WO2014178254A1 - 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 - Google Patents
封止フィルム、その製造方法及び封止フィルムで封止された機能素子 Download PDFInfo
- Publication number
- WO2014178254A1 WO2014178254A1 PCT/JP2014/059623 JP2014059623W WO2014178254A1 WO 2014178254 A1 WO2014178254 A1 WO 2014178254A1 JP 2014059623 W JP2014059623 W JP 2014059623W WO 2014178254 A1 WO2014178254 A1 WO 2014178254A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- gas barrier
- barrier layer
- layer
- sealing film
- resin
- Prior art date
Links
- 238000007789 sealing Methods 0.000 title claims abstract description 127
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 52
- 230000004888 barrier function Effects 0.000 claims abstract description 216
- 229920005989 resin Polymers 0.000 claims abstract description 94
- 239000011347 resin Substances 0.000 claims abstract description 94
- 238000000576 coating method Methods 0.000 claims abstract description 78
- 239000011248 coating agent Substances 0.000 claims abstract description 68
- 239000002608 ionic liquid Substances 0.000 claims abstract description 44
- 229920001709 polysilazane Polymers 0.000 claims abstract description 44
- 238000001035 drying Methods 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 15
- 238000012986 modification Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 243
- -1 aluminum compound Chemical class 0.000 claims description 156
- 238000000034 method Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 38
- 229910052782 aluminium Inorganic materials 0.000 claims description 20
- 150000002500 ions Chemical class 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 8
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 7
- 229910001882 dioxygen Inorganic materials 0.000 claims description 7
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 claims description 4
- 238000007740 vapor deposition Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 6
- 239000010410 layer Substances 0.000 description 343
- 239000010408 film Substances 0.000 description 183
- 239000000243 solution Substances 0.000 description 50
- 230000015572 biosynthetic process Effects 0.000 description 43
- 238000009826 distribution Methods 0.000 description 43
- 239000003822 epoxy resin Substances 0.000 description 36
- 229920000647 polyepoxide Polymers 0.000 description 36
- 239000000758 substrate Substances 0.000 description 35
- 229910052799 carbon Inorganic materials 0.000 description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 28
- 239000001301 oxygen Substances 0.000 description 28
- 229910052760 oxygen Inorganic materials 0.000 description 28
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 21
- 238000005259 measurement Methods 0.000 description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 18
- 239000002904 solvent Substances 0.000 description 17
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 16
- 239000000523 sample Substances 0.000 description 16
- 229910052710 silicon Inorganic materials 0.000 description 16
- 239000010703 silicon Substances 0.000 description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 14
- 230000005525 hole transport Effects 0.000 description 14
- 239000000203 mixture Substances 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 13
- 238000002347 injection Methods 0.000 description 13
- 239000007924 injection Substances 0.000 description 13
- 239000002346 layers by function Substances 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 229910044991 metal oxide Inorganic materials 0.000 description 12
- 150000004706 metal oxides Chemical class 0.000 description 12
- 229920001187 thermosetting polymer Polymers 0.000 description 12
- 150000001768 cations Chemical class 0.000 description 11
- 125000000217 alkyl group Chemical group 0.000 description 10
- 125000004432 carbon atom Chemical group C* 0.000 description 10
- 230000035699 permeability Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 230000006866 deterioration Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 238000004544 sputter deposition Methods 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 8
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 8
- 238000005530 etching Methods 0.000 description 8
- 230000006870 function Effects 0.000 description 8
- 239000011521 glass Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 7
- 125000003118 aryl group Chemical group 0.000 description 7
- 238000000605 extraction Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 150000003377 silicon compounds Chemical class 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 150000001450 anions Chemical class 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000011342 resin composition Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 5
- 229940024606 amino acid Drugs 0.000 description 5
- 235000001014 amino acid Nutrition 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 5
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000011368 organic material Substances 0.000 description 5
- 239000002985 plastic film Substances 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 229920001721 polyimide Polymers 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052814 silicon oxide Inorganic materials 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- AKSROGHADDORBX-UHFFFAOYSA-M 2-acetamidoacetate;tetrabutylphosphanium Chemical compound CC(=O)NCC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC AKSROGHADDORBX-UHFFFAOYSA-M 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 4
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Natural products NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 4
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical class CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- OKJIRPAQVSHGFK-UHFFFAOYSA-N acetylaminoacetic acid Natural products CC(=O)NCC(O)=O OKJIRPAQVSHGFK-UHFFFAOYSA-N 0.000 description 4
- 239000004305 biphenyl Substances 0.000 description 4
- 235000010290 biphenyl Nutrition 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 238000005401 electroluminescence Methods 0.000 description 4
