer by applying and drying a release agent layer forming material, and a coating layer, It can be manufactured by a method including a release agent layer forming step of forming the release agent layer 12 by irradiating and curing an active energy ray.
- the base material 11 is prepared.
- a surface treatment can be applied to the first surface 11A of the substrate 11. Thereby, the adhesiveness of the base material 11 and the releasing agent layer 12 provided in the 1st surface 11A side of the base material 11 can be made especially excellent.
- Examples of the surface treatment include corona discharge treatment, plasma discharge treatment, chromium oxidation treatment (wet), flame treatment, hot air treatment, ozone, and ultraviolet irradiation treatment. These surface treatments are appropriately selected according to the type of the substrate 11, but generally corona discharge treatment is preferably used from the viewpoints of effects and operability.
- the aforementioned release agent layer forming material is applied onto the first surface 11A of the substrate 11 and dried. Thereby, a coating layer is obtained. If the above-mentioned release agent layer forming material is used, the unevenness of the first surface 11A of the substrate 11 can be filled. As a result, the outer surface 12A of the release agent layer 12 can be smoothed.
- Examples of the method for applying the release agent layer forming material include a gravure coating method, a bar coating method, a spray coating method, a spin coating method, an air knife coating method, a roll coating method, a blade coating method, a gate roll coating method, and Examples include a die coating method.
- the method for drying the release agent layer forming material is not particularly limited, and examples thereof include a method of drying in a hot air drying furnace.
- Drying conditions are not particularly limited, but the drying temperature is preferably 50 ° C. or higher and 130 ° C. or lower, and the drying time is preferably 5 seconds or longer and 1 minute or shorter. Thereby, unintentional alteration of the coating layer can be prevented, and the coating layer can be formed particularly efficiently. As a result, productivity of the finally obtained release film 1 can be improved. Further, when the drying temperature is within the above range, when the release agent layer forming material contains a solvent or the like, it is possible to prevent the coating layer from warping or cracking accompanying evaporation of the solvent or the like during drying.
- the release agent layer 12 is formed by irradiating and curing the active energy ray on the coating layer obtained in the coating layer forming step.
- the coating layer in which the unevenness of the first surface 11A of the base material 11 is properly embedded in the coating layer forming step is cured while maintaining the smoothness of the outer surface 12A.
- the release agent layer 12 having a sufficiently smooth outer surface 12A can be obtained.
- the release agent layer forming material contains the constituent components as described above, the release agent layer 12 having appropriate conductivity can be obtained.
- active energy rays include electromagnetic waves (infrared rays, visible rays, ultraviolet rays and X-rays) and particle beams (electron beams, ion beams, neutron rays and ⁇ rays).
- electromagnetic waves infrared rays, visible rays, ultraviolet rays and X-rays
- particle beams electron beams, ion beams, neutron rays and ⁇ rays.
- ultraviolet rays or visible light it is more preferable to use ultraviolet rays.
- the release agent layer 12 can be formed more easily and reliably.
- the coating layer can be uniformly cured while sufficiently shortening the curing time for curing the coating layer.
- a various general means can be utilized.
- a light source lamp such as a pressure mercury lamp, a metal halide lamp, and an excimer lamp can be used as the light source.
- irradiating active energy rays are irradiated amount of the active energy ray is preferably integrated light quantity is 30 mJ / cm 2 or more 400 mJ / cm 2 or less, 50 mJ / cm 2 or more 300mmJ / cm 2 or less It is more preferable that Further, it is preferable that the illuminance of the active energy ray is 0.1 W / cm 2 or more 4.0 W / cm 2 or less. If the irradiation amount and illuminance of ultraviolet rays are within the above ranges, the coating layer can be cured more uniformly and reliably.
- a ceramic capacitor can be manufactured using the release film 1 of the present embodiment.
- a method for manufacturing a ceramic capacitor for example, a ceramic powder dispersion slurry is applied to the surface of the release agent layer 12 of the release film 1 and dried to form a green sheet, and then the green sheet released from the release film 1 is laminated. And the method of forming an electrode in the ceramic sheet obtained by baking is mentioned. Since the release film 1 of the present embodiment hardly causes blocking, both the outer surface 12A of the release agent layer 12 and the second surface 11B of the substrate 11 can be made highly smooth. Thereby, if a ceramic capacitor is formed with a green sheet formed using the release film 1 of the present embodiment, a highly reliable ceramic capacitor in which the occurrence of problems due to a short circuit is prevented can be obtained.
