JPWO2017082319A1 - シール剤 - Google Patents
シール剤 Download PDFInfo
- Publication number
- JPWO2017082319A1 JPWO2017082319A1 JP2017550372A JP2017550372A JPWO2017082319A1 JP WO2017082319 A1 JPWO2017082319 A1 JP WO2017082319A1 JP 2017550372 A JP2017550372 A JP 2017550372A JP 2017550372 A JP2017550372 A JP 2017550372A JP WO2017082319 A1 JPWO2017082319 A1 JP WO2017082319A1
- Authority
- JP
- Japan
- Prior art keywords
- photoelectric conversion
- agent
- sealing agent
- conversion elements
- thermosetting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000565 sealant Substances 0.000 title description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 128
- 238000006243 chemical reaction Methods 0.000 claims abstract description 103
- 238000007789 sealing Methods 0.000 claims abstract description 95
- 239000003822 epoxy resin Substances 0.000 claims abstract description 60
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 60
- 150000001412 amines Chemical class 0.000 claims abstract description 45
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 29
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 10
- LLEASVZEQBICSN-UHFFFAOYSA-N 2-undecyl-1h-imidazole Chemical compound CCCCCCCCCCCC1=NC=CN1 LLEASVZEQBICSN-UHFFFAOYSA-N 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 5
- 229910002026 crystalline silica Inorganic materials 0.000 claims abstract description 5
- 239000005350 fused silica glass Substances 0.000 claims abstract description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 5
- UHNWOJJPXCYKCG-UHFFFAOYSA-L magnesium oxalate Chemical compound [Mg+2].[O-]C(=O)C([O-])=O UHNWOJJPXCYKCG-UHFFFAOYSA-L 0.000 claims abstract description 4
- 239000004065 semiconductor Substances 0.000 claims description 44
- 238000012546 transfer Methods 0.000 claims description 36
- 150000001875 compounds Chemical class 0.000 claims description 14
- 150000002460 imidazoles Chemical class 0.000 claims description 8
- SIWAMVWVZFSANK-UHFFFAOYSA-N 2-(oxiran-2-yl)ethoxysilane Chemical class [SiH3]OCCC1CO1 SIWAMVWVZFSANK-UHFFFAOYSA-N 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- HRXKFBUJRIYOTJ-UHFFFAOYSA-N 3-(oxiran-2-yl)propoxysilane Chemical group C(C1CO1)CCO[SiH3] HRXKFBUJRIYOTJ-UHFFFAOYSA-N 0.000 claims description 2
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims 3
- 230000005693 optoelectronics Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 45
- 239000000975 dye Substances 0.000 description 39
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical class C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 21
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 20
- 239000000758 substrate Substances 0.000 description 20
- 239000002904 solvent Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 238000001723 curing Methods 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- 239000003792 electrolyte Substances 0.000 description 13
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 12
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 12