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 description 4
- 239000000395 magnesium oxide Substances 0.000 description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 150000007524 organic acids Chemical group 0.000 description 4
- 125000004430 oxygen atom Chemical group O* 0.000 description 4
- 229920006255 plastic film Polymers 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- NQTSHWFAOMOLDB-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;formate Chemical compound [O-]C=O.CC[N+]=1C=CN(C)C=1 NQTSHWFAOMOLDB-UHFFFAOYSA-M 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000004471 Glycine Substances 0.000 description 3
- QIAFMBKCNZACKA-UHFFFAOYSA-N Hippuric acid Natural products OC(=O)CNC(=O)C1=CC=CC=C1 QIAFMBKCNZACKA-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 208000002564 X-linked cardiac valvular dysplasia Diseases 0.000 description 3
- OBOXTJCIIVUZEN-UHFFFAOYSA-N [C].[O] Chemical compound [C].[O] OBOXTJCIIVUZEN-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 229960003767 alanine Drugs 0.000 description 3
- 235000004279 alanine Nutrition 0.000 description 3
- 125000002723 alicyclic group Chemical group 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000013522 chelant Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- NEXSMEBSBIABKL-UHFFFAOYSA-N hexamethyldisilane Chemical compound C[Si](C)(C)[Si](C)(C)C NEXSMEBSBIABKL-UHFFFAOYSA-N 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 201000006747 infectious mononucleosis Diseases 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000004843 novolac epoxy resin Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 229920005668 polycarbonate resin Polymers 0.000 description 3
- 239000004431 polycarbonate resin Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BJQWBACJIAKDTJ-UHFFFAOYSA-N tetrabutylphosphanium Chemical compound CCCC[P+](CCCC)(CCCC)CCCC BJQWBACJIAKDTJ-UHFFFAOYSA-N 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- XIYUIMLQTKODPS-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CC[N+]=1C=CN(C)C=1 XIYUIMLQTKODPS-UHFFFAOYSA-M 0.000 description 2
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 2
- MCTWTZJPVLRJOU-UHFFFAOYSA-O 1-methylimidazole Chemical class CN1C=C[NH+]=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-O 0.000 description 2
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical group C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 description 2
- MFYNHXMPPRNECN-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine;phenol Chemical class OC1=CC=CC=C1.C1CCCCN2CCCN=C21 MFYNHXMPPRNECN-UHFFFAOYSA-N 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-L L-tartrate(2-) Chemical compound [O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O FEWJPZIEWOKRBE-JCYAYHJZSA-L 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000004840 adhesive resin Substances 0.000 description 2
- 229920006223 adhesive resin Polymers 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- AGBQKNBQESQNJD-UHFFFAOYSA-N alpha-Lipoic acid Natural products OC(=O)CCCCC1CCSS1 AGBQKNBQESQNJD-UHFFFAOYSA-N 0.000 description 2
- MQQXUGFEQSCYIA-OAWHIZORSA-M aluminum;(z)-4-ethoxy-4-oxobut-2-en-2-olate;propan-2-olate Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CCOC(=O)\C=C(\C)[O-] MQQXUGFEQSCYIA-OAWHIZORSA-M 0.000 description 2
- YNCDEEFMDXHURQ-UHFFFAOYSA-N aluminum;ethyl 3-oxobutanoate Chemical compound [Al].CCOC(=O)CC(C)=O YNCDEEFMDXHURQ-UHFFFAOYSA-N 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 229940009098 aspartate Drugs 0.000 description 2
- 238000007611 bar coating method Methods 0.000 description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 2
- XJHCXCQVJFPJIK-UHFFFAOYSA-M caesium fluoride Chemical compound [F-].[Cs+] XJHCXCQVJFPJIK-UHFFFAOYSA-M 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000011247 coating layer Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 238000002788 crimping Methods 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 2
- 229940093858 ethyl acetoacetate Drugs 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 2
- 238000007646 gravure printing Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 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 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003230 hygroscopic agent Substances 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 235000019136 lipoic acid Nutrition 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229920003986 novolac Polymers 0.000 description 2
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-M phenolate Chemical compound [O-]C1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-M 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 238000002407 reforming Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000007962 solid dispersion Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- 229960002663 thioctic acid Drugs 0.000 description 2
- 125000005369 trialkoxysilyl group Chemical group 0.000 description 2
- 239000013638 trimer Substances 0.000 description 2
- 239000002966 varnish Substances 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- DWDIKSBLKQGHDF-CICJTZRQSA-M (2s)-2-acetamido-3-phenylpropanoate;tetrabutylphosphanium Chemical compound CC(=O)N[C@H](C([O-])=O)CC1=CC=CC=C1.CCCC[P+](CCCC)(CCCC)CCCC DWDIKSBLKQGHDF-CICJTZRQSA-M 0.000 description 1
- ZQMBCBBSUSLRKI-WNQIDUERSA-M (2s)-2-amino-4-hydroxy-4-oxobutanoate;tetrabutylphosphanium Chemical compound [O-]C(=O)[C@@H](N)CC(O)=O.CCCC[P+](CCCC)(CCCC)CCCC ZQMBCBBSUSLRKI-WNQIDUERSA-M 0.000 description 1
- KWEKXPWNFQBJAY-UHFFFAOYSA-N (dimethyl-$l^{3}-silanyl)oxy-dimethylsilicon Chemical compound C[Si](C)O[Si](C)C KWEKXPWNFQBJAY-UHFFFAOYSA-N 0.000 description 1
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- ISHFYECQSXFODS-UHFFFAOYSA-M 1,2-dimethyl-3-propylimidazol-1-ium;iodide Chemical compound [I-].CCCN1C=C[N+](C)=C1C ISHFYECQSXFODS-UHFFFAOYSA-M 0.000 description 1