- the release agent layer forming material containing the energy ray curable compound (A) can easily embed the unevenness of the first surface 11A of the substrate 11 and can maintain the embedded state. it can. As a result, the unevenness of the base material 11 can be prevented from affecting the outer surface 12A side of the release agent layer 12 opposite to the base material 11, and the outer surface 12A of the release agent layer 12 can be smoothed. .
- the green sheet forming release film according to this embodiment include the following green sheet forming release films, but the present invention is not limited to such examples.
- the release film for forming a green sheet according to the present embodiment a substrate and a release agent layer provided on one side of the substrate are provided, and the release agent layer is (A) an energy ray curable compound.
- a release film for forming a green sheet comprising a cured product of a release agent-forming material containing a hydroxyl group-containing acrylic compound, (B) a hydrophobized silica sol, and (C) a silicone compound as a release imparting component. It is done.
- the release film for forming a green sheet As an example of the release film for forming a green sheet according to the present embodiment, a substrate and a release agent layer provided on one side of the substrate are provided, and the release agent layer is (A) an energy ray curable compound.
- a cured product of a release agent-forming material comprising: (B) a hydrophobized silica sol; (C) a silicone compound as a release imparting component; and (D) a photopolymerization initiator. And a release film for forming a green sheet.
- the present invention is not limited to the above-described embodiments, and modifications, improvements, and the like within the scope that can achieve the object of the present invention are included in the present invention.
- the base material 11 has been described as having a single-layer structure, but is not limited thereto.
- the substrate 11 may have a multilayer structure of two or more layers of the same type or different types.
- the release agent layer 12 has been described as having a single layer structure, but is not limited thereto.
- the release agent layer 12 may also have a multilayer structure of two or more layers of the same type or different types.
- the green sheet forming release film in which the release agent layer 12 is provided on the first surface 11A of the substrate 11 has been described, but the present invention is not limited thereto.
- the release agent layer 12 may be provided on the second surface 11B side of the substrate 11.
- Example and a comparative example demonstrate this invention further in detail, this invention is not limited at all by these examples.
- material used in the Example and the comparative example is shown below.
- (A) component) Energy ray-curable compound: pentaerythritol triacrylate, trade name “NK Ester A-TMM-3L”, manufactured by Shin-Nakamura Chemical Co., Ltd., solid content: 100% by mass
- (B) component) Silica sol A: Hydrophobized silica sol, average particle size 30 nm, trade name “SIRPGM15WT% -E26”, manufactured by CIK Nanotech, Inc.
- Silica sol B Hydrophobized silica sol, average particle size 30 nm, trade name “SIRMIBK15WT% -E83”, manufactured by CIK Nanotech Co., Ltd.
- Silica sol C Silica sol, average particle size 100 nm, trade name “SIRMIBK15WT% -K18”, CIK Nanotech's silica sol
- D Silica sol, average particle size 30 nm, trade name “OSCAL-1632”, JGC Catalysts & Chemicals silica sol
- Silica sol F Silica sol average particle size 100 nm, trade name “SIRMIBK-E65”, manufactured by CIK Nanotech (component (C)) Peeling imparting component: Trade name “SH-28”, manufactured by Toray Dow Corning (component (D)) Photopolymerization initiator: trade name “Irgacure 184”, manufactured by BASF
- Example 1 First, a polyethylene terephthalate film (trade name “Lumirror U48”, manufactured by Toray Industries, Inc., thickness: 38 ⁇ m, arithmetic average roughness Ra (Ra 1 ) of the first surface: 2 nm, maximum protrusion on the first surface as a base material Height Rp (Rp 1 ): 15 nm, arithmetic average roughness Ra (Ra 2 ): 2 nm of the second surface, maximum protrusion height Rp (Rp 2 ): 15 nm of the second surface were prepared.
- a polyethylene terephthalate film trade name “Lumirror U48”, manufactured by Toray Industries, Inc., thickness: 38 ⁇ m, arithmetic average roughness Ra (Ra 1 ) of the first surface: 2 nm, maximum protrusion on the first surface as a base material Height Rp (Rp 1 ): 15 nm, arithmetic average roughness Ra (Ra 2 ): 2
- a release agent layer (thickness: 1 ⁇ m) was formed by light quantity: 300 mJ / cm 2 ) to obtain a release film for forming a green sheet.
- Examples 2 to 7 and Comparative Examples 1 to 5 A release agent layer-forming material was obtained in the same manner as in Example 1 except that each material was blended according to the composition shown in Table 1. Further, a release film for forming a green sheet was produced in the same manner as in Example 1 except that the obtained release agent layer forming material was used.
