WO2019159852A1 - 合わせガラス中間膜または太陽電池封止材用樹脂組成物、合わせガラス中間膜、合わせガラス、太陽電池封止材および太陽電池モジュール - Google Patents
合わせガラス中間膜または太陽電池封止材用樹脂組成物、合わせガラス中間膜、合わせガラス、太陽電池封止材および太陽電池モジュール Download PDFInfo
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- WO2019159852A1 WO2019159852A1 PCT/JP2019/004704 JP2019004704W WO2019159852A1 WO 2019159852 A1 WO2019159852 A1 WO 2019159852A1 JP 2019004704 W JP2019004704 W JP 2019004704W WO 2019159852 A1 WO2019159852 A1 WO 2019159852A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- resin composition
- laminated glass
- ethylene
- solar cell
- ester copolymer
- Prior art date
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- 239000005340 laminated glass Substances 0.000 title claims abstract description 118
- 239000011342 resin composition Substances 0.000 title claims abstract description 111
- 239000011229 interlayer Substances 0.000 title claims abstract description 42
- 239000003566 sealing material Substances 0.000 title abstract description 31
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 103
- 239000005977 Ethylene Substances 0.000 claims abstract description 103
- 229920001577 copolymer Polymers 0.000 claims abstract description 89
- 238000005259 measurement Methods 0.000 claims abstract description 37
- 238000004132 cross linking Methods 0.000 claims abstract description 32
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims description 36
- 239000011521 glass Substances 0.000 claims description 25
- 239000008393 encapsulating agent Substances 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 9
- 150000001451 organic peroxides Chemical class 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 5
- 229920001567 vinyl ester resin Polymers 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 description 23
- 238000004519 manufacturing process Methods 0.000 description 20
- 239000000758 substrate Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- -1 acryl Chemical group 0.000 description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 13
- 239000005357 flat glass Substances 0.000 description 11
- 230000001681 protective effect Effects 0.000 description 10
- DLSMLZRPNPCXGY-UHFFFAOYSA-N tert-butylperoxy 2-ethylhexyl carbonate Chemical compound CCCCC(CC)COC(=O)OOOC(C)(C)C DLSMLZRPNPCXGY-UHFFFAOYSA-N 0.000 description 9
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 7
- 239000003963 antioxidant agent Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000004611 light stabiliser Substances 0.000 description 7
- 239000006087 Silane Coupling Agent Substances 0.000 description 6
- 238000011074 autoclave method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 5
- 239000011324 bead Substances 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 150000001733 carboxylic acid esters Chemical class 0.000 description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 2
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 2
- ZQBAKBUEJOMQEX-UHFFFAOYSA-N phenyl salicylate Chemical compound OC1=CC=CC=C1C(=O)OC1=CC=CC=C1 ZQBAKBUEJOMQEX-UHFFFAOYSA-N 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- KDGNCLDCOVTOCS-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy propan-2-yl carbonate Chemical compound CC(C)OC(=O)OOC(C)(C)C KDGNCLDCOVTOCS-UHFFFAOYSA-N 0.000 description 1
- VRWOEFJNMPHSTD-UHFFFAOYSA-N (2-octoxyphenyl)-phenylmethanone Chemical compound CCCCCCCCOC1=CC=CC=C1C(=O)C1=CC=CC=C1 VRWOEFJNMPHSTD-UHFFFAOYSA-N 0.000 description 1
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OXYKVVLTXXXVRT-UHFFFAOYSA-N (4-chlorobenzoyl) 4-chlorobenzenecarboperoxoate Chemical compound C1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1 OXYKVVLTXXXVRT-UHFFFAOYSA-N 0.000 description 1
- VNFXPOAMRORRJJ-UHFFFAOYSA-N (4-octylphenyl) 2-hydroxybenzoate Chemical compound C1=CC(CCCCCCCC)=CC=C1OC(=O)C1=CC=CC=C1O VNFXPOAMRORRJJ-UHFFFAOYSA-N 0.000 description 1
- 229920003067 (meth)acrylic acid ester copolymer Polymers 0.000 description 1
- NALFRYPTRXKZPN-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane Chemical compound CC1CC(C)(C)CC(OOC(C)(C)C)(OOC(C)(C)C)C1 NALFRYPTRXKZPN-UHFFFAOYSA-N 0.000 description 1
- HSLFISVKRDQEBY-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)cyclohexane Chemical compound CC(C)(C)OOC1(OOC(C)(C)C)CCCCC1 HSLFISVKRDQEBY-UHFFFAOYSA-N 0.000 description 1
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- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 description 1
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- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- ZMWRRFHBXARRRT-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4,6-bis(2-methylbutan-2-yl)phenol Chemical compound CCC(C)(C)C1=CC(C(C)(C)CC)=CC(N2N=C3C=CC=CC3=N2)=C1O ZMWRRFHBXARRRT-UHFFFAOYSA-N 0.000 description 1
- IYAZLDLPUNDVAG-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4-(2,4,4-trimethylpentan-2-yl)phenol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 IYAZLDLPUNDVAG-UHFFFAOYSA-N 0.000 description 1
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- LZMNXXQIQIHFGC-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propyl 2-methylprop-2-enoate Chemical compound CO[Si](C)(OC)CCCOC(=O)C(C)=C LZMNXXQIQIHFGC-UHFFFAOYSA-N 0.000 description 1
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 description 1
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
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- KBQVDAIIQCXKPI-UHFFFAOYSA-N 3-trimethoxysilylpropyl prop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C=C KBQVDAIIQCXKPI-UHFFFAOYSA-N 0.000 description 1
- FETUUKHOLDNMQO-UHFFFAOYSA-N 6-benzoyl-1-hydroxy-3-methoxycyclohexa-2,4-diene-1-carboxylic acid Chemical compound C1=CC(OC)=CC(O)(C(O)=O)C1C(=O)C1=CC=CC=C1 FETUUKHOLDNMQO-UHFFFAOYSA-N 0.000 description 1
- QLZINFDMOXMCCJ-UHFFFAOYSA-N 7-(7-hydroxyheptylperoxy)heptan-1-ol Chemical compound OCCCCCCCOOCCCCCCCO QLZINFDMOXMCCJ-UHFFFAOYSA-N 0.000 description 1
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- 229920000178 Acrylic resin Polymers 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical group [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- XLYMOEINVGRTEX-ARJAWSKDSA-N Ethyl hydrogen fumarate Chemical compound CCOC(=O)\C=C/C(O)=O XLYMOEINVGRTEX-ARJAWSKDSA-N 0.000 description 1
- 101000969770 Homo sapiens Myelin protein zero-like protein 2 Proteins 0.000 description 1
- 102100021272 Myelin protein zero-like protein 2 Human genes 0.000 description 1
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- 239000004793 Polystyrene Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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- MOVRNJGDXREIBM-UHFFFAOYSA-N aid-1 Chemical compound O=C1NC(=O)C(C)=CN1C1OC(COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C(NC(=O)C(C)=C2)=O)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)COP(O)(=O)OC2C(OC(C2)N2C3=C(C(NC(N)=N3)=O)N=C2)CO)C(O)C1 MOVRNJGDXREIBM-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
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- 125000003277 amino group Chemical group 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- ZPOLOEWJWXZUSP-AATRIKPKSA-N bis(prop-2-enyl) (e)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C\C(=O)OCC=C ZPOLOEWJWXZUSP-AATRIKPKSA-N 0.000 description 1
- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 150000001649 bromium compounds Chemical class 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- RPPBZEBXAAZZJH-UHFFFAOYSA-N cadmium telluride Chemical compound [Te]=[Cd] RPPBZEBXAAZZJH-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 229910052718 tin Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
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Images
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- 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 laminated glass interlayer film or a resin composition for a solar cell sealing material, a laminated glass interlayer film, a laminated glass, a solar cell sealing material, and a solar cell module.
- films composed of an ethylene / unsaturated ester copolymer and a crosslinking agent are known.
- Patent Document 1 International Publication No. 2014/208756
- Patent Document 2 Japanese Patent Application Laid-Open No. 2007-331952.
- Patent Document 1 discloses a laminate-forming sheet for use in a laminate production method including a step of applying pressure using a nip roll, comprising a composition containing an ethylene-vinyl acetate copolymer and a crosslinking agent,
- the vinyl acetate content of the ethylene-vinyl acetate copolymer is 30% by mass or more based on the ethylene-vinyl acetate copolymer, and the melt flow rate of the ethylene-vinyl acetate copolymer (JIS-K7210).
- JIS-K7210 melt flow rate of the ethylene-vinyl acetate copolymer
- Patent Document 2 discloses an interlayer film for laminated glass comprising an organic peroxide in an ethylene / vinyl acetate copolymer, wherein the organic peroxide is represented by a specific chemical formula and has a 10-hour half-life.
- An interlayer film for laminated glass is described which is a peroxyketal having a temperature of 100 ° C. or lower.
- a laminated glass interlayer film composed of an ethylene / unsaturated ester copolymer and a crosslinking agent has optical properties and adhesiveness under high humidity (hereinafter referred to as moisture-resistant adhesion).
- moisture-resistant adhesion a laminated glass interlayer film composed of an ethylene / unsaturated ester copolymer and a crosslinking agent.
- the present inventors have room for improvement in terms of improving optical properties and moisture-resistant adhesion in a well-balanced manner for a laminated glass intermediate film composed of a conventional ethylene / unsaturated ester copolymer and a crosslinking agent. Found that there is.
- the solar cell sealing material also had the same problem as the laminated glass intermediate film.
- the present invention has been made in view of the above circumstances, and provides a laminated glass interlayer film or a resin composition for a solar cell encapsulant that is excellent in performance balance between optical properties and moisture-resistant adhesion.