- 229920003986 novolac Polymers 0.000 description 11
- -1 p-hydroxyl Tophenone Chemical compound 0.000 description 11
- 239000010419 fine particle Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 239000002002 slurry Substances 0.000 description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000004593 Epoxy Substances 0.000 description 8
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 238000011109 contamination Methods 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 7
- 239000000460 chlorine Substances 0.000 description 7
- 229910052801 chlorine Inorganic materials 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 229910052736 halogen Inorganic materials 0.000 description 7
- 238000007654 immersion Methods 0.000 description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 7
- 230000001235 sensitizing effect Effects 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 150000002367 halogens Chemical class 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 6
- OOWFYDWAMOKVSF-UHFFFAOYSA-N 3-methoxypropanenitrile Chemical compound COCCC#N OOWFYDWAMOKVSF-UHFFFAOYSA-N 0.000 description 5
- 239000010408 film Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 238000007650 screen-printing Methods 0.000 description 5
- 230000008961 swelling Effects 0.000 description 5
- JECYUBVRTQDVAT-UHFFFAOYSA-N 2-acetylphenol Chemical compound CC(=O)C1=CC=CC=C1O JECYUBVRTQDVAT-UHFFFAOYSA-N 0.000 description 4
- VPWNQTHUCYMVMZ-UHFFFAOYSA-N 4,4'-sulfonyldiphenol Chemical compound C1=CC(O)=CC=C1S(=O)(=O)C1=CC=C(O)C=C1 VPWNQTHUCYMVMZ-UHFFFAOYSA-N 0.000 description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 description 4
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- IMHDGJOMLMDPJN-UHFFFAOYSA-N biphenyl-2,2'-diol Chemical compound OC1=CC=CC=C1C1=CC=CC=C1O IMHDGJOMLMDPJN-UHFFFAOYSA-N 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 239000000434 metal complex dye Substances 0.000 description 4
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 4
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 4
- 150000001451 organic peroxides Chemical class 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000003566 sealing material Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 3
- 235000019416 cholic acid Nutrition 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- KXGVEGMKQFWNSR-UHFFFAOYSA-N deoxycholic acid Natural products C1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 KXGVEGMKQFWNSR-UHFFFAOYSA-N 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000002612 dispersion medium Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000003365 glass fiber Substances 0.000 description 3
- 230000005525 hole transport Effects 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Inorganic materials [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 150000002989 phenols Chemical class 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000011342 resin composition Substances 0.000 description 3