- a release film is cut into a size of 100 mm ⁇ 100 mm, and two or more of the same release films are stacked. Then, a load was applied so as to be 10 kg / m 2, and the presence or absence of blocking was confirmed visually under a fluorescent lamp on the peeled film superposed after 5 days. And antiblocking property was evaluated in accordance with the following criteria. A: Adhesion between film surfaces does not occur. B: Sticking of film surfaces occurs.
- the surface roughness (arithmetic average roughness Ra 0 and maximum protrusion height Rp 0 , unit: nm) of the release agent layer of the release film was determined as the optical interference type surface roughness manufactured by Veeco. The measurement was performed in a PSI mode using a total meter “WYKO-1100” at a lens magnification of 50 times.
- Elastic modulus of release agent layer Using a nanoindenter (trade name “Nano Indenter SA4” manufactured by MTS), the maximum indentation depth of the indenter is 100 nm, the strain rate is 0.05 sec ⁇ 1 , the displacement amplitude is 2 nm, and the vibration frequency. A nanoindentation test was performed under the condition of 45 Hz, and the coating elastic modulus of the release film was measured.
- the release film for forming a green sheet of the present invention can be suitably used as a technique for forming a ceramic green sheet.
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Abstract
Description
また、剥離フィルムを用いてグリーンシートを製造する場合、剥離フィルムの表面の凹凸がグリーンシートに転写されることで、グリーンシートの表面にピンホールが生じるなどの問題があった。そこで、剥離フィルムには、表面の凹凸が少ないという平滑性が求められている。一方で、近年のセラミックコンデンサの小型化、高密度化に伴って、グリーンシートの更なる薄膜化が求められている。そして、グリーンシートの更なる薄膜化により、剥離フィルムには、平滑性の更なる向上が求められている。
剥離フィルムのアンチブロッキング性を向上させる技術として、例えば、特許文献1には、ポリエステルフィルムの少なくとも片面に、不活性微粒子を含有する離形層を設けた離形フィルムが記載されている。この離形フィルムにおいて、離形層表面の十点平均粗さ(Rz)は20~500nmである。
本発明の一態様に係るグリーンシート形成用剥離フィルムにおいては、前記(B)疎水化シリカゾルの塗膜を形成した場合、前記塗膜に対する水の接触角が100°以上であることが好ましい。
本発明の一態様に係るグリーンシート形成用剥離フィルムにおいては、前記剥離剤層の平均厚さが、0.2μm以上2μm以下であることが好ましい。
本発明の一態様に係るグリーンシート形成用剥離フィルムにおいては、前記剥離剤層の外表面の算術平均粗さRaが8nm以下であり、かつ、前記剥離剤層の外表面の最大突起高さRpが50nm以下であることが好ましい。
本実施形態に係る基材11は、第1の面11Aと第2の面11Bとを有する。