- the inventors of the present invention have made extensive studies in order to achieve the above problems. As a result, it has been clarified that the resin composition having a high crosslinking rate tends to be inferior in moisture-resistant adhesion and air bubble removal during the production of laminated glass. On the other hand, it has been found that by reducing the crosslinking rate of the resin composition, the moisture-resistant adhesion is improved while keeping the optical properties of the resulting crosslinked film good. As a result of further investigation based on the above knowledge, the present inventors have found that the torque value after 60 minutes from the start of measurement when the torque of the resin composition was measured over time at 130 ° C. using a movable direometer.
- T 100 [dN ⁇ m] a torque value of 10% of T 100 is set to T 10
- a torque value of 50% of T 100 is set to T 50
- a minimum value of torque being measured is set to T min, and measurement is started.
- the laminated glass interlayer film or the solar cell encapsulating material As a result of intensive studies based on these findings, as a result of adjusting the crosslinking rate represented by (T 50 -T 10 ) / (YX) to a specific range, the laminated glass interlayer film or the solar cell encapsulating material The present inventors have found that the performance balance between optical properties and moisture-resistant adhesion can be effectively improved, and have completed the present invention.
- the following laminated glass interlayer film or resin composition for solar cell sealing material, laminated glass interlayer film, laminated glass, solar cell sealing material, and solar cell module are provided.
- a resin composition for laminated glass interlayer film or solar cell encapsulant An ethylene / unsaturated ester copolymer (A) and a crosslinking agent (B),
- the torque value 60 minutes after the start of measurement was T 100 [dN ⁇ m]
- 10% of T 100 and the torque value T 10 50% of the torque value of the T 100 and T 50, the minimum value of the torque being measured and T min
- the time from the start of measurement reaches T 10 and X [min]
- measurement start When the time from T to T 50 is Y [minutes]
- T min is a resin composition having a value exceeding 0.01 dN ⁇ m / min and not more than 0.25 dN ⁇ m / min.
- MFR melt flow rate
- a resin composition comprising the ethylene / unsaturated ester copolymer (A) comprising at least one polymer selected from an ethylene / vinyl ester copolymer and an ethylene / unsaturated carboxylic acid ester copolymer.
- the obtained film is sandwiched between glass plates of 120 mm ⁇ 75 mm ⁇ 3.2 mm, and heat-pressed with a vacuum laminator at 130 ° C. and 1 atm for 60 minutes to obtain a laminated glass.
- the protruding length of the resin composition protruding from the end portion of the obtained laminated glass in the direction perpendicular to the end surface of the laminated glass is measured.
- the resin composition which is a sheet form or a film form.
- the present invention it is possible to provide a laminated glass interlayer film or a resin composition for a solar cell encapsulant that has an excellent performance balance between optical properties and moisture-resistant adhesion.
- FIG. 1 is a diagram schematically showing a relationship between a torque value obtained by measurement using a movable direometer and measurement time.
- FIG. 2 is a cross-sectional view schematically showing an example of the structure of the laminated glass 10 according to the embodiment of the present invention.
- the resin composition (P) according to the present embodiment is a resin composition used for forming the laminated glass intermediate film 11 or the solar cell sealing material, and includes an ethylene / unsaturated ester copolymer (A) and The torque value after 60 minutes from the start of measurement when the torque of the resin composition was measured with time at 130 ° C.
- the measurement of the torque values (T 10 , T 50 , T 100 ) of the resin composition (P) according to this embodiment using a movable direometer can be performed according to the following conditions.
- a measuring device for example, a moveable rheometer (product name: MDR-2000P) manufactured by Alpha Technology Co., Ltd. is used, and the melting torque of the resin composition (P) is measured with time at a measurement temperature of 130 ° C. and a frequency of 1.66 Hz. It is possible to measure the torque values (T 10 , T 50 , T 100 ) of the resin composition (P) according to the present embodiment by performing measurement.
- a laminated glass interlayer film composed of an ethylene / unsaturated ester copolymer and a crosslinking agent as described in Patent Documents 1 and 2 has optical properties and high humidity. It became clear that the adhesiveness of was not fully satisfactory. That is, the present inventors have room for improvement in terms of improving optical properties and moisture-resistant adhesion in a well-balanced manner for a laminated glass intermediate film composed of a conventional ethylene / unsaturated ester copolymer and a crosslinking agent. Found that there is. Moreover, the solar cell sealing material also had the same problem as the laminated glass intermediate film.
- the inventors of the present invention have made extensive studies in order to achieve the above problems. As a result, it became clear that the resin composition having a high crosslinking rate tends to be inferior in moisture-resistant adhesion. On the other hand, it has been found that by reducing the crosslinking rate of the resin composition, the moisture-resistant adhesion is improved while keeping the optical properties of the resulting crosslinked film good. As a result of further investigation based on the above knowledge, the present inventors have found that the torque value after 60 minutes from the start of measurement when the torque of the resin composition was measured over time at 130 ° C. using a movable direometer.
- T 100 [dN ⁇ m] a torque value of 10% of T 100 is set to T 10
- a torque value of 50% of T 100 is set to T 50
- a minimum value of torque being measured is set to T min, and measurement is started.
- the crosslinking rate represented by (T 50 -T 10 ) / (YX) As a result of intensive studies based on these findings, as a result of adjusting the crosslinking rate represented by (T 50 -T 10 ) / (YX) to a specific range, the laminated glass interlayer film or the solar cell encapsulating material
- the present inventors have found that the performance balance between optical properties and moisture-resistant adhesion can be effectively improved, and have completed the present invention. That is, in the resin composition (P) according to the present embodiment, the crosslinking rate represented by (T 50 -T 10 ) / (YX) exceeds 0.01 dN ⁇ m / min and is 0.25 dN ⁇ m / min.
- the performance balance of the optical characteristic and moisture-proof adhesiveness of a laminated glass intermediate film or a solar cell sealing material can be made favorable.
- the crosslinking rate represented by (T 50 -T 10 ) / (YX) within the above range, the performance balance between the optical characteristics and the moisture-resistant adhesive property of the laminated glass interlayer film or solar cell encapsulant is improved.
- the resin composition can be cross-linked, by adjusting the cross-linking rate of the resin composition within the above range, the cross-linking of the resin composition proceeds more moderately and at an appropriate rate. When the reaction is in progress, moisture and bubbles contained in the resin composition are easily degassed.
- the amount of bubbles in the resulting crosslinked film can be suppressed, and optical characteristics and moisture-resistant adhesiveness can be suppressed. Is considered to be better.
- the optical characteristics refer to, for example, haze, total light transmittance, and the like.
- the crosslinking rate represented by (T 50 -T 10 ) / (YX) exceeds 0.01 dN ⁇ m / min. From the viewpoint of further improving the mechanical properties and heat resistance, and further suppressing the resin protrusion from the end of the laminated glass or solar cell module, it is preferably 0.02 dN ⁇ m / min or more, More preferably, it is 0.03 dN ⁇ m / min or more. In this embodiment, the crosslinking rate represented by (T 50 -T 10 ) / (YX) is 0.25 dN ⁇ m / min or less.
- it is preferably 0.20 dN ⁇ m / min or less, more preferably 0.17 dN ⁇ m / min or less, and It is particularly preferably 15 dN ⁇ m / min or less.
- the resin composition when the periodically measured torque (P), the lower limit value of the torque value T 100 of 60 minutes after the start of measurement is, for example 1.5dN ⁇ m or more, preferably 1.8 dN ⁇ m or more.
- the upper limit torque value T 100 is, for example, less 12.0dN ⁇ m, preferably not more than 8.0dN ⁇ m, more preferably not more than 6.0dN ⁇ m.
- the present embodiment for example, by appropriately selecting the type of the ethylene / unsaturated ester copolymer (A), the one-hour half-life temperature of the crosslinking agent (B), the content of the crosslinking agent (B), etc. It is possible to control the crosslinking rate indicated by (T 50 -T 10 ) / (YX) of the resin composition (P) according to the embodiment and the torque value T 100 within a desired range.
- Examples of the resin composition (P) include a crosslinking rate represented by (T 50 -T 10 ) / (YX) and an element for setting the torque value T 100 in a desired numerical range. For example, when the MFR of the ethylene / unsaturated ester copolymer (A) is lowered, the one-hour half-life temperature of the crosslinking agent (B) is increased, or the content of the crosslinking agent (B) is reduced, the crosslinking rate is increased. Can be reduced.
- the ethylene / unsaturated ester copolymer (A) is a polymer obtained by copolymerizing ethylene and at least one unsaturated ester.
- Examples of the ethylene / unsaturated ester copolymer (A) include a copolymer containing ethylene and an unsaturated ester.
- the ethylene / unsaturated ester copolymer (A) according to this embodiment may contain at least one polymer selected from ethylene / vinyl ester copolymers and ethylene / unsaturated carboxylic acid ester copolymers. preferable.
- the ethylene / unsaturated ester copolymer (A) may contain a polymerizable monomer other than ethylene and the unsaturated ester, and examples thereof include olefins such as propylene, butene, and hexene. Can do.
- Examples of the ethylene / vinyl ester copolymer according to this embodiment include an ethylene / vinyl acetate copolymer, an ethylene / vinyl propionate copolymer, an ethylene / vinyl butyrate copolymer, and an ethylene / vinyl stearate copolymer. 1 type, or 2 or more types selected from etc. can be used.
- the ethylene / unsaturated carboxylic acid ester copolymer according to this embodiment is a polymer obtained by copolymerizing ethylene and at least one unsaturated carboxylic acid ester. Specifically, a copolymer composed of ethylene and an unsaturated carboxylic acid alkyl ester can be exemplified.
- the unsaturated carboxylic acid in the unsaturated carboxylic acid ester examples include acrylic acid, methacrylic acid, 2-ethylacrylic acid, crotonic acid, maleic acid, fumaric acid, itaconic acid, maleic anhydride, fumaric anhydride, itaconic anhydride , Monomethyl maleate, monoethyl maleate and the like.