- YJTKZCDBKVTVBY-UHFFFAOYSA-N 1,3-Diphenylbenzene Chemical group C1=CC=CC=C1C1=CC=CC(C=2C=CC=CC=2)=C1 YJTKZCDBKVTVBY-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- HYYJOCXNESGFSB-UHFFFAOYSA-N 1-(oxiran-2-yl)-n-(oxiran-2-ylmethyl)methanamine Chemical compound C1OC1CNCC1CO1 HYYJOCXNESGFSB-UHFFFAOYSA-N 0.000 description 1
- FBHPRUXJQNWTEW-UHFFFAOYSA-N 1-benzyl-2-methylimidazole Chemical compound CC1=NC=CN1CC1=CC=CC=C1 FBHPRUXJQNWTEW-UHFFFAOYSA-N 0.000 description 1
- XZKLXPPYISZJCV-UHFFFAOYSA-N 1-benzyl-2-phenylimidazole Chemical compound C1=CN=C(C=2C=CC=CC=2)N1CC1=CC=CC=C1 XZKLXPPYISZJCV-UHFFFAOYSA-N 0.000 description 1
- CYFFKUDZLZREEX-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;2-hydroxypropanoate Chemical compound CC(O)C([O-])=O.CCCC[N+]=1C=CN(C)C=1 CYFFKUDZLZREEX-UHFFFAOYSA-M 0.000 description 1
- RJCLZEKYUQKDAL-WNQIDUERSA-M 1-ethyl-3-methylimidazol-3-ium;(2s)-2-hydroxypropanoate Chemical compound C[C@H](O)C([O-])=O.CCN1C=C[N+](C)=C1 RJCLZEKYUQKDAL-WNQIDUERSA-M 0.000 description 1
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 description 1
- NBUKAOOFKZFCGD-UHFFFAOYSA-N 2,2,3,3-tetrafluoropropan-1-ol Chemical compound OCC(F)(F)C(F)F NBUKAOOFKZFCGD-UHFFFAOYSA-N 0.000 description 1
- GQHTUMJGOHRCHB-UHFFFAOYSA-N 2,3,4,6,7,8,9,10-octahydropyrimido[1,2-a]azepine Chemical compound C1CCCCN2CCCN=C21 GQHTUMJGOHRCHB-UHFFFAOYSA-N 0.000 description 1
- DDAGEIJSXQDDKX-UHFFFAOYSA-L 2,3-dihydroxybutanedioate;tetrabutylphosphanium Chemical compound [O-]C(=O)C(O)C(O)C([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC.CCCC[P+](CCCC)(CCCC)CCCC DDAGEIJSXQDDKX-UHFFFAOYSA-L 0.000 description 1
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
- FRTOXZBDQNPXDU-UHFFFAOYSA-M 2-[benzoyl(methyl)amino]acetate;tetrabutylphosphanium Chemical compound [O-]C(=O)CN(C)C(=O)C1=CC=CC=C1.CCCC[P+](CCCC)(CCCC)CCCC FRTOXZBDQNPXDU-UHFFFAOYSA-M 0.000 description 1
- KBAPFNXJKSYUBJ-UHFFFAOYSA-M 2-acetamidoacetate;1-ethyl-3-methylimidazol-3-ium Chemical compound CC[N+]=1C=CN(C)C=1.CC(=O)NCC([O-])=O KBAPFNXJKSYUBJ-UHFFFAOYSA-M 0.000 description 1
- KZECYDSUKLPVOF-UHFFFAOYSA-M 2-aminoacetate;tetrabutylphosphanium Chemical compound NCC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC KZECYDSUKLPVOF-UHFFFAOYSA-M 0.000 description 1
- YWMVIXRVDXTEFL-UHFFFAOYSA-M 2-benzamidopropanoate;tetrabutylphosphanium Chemical compound [O-]C(=O)C(C)NC(=O)C1=CC=CC=C1.CCCC[P+](CCCC)(CCCC)CCCC YWMVIXRVDXTEFL-UHFFFAOYSA-M 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- PVQBTSVRNJNNLV-UHFFFAOYSA-M 2-hydroxypropanoate;tetrabutylphosphanium Chemical compound CC(O)C([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC PVQBTSVRNJNNLV-UHFFFAOYSA-M 0.000 description 1
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 1
- 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 1
- CXXSQMDHHYTRKY-UHFFFAOYSA-N 4-amino-2,3,5-tris(oxiran-2-ylmethyl)phenol Chemical compound C1=C(O)C(CC2OC2)=C(CC2OC2)C(N)=C1CC1CO1 CXXSQMDHHYTRKY-UHFFFAOYSA-N 0.000 description 1
- YJEUORONVNFKJX-UHFFFAOYSA-M 5-oxopyrrolidine-2-carboxylate;tetrabutylphosphanium Chemical compound [O-]C(=O)C1CCC(=O)N1.CCCC[P+](CCCC)(CCCC)CCCC YJEUORONVNFKJX-UHFFFAOYSA-M 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical group CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- SLBGTSBCTWNRMX-UHFFFAOYSA-M CCn1cc[n+](C)c1.CN(CC([O-])=O)C(=O)c1ccccc1 Chemical compound CCn1cc[n+](C)c1.CN(CC([O-])=O)C(=O)c1ccccc1 SLBGTSBCTWNRMX-UHFFFAOYSA-M 0.000 description 1
- MOIOYLNJXGOCNR-UHFFFAOYSA-M C[N+]1(CCCC1)C.C(C)(=O)NCC(=O)[O-] Chemical compound C[N+]1(CCCC1)C.C(C)(=O)NCC(=O)[O-] MOIOYLNJXGOCNR-UHFFFAOYSA-M 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-O Imidazolium Chemical compound C1=C[NH+]=CN1 RAXXELZNTBOGNW-UHFFFAOYSA-O 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 1
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- 229910013528 LiN(SO2 CF3)2 Inorganic materials 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 1
- PKCSYDDSNIJRIX-UHFFFAOYSA-N N-methylhippuric acid Chemical compound OC(=O)CN(C)C(=O)C1=CC=CC=C1 PKCSYDDSNIJRIX-UHFFFAOYSA-N 0.000 description 1
- 229910020808 NaBF Inorganic materials 0.000 description 1
- ZOPVZDIHLDQBRB-UHFFFAOYSA-N P(OC(C(F)(F)F)(F)F)(O)=O Chemical compound P(OC(C(F)(F)F)(F)F)(O)=O ZOPVZDIHLDQBRB-UHFFFAOYSA-N 0.000 description 1
- 229920000144 PEDOT:PSS Polymers 0.000 description 1
- 241000199911 Peridinium Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004697 Polyetherimide Substances 0.000 description 1
- 229910007991 Si-N Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 229910006294 Si—N Inorganic materials 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 1
- 125000004062 acenaphthenyl group Chemical group C1(CC2=CC=CC3=CC=CC1=C23)* 0.000 description 1
- 125000004054 acenaphthylenyl group Chemical group C1(=CC2=CC=CC3=CC=CC1=C23)* 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-M acetoacetate Chemical compound CC(=O)CC([O-])=O WDJHALXBUFZDSR-UHFFFAOYSA-M 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000005210 alkyl ammonium group Chemical group 0.000 description 1
- 150000001343 alkyl silanes Chemical class 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 1
- IKHOZNOYZQPPCK-UHFFFAOYSA-K aluminum;4,4-diethyl-3-oxohexanoate Chemical compound [Al+3].CCC(CC)(CC)C(=O)CC([O-])=O.CCC(CC)(CC)C(=O)CC([O-])=O.CCC(CC)(CC)C(=O)CC([O-])=O IKHOZNOYZQPPCK-UHFFFAOYSA-K 0.000 description 1
- KEBBHXFLBGHGMA-UHFFFAOYSA-K aluminum;4-ethyl-3-oxohexanoate Chemical compound [Al+3].CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O.CCC(CC)C(=O)CC([O-])=O KEBBHXFLBGHGMA-UHFFFAOYSA-K 0.000 description 1
- GMARCGBNZNYETI-UHFFFAOYSA-N aluminum;oxygen(2-);propan-2-olate Chemical compound [O-2].[Al+3].CC(C)[O-] GMARCGBNZNYETI-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 125000005428 anthryl group Chemical group [H]C1=C([H])C([H])=C2C([H])=C3C(*)=C([H])C([H])=C([H])C3=C([H])C2=C1[H] 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- 125000003828 azulenyl group Chemical group 0.000 description 1
- 125000003236 benzoyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C(*)=O 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 229940006460 bromide ion Drugs 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N butadiene group Chemical group C=CC=C KAKZBPTYRLMSJV-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