基材11を構成する材料としては、特に限定されず、例えば、ポリエステル樹脂(ポリブチレンテレフタレート樹脂、ポリエチレンテレフタレート樹脂およびポリエチレンナフタレート樹脂など)、ポリオレフィン樹脂(ポリプロピレン樹脂およびポリメチルペンテン樹脂など)、およびポリカーボネートなどのプラスチックからなるフィルムなどが挙げられる。基材11は、単層フィルムであってもよく、同種または異種の2層以上の多層フィルムであってもよい。これらの中でも、加工時または使用時などにおいて、埃などが発生しにくいという観点から、ポリエステルフィルムが好ましく、二軸延伸ポリエチレンテレフタレートフィルムがより好ましい。ポリエステルフィルムを用いて製造した剥離フィルム1を使用して、グリーンシートを製造する場合には、埃などによるセラミックスラリーの塗工不良などを効果的に防止できる。
高平滑グレードの場合、基材11の第1の面11Aの最大突起高さRp(Rp1)は、10nm以上500nm以下であることが好ましく、15nm以上350nm以下であることがより好ましい。これにより、後述するように、基材11の第1の面11A上には、第1の面11Aの凹凸を埋めて平滑化された剥離剤層12が形成される。そのため、最大突起高さRp1が前記範囲内であれば、剥離剤層の外表面12Aの平滑化作用が特に顕著となる。
このように高平滑グレードの基材を使用することにより、剥離フィルム1とこれに製膜されたセラミックグリーンシートが巻き取られても、塗布表面に接触する剥離フィルム1の裏面側(第2の面11B側)が平滑であるため、セラミックグリーンシートが押圧されて受けるダメージが無くなり、セラミックコンデンサの品質が向上する。
なお、汎用グレードの場合、基材11の第1の面11Aの算術平均粗さRa(Ra1)は、通常、5nm以上80nm以下であり、基材11の第1の面11Aの最大突起高さRp(Rp1)は、通常、100nm以上700nm以下である。また、汎用グレードの場合、基材11の第2の面11Bの算術平均粗さRa(Ra2)は、通常、5nm以上80nm以下であり、基材11の第2の面11Bの最大突起高さRp(Rp2)は、通常、100以上700nm以下である。
本実施形態に係る剥離剤層12は、基材11の第1の面11A上に設けられている。剥離剤層12は、剥離剤形成用材料の硬化物からなる。そして、本実施形態では、(A)エネルギー線硬化性化合物を用いるので、剥離剤層12は、剥離剤層形成用材料に活性エネルギー線を照射して硬化することにより形成される。この剥離剤層12は、剥離フィルム1に平滑性、剥離性およびアンチブロッキング性を付与できる。
本実施形態による剥離剤層12であれば、外表面12Aが上記のような高平滑であって、かつ、基材11の第2の面11Bも高平滑である場合であっても、ブロッキングを起こすことはない。
なお、後述する剥離剤層形成用材料は、基材11の第1の面11A上に塗布するに際し、適度な流動性を有している。したがって、かかる剥離剤層形成用材料を用いれば、基材11の第1の面11Aの凹凸を容易に埋め込むことができ、その埋め込んだ状態を保持することができる。その結果、剥離剤層12の基材11と反対の外表面12A側に、基材11の凹凸が影響するのを防ぐことができ、剥離剤層12の外表面12Aを平滑にすることができる。
ここで、本実施形態に係る剥離剤層12を形成するために用いる剥離剤層形成用材料について説明する。
本実施形態に係る剥離剤層形成用材料は、(A)エネルギー線硬化性化合物と、(B)疎水化シリカゾルと、(C)剥離付与成分とを含有するものである。
本実施形態に係る(A)エネルギー線硬化性化合物としては、特に制限はなく、従来公知のものの中から選択できる。(A)エネルギー線硬化性化合物としては、エネルギー線硬化性のモノマー、オリゴマーおよび樹脂、並びにこれらを含む組成物などが挙げられる。
具体例としては、多官能(メタ)アクリレート、ウレタン(メタ)アクリレート、ポリエステル(メタ)アクリレート、ポリエーテル(メタ)アクリレート、シリコーン(メタ)アクリレートなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。
多官能(メタ)アクリレートとしては、1,4-ブタンジオールジ(メタ)アクリレート、1,6-ヘキサンジオールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、エチレングリコールジ(メタ)アクリレート、プロピレングリコールジ(メタ)アクリレート、ヘキサンジオールジ(メタ)アクリレート、トリメチロールエタントリ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート、ペンタエリスリトールテトラ(メタ)アクリレート、ジペンタエリスリトールヘキサ(メタ)アクリレート、グリセロールトリ(メタ)アクリレート、並びに、トリアリル(メタ)アクリレートなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。これらの中でも、剥離剤層12に適度な堅硬性を付与できることから、ペンタエリスリトールテトラ(メタ)アクリレートまたはジペンタエリスリトールヘキサ(メタ)アクリレートを用いることがより好ましい。