- the unsaturated carboxylic acid preferably contains at least one selected from acrylic acid and methacrylic acid from the viewpoints of productivity and hygiene of the ethylene / unsaturated ester copolymer (A).
- These unsaturated carboxylic acids may be used individually by 1 type, and may be used in combination of 2 or more type.
- alkyl moiety in the unsaturated carboxylic acid alkyl ester examples include those having 1 to 12 carbon atoms, and more specifically, methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, secondary butyl, Examples include alkyl groups such as 2-ethylhexyl and isooctyl.
- the alkyl moiety of the alkyl ester preferably has 1 to 8 carbon atoms.
- unsaturated carboxylic acid esters examples include methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, n-propyl (meth) acrylate, isobutyl (meth) acrylate, (meth) acrylic acid It is preferable to include one or more selected from (meth) acrylic acid esters such as n-butyl, isooctyl (meth) acrylate, and 2-ethylhexyl (meth) acrylate. These unsaturated carboxylic acid esters may be used alone or in combination of two or more.
- methyl (meth) acrylate, ethyl (meth) acrylate, isopropyl (meth) acrylate, n-propyl (meth) acrylate, isobutyl (meth) acrylate, and n-butyl (meth) acrylate It is more preferable that 1 type or 2 types or more selected from are included.
- a preferable ethylene / unsaturated carboxylic acid ester copolymer is an ethylene / (meth) acrylic acid ester copolymer.
- a copolymer composed of one kind of compound is preferable as the (meth) acrylic acid ester.
- examples of such copolymers include ethylene / methyl (meth) acrylate copolymer, ethylene / (meth) ethyl acrylate copolymer, ethylene / (meth) isopropyl acrylate copolymer, ethylene / (meth).
- N-propyl acrylate copolymer ethylene / (meth) acrylate isobutyl copolymer, ethylene / (meth) acrylate n-butyl copolymer, ethylene / (meth) acrylate isooctyl copolymer, ethylene / ( And (meth) acrylic acid 2-ethylhexyl copolymer.
- Ethylene / unsaturated ester copolymer (A) includes ethylene / vinyl acetate copolymer, ethylene / (meth) methyl acrylate copolymer, ethylene / (meth) ethyl acrylate copolymer, ethylene / (meth) Selected from isopropyl acrylate copolymer, ethylene / (meth) acrylic acid n-propyl copolymer, ethylene / (meth) acrylic acid isobutyl copolymer, ethylene / (meth) acrylic acid n-butyl copolymer It is preferable to include one or more types, and it is more preferable to include an ethylene / vinyl acetate copolymer. In the present embodiment, the ethylene / unsaturated ester copolymer (A) may be used alone or in combination of two or more.
- the melt flow rate (MFR) of the unsaturated ester copolymer (A) is preferably 10 g / 10 min or less, more preferably 9 g / 10 min or less, and 8 g / 10 min or less. More preferably, it is particularly preferably 7 g / 10 min or less. Further, if the MFR is not more than the above upper limit value, the heat resistance, mechanical strength, optical properties, etc.
- an ethylene / unsaturated ester copolymer (measured under conditions of 190 ° C. and 2160 g load in accordance with JIS K7210: 1999)
- the melt flow rate (MFR) of A) is preferably 0.1 g / 10 minutes or more, more preferably 1 g / 10 minutes or more, and particularly preferably 2 g / 10 minutes or more.
- the MFR of the ethylene / unsaturated ester copolymer (A) may be adjusted by blending a plurality of ethylene / unsaturated ester copolymers (A) having different MFRs.
- the MFR of the blend is defined as the MFR of the ethylene / unsaturated ester copolymer (A).
- the content of the structural unit derived from ethylene is preferably 52.
- the content is from mass% to 72 mass%, more preferably from 54 mass% to 70 mass%.
- the heat resistance, mechanical strength, water resistance, workability, etc. of the obtained laminated glass interlayer film or solar cell encapsulant should be improved. Can do.
- flexibility, adhesiveness, etc. of the laminated glass intermediate film and solar cell sealing material which can be obtained as content of the structural unit derived from ethylene is below the said upper limit can be made more favorable. .
- the content of the structural unit derived from the unsaturated ester is preferably Is 28 mass% or more and 48 mass% or less, More preferably, it is 30 mass% or more and 46 mass% or less.
- the content of the structural unit derived from the unsaturated ester is not less than the above lower limit, the transparency, flexibility, adhesiveness, and the like of the obtained laminated glass interlayer film and solar cell sealing material can be improved. . Further, if the content of the structural unit derived from the unsaturated ester is not more than the above upper limit value, the heat resistance, mechanical strength, water resistance, workability, etc. of the laminated glass intermediate film and solar cell sealing material obtained are more Can be good.
- the method for producing the ethylene / unsaturated ester copolymer (A) according to the present embodiment is not particularly limited, and can be produced by a known method.
- each polymerization component can be obtained by radical copolymerization at high temperature and high pressure.
- a commercially available ethylene / unsaturated ester copolymer (A) may be used.
- the total content of the ethylene / unsaturated ester copolymer (A) and the crosslinking agent (B) is 100% by mass of the entire resin composition (P).
- it is preferably 60% by mass or more, more preferably 70% by mass or more, further preferably 80% by mass or more, and particularly preferably 90% by mass or more.
- the optical properties, adhesiveness, and water resistance of the resulting laminated glass interlayer film and solar cell encapsulant are obtained. The balance of mechanical properties, heat resistance, handleability, workability, etc. can be made even better.
- the resin composition (P) according to the present embodiment contains a crosslinking agent (B) as an essential component. Heat resistance can be provided to the laminated glass intermediate film and solar cell sealing material which are obtained because the resin composition (P) which concerns on this embodiment contains a crosslinking agent (B).
- the crosslinking agent (B) is preferably an organic peroxide, more preferably an organic peroxide having a one-hour half-life temperature (decomposition temperature) of preferably 90 to 180 ° C, more preferably 100 to 150 ° C.
- organic peroxides examples include t-butyl peroxyisopropyl carbonate, t-butyl peroxy-2-ethylhexyl carbonate, t-butyl peroxyacetate, t-butyl peroxybenzoate, dicumyl peroxide, 2,5-dimethyl-2,5-bis (t-butylperoxy) hexane, di-t-butyl peroxide, 2,5-dimethyl-2,5-bis (t-butylperoxy) hexyne-3, 1 , 1-bis (t-butylperoxy) -3,3,5-trimethylcyclohexane, 1,1-bis (t-butylperoxy) cyclohexane, methyl ethyl ketone peroxide, 2,5-dimethylhexyl-2,5- Bisperoxybenzoate, t-butyl hydroperoxide, p-menthane hydride Peroxide, benzoyl
- TBEC t-butylperoxy-2- Ethyl hexyl carbonate
- the crosslinking agent (B) is preferably 0.1 to 1.5 parts by weight, more preferably 0.2 to 1.0 parts by weight, based on 100 parts by weight of the ethylene / unsaturated ester copolymer (A). It can be contained in an amount of preferably 0.3 to 1.0 part by mass, particularly preferably 0.4 to 1.0 part by mass.
- t-butylperoxy-2-ethylhexyl carbonate (TBEC) is included as the crosslinking agent (B)
- t-butylperoxy-2-ethylhexyl carbonate (TBEC) is an ethylene / unsaturated ester copolymer (A) 100
- A ethylene / unsaturated ester copolymer
- the resin composition (P) according to the present embodiment may contain components other than the ethylene / unsaturated ester copolymer (A) and the crosslinking agent (B) within a range not impairing the object of the present invention. it can. Although it does not specifically limit as another component, For example, a crosslinking adjuvant, a silane coupling agent, a ultraviolet absorber, a light stabilizer, antioxidant, etc. can be mentioned. Other components may be used individually by 1 type, and may be used in combination of 2 or more type.
- crosslinking aid examples include polyunsaturated compounds such as polyallyl compounds and poly (meth) acryloxy compounds. More specifically, polyallyl compounds such as triallyl isocyanurate, triallyl cyanurate, diallyl phthalate, diallyl fumarate, diallyl maleate; poly ( (Meth) acryloxy compounds; divinylbenzene and the like.
- the crosslinking aid is, for example, 5 parts by mass or less, preferably 0.1 to 3 parts by mass, more preferably 0.1 to 1 part by mass with respect to 100 parts by mass of the ethylene / unsaturated ester copolymer (A). It can be made to contain.
- silane coupling agent examples include a silane coupling agent having a vinyl group, an amino group or an epoxy group and a hydrolyzable group such as an alkoxy group. More specifically, vinyltrimethoxysilane, vinyltriethoxysilane, ⁇ -methacryloxypropyltrimethoxysilane, ⁇ -methacryloxypropylmethyldimethoxysilane, ⁇ -acryloxypropyltrimethoxysilane, ⁇ -glycidoxypropyltri Methoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, N-2- (aminoethyl) 3-aminopropyltrimethoxysilane, N-2- (aminoethyl) 3- Aminopropylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N
- the silane coupling agent is, for example, 5 parts by mass or less, preferably 0.02 to 3 parts by mass, more preferably 0.05 to 1 part by mass with respect to 100 parts by mass of the ethylene / unsaturated ester copolymer (A). It can be contained in an amount. When the silane coupling agent is contained in the above range, the adhesiveness of the resin composition (P) can be further improved.
- the resin composition (P) according to this embodiment preferably contains an ultraviolet absorber, a light stabilizer, an antioxidant, and the like.
- the ultraviolet absorber examples include 2-hydroxy-4-methoxybenzophenone, 2,2′-dihydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-2-carboxybenzophenone, 2-hydroxy-4-n- Benzophenone ultraviolet absorbers such as octoxybenzophenone; 2- (2H-benzotriazol-2-yl) -4,6-di-tert-pentylphenol, 2- (2′-hydroxy-3 ′, 5′-di benzotriazole ultraviolet absorbers such as t-butylphenyl) benzotriazole, 2- (2′-hydroxy-5-methylphenyl) benzotriazole, 2- (2′-hydroxy-5-t-octylphenyl) benzotriazole; Salicylic acid esters such as phenyl salicylate and p-octylphenyl salicylate Ether-based ultraviolet absorbers and the like are used.