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- 125000006850 spacer group Chemical group 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 150000003505 terpenes Chemical class 0.000 description 3
- 235000007586 terpenes Nutrition 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BHQCQFFYRZLCQQ-UHFFFAOYSA-N (3alpha,5alpha,7alpha,12alpha)-3,7,12-trihydroxy-cholan-24-oic acid Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)C(O)C2 BHQCQFFYRZLCQQ-UHFFFAOYSA-N 0.000 description 2
- RUDATBOHQWOJDD-UHFFFAOYSA-N (3beta,5beta,7alpha)-3,7-Dihydroxycholan-24-oic acid Natural products OC1CC2CC(O)CCC2(C)C2C1C1CCC(C(CCC(O)=O)C)C1(C)CC2 RUDATBOHQWOJDD-UHFFFAOYSA-N 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical group C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 2
- MODAACUAXYPNJH-UHFFFAOYSA-N 1-(methoxymethyl)-4-[4-(methoxymethyl)phenyl]benzene Chemical group C1=CC(COC)=CC=C1C1=CC=C(COC)C=C1 MODAACUAXYPNJH-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical class C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-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
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical compound OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- YTWBFUCJVWKCCK-UHFFFAOYSA-N 2-heptadecyl-1h-imidazole Chemical compound CCCCCCCCCCCCCCCCCC1=NC=CN1 YTWBFUCJVWKCCK-UHFFFAOYSA-N 0.000 description 2
- QKPVEISEHYYHRH-UHFFFAOYSA-N 2-methoxyacetonitrile Chemical compound COCC#N QKPVEISEHYYHRH-UHFFFAOYSA-N 0.000 description 2
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 2
- VEORPZCZECFIRK-UHFFFAOYSA-N 3,3',5,5'-tetrabromobisphenol A Chemical compound C=1C(Br)=C(O)C(Br)=CC=1C(C)(C)C1=CC(Br)=C(O)C(Br)=C1 VEORPZCZECFIRK-UHFFFAOYSA-N 0.000 description 2
- VWIIJDNADIEEDB-UHFFFAOYSA-N 3-methyl-1,3-oxazolidin-2-one Chemical compound CN1CCOC1=O VWIIJDNADIEEDB-UHFFFAOYSA-N 0.000 description 2
- TXFPEBPIARQUIG-UHFFFAOYSA-N 4'-hydroxyacetophenone Chemical compound CC(=O)C1=CC=C(O)C=C1 TXFPEBPIARQUIG-UHFFFAOYSA-N 0.000 description 2
- HDPBBNNDDQOWPJ-UHFFFAOYSA-N 4-[1,2,2-tris(4-hydroxyphenyl)ethyl]phenol Chemical compound C1=CC(O)=CC=C1C(C=1C=CC(O)=CC=1)C(C=1C=CC(O)=CC=1)C1=CC=C(O)C=C1 HDPBBNNDDQOWPJ-UHFFFAOYSA-N 0.000 description 2
- WFCQTAXSWSWIHS-UHFFFAOYSA-N 4-[bis(4-hydroxyphenyl)methyl]phenol Chemical compound C1=CC(O)=CC=C1C(C=1C=CC(O)=CC=1)C1=CC=C(O)C=C1 WFCQTAXSWSWIHS-UHFFFAOYSA-N 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- IXCOKTMGCRJMDR-UHFFFAOYSA-N 9h-fluorene;phenol Chemical compound OC1=CC=CC=C1.OC1=CC=CC=C1.C1=CC=C2CC3=CC=CC=C3C2=C1 IXCOKTMGCRJMDR-UHFFFAOYSA-N 0.000 description 2
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- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000004380 Cholic acid Substances 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 2
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- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
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- BHQCQFFYRZLCQQ-OELDTZBJSA-N cholic acid Chemical compound C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)[C@@H](O)C1 BHQCQFFYRZLCQQ-OELDTZBJSA-N 0.000 description 2