また、多官能(メタ)アクリレートとしては、官能基を含有する多官能(メタ)アクリレートであってもよい。使用される官能基としては水酸基が好ましく、(B)成分の疎水化シリカゾルの剥離剤層形成用材料中での分散性および形成された剥離剤層12における遍在性を最適化させることができる。水酸基含有アクリル系化合物の具体例としては、ペンタエリスリトールトリ(メタ)アクリレート、ジペンタエリスリトールトリ(メタ)アクリレート、ジペンタエリスリトールテトラ(メタ)アクリレート、ジペンタエリスリトールペンタ(メタ)アクリレート、トリメチロールプロパンジ(メタ)アクリレート、およびペンタエリスリトールジ(メタ)アクリレートなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。これらの中でも、剥離剤層12に適度な堅硬性を付与できることから、ペンタエリスリトールトリ(メタ)アクリレートを用いることがより好ましい。また、多官能(メタ)アクリレートが官能基を有していれば架橋剤による架橋によって、剥離剤層12をエネルギー線と加熱の2系統の手段で硬化することができ、硬化の程度を所望のレベルとすることができる。
EO(エチレンオキサイド)またはPO(プロピレンオキサイド)付加型の多官能(メタ)アクリレートとは、EOまたはPO付加型の多価アルコールをアクリル酸でエステル化することによって得られる化合物である。具体的には、EOまたはPO変性グリセロールトリアクリレート、EOまたはPO変性トリメチロールプロパンアクリレート、EOまたはPO変性ペンタエリスリトールテトラアクリレート、並びに、EOまたはPO変性ジペンタエリスリトールヘキサアクリレートなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。これらの中でも、剥離剤層12に適度な柔軟性を付与することで剥離剤層12のクラックまたは割れを防止できることから、EOまたはPO変性ジペンタエリスリトールヘキサアクリレート、EOまたはPO変性トリメチロールプロパンテトラアクリレートを用いても良い。
本実施形態に係る(B)疎水化シリカゾルの種類としては、アルコキシシラン化合物およびクロロシラン化合物などのシリカ微粒子のゾルが挙げられる。(B)疎水化シリカゾルにより、剥離剤層12にアンチブロッキング性を付与できる。
アルコキシシラン化合物としては、加水分解性のアルコキシル基を有するケイ素化合物であれば、特に限定されず、例えば一般式(1)で表される化合物が挙げられる。
R1 nSi(OR2)4-n ・・・(1)
前記一般式において、R1は、水素原子または非加水分解性基を示す。非加水分解性基としては、アルキル基、置換アルキル基(置換基:ハロゲン原子、エポキシ原子、(メタ)アクリロイルオキシ基など)、アルケニル基、アリール基、およびアラルキル基などが挙げられる。R2は、低級アルキル基(炭素数が1から10(好ましくは、炭素数が1から4)のアルキル基)を示す。nは、0から2の整数であり、R1およびOR2がそれぞれ複数である場合、複数のR1は同一でも異なっていてもよく、また複数のOR2は、同一でも異なっていてもよい。
一方、nが1または2で、R1が非加水分解性基である化合物では、非加水分解性基を有するので、部分または完全加水分解により、ポリオルガノシロキサン系硬化物が得られる。
クロロシラン化合物としては、エチルジクロロシラン、エチルトリクロロシラン、ジメチルジクロロシラン、トリクロロシラン、トリメチルクロロシラン、ジメチルジクロロシラン、およびメチルトリクロロシランなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。
かかる有機溶媒に特に制限はなく、メタノール、エタノール、イソプロパノール、エチレングリコール、n-プロピルセロソルブ、メチルエチルケトン、メチルイソブチルケトン、ジメチルアセトアミド、プロピレングリコールモノメチルエーテル、シクロヘキサン、ベンゼン、およびトルエンなどが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。これらの中でも、比較的沸点が高いという観点から、メチルイソブチルケトン、プロピレングリコールモノメチルエーテルがより好ましい。
ここで、表面改質剤としては、シリカ粒子表面上のシラノール基に対して、反応可能な官能基と、疎水基とを併せ持つシランカップリング剤が挙げられる。
(B)疎水化シリカゾルの市販品としては、例えば、CIKナノテック社製SIRPGM15WT%-E26などが挙げられる。
より具体的には、(B)疎水化シリカゾルの塗膜を形成した場合に、この塗膜に対する水の接触角は、100°以上であることが好ましい。
すなわち、シリカゾルの塗膜に対する水の接触角が100°以上の値であれば、シリカゾルの表面が疎水性であると判断できる。
ここで、図2に(B)疎水化シリカゾルの偏析状態を概念的に説明するための模式図を示す。