- 150000001721 carbon Chemical group 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 125000002676 chrysenyl group Chemical group C1(=CC=CC=2C3=CC=C4C=CC=CC4=C3C=CC12)* 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000004643 cyanate ester Substances 0.000 description 1
- 125000006165 cyclic alkyl group Chemical group 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 125000001559 cyclopropyl group Chemical group [H]C1([H])C([H])([H])C1([H])* 0.000 description 1
- DEKLIKGLDMCMJG-UHFFFAOYSA-M decanoate;tetrabutylphosphanium Chemical compound CCCCCCCCCC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC DEKLIKGLDMCMJG-UHFFFAOYSA-M 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 150000001983 dialkylethers Chemical class 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- UCXUKTLCVSGCNR-UHFFFAOYSA-N diethylsilane Chemical compound CC[SiH2]CC UCXUKTLCVSGCNR-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- WEIQRLLXVVSKIL-UHFFFAOYSA-N ethyl 2,2-diethyl-3-oxobutanoate Chemical compound CCOC(=O)C(CC)(CC)C(C)=O WEIQRLLXVVSKIL-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 125000003914 fluoranthenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC=C4C1=C23)* 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229930195712 glutamate Natural products 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 125000003454 indenyl group Chemical group C1(C=CC2=CC=CC=C12)* 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 1
- 229940006461 iodide ion Drugs 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- FCCDDURTIIUXBY-UHFFFAOYSA-N lipoamide Chemical compound NC(=O)CCCCC1CCSS1 FCCDDURTIIUXBY-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000113 methacrylic resin Substances 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- JAYXSROKFZAHRQ-UHFFFAOYSA-N n,n-bis(oxiran-2-ylmethyl)aniline Chemical compound C1OC1CN(C=1C=CC=CC=1)CC1CO1 JAYXSROKFZAHRQ-UHFFFAOYSA-N 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000003136 n-heptyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052756 noble gas Inorganic materials 0.000 description 1
- 150000002835 noble gases Chemical class 0.000 description 1
- RNVCVTLRINQCPJ-UHFFFAOYSA-N o-toluidine Chemical compound CC1=CC=CC=C1N RNVCVTLRINQCPJ-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 125000001828 phenalenyl group Chemical group C1(C=CC2=CC=CC3=CC=CC1=C23)* 0.000 description 1
- 125000005561 phenanthryl group Chemical group 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- IGALFTFNPPBUDN-UHFFFAOYSA-N phenyl-[2,3,4,5-tetrakis(oxiran-2-ylmethyl)phenyl]methanediamine Chemical compound C=1C(CC2OC2)=C(CC2OC2)C(CC2OC2)=C(CC2OC2)C=1C(N)(N)C1=CC=CC=C1 IGALFTFNPPBUDN-UHFFFAOYSA-N 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- UIDUKLCLJMXFEO-UHFFFAOYSA-N propylsilane Chemical compound CCC[SiH3] UIDUKLCLJMXFEO-UHFFFAOYSA-N 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 125000001725 pyrenyl group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium group Chemical group [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 230000002194 synthesizing 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
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- TXMIUMUSEKVUBH-UHFFFAOYSA-M tetrabutylphosphanium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CCCC[P+](CCCC)(CCCC)CCCC TXMIUMUSEKVUBH-UHFFFAOYSA-M 0.000 description 1
- GFZMLBWMGBLIDI-UHFFFAOYSA-M tetrabutylphosphanium;acetate Chemical compound CC([O-])=O.CCCC[P+](CCCC)(CCCC)CCCC GFZMLBWMGBLIDI-UHFFFAOYSA-M 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- WHDWTYUVZOXXKX-UHFFFAOYSA-M tetrabutylphosphanium;formate Chemical compound [O-]C=O.CCCC[P+](CCCC)(CCCC)CCCC WHDWTYUVZOXXKX-UHFFFAOYSA-M 0.000 description 1
- 125000001935 tetracenyl group Chemical group C1(=CC=CC2=CC3=CC4=CC=CC=C4C=C3C=C12)* 0.000 description 1
- DDFYFBUWEBINLX-UHFFFAOYSA-M tetramethylammonium bromide Chemical compound [Br-].C[N+](C)(C)C DDFYFBUWEBINLX-UHFFFAOYSA-M 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- BRKFQVAOMSWFDU-UHFFFAOYSA-M tetraphenylphosphanium;bromide Chemical compound [Br-].C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 BRKFQVAOMSWFDU-UHFFFAOYSA-M 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 150000004992 toluidines Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 description 1
- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 125000003960 triphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C3=CC=CC=C3C12)* 0.000 description 1
- MDDPTCUZZASZIQ-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] MDDPTCUZZASZIQ-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/84—Passivation; Containers; Encapsulations
- H10K50/844—Encapsulations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- 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
- H01L31/048—Encapsulation of modules
-
- 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
- H01L31/048—Encapsulation of modules
- H01L31/0481—Encapsulation of modules characterised by the composition of the encapsulation material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/26—Polymeric coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/724—Permeability to gases, adsorption
- B32B2307/7242—Non-permeable
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/202—LCD, i.e. liquid crystal displays
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/805—Electrodes
- H10K50/81—Anodes
- H10K50/814—Anodes combined with auxiliary electrodes, e.g. ITO layer combined with metal lines
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to a sealing film, a manufacturing method thereof, and a functional element sealed with the sealing film. More specifically, a sealing film excellent in moisture permeability even if it is used after being stored in a high-humidity environment, its production method, and functions such as an organic electroluminescence element and a solar cell element sealed with the sealing film It relates to an element.