- 229960002471 cholic acid Drugs 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- WHGNXNCOTZPEEK-UHFFFAOYSA-N dimethoxy-methyl-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](C)(OC)CCCOCC1CO1 WHGNXNCOTZPEEK-UHFFFAOYSA-N 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 238000007606 doctor blade method Methods 0.000 description 2
- SEQGYYCJHIYNRE-UHFFFAOYSA-N ethoxy(oxiran-2-ylmethyl)silane Chemical class CCO[SiH2]CC1CO1 SEQGYYCJHIYNRE-UHFFFAOYSA-N 0.000 description 2
- 239000005038 ethylene vinyl acetate Substances 0.000 description 2
- 150000002366 halogen compounds Chemical class 0.000 description 2
- 238000013007 heat curing Methods 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
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- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 150000002148 esters Chemical class 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
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
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- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 1
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- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 239000004845 glycidylamine epoxy resin Substances 0.000 description 1
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- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 229920000193 polymethacrylate Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920006295 polythiol Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
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- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
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- 239000004576 sand Substances 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- NRHMKIHPTBHXPF-TUJRSCDTSA-M sodium cholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 NRHMKIHPTBHXPF-TUJRSCDTSA-M 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- CURCMGVZNYCRNY-UHFFFAOYSA-N trimethylazanium;iodide Chemical compound I.CN(C)C CURCMGVZNYCRNY-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- RUDATBOHQWOJDD-UZVSRGJWSA-N ursodeoxycholic acid Chemical compound C([C@H]1C[C@@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(O)=O)C)[C@@]2(C)CC1 RUDATBOHQWOJDD-UZVSRGJWSA-N 0.000 description 1
- 229960001661 ursodiol Drugs 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000001018 xanthene dye Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—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
- 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
- H01L31/042—PV modules or arrays of single PV cells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—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
- 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
- H01L31/042—PV modules or arrays of single PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
Description
即ち、本発明の各態様は、以下のとおりである。
[1].(a)エポキシ樹脂及び(b)熱硬化剤としてアミン類を含有することを特徴とする、光電子変換素子用シール剤。