本実施形態に係る剥離剤層形成用材料を用いて塗膜を形成した場合、図2に示すように、疎水化シリカゾルPは、剥離剤層12内で、剥離剤層12の外表面12Aに多く存在し、基材11の第1の面11A付近および剥離剤層12内に存在する割合は低いことが理解される。
したがって、少量の疎水化シリカゾルの添加で、剥離剤層12の表面に、適度な表面粗さを付与できる。そのため、剥離フィルム1同士が重なって時間が経過した場合であっても、基材11の第2の面11Bと、剥離剤層12とのブロッキングが生じることを防止することができる。
すなわち、比較的少量の添加で所定のアンチブロッキング性の効果を発揮可能であるため、平滑性に優れる剥離剤層を形成できることが理解される。
なお、(B)疎水化シリカゾルの塗膜を形成した場合に、この塗膜に対する水の接触角は、100°以上130°以下であることがより好ましい。
一方、シリカゾルの塗膜を形成した場合に、この塗膜に対する水の接触角が100°未満の値となり、シリカゾルの親水性が高くなると、シリカゾルは、剥離剤層12の外表面12Aに偏析することなく、剥離剤層12内全体に分散した状態で存在することが確認されている。
したがって、剥離剤層12にアンチブロッキング性を付与できないことが理解される。
なお、シリカゾルの塗膜を形成した場合に、この塗膜に対する水の接触角を測定する方法は、実施例1において、具体的に説明する。
したがって、(B)疎水化シリカゾルの平均粒子径は、10nm以上50nm以下であることがより好ましく、15nm以上40nm以下であることがさらに好ましい。
なお、(B)疎水化シリカゾルの平均粒子径は、レーザー回折錯乱式粒度分布測定装置を用いて求めた粒度分布における積算値50%での粒径(メジアン径D50)である。
本実施形態に係る(C)剥離付与成分としては、例えば、シリコーン化合物、フッ素化合物、及び長鎖アルキル変性化合物等が挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。特に、(C)剥離付与成分としては、シリコーン化合物が好ましく、直鎖状または分岐状の分子鎖を有するポリオルガノシロキサンが挙げられる。(C)剥離付与成分により、剥離剤層12の剥離性を付与できる。また、ポリオルガノシロキサンは、分子鎖の末端および側鎖の少なくともいずれかに、(メタ)アクリロイル基、ビニル基、水酸基、チオール基、およびマレイミド基よりなる群から選択される少なくとも1種を有する反応性官能基を有することが好ましい。また、ポリオルガノシロキサンは、前記反応性官能基が、直接または2価の連結基を介して、前記分子鎖中のケイ素原子と結合したものであることがより好ましい。前記反応性官能基は、1分子中に少なくとも1個有していればよい。
また、2価の連結基としては、例えば、アルキレン基、アルキレンオキシ基、オキシ基、イミノ基、カルボニル基およびそれらを組み合わせた2価の連結基などが挙げられる。
2価の連結基の炭素数は、1から30であることが好ましく、1から10であることがより好ましい。
また、ポリオルガノシロキサンは、必要に応じて2種以上を組み合わせて使用することができる。
1価の炭化水素基としては、炭素数が1から12のものが好ましく、炭素数が1から10のものがより好ましい。
1価の炭化水素基としては、アルキル基(メチル基、エチル基およびプロピル基など)、およびアリール基(フェニル基、トリル基など)などが挙げられる。
また、1価の炭化水素基としては、1価の炭化水素基のうちの80モル%以上がメチル基であることが好ましい。これにより、剥離剤層12の剥離性を特に優れたものとすることができる。
剥離剤層形成用材料を硬化させるために、剥離剤層形成用材料は、(D)光重合開始剤を含んでいてもよい。(D)光重合開始剤を含有させることにより、剥離剤層形成用材料に対して活性エネルギー線を照射した際に、効率的に剥離剤層12を形成することができる。ここで、光重合開始剤とは、紫外線などの活性エネルギー線の照射により、ラジカル種を発生させる化合物をいう。
その他の成分を用いる場合、その含有量は、固形分換算で、前記(A)エネルギー線硬化性化合物100質量部に対して、0.01質量部以上5質量部以下であることが好ましく、0.02質量部以上3質量部以下であることがより好ましく、0.05質量部以上2質量部以下であることが特に好ましい。
本実施形態に係る溶剤としては、例えば、メチルアルコール、エチルアルコール、n-プロピルアルコール、イソプロピルアルコール、n-ブチルアルコール、イソブチルアルコール、ペンチルアルコール、エチルセロソルブ、ベンゼン、トルエン、キシレン、エチルベンゼン、シクロヘキサン、エチルシクロヘキサン、酢酸エチル、酢酸ブチル、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン、テトラヒドロフラン、プロピレングリコールモノメチルエーテル、および水などが挙げられる。これらは一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。