- Functional elements made of organic materials such as organic EL elements and organic thin film solar cells have extremely low resistance to oxygen and moisture.
- the organic material itself is altered by oxygen or moisture, resulting in a decrease in luminance, a non-luminous defect called a dark spot, or a light emission. There is a drawback that it disappears.
- a sealing film composed of a base material and an adhesive resin is used.
- the sealing film is rarely used immediately after production, and is usually used after being stored for several days to several months.
- the moisture permeation resistance deteriorates, and the dark spots are likely to occur when the sealed film after storage is used as a sealing substrate for an organic EL device. I understood it.
- the present invention has been made in view of the above-described problems and situations, and its solution is to provide a sealing film excellent in moisture permeability even when used after being stored in a high-humidity environment, a manufacturing method thereof, and the sealing. It is to provide a functional element sealed with a stop film.
- the present inventor has a gas barrier layer formed by applying a modification treatment to a dried layer by applying a coating liquid containing at least polysilazane in the course of examining the cause of the above-described problem. It was found that by forming a resin layer containing at least an ionic liquid on the sealing film, a sealing film having excellent moisture permeation resistance can be obtained even if used after being stored in a high humidity environment. It came.
- a sealing film comprising a base material, a gas barrier layer formed on one surface of the base material, and a resin layer in this order, wherein the gas barrier layer is coated with a coating liquid containing at least polysilazane.
- a sealing film which is a layer obtained by subjecting a dried layer to a modification treatment, and wherein the resin layer contains at least an ionic liquid.
- Item 1 or Item 2 is characterized in that the ionic liquid contained in the resin layer comprises at least an ammonium cation or a phosphonium cation and an N-acylamino acid ion or a carboxylic acid anion. Sealing film.
- Discharge plasma chemistry having a discharge space between a pair of rollers to which a magnetic field is applied using a source gas containing an organosilicon compound and an oxygen gas on the surface of the base material between the base material and the gas barrier layer.
- the sealing film according to any one of items 1 to 3, wherein a gas barrier layer is further formed by a vapor deposition method.
- Forming a gas barrier layer Applying a resin layer solution containing at least an ionic liquid on the gas barrier layer and drying to form a resin layer; and
- the manufacturing method of the sealing film characterized by having.
- the adhesive resin side in contact with the organic EL element directly touches the atmosphere and absorbs moisture, and this moisture evaporates by heating during solid sealing, causing deterioration of the element and generating dark spots. It is considered that moisture remaining without being allowed to evaporate or to evaporate also causes deterioration of moisture permeability resistance during subsequent storage over time.
- the water absorbing agent contained in the water absorbing layer absorbs the moisture and the influence of moisture on the organic EL element is improved. It was insufficient.
- the ionic liquid contained in the resin layer formed on the sealing film is a hygroscopic agent. As described above, it has the ability to supply moisture to the unmodified portion of the polysilazane remaining in the gas barrier layer at the same time as absorbing the moisture, and the unmodified portion of the polysilazane reacts with the moisture to be modified. It is presumed that this is due to the formation of a gas barrier film with higher moisture resistance that is closer to glass.
- Sectional drawing of the sealing film of this invention The schematic diagram which shows an example of the vacuum plasma CVD apparatus used for formation of the gas barrier layer based on this invention
- Sectional drawing which shows schematic structure of organic EL element Schematic diagram showing an example of vacuum ultraviolet irradiation equipment
- the sealing film of the present invention is a sealing film comprising a gas barrier layer and a resin layer formed on a base material in this order, and the gas barrier layer is dried by applying a coating liquid containing at least polysilazane. And the resin layer contains at least an ionic liquid, and this configuration makes it moisture resistant even when used after being stored in a high humidity environment.
- An excellent sealing film is provided. This feature is a technical feature common to the inventions according to claims 1 to 6.
- the gas barrier layer preferably further contains an aluminum compound, and the ionic liquid contained in the resin layer is at least an ammonium cation or phosphonium. More preferably, it is composed of a cation and an N-acylamino acid ion or a carboxylic acid anion. With this configuration, a sealing film having further improved moisture resistance can be obtained.
- a discharge having a discharge space between a pair of rollers to which a magnetic field is applied between the base material and the gas barrier layer using a source gas containing an organosilicon compound and an oxygen gas on the surface of the base material is preferable that a gas barrier layer is further formed by the plasma chemical vapor deposition method from the viewpoint of further improving the flexibility and gas barrier properties of the sealing film.
- the method for producing a sealing film of the present invention includes a step of applying a coating liquid containing at least polysilazane, subjecting the dried layer to a modification treatment to form a gas barrier layer, and at least an ionic liquid on the gas barrier layer.
- the step of applying and drying the resin layer solution contained to form a resin layer is preferable.
- the functional element sealed with the sealing film of the present invention is preferable because, for example, a stable organic EL element in which generation of dark spots and reduction in luminance are suppressed over time can be obtained.
- ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
- the sealing film of the present invention is a sealing film comprising a base material, a gas barrier layer formed on one surface of the base material, and a resin layer in this order, and the gas barrier layer contains at least polysilazane. It is a layer formed by applying a modification treatment to a layer that has been coated with a coating solution and dried, and the resin layer is a layer containing at least an ionic liquid.
- FIG. 1 is a sectional view showing an example of the sealing film of the present invention.
- the sealing film 1 of the present invention is obtained by forming a gas barrier layer 1b and a resin layer 1c in this order on at least a base material 1a.
- a gas barrier film the form in which the gas barrier layer 1b is formed on the substrate 1a is also referred to as a gas barrier film.