- the light stabilizer a hindered amine light stabilizer or the like is used.
- the antioxidant various hindered phenol antioxidants, phosphite antioxidants, and the like are used.
- the antioxidant, light stabilizer and ultraviolet absorber are each, for example, 5 parts by mass or less, preferably 0.001 to 3 parts by mass, more preferably 100 parts by mass of the ethylene / unsaturated ester copolymer (A). Can be contained in an amount of 0.01 to 1 part by mass.
- the resin composition (P) according to the present embodiment can contain additives such as a colorant, a light diffusing agent, and a flame retardant as necessary.
- the colorant include pigments, inorganic compounds, and dyes.
- white colorants include titanium oxide, aluminum oxide, zinc oxide, calcium oxide, calcium carbonate, barium carbonate, barium sulfate, and the like.
- Examples of the light diffusing agent include glass beads, silica beads, silicon alkoxide beads, and hollow glass beads as inorganic spherical substances.
- Examples of the organic spherical material include acrylic and vinylbenzene plastic beads.
- flame retardants examples include halogen flame retardants such as bromides, phosphorus flame retardants, silicone flame retardants, metal hydrates such as magnesium hydroxide and aluminum hydroxide, and the like.
- the haze measured by the following method is preferably less than 2.5%, more preferably less than 2.0%, and less than 1.0%. More preferably, it is more preferably less than 0.6%, and particularly preferably less than 0.5%.
- the transparency of the obtained laminated glass or solar cell module can be further improved.
- the crosslinking rate represented by (T 50 -T 10 ) / (YX) and the ethylene / unsaturated ester content in the resin composition (P) according to the present embodiment are used. What is necessary is just to adjust suitably the kind, content, etc.
- the lower limit of the said haze of the resin composition (P) which concerns on this embodiment is not specifically limited, For example, it is 0.01% or more.
- the haze of the laminated glass according to this embodiment can be made less than 2.5%.
- the preferred haze of the laminated glass is the same as described above.
- the protrusion length of the resin composition (P) measured by the following method is preferably less than 10 mm, more preferably 9 mm or less, further preferably 5 mm or less, and 1 mm or less. It is particularly preferred that When the protrusion length is not more than the above upper limit value, the appearance of the resulting laminated glass or solar cell module can be improved.
- the crosslinking rate represented by (T 50 -T 10 ) / (YX), and the ethylene / undissolved amount in the resin composition (P) according to this embodiment can be obtained.
- the type and content of the saturated ester copolymer (A) and the crosslinking agent (B) may be appropriately adjusted.
- the MFR of the saturated ester copolymer (A) is particularly important.
- the lower limit value of the protruding length of the resin composition (P) according to this embodiment is preferably 0.0 mm.
- (Method) A 120 mm ⁇ 75 mm film composed of the resin composition (P) according to this embodiment is obtained. Next, the obtained film is sandwiched between glass plates of 120 mm ⁇ 75 mm ⁇ 3.2 mm, and heat-pressed with a vacuum laminator at 130 ° C. and 1 atm for 60 minutes to obtain a laminated glass.
- the protruding length of the resin composition protruding from the end portion of the obtained laminated glass in the direction perpendicular to the end surface of the laminated glass is measured.
- the protruding length is a length measured perpendicularly from the center point of the long side of the glass, and is an average value of two points measured at each long side.
- Examples of the shape of the resin composition (P) according to this embodiment include a sheet shape and a film shape.
- the laminated glass intermediate film 11 according to the present embodiment is composed of the resin composition (P) according to the present embodiment.
- the thickness of the laminated glass intermediate film 11 according to the present embodiment is, for example, 0.1 mm or more and 10 mm or less, preferably 0.2 mm or more and 5 mm or less, more preferably 0.3 mm or more and 2 mm or less.
- the mechanical strength of the glass intermediate film 11 can be made more favorable as the thickness of the glass intermediate film 11 is more than the said lower limit.
- the optical characteristic and interlayer adhesiveness of the laminated glass obtained can be made more favorable as the thickness of the glass intermediate film 11 is below the said upper limit.
- the manufacturing method of the laminated glass intermediate film 11 which concerns on this embodiment is not specifically limited, A conventionally well-known manufacturing method can be used.
- Examples of the method for producing the laminated glass interlayer film 11 according to the present embodiment include a press molding method, an extrusion molding method, a T-die molding method, an injection molding method, a compression molding method, a cast molding method, a calendar molding method, and an inflation molding method. Etc. can be used.
- the solar cell sealing material which concerns on this embodiment is comprised by the resin composition (P) which concerns on this embodiment.
- the solar cell encapsulant according to the present embodiment also preferably has the same film thickness as the laminated glass intermediate film, and can be manufactured by the same manufacturing method.
- FIG. 2 is a cross-sectional view schematically showing an example of the structure of the laminated glass 10 according to the embodiment of the present invention.
- a laminated glass 10 according to the present embodiment includes a laminated glass intermediate film 11 according to the present embodiment, and a transparent plate-like member 13 provided on both surfaces of the laminated glass intermediate film 11.
- the laminated glass 10 according to the present embodiment is excellent in performance balance of optical characteristics and moisture resistance adhesion between the glass intermediate film 11 and the transparent plate member 13. ing.
- Two or more layers of laminated glass intermediate film 11 may be used, or a layer made of another resin may be sandwiched between two laminated glass intermediate films 11 to form three or more layers.
- the transparent plate-like member 13 is not particularly limited.
- a commonly used transparent plate glass can be used.
- Inorganic glass such as heat ray absorbing plate glass, heat ray reflecting plate glass, and green glass.
- organic plastics plates such as polycarbonate plates, poly (meth) acrylate plates, polymethyl (meth) acrylate plates, polystyrene plates, cyclic polyolefin plates, polyethylene terephthalate plates, polyethylene naphthalate plates, polyethylene butyrate plates may be used. it can.
- the transparent plate-like member 13 may be appropriately subjected to surface treatment such as corona treatment, plasma treatment, and flame treatment.
- the thickness of the transparent plate member 13 is, for example, 1 mm or more and 20 mm or less.
- the transparent plate-like members 13 provided on both surfaces of the laminated glass intermediate film 11 may be the same or may be used in combination with different plate-like members.
- the manufacturing method of the laminated glass 10 which concerns on this embodiment is not specifically limited, For example, conventionally well-known manufacturing methods, such as a nip roll method, an autoclave method, a vacuum bag method, a vacuum laminator method, can be used. Manufacture may be performed using one of these methods, or two or more manufacturing methods may be combined.
- a manufacturing method of the laminated glass 10 according to the present embodiment for example, as shown in FIG. 2, after sandwiching the laminated glass intermediate film 11 according to the present embodiment between two transparent plate-like members 13, A method of heating and pressurizing is used.
- a method for producing the laminated glass 10 according to the present embodiment a method combining the nip roll method and the autoclave method, or a method combining the vacuum bag method and the autoclave method is preferable.
- a method combining the nip roll method and the autoclave method is, for example, by temporarily pressing a laminated body obtained by sandwiching the laminated glass interlayer film 11 according to the present embodiment between two transparent plate-like members 13 with a nip roll. Then, the laminated body is heat-pressed by heating and pressurizing using an autoclave to obtain a laminated glass 10.
- a method combining the vacuum bag method and the autoclave method is, for example, that a laminated body obtained by sandwiching the laminated glass interlayer film 11 according to the present embodiment between two transparent plate members 13 is placed in a vacuum bag. Then, the inside of the vacuum bag is depressurized to temporarily press-bond the laminated body, and then the laminated body is heat-pressed by heating and pressurizing using an autoclave to obtain a laminated glass 10.
- laminated glasses can be used for various applications, such as laminated glass for buildings, laminated glass for automobiles, general buildings, agricultural buildings, railway windows, etc. It is not limited to.
- Solar cell module The solar cell module according to this embodiment includes at least a substrate on which sunlight is incident, a solar cell element, and a solar cell sealing material according to this embodiment.
- the solar cell module according to the present embodiment may further include a protective material as necessary.
- a substrate on which sunlight is incident may be simply referred to as a substrate.
- the solar cell module according to the present embodiment can be produced by fixing the solar cell element sealed with the solar cell sealing material according to the present embodiment on the substrate.
- Examples of such solar cell modules include various types. For example, a substrate / sealing material / solar cell element / sealing material / protective material sandwiched between both sides of a solar cell element; a solar cell previously formed on the surface of a substrate such as glass
- the element is configured as a substrate / solar cell element / sealing material / protective material; a solar cell element formed on the inner peripheral surface of the substrate, for example, sputtering an amorphous solar cell element on a fluororesin-based sheet, etc.
- the protective material is sometimes referred to as a lower protective material because it is provided on the side opposite to the substrate side of the solar cell module, that is, on the lower side when the substrate on which sunlight is incident is the upper part of the solar cell module.
- solar cell elements examples include silicon-based materials such as single crystal silicon, polycrystalline silicon, and amorphous silicon, III-V groups such as gallium-arsenic, copper-indium-selenium, copper-indium-gallium-selenium, and cadmium-tellurium, and II.
- Various solar cell elements such as a group VI compound semiconductor can be used.
- the solar cell sealing material according to the present embodiment is particularly useful for sealing an amorphous silicon solar cell element and a heterojunction type solar cell element of amorphous silicon and single crystal silicon.
- the substrate constituting the solar cell module according to the present embodiment examples include a glass substrate, an acrylic resin substrate, a polycarbonate substrate, a polyester substrate, and a fluorine-containing resin substrate.