[2].(a)エポキシ樹脂中のエポキシ基1当量に対して(b)熱硬化剤中の活性水素が0.8〜3.0当量となる量の(b)熱硬化剤を含有する、上記[1]項に記載の光電子変換素子用シール剤。
[3].(b)熱硬化剤がアミンアダクトであることを特徴とする、上記[1]又は[2]項に記載の光電変換素子用シール剤。
[4].(b)熱硬化剤が、グアナミン類及び/又はイミダゾール類の少なくとも1種と、それ以外のアミン類の少なくとも1種とを含む少なくとも2種のアミン類を含む、上記[1]乃至[3]項のいずれか一項に記載の光電変換素子用シール剤。
[5].イミダゾール類が、2−ウンデシルイミダゾールを含むことを特徴とする、上記[4]項に記載の光電変換素子用シール剤。
[6].(c)充填剤を含有する、上記[1]乃至[5]項のいずれか一項に記載の光電変換素子用シール剤。
[7].(c)充填剤が、含水硅酸マグネシウム、炭酸カルシウム、酸化アルミニウム、結晶シリカ及び溶融シリカからなる群から選ばれる1種または2種以上であり、且つその平均粒径が50μm以下である、上記[6]項に記載の光電変換素子用シール剤。
[8].(d)シランカップリング剤を含有する、上記[1]乃至[7]項のいずれか一項に記載の光電変換素子用シール剤。
[9].(d)シランカップリング剤が、グリシジルエトキシシラン類またはグリシジルメトキシシラン類である、上記[8]項に記載の光電変換素子用シール剤。
[10].半導体含有層を有する第一の導電性支持体、該半導体含有層と対向電極とが所定の間隔で対向する位置に設けられた対向電極を有する第二の導電性支持体、第一及び第二の導電性支持体の間隙に挟持された電荷移動層、並びに第一及び第二の導電性支持体の周辺部に設けられ、電荷移動層を包囲するシールを含む光電変換素子であって、該シールが上記[1]乃至[9]項のいずれか一項に記載の光電変換素子用シール剤から形成されたシールである、光電変換素子。
[11].上記[10]項に記載の光電変換素子を有してなる太陽電池。
本発明のシール剤は、別途言及しない限り、熱硬化プロセスにかける前の状態の組成物を指す。
なお、本願における熱硬化剤としては、120℃未満でシール硬化を可能とする硬化剤が好ましく使用できる。より好ましくは、110℃未満でシール硬化を可能とする硬化剤が使用できる。更に好ましくは105℃未満で、最も好ましくは100℃前後で(又は100℃以下で)、シール硬化を可能とする硬化剤が使用できる。
なお、ここで言及される本発明のシール剤の成分としての「アミンアダクト」は、シール剤を熱硬化プロセスにかけることで得られる(a)エポキシ樹脂と(b)アミン類との反応生成物の一つとしてのアミンアダクトを含まない。理論に拘束される意図はないが、このアミンアダクトは、主に熱硬化の温度を低下させる目的で添加されるので、熱硬化にかける前にアダクトの形態である必要がある。
これらの併用できる熱硬化剤の使用量は、本発明のシール剤中の(b)熱硬化剤の総量に対して通常0質量%以上50質量%以下、好ましくは30質量%以下である。一実施形態において、シール剤は、これらの併用できる熱硬化剤(アミン類以外)を含まない。別の実施形態において、シール剤の熱硬化剤は、アミン類(特に好ましくはアミンアダクト類)のみ、又は、グアナミン類もしくはイミダゾール類及びそれ以外のアミン類(特に好ましくはアミンアダクト類)のみからなってよい。
一実施態様として、本発明の光電変換素子用シール剤は、硬化剤として、分子内にチオール基を2個以上有するポリチオール化合物及び分子内にヒドラジド基を2個以上有するポリヒドラジド化合物のいずれか又は両方を含まないものであってよい。
一般に、色素増感型光電変換素子は、色素で増感された半導体含有層を表面に有する第一の導電性支持体(酸化物半導体電極)、対向電極としての第二の導電性支持体、及び電荷移動層を主要な構成要素として構成される。本発明の光電変換素子用シール剤は、第一と第二の導電性支持体を接着し、かつ両支持体間に電荷移動層を保持する目的で用いられる。導電性支持体としては、例えばFTO(フッ素ドープ酸化スズ)、ATO(アンチモンドープ酸化スズ)、ITO(インジウムドープ酸化スズ)に代表される導電性物質を、ガラス、プラスチック、ポリマーフィルム、石英、シリコン等の基板の表面に薄膜化させたものが用いられる。基板の厚みは、通常0.01〜10mmであり、その形状はフィルム状から板状まで様々な態様を取り得るが、2枚の基板のうち少なくとも一方には光透過性のある基板が用いられる。導電性支持体の導電性は、通常1000Ω/cm2以下、好ましくは100Ω/cm2以下である。
また、色素を担持させた後、4−t−ブチルピリジン等のアミン化合物で半導体含有層を処理しても良い。処理方法は、例えばアミン化合物のエタノール溶液に色素を担持した半導体含有層が設けられた導電性支持体を浸す方法等が採られる。
まず、スペーサー(間隙制御材)を添加した本発明のシール剤を、いずれか一方の導電性支持体の導電面の周辺部に、電荷移動層の注入口を残してディスペンサー、スクリーン印刷機等により堰状に塗布した後、第一と第二の導電性支持体の導電面が対面するように他方の導電性支持体を重ね合わせ、加熱してシール剤を硬化させることができる。ここでスペーサーとしては、例えばグラスファイバー、シリカビーズ、ポリマービーズ等、さらには金パール、銀パール等の金属コーティングした微粒子等が用いられる。その平均直径は、目的に応じて異なるが、通常1〜100μm、好ましくは10〜40μmである。その使用量は、本発明のシール剤100質量部に対し通常0.1〜10質量部、好ましくは0.5〜5質量部、更に、好ましくは1〜2.5質量部である。シール剤の加熱硬化の条件は、通常80〜120℃で1〜3時間である。尚、加熱硬化の方法としては、熱盤を2枚有する熱プレス機でサンドイッチ上に挟んで行う方法、冶具で固定した後オーブン中で行なう方法等が採用できる。第一と第二の導電性支持体の間隙は通常1〜100μm、好ましくは4〜50μmである。
(a)エポキシ樹脂としてRE−310S(商品名、ビスフェノールA型エポキシ樹脂、日本化薬株式会社製、エポキシ当量185g/eq.、加水分解塩素量400ppm以下)90質量部にEP−1001(商品名、ビスフェノールA型エポキシ樹脂、三菱化学株式会社製、エポキシ当量475g/eq.)10質量部を添加して加熱溶解させた。このエポキシ樹脂を室温まで冷却後、(c)充填剤としてSSP−07DM(商品名、表面処理シリカ、最大粒径が0.7μm)90質量部、(d)シランカップリング剤としてKBM−403(商品名、エポキシシランカップリング剤(γ−グリシドキシプロピルトリメトキシシラン)、信越シリコーン株式会社製)1質量部を添加して3本ロールにより混合分散し、(b)熱硬化剤としてPN−31(商品名、エポキシ樹脂アミンアダクト、味の素ファインテクノ株式会社製、平均粒径8.8μm)20質量部を添加してさらに3本ロールにより混合分散して、本発明の光電変換素子用シール剤(1)を得た。このシール剤(1)の25℃における粘度をE型粘度計で測定したところ、73Pa・sであった。