- the surface of the substrate 1a opposite to the gas barrier layer, between the substrate 1a and the gas barrier layer 1b, between the gas barrier layer 1b and the resin layer 1c, and the surface of the resin layer 1c opposite to the gas barrier layer can be formed as long as the effects of the present invention are not impaired.
- a smoothing layer is provided between the base material 1a and the gas barrier layer 1b to smooth the unevenness of the base material surface, or a separator film that can be peeled off on the surface of the resin layer 1c opposite to the gas barrier layer.
- a layer may be provided.
- functional layers such as an intermediate layer, a protective layer, a bleed-out prevention layer, and an antistatic layer can be used.
- gas barrier layer 1b and the resin layer 1c according to the present invention may be composed of a plurality of layers, and the gas barrier layer is preferably formed by laminating a plurality of barrier layers.
- the resin layer according to the present invention is a layer containing at least an ionic liquid, but contains at least a thermosetting resin together with the ionic liquid, and has a function as an adhesive layer when sealing a functional element. Preferably there is.
- the resin layer may contain a hygroscopic metal oxide, an inorganic filler, a curing accelerator, and the like from the viewpoint of moisture permeability.
- the ionic liquid in the present invention is a salt that can melt in a temperature range of 140 ° C. or lower (preferably 120 ° C. or lower). As a function, it absorbs moisture like a hygroscopic agent and at the same time has the ability to supply moisture to the unreacted polysilazane remaining in the gas barrier layer, contributing to the modification of the unreacted portion of the polysilazane. It is preferable.
- the ionic liquid for example, a salt having a curing action of an epoxy resin, which is a thermosetting resin described later, is particularly preferably used, which acts advantageously on improving moisture resistance of a cured product of the resin layer.
- the ionic liquid is preferably used in a state where the ionic liquid is uniformly dissolved in the epoxy resin.
- Examples of cations constituting such an ionic liquid include imidazolium ions, pyrimidinium ions, pyridinium ions, pyrrolidinium ions, piperidinium ions, pyrazonium ions, guanidinium ions and other ammonium cations; tetraalkylphosphonium cations (for example, Phosphonium cations such as tetrabutylphosphonium ion and tributylhexylphosphonium ion; sulfonium cations such as triethylsulfonium ion and the like.
- ammonium cation examples include, for example, 1,3-dimethylimidazolium cation, 1,3-diethylimidazolium cation, 1-ethyl-3-methylimidazolium cation, 1-propyl-3-methylimidazolium ion.
- the cation is preferably an ammonium cation or a phosphonium cation, and more preferably an imidazolium ion or a phosphonium ion.
- anion constituting the ionic liquid examples include halide anions such as fluoride ion, chloride ion, bromide ion and iodide ion; alkyl sulfate anions such as methanesulfonate ion; trifluoromethanesulfonate ion, Fluorine-containing compound anions such as hexafluorophosphonate ion, trifluorotris (pentafluoroethyl) phosphonate ion, bis (trifluoromethanesulfonyl) imide ion, trifluoroacetate ion, tetrafluoroborate ion; phenol ion, 2-methoxy Phenolic anions such as phenol ion and 2,6-di-tert-butylphenol ion; acidic amino acid ions such as aspartate ion and glutamate ion; glycine ion, alan
- R—CO— is an acyl group derived from a linear or branched fatty acid having 1 to 5 carbon atoms, or a substituted or unsubstituted benzoyl group, and —NH—CHX—CO 2 — is aspartic acid.
- Acidic amino acid ions such as glutamic acid, or neutral amino acid ions such as glycine, alanine and phenylalanine.
- the anion is preferably an N-acylamino acid ion or a carboxylic acid anion represented by the general formula (1).
- carboxylate anion examples include acetate ion, decanoate ion, 2-pyrrolidone-5-carboxylate ion, formate ion, ⁇ -lipoic acid ion, lactate ion, tartaric acid ion, hippuric acid ion, and N-methyl horse.
- Uric acid ions and the like are mentioned.
- acetate ion, 2-pyrrolidone-5-carboxylate ion, formate ion, lactate ion, tartrate ion, hippurate ion, N-methyl hippurate ion are preferable
- acetate ion, N-methyl Hippurate ion and formate ion are more preferable.
- N-acylamino acid ion represented by the general formula (1) examples include N-benzoylalanine ion, N-acetylphenylalanine ion, aspartate ion, glycine ion, N-acetylglycine ion, and the like. Of these, N-benzoylalanine ion, N-acetylphenylalanine ion, and N-acetylglycine ion are preferable, and N-acetylglycine ion is more preferable.
- Specific ionic liquids include, for example, 1-butyl-3-methylimidazolium lactate, tetrabutylphosphonium-2-pyrrolidone-5-carboxylate, tetrabutylphosphonium acetate, tetrabutylphosphonium decanoate, tetrabutylphosphonium tri Fluoroacetate, tetrabutylphosphonium ⁇ -lipoate, tetrabutylphosphonium formate, tetrabutylphosphonium lactate, bis (tetrabutylphosphonium) tartrate, tetrabutylphosphonium hippurate, tetrabutylphosphonium N-methylhippurate, benzoyl-DL -Alanine tetrabutylphosphonium salt, N-acetylphenylalanine tetrabutylphosphonium salt, 2,6-di-tert-butylphenoltetrabutylphospho Um salt,
- a precursor composed of a cation moiety such as an alkylimidazolium, alkylpyridinium, alkylammonium and alkylsulfonium ions and an anion moiety containing a halogen is added to NaBF 4 , NaPF 6 , CF 3 SO 3
- the content of the ionic liquid according to the present invention is preferably in the range of 0.1 to 50% by mass, more preferably in the range of 0.5 to 25% by mass with respect to the entire resin layer. If it is in this range, the effect of the present invention is sufficiently obtained, and the storage stability of the resin layer is not impaired.
- the resin contained in the resin layer is preferably a thermosetting resin, and the thermoplastic resin is not particularly limited. Specifically, an epoxy resin, a cyanate ester resin, a phenol resin, a bismaleimide-triazine resin, Various thermosetting resins such as a polyimide resin, an acrylic resin, and a vinyl benzyl resin can be used. Of these, epoxy resins are preferred from the viewpoints of low-temperature curability and adhesiveness.