- the protective material lower protective material
- a single or multilayer sheet made of metal or various thermoplastic resins can be used.
- metals such as tin, aluminum, stainless steel, and inorganic materials such as glass
- examples thereof include single-layer or multi-layer sheets formed of polyester, inorganic material-deposited polyester, fluorine-containing resin, polyolefin, and the like.
- the solar cell sealing material according to the present embodiment exhibits good adhesion to these substrates or protective materials.
- the manufacturing method of the solar cell module according to the present embodiment is not particularly limited, and conventionally known manufacturing methods such as a nip roll method, an autoclave method, a vacuum bag method, and a vacuum laminator method can be used. Manufacture may be performed using one of these methods, or two or more manufacturing methods may be combined. Among these, as a manufacturing method of the solar cell module according to this embodiment, a manufacturing method using a vacuum laminator is preferable.
- a method using a vacuum laminator is, for example, heating a laminated body obtained by sandwiching a solar cell sealing material and a solar cell element according to this embodiment between a substrate and a protective material in a double vacuum apparatus. After the vacuum deaeration, the diaphragm rubber is thermocompression-bonded by heating and pressurizing the laminated body from the upper part of the double vacuum in the pressurizing step to obtain a solar cell module.
- the apparatus used was a movable direometer (MDR), MDR-2000P manufactured by Alpha Technology Co., Ltd.
- the laminated glass interlayer film having a thickness of 450 ⁇ m obtained in the examples and comparative examples was cut into about 30 mm squares to obtain measurement samples.
- the apparatus was set to a measurement condition of 130 ° C., it was confirmed that the temperature of the apparatus was stable, the sample was set in the apparatus, and measurement of the melting torque of the sample was started (frequency: 1.66 Hz). Generally, after the measurement is started, the torque once decreases (the minimum viscosity is T min ). Thereafter, the degree of increase in torque changes depending on the degree of progress of crosslinking.
- the torque value 60 minutes after the start of measurement is T 100 [dN ⁇ m]
- the torque value of 10% of T 100 is T 10
- the torque value of 50% of T 100 is T 50
- the torque being measured When the minimum value is T min
- the time to reach T 10 from the start of measurement is X [minutes]
- T 10 (T 100 ⁇ T min ) ⁇ 0.1 + T min ) as the crosslinking rate of the resin composition evaluated.
- the test piece was pulled away from the glass plate at a tensile speed of 100 mm / min, and the maximum stress was calculated as the adhesive strength (N) to the glass plate.
- the adhesive strength was measured about the adhesive strength of the laminated body after each storing for 500 hours and 1000 hours in 85 degreeC and 90% RH environment, and the adhesive strength of the laminated body before storage, respectively.
- Crosslinker 1 2,5-dimethyl-2,5-bis (t-butylperoxy) hexane (1 hour half-life temperature: 140 ° C.)
- Cross-linking agent 2 t-butylperoxy-2-ethylhexyl carbonate (1 hour half-life temperature: 121 ° C.)
- Crosslinking aid 1 Triallyl isocyanurate UV absorber 1: Benzophenone UV absorber Light stabilizer 1: Hindered amine light stabilizer Antioxidant 1: Hindered phenol antioxidant Silane coupling agent 1: ⁇ -methacrylic Roxypropyltrimethoxysilane
- the laminated glass interlayer of the example was excellent in the performance balance between optical properties and moisture-resistant adhesion. Furthermore, the obtained laminated glass had a short resin protrusion and was excellent in appearance. On the other hand, the laminated glass interlayer film of the comparative example was inferior in the performance balance between optical properties and moisture-resistant adhesion.
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Abstract
Description
まず、特許文献1および2に記載されているような、エチレン・不飽和エステル共重合体および架橋剤により構成された合わせガラス中間膜は光学特性および高湿度下での接着性(以下、耐湿接着性とも呼ぶ。)が十分に満足するものではなかった。
すなわち、本発明者らは、従来のエチレン・不飽和エステル共重合体および架橋剤により構成された合わせガラス中間膜には、光学特性および耐湿接着性をバランスよく向上させるという観点において、改善の余地があることを見出した。
また、太陽電池封止材も上記合わせガラス中間膜と同様の課題があった。
本発明者らは、上記知見を基にさらに検討したところ、可動ダイレオメータを用いて、130℃にて樹脂組成物のトルクを経時的に測定した際の、測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最小値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、(T50-T10)/(Y-X)で示される値(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)を樹脂組成物の架橋速度を評価する指標として利用できることを見出した。
こうした知見に基づいて、鋭意検討した結果、(T50-T10)/(Y-X)で示される架橋速度を特定の範囲に調整することによって、合わせガラス中間膜または太陽電池封止材の光学特性および耐湿接着性の性能バランスを効果的に向上できることを見出し、本発明を完成するに至った。
合わせガラス中間膜または太陽電池封止材用樹脂組成物であって、
エチレン・不飽和エステル共重合体(A)および架橋剤(B)を含み、
可動ダイレオメータを用いて、130℃にて当該樹脂組成物のトルクを経時的に測定した際の、測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最小値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、
(T50-T10)/(Y-X)で示される架橋速度(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)が0.01dN・m/分を超え0.25dN・m/分以下である樹脂組成物。
[2]
上記[1]に記載の樹脂組成物において、
JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定される、エチレン・不飽和エステル共重合体(A)のメルトフローレート(MFR)が10g/10分以下である樹脂組成物。
[3]
上記[1]または[2]に記載の樹脂組成物において、
上記エチレン・不飽和エステル共重合体(A)がエチレン・ビニルエステル共重合体およびエチレン・不飽和カルボン酸エステル共重合体から選択される少なくとも一種の重合体を含む樹脂組成物。
[4]
上記[3]に記載の樹脂組成物において、
上記エチレン・不飽和エステル共重合体(A)がエチレン・酢酸ビニル共重合体を含む樹脂組成物。
[5]
上記[1]乃至[4]のいずれか一つに記載の樹脂組成物において、
上記エチレン・不飽和エステル共重合体(A)の全体を100質量%としたとき、上記エチレン・不飽和エステル共重合体(A)中の不飽和エステルに由来する構成単位の含有量が28質量%以上48質量%以下である樹脂組成物。
[6]
上記[1]乃至[5]のいずれか一つに記載の樹脂組成物において、