次に、前述した本実施形態の剥離フィルム1を製造する方法について説明する。
本実施形態の剥離フィルム1は、基材11を準備する基材準備工程と、剥離剤層形成用材料を塗布して乾燥させることで塗布層を形成する塗布層形成工程と、塗布層に、活性エネルギー線を照射して硬化させることにより剥離剤層12を形成する剥離剤層形成工程とを備える方法で製造できる。
基材11の第1の面11Aに、表面処理を施すことができる。これにより、基材11と、基材11の第1の面11A側に設けられる剥離剤層12との密着性を特に優れたものとすることができる。
前述の剥離剤層形成用材料を用いれば、基材11の第1の面11Aの凹凸を埋めることができる。その結果、剥離剤層12の外表面12Aを平滑にすることができる。
剥離剤層形成用材料を乾燥する方法としては、特に限定されないが、例えば、熱風乾燥炉などで乾燥する方法などが挙げられる。
この工程において、前記塗布層形成工程にて、基材11の第1の面11Aの凹凸を的確に埋め込んだ塗布層を、その外表面12Aの平滑性を保持したまま硬化する。その結果、外表面12Aが十分に平滑な剥離剤層12を得ることができる。また、剥離剤層形成用材料が、前述したような構成成分を含むことにより、適度の導電性を有する剥離剤層12を得ることができる。
次に、前述した本実施形態の剥離フィルム1を使用する方法について説明する。
本実施形態の剥離フィルム1を用いてセラミックコンデンサを製造できる。セラミックコンデンサの製造方法としては、例えば、剥離フィルム1の剥離剤層12の表面に、セラミック粉末分散スラリーを塗布し、乾燥してグリーンシートを形成した後、剥離フィルム1から剥離したグリーンシートを積層し、焼成して得られたセラミックシートに電極を形成する方法が挙げられる。本実施形態の剥離フィルム1は、ブロッキングを起こしにくいため、剥離剤層12の外表面12Aおよび基材11の第2の面11Bの両方を高平滑にできる。これにより、本実施形態の剥離フィルム1を用いて形成されたグリーンシートによりセラミックコンデンサを形成すれば、短絡による不具合の発生が防止された信頼性の高いセラミックコンデンサを得ることができる。
本実施形態によれば、次のような作用効果を奏することができる。
(1)(A)エネルギー線硬化性化合物を含有する剥離剤層形成用材料は、基材11の第1の面11Aの凹凸を容易に埋め込むことができ、その埋め込んだ状態を保持することができる。その結果、剥離剤層12の基材11と反対の外表面12A側に、基材11の凹凸が影響するのを防ぐことができ、剥離剤層12の外表面12Aを平滑にすることができる。
(2)(B)疎水化シリカゾルによれば、少ない含有量でも、剥離剤層12に十分なアンチブロッキング性を付与できる。そして、(B)疎水化シリカゾルを用いても、剥離剤層12の外表面12Aの平滑性を維持できる。さらに、(C)剥離付与成分により、剥離剤層12に剥離性も付与できる。
本実施形態に係るグリーンシート形成用剥離フィルムの一例として、基材と、前記基材の片面に設けられた剥離剤層とを備え、前記剥離剤層は、(A)エネルギー線硬化性化合物としての水酸基含有アクリル系化合物と、(B)疎水化シリカゾルと、(C)剥離付与成分としてのシリコーン化合物と、を含有する剥離剤形成用材料の硬化物からなる、グリーンシート形成用剥離フィルムが挙げられる。
本実施形態に係るグリーンシート形成用剥離フィルムの一例として、基材と、前記基材の片面に設けられた剥離剤層とを備え、前記剥離剤層は、(A)エネルギー線硬化性化合物としての水酸基含有アクリル系化合物と、(B)疎水化シリカゾルと、(C)剥離付与成分としてのシリコーン化合物と、(D)光重合開始剤と、を含有する剥離剤形成用材料の硬化物からなる、グリーンシート形成用剥離フィルムが挙げられる。
本発明は前述の実施形態に限定されるものではなく、本発明の目的を達成できる範囲での変形、改良などは本発明に含まれるものである。
例えば、前述の実施形態では、基材11は単層構造のものとして説明したが、これに限定されない。基材11は、同種または異種の2層以上の多層構造をなすものであってもよい。また、剥離剤層12についても同様に、単層構造のものとして説明したが、これに限定されない。剥離剤層12についても、同種または異種の2層以上の多層構造をなすものであってもよい。
また、例えば、前述した実施形態では、基材11の第1の面11Aに剥離剤層12を設けたグリーンシート形成用剥離フィルムについて説明したが、これに限定されない。基材11の第2の面11B側に剥離剤層12を設けてもよい。
((A)成分)
エネルギー線硬化性化合物:ペンタエリスリトールトリアクリレート、商品名「NKエステル A-TMM-3L」、新中村化学工業社製、固形分100質量%
((B)成分)
シリカゾルA:疎水化シリカゾル、平均粒子径30nm、商品名「SIRPGM15WT%-E26」、CIKナノテック社製