- epoxy resin those having an average of two or more epoxy groups per molecule may be used.
- bisphenol A type epoxy resin biphenyl type epoxy resin, biphenyl aralkyl type epoxy resin, and naphthol type epoxy are used.
- alicyclic epoxy resin aliphatic chain epoxy resin
- phenol novolac epoxy resin cresol novolac epoxy resin
- bisphenol A novolac epoxy resin Epoxy resin having a butadiene structure, phenol aralkyl type epoxy resin, epoxy resin having a dicyclopentadiene structure, diglycidyl ether
- bisphenol A type epoxy resin bisphenol F type epoxy resin, phenol novolac type epoxy resin, biphenyl aralkyl type epoxy resin, phenol aralkyl type epoxy from the viewpoint of maintaining high heat resistance and low moisture permeability of the resin composition.
- a resin, an aromatic glycidylamine type epoxy resin, an epoxy resin having a dicyclopentadiene structure, and the like are preferable.
- the epoxy resin may be liquid, solid, or both liquid and solid.
- “liquid” and “solid” are states of the epoxy resin at 25 ° C. From the viewpoints of coatability, processability, adhesiveness, etc., it is preferable that 10% by mass or more of the entire epoxy resin to be used is liquid.
- the epoxy resin preferably has an epoxy equivalent in the range of 100 to 1000, more preferably in the range of 120 to 1000, from the viewpoint of reactivity.
- the epoxy equivalent is the number of grams (g / eq) of a resin containing 1 gram equivalent of an epoxy group, and is measured according to the method defined in JIS K-7236.
- the curing agent for the epoxy resin is not particularly limited as long as it has a function of curing the epoxy resin, but from the viewpoint of suppressing thermal deterioration of the element (particularly the organic EL element) during the curing treatment of the resin composition.
- the curing treatment of the composition is preferably performed at 140 ° C. or lower, more preferably 120 ° C. or lower, and the curing agent preferably has an epoxy resin curing action in such a temperature range.
- amine adduct-based compounds Amicure PN-23, Amicure MY-24, Amicure PN-D, Amicure MY-D, Amicure PN-H, Amicure MY-H, Amicure PN-31, Amicure PN-40, Amicure PN-40J, etc. (all Ajinomoto Fine Techno)
- organic acid dihydrazide Amicure VDH-J, Amicure UDH, Amicure LDH, etc. (all manufactured by Ajinomoto Fine Techno Co.)
- these may be used alone or in combination of two or more.
- the resin layer according to the present invention preferably contains a hygroscopic metal oxide from the viewpoint of adjusting moisture permeability.
- the “hygroscopic metal oxide” as used in the present invention is a metal oxide that has the ability to absorb moisture and chemically reacts with moisture that has been absorbed to become a hydroxide, so long as the object of the present invention can be achieved.
- a metal oxide that has the ability to absorb moisture and chemically reacts with moisture that has been absorbed to become a hydroxide, so long as the object of the present invention can be achieved.
- calcined dolomite a mixture containing calcium oxide and magnesium oxide
- calcined hydrotalcite solid solution of calcium oxide and aluminum oxide
- Such a hygroscopic metal oxide is known as a hygroscopic material in various technical fields, and a commercially available product can be used. Specifically, calcined dolomite (such as “KT” manufactured by Yoshizawa Lime Co., Ltd.), calcium oxide (such as “Moystop # 10” manufactured by Sankyo Flour Mills), magnesium oxide (“Kyowa Mag MF-150” manufactured by Kyowa Chemical Industry Co., Ltd.), “ Kyowa Mag MF-30 ”,“ Pure Mag FNMG ”manufactured by Tateho Chemical Industry Co., Ltd.), lightly burned magnesium oxide (“ # 500 ”,“ # 1000 ”,“ # 5000 ”etc. manufactured by Tateho Chemical Industry Co., Ltd.), and the like.
- dolomite such as “KT” manufactured by Yoshizawa Lime Co., Ltd.
- calcium oxide such as “Moystop # 10” manufactured by Sankyo Flour Mills
- magnesium oxide (“Kyowa Mag MF
- the average particle diameter of the hygroscopic metal oxide is not particularly limited, but is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, and even more preferably 1 ⁇ m or less.
- the hygroscopic metal oxide may be a surface treated with a higher fatty acid such as stearic acid, or a surface treatment agent such as a known alkylsilane or silane coupling agent. By performing such surface treatment, it is possible to prevent the moisture in the resin from reacting with the hygroscopic metal oxide.
- the content of the hygroscopic metal oxide in the resin layer is preferably in the range of 1 to 40% by mass with respect to 100% by mass of the nonvolatile content in the resin composition.
- the resin composition constituting the resin layer can further contain a filler having a plate shape in the form of particles such as talc, clay, mica, boehmite and the like, and the moisture resistance of the resin layer can be further enhanced.
- rubber particles can be contained. By containing the rubber particles, the mechanical strength of the resin layer can be improved and the stress can be relaxed.
- core-shell type rubber particles are preferably used. Specific examples include Staphyloid AC3832, AC3816N (manufactured by Ganz Kasei Co., Ltd.), Metabrene KW-4426 (manufactured by Mitsubishi Rayon Co., Ltd.), F351 (Nippon Zeon Corporation) Manufactured) and the like.
- Specific examples of acrylonitrile butadiene rubber (NBR) particles include XER-91 (manufactured by JSR).
- SBR styrene butadiene rubber
- acrylic rubber particles include Methbrene W300A and W450A (manufactured by Mitsubishi Rayon Co., Ltd.).
- the resin composition constituting the resin layer according to the present invention may further contain a curing accelerator for adjusting the curing temperature, the curing time, and the like.
- a curing accelerator for adjusting the curing temperature, the curing time, and the like.
- the curing accelerator include quaternary ammonium salts such as tetramethylammonium bromide and tetrabutylammonium bromide, quaternary sulfonium salts such as tetraphenylphosphonium bromide and tetrabutylphosphonium bromide, DBU (1,8-diazabicyclo (5.4.0).