上記架橋剤(B)が有機過酸化物を含む樹脂組成物。
[7]
上記[1]乃至[6]のいずれか一つに記載の樹脂組成物において、
下記方法により測定されるヘイズが2.5%未満である樹脂組成物。
(方法)
上記樹脂組成物により構成された120mm×75mmの膜を得る。次いで、得られた上記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた上記合わせガラスのヘイズをJIS K7136:2000に準じてヘイズメータにより測定する。
[8]
上記[1]乃至[7]のいずれか一つに記載の樹脂組成物において、
下記方法により測定される樹脂組成物のはみ出し長さが10mm未満である樹脂組成物。
(方法)
上記樹脂組成物により構成された120mm×75mmの膜を得る。次いで、得られた上記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた上記合わせガラスの端部からはみ出した樹脂組成物の、上記合わせガラスの端面に対して垂直方向のはみ出し長さを測定する。
[9]
上記[1]乃至[8]のいずれか一つに記載の樹脂組成物において、
シート状またはフィルム状である樹脂組成物。
[10]
上記[1]乃至[9]のいずれか一つに記載の樹脂組成物により構成された合わせガラス中間膜。
[11]
上記[10]に記載の合わせガラス中間膜と、
上記合わせガラス中間膜の両面に設けられた透明板状部材と、
を備える合わせガラス。
[12]
上記[1]乃至[9]のいずれか一つに記載の樹脂組成物により構成された太陽電池封止材。
[13]
上記[12]に記載の太陽電池封止材を含む太陽電池モジュール。
図1は、可動ダイレオメータを用いた測定により得られるトルク値と測定時間との関係を模式的に示した図である。図2は、本発明に係る実施形態の合わせガラス10の構造の一例を模式的に示した断面図である。
本実施形態に係る樹脂組成物(P)は、合わせガラス中間膜11または太陽電池封止材を形成するために用いられる樹脂組成物であって、エチレン・不飽和エステル共重合体(A)および架橋剤(B)を含み、可動ダイレオメータを用いて、130℃にて当該樹脂組成物のトルクを経時的に測定した際の、測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最小値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、(T50-T10)/(Y-X)で示される架橋速度(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)が0.01dN・m/分を超え0.25dN・m/分以下である。
測定装置としては、例えば、アルファテクノロジー社製の可動ダイレオメータ(製品名:MDR-2000P)を使用し、測定温度130℃、周波数1.66Hzの条件で樹脂組成物(P)の溶融トルクを経時的に測定することにより本実施形態に係る樹脂組成物(P)のトルク値(T10、T50、T100)を測定することができる。
すなわち、本発明者らは、従来のエチレン・不飽和エステル共重合体および架橋剤により構成された合わせガラス中間膜には、光学特性および耐湿接着性をバランスよく向上させるという観点において、改善の余地があることを見出した。
また、太陽電池封止材も上記合わせガラス中間膜と同様の課題があった。
本発明者らは、上記知見を基にさらに検討したところ、可動ダイレオメータを用いて、130℃にて樹脂組成物のトルクを経時的に測定した際の、測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最低値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、(T50-T10)/(Y-X)で示される値(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)を樹脂組成物の架橋速度を評価する指標として利用できることを見出した。
こうした知見に基づいて、鋭意検討した結果、(T50-T10)/(Y-X)で示される架橋速度を特定の範囲に調整することによって、合わせガラス中間膜または太陽電池封止材の光学特性および耐湿接着性の性能バランスを効果的に向上できることを見出し、本発明を完成するに至った。
すなわち、本実施形態に係る樹脂組成物(P)は、(T50-T10)/(Y-X)で示される架橋速度が0.01dN・m/分を超え0.25dN・m/分以下の範囲内になるように構成されることによって、合わせガラス中間膜または太陽電池封止材の光学特性および耐湿接着性の性能バランスを良好にすることができる。
(T50-T10)/(Y-X)で示される架橋速度を上記範囲内にすることによって、合わせガラス中間膜または太陽電池封止材の光学特性および耐湿接着性の性能バランスを良好にすることができる理由は明らかではないが、樹脂組成物の架橋速度を上記範囲内に調整することによって、樹脂組成物の架橋がより穏やかで、かつ、適切な速度で進み、樹脂組成物の架橋反応が進行している際に、樹脂組成物中に含まれる水分や気泡等が脱気しやすくなり、その結果、得られる架橋膜中の気泡の量等を抑制でき、光学特性および耐湿接着性が良好になるからだと考えられる。
なお、本実施形態では、光学特性とは、例えばヘイズ、全光線透過率等をいう。
また、本実施形態において、(T50-T10)/(Y-X)で示される架橋速度は0.25dN・m/分以下であるが、得られる合わせガラス中間膜や太陽電池封止材の光学特性および耐湿接着性の性能バランスをより一層良好にする観点から、0.20dN・m/分以下であることが好ましく、0.17dN・m/分以下であることがより好ましく、0.15dN・m/分以下であることが特に好ましい。
これらの中でも、例えば、後述するエチレン・不飽和エステル共重合体(A)のMFRや架橋剤(B)の1時間半減期温度、架橋剤(B)の含有量等が、本実施形態に係る樹脂組成物(P)の(T50-T10)/(Y-X)で示される架橋速度や、トルク値T100を所望の数値範囲とするための要素として挙げられる。例えば、エチレン・不飽和エステル共重合体(A)のMFRを低くする、架橋剤(B)の1時間半減期温度を高くする、あるいは架橋剤(B)の含有量を減らすと、上記架橋速度を低下させることができる。
本実施形態に係るエチレン・不飽和エステル共重合体(A)は、エチレンと、不飽和エステルの少なくとも1種とを共重合した重合体である。エチレン・不飽和エステル共重合体(A)としては、エチレンと不飽和エステルとを含む共重合体を例示することができる。
また、本実施形態に係るエチレン・不飽和エステル共重合体(A)はエチレン・ビニルエステル共重合体およびエチレン・不飽和カルボン酸エステル共重合体から選択される少なくとも一種の重合体を含むことが好ましい。
また、本実施形態に係るエチレン・不飽和エステル共重合体(A)は、エチレンおよび不飽和エステル以外の重合性モノマーを含んでいてもよく、例えばプロピレン、ブテン、ヘキセン等のオレフィンを例示することができる。
具体的には、エチレンと、不飽和カルボン酸アルキルエステルと、からなる共重合体を例示することができる。
これらの中でも、上記不飽和カルボン酸は、エチレン・不飽和エステル共重合体(A)の生産性、衛生性等の観点から、アクリル酸およびメタクリル酸から選ばれる少なくとも一種を含むことが好ましい。これらの不飽和カルボン酸は1種単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
なお、本実施形態においてはエチレン・不飽和エステル共重合体(A)は、単独で用いてもよいし、二種以上を組み合わせて用いてもよい。
また、本実施形態において、樹脂組成物の加工性をより一層向上させる観点から、JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定される、エチレン・不飽和エステル共重合体(A)のメルトフローレート(MFR)は、0.1g/10分以上であることが好ましく、1g/10分以上であることがより好ましく、2g/10分以上であることが特に好ましい。
エチレン・不飽和エステル共重合体(A)のMFRは、異なるMFRを有するエチレン・不飽和エステル共重合体(A)を複数ブレンドして調整してもよい。ここで、異なるMFRを有するエチレン・不飽和エステル共重合体(A)を複数ブレンドした場合、ブレンド物のMFRをエチレン・不飽和エステル共重合体(A)のMFRとする。
エチレンに由来する構成単位の含有量が上記下限値以上であると、得られる合わせガラス中間膜や太陽電池封止材の耐熱性や機械的強度、耐水性、加工性等をより良好にすることができる。また、エチレンに由来する構成単位の含有量が上記上限値以下であると、得られる合わせガラス中間膜や太陽電池封止材の透明性や柔軟性、接着性等をより良好にすることができる。
不飽和エステルに由来する構成単位の含有量が上記下限値以上であると、得られる合わせガラス中間膜や太陽電池封止材の透明性や柔軟性、接着性等をより良好にすることができる。また、不飽和エステルに由来する構成単位の含有量が上記上限値以下であると、得られる合わせガラス中間膜や太陽電池封止材の耐熱性や機械的強度、耐水性、加工性等をより良好にすることができる。
本実施形態に係る樹脂組成物(P)は、必須成分として架橋剤(B)を含む。
本実施形態に係る樹脂組成物(P)が架橋剤(B)を含有することで、得られる合わせガラス中間膜や太陽電池封止材に耐熱性を付与することができる。
架橋剤(B)としては、有機過酸化物が好ましく、1時間半減期温度(分解温度)が好ましくは90~180℃、より好ましくは100~150℃の有機過酸化物がより好ましい。
これらの中でも、少なくとも、炭素数3~6の分岐アルキルパーオキシ基を有する化合物が好ましく、少なくとも、t-ブチルパーオキシ基を有する化合物がより好ましく、2,5-ジメチル-2,5-ビス(t-ブチルパーオキシ)ヘキサン〔1時間半減期温度=140℃〕およびt-ブチルパーオキシ-2-エチルヘキシルカーボネート〔1時間半減期温度=121℃〕がさらに好ましく、t-ブチルパーオキシ-2-エチルヘキシルカーボネート(TBEC)が架橋速度の点と合わせガラスの製造プロセスの観点から特に好ましい。
架橋剤(B)は、エチレン・不飽和エステル共重合体(A)100質量部に対し、好ましくは0.1~1.5質量部、より好ましくは0.2~1.0質量部、さらに好ましくは0.3~1.0質量部、特に好ましくは0.4~1.0質量部の量で含有させることができる。
架橋剤(B)としてt-ブチルパーオキシ-2-エチルヘキシルカーボネート(TBEC)を含む場合、t-ブチルパーオキシ-2-エチルヘキシルカーボネート(TBEC)は、エチレン・不飽和エステル共重合体(A)100質量部に対し、好ましくは0.2~1.5質量部、より好ましくは0.3~1.0質量部、さらに好ましくは0.4~1.0質量部、特に好ましくは0.4~0.8質量部の量で含有させることができる。
本実施形態に係る樹脂組成物(P)には、本発明の目的を損なわない範囲内において、エチレン・不飽和エステル共重合体(A)および架橋剤(B)以外の成分を含有させることができる。その他の成分としては特に限定されないが、例えば、架橋助剤、シランカップリング剤、紫外線吸収剤、光安定剤および酸化防止剤等を挙げることができる。その他の成分は1種単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
架橋助剤は、エチレン・不飽和エステル共重合体(A)100質量部に対し、例えば5質量部以下、好ましくは0.1~3質量部、より好ましくは0.1~1質量部の量で含有させることができる。
シランカップリング剤は、エチレン・不飽和エステル共重合体(A)100質量部に対し、例えば5質量部以下、好ましくは0.02~3質量部、より好ましくは0.05~1質量部の量で含有させることができる。シランカップリング剤が上記範囲で含まれていると、樹脂組成物(P)の接着性をより一層向上させることができる。
酸化防止剤として各種ヒンダードフェノール系酸化防止剤やホスファイト系酸化防止剤等が用いられる。
酸化防止剤、光安定剤および紫外線吸収剤は、エチレン・不飽和エステル共重合体(A)100質量部に対し、各々、例えば5質量部以下、好ましくは0.001~3質量部、より好ましくは0.01~1質量部の量で含有させることができる。
着色剤としては、顔料、無機化合物、染料等が挙げられ、特に白色の着色剤としては、酸化チタン、酸化アルミニウム、酸化亜鉛、酸化カルシウム、炭酸カルシウム、炭酸バリウム、硫酸バリウム等が挙げられる。これらの添加剤を含有する樹脂組成物(P)を太陽電池素子の受光側の封止材として用いる場合は、透明性を損なう場合があるが、太陽電池素子の受光側と反対面の封止材として用いる場合には好適に用いられる。