(a)エポキシ樹脂としてRE−310Sの70質量部、EPPN−501H(商品名、トリスフェノールメタンノボラック型エポキシ樹脂、日本化薬株式会社製、エポキシ当量165g/eq.、加水分解塩素量550ppm以下)20質量部及びYD−017(商品名、ビスフェノールA型固形エポキシ樹脂、東都化成工業株式会社製、エポキシ当量1900g/eq.)10質量部、(b)熱硬化剤としてPN−152(商品名、フェノールノボラック樹脂、日本化薬株式会社製、活性水素当量100g/eq.)7.5質量部、(d)シランカップリング剤としてKBM−403の1質量部、を溶剤としてエチレングリコールジブチルエーテル30質量部に加熱溶解させた。この溶解液を室温まで冷却後、さらに、(b)熱硬化剤としてイソフタル酸ジヒドラジドのジェットミルで微粉砕したもの(融点224℃、活性水素当量48.5g/eq.、平均粒径1.7μm、最大粒径7μm)19質量部、(c)充填剤として平均粒径が0.5μm以下のアルミナを90質量部及びフュームドシリカを3.5質量部、を添加して3本ロールにより混合分散し、ここに硬化促進剤として平均粒径が3μm以下の2,4−ジアミノ−6−[2’−メチルイミダゾリル−(1’)]−エチル−s−トリアジンイソシアヌル酸付加物の5質量部を添加して光電変換素子用シール剤(2)を得た。このシール剤(2)の25℃における粘度をE型粘度計で測定したところ47Pa・sであった。
実施例1における(a)RE−310Sの90質量部を80質量部に変更し、新たに多官能エポキシ樹脂EPPN−501(商品名、トリスフェノールメタンノボラック型エポキシ樹脂、日本化薬株式会社製、エポキシ当量165g/eq.、加水分解塩素量550ppm以下)10部を添加し、(d)シランカップリング剤としてKBM−403の1質量部を3質量部に変更し、(b)熱硬化剤としてC11Z(商品名、2−ウンデシルイミダゾール、四国化成株式会社製)3質量部を加えること以外は実施例1と同様にして、本発明の光電変換素子用シール剤(3)を得た。このシール剤(3)の25℃における粘度をE型粘度計で測定したところ278Pa・sであった。
実施例1における(a)RE−310Sの90質量部を80質量部に変更し、新たに多官能エポキシ樹脂EPPN−501(商品名、トリスフェノールメタンノボラック型エポキシ樹脂、日本化薬株式会社製、エポキシ当量165g/eq.、加水分解塩素量550ppm以下)10部を加えること以外は実施例1と同様にして、本発明の光電変換素子用シール剤(4)を得た。このシール剤(4)の25℃における粘度をE型粘度計で測定したところ443Pa・sであった。
実施例1における(d)シランカップリング剤としてKBM−403の1質量部を3質量部に変更する以外は実施例1と同様にして、本発明の光電変換素子用シール剤(5)を得た。このシール剤(5)の25℃における粘度をE型粘度計で測定したところ31Pa・sであった。
実施例1における(b)熱硬化剤としてC11Z(商品名、2−ウンデシルイミダゾール、四国化成株式会社製)3質量部を加えること以外は実施例1と同様にして、本発明の光電変換素子用シール剤(6)を得た。このシール剤(6)の25℃における粘度をE型粘度計で測定したところ80Pa・sであった。
実施例1、3、4、5及び比較例1で作製した各シール剤の性能評価として、せん断接着強度を測定した。また、実施例2及び比較例1で作製した各シール剤の性能評価として、対溶媒膨潤度測定を実施した。
各シール剤100質量部にスペーサーとして直径50μmのグラスファイバー1質量部を添加して混合撹拌を行った。このシール剤を50mm×50mmの導電性支持体(FTOガラス基板)上にディスペンサーで塗布し、ホットプレートによる加熱で溶剤を揮発させた後、導電性支持体上のシール剤上に2mm×2mmのガラス片を貼り合わせて100℃下1時間の条件で硬化させ、得られた試験片のせん断接着強度を測定した。
各シール剤をアプリケーター(膜厚200μm)を用いて耐熱フィルム上に塗布し、100℃下1時間の条件で硬化させた。得られた硬化膜に対して3cm×3cmのパンチ刃を適用して打ち抜き試験片を4枚作製した。各試験片の質量(浸漬前質量)を測定した後、3−メトキシプロピオニトリル(3MPN)と共に耐圧容器に入れ,耐圧容器を85℃下2時間加熱した。加熱終了後、耐圧容器を室温まで冷却し、取り出した試験片に付着している3MPNをふき取り、試験片の質量(浸漬後質量)を測定した。{(浸漬後質量/浸漬前質量)−1}×100の計算から溶媒浸漬前後の質量増加率を求め、4枚の質量増加率の平均値を膨潤度(%)とした。
2.色素によって増感された半導体含有層
3.対向電極
4.電荷移動層
5.シール剤
6.ガラス基板
Claims (11)
- (a)エポキシ樹脂及び(b)熱硬化剤としてアミン類を含有することを特徴とする、光電子変換素子用シール剤。
- (a)エポキシ樹脂中のエポキシ基1当量に対して(b)熱硬化剤中の活性水素が0.8〜3.0当量となる量の(b)熱硬化剤を含有する、請求項1に記載の光電子変換素子用シール剤。
- (b)熱硬化剤がアミンアダクトであることを特徴とする、請求項1または2に記載の光電変換素子用シール剤。
- (b)熱硬化剤が、グアナミン類及び/又はイミダゾール類の少なくとも1種と、それ以外のアミン類の少なくとも1種とを含む少なくとも2種のアミン類を含む、請求項1乃至3のいずれか一項に記載の光電変換素子用シール剤。
- イミダゾール類が、2−ウンデシルイミダゾールを含むことを特徴とする、請求項4に記載の光電変換素子用シール剤。
- (c)充填剤を含有する、請求項1乃至5のいずれか一項に記載の光電変換素子用シール剤。
- (c)充填剤が、含水硅酸マグネシウム、炭酸カルシウム、酸化アルミニウム、結晶シリカ及び溶融シリカからなる群から選ばれる1種または2種以上であり、且つその平均粒径が50μm以下である、請求項6に記載の光電変換素子用シール剤。
- (d)シランカップリング剤を含有する、請求項1乃至7のいずれか一項に記載の光電変換素子用シール剤。
- (d)シランカップリング剤が、グリシジルエトキシシラン類またはグリシジルメトキシシラン類である、請求項8に記載の光電変換素子用シール剤。
- 半導体含有層を有する第一の導電性支持体、該半導体含有層と対向電極とが所定の間隔で対向する位置に設けられた対向電極を有する第二の導電性支持体、第一及び第二の導電性支持体の間隙に挟持された電荷移動層、並びに第一及び第二の導電性支持体の周辺部に設けられ、電荷移動層を包囲するシールを含む光電変換素子であって、該シールが請求項1乃至9のいずれか一項に記載の光電変換素子用シール剤から形成されたシールである、光電変換素子。
- 請求項10に記載の光電変換素子を有してなる太陽電池。
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