シリカゾルB:疎水化シリカゾル、平均粒子径30nm、商品名「SIRMIBK15WT%-E83」、CIKナノテック社製
(他の成分)
シリカゾルC:シリカゾル、平均粒子径100nm、商品名「SIRMIBK15WT%-K18」、CIKナノテック社製
シリカゾルD:シリカゾル、平均粒子径30nm、商品名「OSCAL-1632」、日揮触媒化成社製
シリカゾルE:シリカゾル、平均粒子径15nm、商品名「MIBK-ST」、日産化学工業社製
シリカゾルF:シリカゾル平均粒子径100nm、商品名「SIRMIBK-E65」、CIKナノテック社製
((C)成分)
剥離付与成分:商品名「SH-28」、東レ・ダウコーニング社製
((D)成分)
光重合開始剤:商品名「イルガキュア184」、BASF社製
先ず、基材としてのポリエチレンテレフタレートフィルム(商品名「ルミラーU48」、東レ社製、厚さ:38μm、第1の面の算術平均粗さRa(Ra1):2nm、第1の面の最大突起高さRp(Rp1):15nm、第2の面の算術平均粗さRa(Ra2):2nm、第2の面の最大突起高さRp(Rp2):15nm)を準備した。
次に、エネルギー線硬化性化合物100質量部と、シリカゾルA0.4質量部と、剥離付与成分5質量部と、光重合開始剤5質量部と、を混合し、プロピレングリコールモノメチルエーテルで希釈して、固形分15質量%の剥離剤層形成用材料を得た。
次いで、得られた剥離剤層形成用材料をマイヤーバーで基材の第1の面上に塗布して、70℃で1分間乾燥させた後、高圧水銀ランプを用いて、紫外線を照射(積算光量:300mJ/cm2)して剥離剤層(厚さ:1μm)を形成し、グリーンシート形成用剥離フィルムを得た。
表1に示す組成に従い各材料を配合した以外は実施例1と同様にして、剥離剤層形成用材料を得た。
また、得られた剥離剤層形成用材料を用いた以外は実施例1と同様にして、グリーンシート形成用剥離フィルムを作製した。
シリカゾルの評価(シリカゾルの接触角)、および、剥離フィルムの評価(アンチブロッキング性、剥離剤層の表面粗さ、および剥離剤層の弾性率)を以下のような方法で行った。得られた結果を表1に示す。
(1)シリカゾルの接触角
実施例および比較例で用いたシリカゾルを用いて、平坦なガラス基板上にシリカゾル塗膜を形成した。そして、ガラス基板を静置し、ガラス基板の傾きを0度としたときに、水滴2μLを滴下し、液滴が静止したところで、Youngの式にて水接触角を求めた。
(2)アンチブロッキング性
剥離フィルムを100mm×100mmの大きさに切り出し、2枚以上の同じ剥離フィルムを重ねる。そこに、10kg/m2となるように荷重をかけ、5日後に重ね合わせた
剥離フィルムを蛍光灯下、目視にてブロッキングの有無を確認した。そして、以下の基準に従って、アンチブロッキング性を評価した。
A:フィルム面同士の貼り付きが生じていない。
B:フィルム面同士の貼り付きが生じている。
剥離フィルムの剥離剤層の表面粗さ(算術平均粗さRa0および最大突起高さRp0、単位:nm)を、Veeco社製の光干渉式表面粗さ計「WYKO-1100」を用いて、PSIモードで、レンズ倍率50倍の条件で、測定した。
(4)剥離剤層の弾性率
ナノインデンター(MTS社製、商品名「Nano Indenter SA4」)を用い、圧子の最大押込み深さ100nm、歪速度0.05sec-1、変位振幅2nm、振動周波数45Hzの条件にてナノインデンテーション試験を行い、上記剥離フィルムの被膜弾性率を測定した。
Claims (5)
- グリーンシートの形成に用いられるグリーンシート形成用剥離フィルムであって、
基材と、前記基材の片面に設けられた剥離剤層とを備え、
前記剥離剤層は、(A)エネルギー線硬化性化合物と、(B)疎水化シリカゾルと、(C)剥離付与成分と、を含有する剥離剤形成用材料の硬化物からなる
ことを特徴とするグリーンシート形成用剥離フィルム。 - 請求項1に記載のグリーンシート形成用剥離フィルムにおいて、
前記(B)疎水化シリカゾルの平均粒子径が、10nm以上100nm以下である
ことを特徴とするグリーンシート形成用剥離フィルム。 - 請求項1または請求項2に記載のグリーンシート形成用剥離フィルムにおいて、
前記(B)疎水化シリカゾルの塗膜を形成した場合、前記塗膜に対する水の接触角が100°以上である
ことを特徴とするグリーンシート形成用剥離フィルム。 - 請求項1から請求項3のいずれか1項に記載のグリーンシート形成用剥離フィルムにおいて、
前記剥離剤層の平均厚さが、0.2μm以上2μm以下である
ことを特徴とするグリーンシート形成用剥離フィルム。 - 請求項1から請求項4のいずれか1項に記載のグリーンシート形成用剥離フィルムにおいて、
前記剥離剤層の外表面の算術平均粗さRaが8nm以下であり、かつ、前記剥離剤層の外表面の最大突起高さRpが50nm以下である
ことを特徴とするグリーンシート形成用剥離フィルム。
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