本実施形態に係る樹脂組成物(P)において、下記方法により測定されるヘイズが2.5%未満であることが好ましく、2.0%未満であることがより好ましく、1.0%未満であることがより好ましく、0.6%未満であることがさらに好ましく、0.5%未満であることが特に好ましい。上記ヘイズが上記上限値以下であると、得られる合わせガラスや太陽電池モジュールの透明性をより良好にすることができる。
このようなヘイズを達成するためには、(T50-T10)/(Y-X)で示される架橋速度や、本実施形態に係る樹脂組成物(P)中のエチレン・不飽和エステル共重合体(A)および架橋剤(B)の種類や含有量等を適宜調整すればよい。
本実施形態に係る樹脂組成物(P)の上記ヘイズの下限値は特に限定されないが、例えば、0.01%以上である。
本実施形態に係る樹脂組成物(P)を使用することにより、本実施形態に係る合わせガラスのヘイズを2.5%未満とすることができる。合わせガラスの好ましいヘイズは上記と同じある。
(方法)
本実施形態に係る樹脂組成物(P)により構成された120mm×75mmの膜を得る。次いで、得られた上記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた上記合わせガラスのヘイズをJIS K7136:2000に準じてヘイズメータにより測定する。
本実施形態において、下記方法により測定される樹脂組成物(P)のはみ出し長さが10mm未満であることが好ましく、9mm以下であることがより好ましく、5mm以下であることがさらに好ましく、1mm以下であることが特に好ましい。上記はみ出し長さが上記上限値以下であると、得られる合わせガラスや太陽電池モジュールの外観をより良好にすることができる。
このような白濁部の長さを達成するためには(T50-T10)/(Y-X)で示される架橋速度や、本実施形態に係る樹脂組成物(P)中のエチレン・不飽和エステル共重合体(A)および架橋剤(B)の種類や含有量等を適宜調整すればよいが、(T50-T10)/(Y-X)で示される架橋速度やエチレン・不飽和エステル共重合体(A)のMFRが特に重要となる。
本実施形態に係る樹脂組成物(P)の上記はみ出し長さの下限値は0.0mmが好ましい。
(方法)
本実施形態に係る樹脂組成物(P)により構成された120mm×75mmの膜を得る。次いで、得られた上記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた上記合わせガラスの端部からはみ出した樹脂組成物の、上記合わせガラスの端面に対して垂直方向のはみ出し長さを測定する。はみ出し長さは、上記ガラスの長辺の中心点から垂直に測定した長さであり、各長辺で測定した2点の平均値とする。
本実施形態に係る合わせガラス中間膜11は、本実施形態に係る樹脂組成物(P)により構成される。
本実施形態に係る合わせガラス中間膜11の厚みは、例えば、0.1mm以上10mm以下、好ましくは0.2mm以上5mm以下、より好ましくは0.3mm以上2mm以下である。
ガラス中間膜11の厚みが上記下限値以上であると、ガラス中間膜11の機械的強度をより良好にすることができる。また、ガラス中間膜11の厚みが上記上限値以下であると、得られる合わせガラスの光学特性や層間接着性をより良好にすることができる。
本実施形態に係る合わせガラス中間膜11の製造方法としては、例えば、プレス成形法、押出成形法、Tダイ成形法、射出成形法、圧縮成形法、キャスト成形法、カレンダー成形法、インフレーション成形法等を用いることができる。
本実施形態に係る太陽電池封止材も合せガラス中間膜と同様の膜厚が好ましく、同様の製造方法で製造することができる。
図2は、本発明に係る実施形態の合わせガラス10の構造の一例を模式的に示した断面図である。
本実施形態に係る合わせガラス10は、本実施形態に係る合わせガラス中間膜11と、合わせガラス中間膜11の両面に設けられた透明板状部材13と、を備える。本実施形態に係る合わせガラス10は、本実施形態に係る合わせガラス中間膜11を備えることにより、光学特性およびガラス中間膜11と透明板状部材13との間の耐湿接着性の性能バランスに優れている。
合わせガラス中間膜11は2層以上使用してもよく、また他の樹脂からなる層を2枚の合わせガラス中間膜11の間に挟んで3層以上としてもよい。
また透明板状部材13は、コロナ処理、プラズマ処理、フレーム処理等の表面処理を適宜施していてもよい。
本実施形態に係る合わせガラス10の製造方法としては、例えば、図2に示すように、本実施形態に係る合わせガラス中間膜11を2枚の透明板状部材13の間に狭持した後、加熱加圧する方法等が用いられる。
これらの中でも、本実施形態に係る合わせガラス10の製造方法としてはニップロール法とオートクレーブ法を組み合わせた方法、あるいは真空バッグ法とオートクレーブ法を組み合わせた方法が好ましい。
ニップロール法とオートクレーブ法を組み合わせた方法は、例えば、本実施形態に係る合わせガラス中間膜11を2枚の透明板状部材13の間に狭持して得られた積層体をニップロールにより仮圧着し、次いで、オートクレーブを用いて上記積層体を加熱・加圧処理することによって熱圧着し、合わせガラス10を得る方法である。
真空バッグ法とオートクレーブ法を組み合わせた方法は、例えば、本実施形態に係る合わせガラス中間膜11を2枚の透明板状部材13の間に狭持して得られた積層体を真空バッグ内に入れ、次いで、真空バック内を減圧して上記積層体を仮圧着し、次いで、オートクレーブを用いて上記積層体を加熱・加圧処理することによって熱圧着し、合わせガラス10を得る方法である。
本実施形態に係る太陽電池モジュールは、少なくとも、太陽光が入射する基板と、太陽電池素子と、本実施形態に係る太陽電池封止材とを備える。本実施形態に係る太陽電池モジュールは、必要に応じて、さらに保護材を備えていてもよい。なお、太陽光が入射する基板を、単に基板と称することもある。
本実施形態に係る太陽電池モジュールは、上記基板上に、本実施形態に係る太陽電池封止材により封止された太陽電池素子を固定することで作製することができる。
なお、保護材は、太陽光が入射する基板を太陽電池モジュールの上部としたとき、太陽電池モジュールの基板側とは反対側、すなわち下部に備えられるため、下部保護材と称することもある。
保護材(下部保護材)としては、金属や各種熱可塑性樹脂等により形成された単体もしくは多層のシート等を用いることができ、例えば、錫、アルミ、ステンレススチール等の金属、ガラス等の無機材料、ポリエステル、無機物蒸着ポリエステル、フッ素含有樹脂、ポリオレフィン等により形成された1層もしくは多層のシートを例示することができる。本実施形態に係る太陽電池封止材は、これらの基板または保護材に対して良好な接着性を示す。
これらの中でも、本実施形態に係る太陽電池モジュールの製造方法としては真空ラミネーターを用いた製造方法が好ましい。
真空ラミネーターを用いた方法は、例えば、本実施形態に係る太陽電池封止材および太陽電池素子を基板や保護材の間に狭持して得られた積層体を二重真空装置の中で加熱、真空脱気を実施したのち、加圧工程でダイアフラムゴムを二重真空上部から、上記積層体を加熱・加圧処理することによって熱圧着し、太陽電池モジュールを得る方法である。
[架橋速度]
装置はアルファテクノロジー株式会社製可動ダイレオメータ(MDR)、MDR-2000Pを用いた。
実施例および比較例で得られた、厚さ450μmの合わせガラス中間膜を約30mm角にカットし、測定試料とした。
装置を測定条件である130℃に設定し、装置の温度が安定したことを確認し、試料を装置にセットして、試料の溶融トルクの測定を開始させた(周波数1.66Hz)。測定開始後、一般的にはいったんトルクが下がる(その最低粘度をTminとする)。その後、架橋の進行具合によってトルクの上昇度合が変化する。
測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最低値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、(T50-T10)/(Y-X)、(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)で示される値を樹脂組成物の架橋速度として評価した。
実施例および比較例で得られた合わせガラス中間膜を120mm×75mmのサイズに裁断した。次いで、得られた試験片を120mm×75mm×3.2mmのガラス板(旭硝子社製、製品名:フロート板ガラス、全光線透過率:90.4%、ヘイズ:0.2%)で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得た。なお、得られた合わせガラスは約30分かけて室温に戻るように徐冷にて冷却した。次いで、得られた合わせガラスの全光線透過率およびヘイズをJIS K7136:2000に準じてヘイズメータ(村上色彩社製、製品名:ヘイズメータHM150)により測定した。
実施例および比較例で得られた合わせガラス中間膜を120mm×75mmのサイズに裁断した。次いで、得られた試験片を120mm×75mm×3.2mmのガラス板(旭硝子社製、白板フロートガラス)に積層し、真空ラミネーターにて130℃、1atmで60分間加熱圧着を行い、上記試験片を上記ガラス板に接着させ、積層体を得た。次いで、積層体を85℃、90%RHの環境下に500時間および1000時間保管した。次いで、引張速度100mm/分で上記試験片を上記ガラス板から引き離し、最大応力をガラス板に対する接着強度(N)として算出した。なお、接着強度は、85℃、90%RHの環境下に500時間および1000時間それぞれ保管した後の積層体の接着強度と、保管前の積層体の接着強度についてそれぞれ測定した。
実施例および比較例で得られた合わせガラス中間膜を120mm×75mmのサイズに裁断した。次いで、得られた試験片を120mm×75mm×3.2mmのガラス板(旭硝子社製、製品名:フロート板ガラス)で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得た。なお、得られた合わせガラスは約30分かけて室温に戻るように徐冷にて冷却した。次いで、ガラスの長辺側の中心点から垂直にはみ出した樹脂組成物の長さをノギスを用いて測定した。各長辺の中心点での測定の平均値をはみ出し長さとした。
合わせガラスの作製に用いた材料の詳細は以下の通りである。
<エチレン・不飽和エステル共重合体(A)>
EVA1:エチレン・酢酸ビニル共重合体(MFR=14g/10min、エチレン含量=67質量%、酢酸ビニル含量=33質量%)
EVA2:エチレン・酢酸ビニル共重合体(MFR=1.0g/10min、エチレン含量=67質量%、酢酸ビニル含量=33質量%)
EVA3:エチレン・酢酸ビニル共重合体(MFR=30g/10min、エチレン含量=65質量%、酢酸ビニル含量=35質量%)
EVA4:エチレン・酢酸ビニル共重合体(MFR=4.3g/10min、エチレン含量=74質量%、酢酸ビニル含量=26質量%)
架橋剤1:2,5-ジメチル-2,5-ビス(t-ブチルパーオキシ)ヘキサン(1時間半減期温度:140℃)
架橋剤2:t-ブチルパーオキシ-2-エチルヘキシルカーボネート(1時間半減期温度:121℃)
架橋助剤1:トリアリルイソシアヌレート
紫外線吸収剤1:ベンゾフェノン系紫外線吸収剤
光安定剤1:ヒンダードアミン系光安定剤
酸化防止剤1:ヒンダードフェノール系酸化防止剤
シランカップリング剤1:γ-メタクリロキシプロピルトリメトキシシラン
表1および2に示す配合割合で、各成分を事前にブレンドし、次いで、シリンダー温度をC1(先端部):70℃、C2(中間部):80℃、C3(後部):90℃に設定した40mmφ異型押出機(L/D=26)を用いて、得られた樹脂組成物を押出成形することにより、厚さ450μmの合わせガラス中間膜を得た。
得られた合わせガラス中間膜について上記の評価をそれぞれおこなった。得られた結果を表1および2にそれぞれ示す。
Claims (13)
- 合わせガラス中間膜または太陽電池封止材用樹脂組成物であって、
エチレン・不飽和エステル共重合体(A)および架橋剤(B)を含み、
可動ダイレオメータを用いて、130℃にて当該樹脂組成物のトルクを経時的に測定した際の、測定開始から60分後のトルク値をT100[dN・m]とし、T100の10%のトルク値をT10とし、T100の50%のトルク値をT50とし、測定中のトルクの最小値をTminとし、測定開始からT10に達する時間をX[分]とし、測定開始からT50に達する時間をY[分]としたとき、
(T50-T10)/(Y-X)で示される架橋速度(ただし、T50=(T100-Tmin)×0.5+Tmin、T10=(T100-Tmin)×0.1+Tmin)が0.01dN・m/分を超え0.25dN・m/分以下である樹脂組成物。 - 請求項1に記載の樹脂組成物において、
JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定される、エチレン・不飽和エステル共重合体(A)のメルトフローレート(MFR)が10g/10分以下である樹脂組成物。 - 請求項1または2に記載の樹脂組成物において、
前記エチレン・不飽和エステル共重合体(A)がエチレン・ビニルエステル共重合体およびエチレン・不飽和カルボン酸エステル共重合体から選択される少なくとも一種の重合体を含む樹脂組成物。 - 請求項3に記載の樹脂組成物において、
前記エチレン・不飽和エステル共重合体(A)がエチレン・酢酸ビニル共重合体を含む樹脂組成物。 - 請求項1乃至4のいずれか一項に記載の樹脂組成物において、
前記エチレン・不飽和エステル共重合体(A)の全体を100質量%としたとき、前記エチレン・不飽和エステル共重合体(A)中の不飽和エステルに由来する構成単位の含有量が28質量%以上48質量%以下である樹脂組成物。 - 請求項1乃至5のいずれか一項に記載の樹脂組成物において、
前記架橋剤(B)が有機過酸化物を含む樹脂組成物。 - 請求項1乃至6のいずれか一項に記載の樹脂組成物において、
下記方法により測定されるヘイズが2.5%未満である樹脂組成物。
(方法)
前記樹脂組成物により構成された120mm×75mmの膜を得る。次いで、得られた前記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた前記合わせガラスのヘイズをJIS K7136:2000に準じてヘイズメータにより測定する。 - 請求項1乃至7のいずれか一項に記載の樹脂組成物において、
下記方法により測定される樹脂組成物のはみ出し長さが10mm未満である樹脂組成物。
(方法)
前記樹脂組成物により構成された120mm×75mmの膜を得る。次いで、得られた前記膜を120mm×75mm×3.2mmのガラス板で挟み、真空ラミネーターにて130℃、1atmで60分間加熱圧着し、合わせガラスを得る。次いで、得られた前記合わせガラスの端部からはみ出した樹脂組成物の、前記合わせガラスの端面に対して垂直方向のはみ出し長さを測定する。 - 請求項1乃至8のいずれか一項に記載の樹脂組成物において、
シート状またはフィルム状である樹脂組成物。 - 請求項1乃至9のいずれか一項に記載の樹脂組成物により構成された合わせガラス中間膜。
- 請求項10に記載の合わせガラス中間膜と、
前記合わせガラス中間膜の両面に設けられた透明板状部材と、
を備える合わせガラス。 - 請求項1乃至9のいずれか一項に記載の樹脂組成物により構成された太陽電池封止材。
- 請求項12に記載の太陽電池封止材を含む太陽電池モジュール。
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US16/963,625 A-371-Of-International US20200347215A1 (en) | 2018-02-14 | 2019-02-08 | Resin composition for laminated glass interlayer film or solar cell encapsulant, laminated glass interlayer film, laminated glass, solar cell encapsulant, and solar cell module |
US18/410,535 Division US20240150563A1 (en) | 2018-02-14 | 2024-01-11 | Resin composition for laminated glass interlayer film or solar cell encapsulant, laminated glass interlayer film, laminated glass, solar cell encapsulant, and solar cell module |
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WO2019159852A1 true WO2019159852A1 (ja) | 2019-08-22 |
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PCT/JP2019/004704 WO2019159852A1 (ja) | 2018-02-14 | 2019-02-08 | 合わせガラス中間膜または太陽電池封止材用樹脂組成物、合わせガラス中間膜、合わせガラス、太陽電池封止材および太陽電池モジュール |
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US (2) | US20200347215A1 (ja) |
EP (1) | EP3753910A4 (ja) |
JP (2) | JP7032511B2 (ja) |
CN (1) | CN111801303B (ja) |
BR (1) | BR112020016665A2 (ja) |
WO (1) | WO2019159852A1 (ja) |
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JP2007331952A (ja) | 2006-06-12 | 2007-12-27 | Bridgestone Corp | 合わせガラス用中間膜及びそれを用いた合わせガラス |
WO2014208756A1 (ja) | 2013-06-28 | 2014-12-31 | 株式会社ブリヂストン | 積層体形成用シート、及び積層体の製造方法 |
WO2016194606A1 (ja) * | 2015-06-04 | 2016-12-08 | 株式会社ブリヂストン | 太陽電池用封止膜及び太陽電池モジュール |
WO2017150217A1 (ja) * | 2016-02-29 | 2017-09-08 | 三井化学東セロ株式会社 | 樹脂シート、合わせガラスおよび太陽電池モジュール |
JP2018024177A (ja) | 2016-08-10 | 2018-02-15 | キヤノン株式会社 | 画像形成装置、画像形成装置の制御方法、及びプログラム |
JP2018162175A (ja) * | 2017-03-24 | 2018-10-18 | 日立化成株式会社 | 合わせガラス用中間膜 |
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JP2005001952A (ja) * | 2003-06-13 | 2005-01-06 | Bridgestone Corp | 合わせガラス |
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JP5230905B2 (ja) * | 2006-03-23 | 2013-07-10 | 株式会社ブリヂストン | 合わせガラス用中間膜、それを用いた合わせガラス及びその製造方法 |
CN101410990B (zh) * | 2006-04-05 | 2011-03-30 | 株式会社普利司通 | 太阳能电池用密封膜和使用该密封膜的太阳能电池 |
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CN102318080B (zh) * | 2009-02-12 | 2013-12-11 | 株式会社普利司通 | 太阳能电池用密封膜及使用了该密封膜的太阳能电池 |
JP2012052004A (ja) * | 2010-08-31 | 2012-03-15 | Dainippon Printing Co Ltd | 太陽電池モジュール用封止材の製造方法 |
JP5615645B2 (ja) * | 2010-09-22 | 2014-10-29 | 三井化学東セロ株式会社 | 押し出し成形フィルムの製造方法 |
JP5788712B2 (ja) * | 2011-05-24 | 2015-10-07 | 株式会社ブリヂストン | エチレン−極性モノマー共重合体シート、並びにこれを用いた合わせガラス用中間膜、合わせガラス、太陽電池用封止膜及び太陽電池 |
TW201343352A (zh) * | 2012-03-28 | 2013-11-01 | Sumitomo Chemical Co | 太陽能電池密封材用小粒之防止結塊方法 |
KR101699183B1 (ko) * | 2015-12-24 | 2017-01-23 | 한화토탈 주식회사 | 에틸렌 비닐아세테이트 공중합체 수지의 제조방법 및 이로부터 제조된 수지와 이를 이용하여 제조된 태양전지 봉지재용 시트 |
-
2019
- 2019-02-08 US US16/963,625 patent/US20200347215A1/en not_active Abandoned
- 2019-02-08 JP JP2020500465A patent/JP7032511B2/ja active Active
- 2019-02-08 EP EP19753913.3A patent/EP3753910A4/en active Pending
- 2019-02-08 BR BR112020016665-0A patent/BR112020016665A2/pt unknown
- 2019-02-08 WO PCT/JP2019/004704 patent/WO2019159852A1/ja unknown
- 2019-02-08 CN CN201980013150.7A patent/CN111801303B/zh active Active
-
2022
- 2022-02-24 JP JP2022026433A patent/JP7254226B6/ja active Active
-
2024
- 2024-01-11 US US18/410,535 patent/US20240150563A1/en active Pending
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JP2007331952A (ja) | 2006-06-12 | 2007-12-27 | Bridgestone Corp | 合わせガラス用中間膜及びそれを用いた合わせガラス |
WO2014208756A1 (ja) | 2013-06-28 | 2014-12-31 | 株式会社ブリヂストン | 積層体形成用シート、及び積層体の製造方法 |
WO2016194606A1 (ja) * | 2015-06-04 | 2016-12-08 | 株式会社ブリヂストン | 太陽電池用封止膜及び太陽電池モジュール |
WO2017150217A1 (ja) * | 2016-02-29 | 2017-09-08 | 三井化学東セロ株式会社 | 樹脂シート、合わせガラスおよび太陽電池モジュール |
JP2018024177A (ja) | 2016-08-10 | 2018-02-15 | キヤノン株式会社 | 画像形成装置、画像形成装置の制御方法、及びプログラム |
JP2018162175A (ja) * | 2017-03-24 | 2018-10-18 | 日立化成株式会社 | 合わせガラス用中間膜 |
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EP3753910A1 (en) | 2020-12-23 |
JP7254226B6 (ja) | 2023-04-21 |
BR112020016665A2 (pt) | 2020-12-15 |
JP7254226B2 (ja) | 2023-04-07 |
JP2022075689A (ja) | 2022-05-18 |
JPWO2019159852A1 (ja) | 2021-01-28 |
EP3753910A4 (en) | 2021-11-17 |
CN111801303B (zh) | 2022-11-08 |
JP7032511B2 (ja) | 2022-03-08 |
CN111801303A (zh) | 2020-10-20 |
US20240150563A1 (en) | 2024-05-09 |
US20200347215A1 (en) | 2020-11-05 |
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