- the content is in the range of 0.01 to 7% by mass with respect to the total amount of the thermosetting resin.
- the resin layer according to the present invention is preferably formed by preparing a varnish in which the composition constituting the resin layer is dissolved, and applying and drying on a gas barrier layer described later.
- organic solvent used for the preparation of varnish examples include acetone, methyl ethyl ketone (hereinafter abbreviated as “MEK”), ketones such as cyclohexanone, ethyl acetate, butyl acetate, cellosolve acetate, propylene glycol monomethyl ether acetate.
- acetate esters such as carbitol acetate, carbitols such as cellosolve and butyl carbitol, aromatic hydrocarbons such as toluene and xylene, dimethylformamide, dimethylacetamide, and N-methylpyrrolidone. These may be used alone or in combination of two or more.
- any appropriate method can be adopted as a coating method.
- a coating method includes a roll coating method, a flow coating method, an ink jet method, a spray coating method, a printing method, a dip coating method, a casting film forming method, a bar coating method, and a gravure printing method.
- the drying conditions are not particularly limited, but 3 to 15 minutes at 50 to 100 ° C. is preferable.
- the thickness of the resin layer according to the present invention is not particularly limited, but is preferably in the range of 3 to 200 ⁇ m, more preferably in the range of 5 to 150 ⁇ m, from the viewpoint of blocking moisture by reducing the contact area with the outside air.
- the range of 10 to 100 ⁇ m is more preferable.
- the gas barrier layer according to the present invention is a layer formed by applying a coating treatment containing at least polysilazane and performing a modification treatment on the dried layer. When there are a plurality of gas barrier layers, the gas barrier layer is on the outermost surface.
- Polysilazane is a polymer having a silicon-nitrogen bond, such as SiO 2 , Si 3 N 4 having a bond such as Si—N, Si—H, or N—H, and ceramics such as both intermediate solid solutions SiO x N y. It is a precursor inorganic polymer.
- polysilazane preferably has a structure represented by the following general formula (I).
- R 1 , R 2 and R 3 are each independently a hydrogen atom, a substituted or unsubstituted alkyl group, aryl group, vinyl group or (trialkoxysilyl) alkyl group. .
- R 1 , R 2 and R 3 may be the same or different.
- examples of the alkyl group include linear, branched or cyclic alkyl groups having 1 to 8 carbon atoms.
- the aryl group include aryl groups having 6 to 30 carbon atoms.
- non-condensed hydrocarbon groups such as phenyl group, biphenyl group, terphenyl group; pentarenyl group, indenyl group, naphthyl group, azulenyl group, heptaenyl group, biphenylenyl group, fluorenyl group, acenaphthylenyl group, preadenenyl group , Condensed polycyclic hydrocarbon groups such as acenaphthenyl group, phenalenyl group, phenanthryl group, anthryl group, fluoranthenyl group, acephenanthrenyl group, aceantrirenyl group, triphenylenyl group, pyrenyl group, chrysenyl group, naphthacenyl group, etc.
- non-condensed hydrocarbon groups such as phenyl group, biphenyl group, terphenyl group; pentarenyl group, indenyl group, nap
- the (trialkoxysilyl) alkyl group includes an alkyl group having 1 to 8 carbon atoms having a silyl group substituted with an alkoxy group having 1 to 8 carbon atoms. More specific examples include 3- (triethoxysilyl) propyl group and 3- (trimethoxysilyl) propyl group.
- the substituent optionally present in R 1 to R 3 is not particularly limited, and examples thereof include an alkyl group, a halogen atom, a hydroxy group (—OH), a mercapto group (—SH), a cyano group (—CN), There are a sulfo group (—SO 3 H), a carboxy group (—COOH), a nitro group (—NO 2 ) and the like. Note that the optionally present substituent is not the same as R 1 to R 3 to be substituted. For example, when R 1 to R 3 are alkyl groups, they are not further substituted with an alkyl group.
- R 1 , R 2 and R 3 are preferably a hydrogen atom, a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, an isobutyl group, a tert-butyl group, a phenyl group, a vinyl group, 3 -(Triethoxysilyl) propyl group or 3- (trimethoxysilylpropyl) group.
- n is an integer, and it is preferable that the polysilazane having the structure represented by the general formula (I) is determined to have a number average molecular weight of 150 to 150,000 g / mol.
- one of preferred embodiments is perhydropolysilazane in which all of R 1 , R 2 and R 3 are hydrogen atoms.
- Polysilazane is commercially available in a solution state dissolved in an organic solvent, and the commercially available product can be used as it is as a coating solution for forming a gas barrier layer.
- Examples of commercially available polysilazane solutions include AQUAMICA (registered trademark) NN120-10, NN120-20, NAX120-20, NN110, NN310, NN320, NL110A, NL120A, NL120-20, NL150A, and NP110 manufactured by AZ Electronic Materials Co., Ltd. NP140, SP140 and the like.
- polysilazane examples include, but are not limited to, for example, a silicon alkoxide-added polysilazane obtained by reacting the polysilazane with a silicon alkoxide (Japanese Patent Laid-Open No. 5-23827), and a glycidol reaction.
- a silicon alkoxide-added polysilazane obtained by reacting the polysilazane with a silicon alkoxide
- glycidol-added polysilazane Japanese Patent Laid-Open No. 6-122852
- alcohol-added polysilazane obtained by reacting alcohol
- metal carboxylate obtained by reacting metal carboxylate Addition polysilazane (JP-A-6-299118), acetylacetonate complex-added polysilazane obtained by reacting a metal-containing acetylacetonate complex (JP-A-6-306329), metal obtained by adding metal fine particles Fine particle added policy Zhang such (JP-A-7-196986), and a polysilazane ceramic at low temperatures.
- the content of polysilazane in the gas barrier layer before the reforming treatment may be 100% by mass when the total mass of the gas barrier layer is 100% by mass.
- the content of polysilazane in the layer is preferably in the range of 10 to 99% by mass, and more preferably in the range of 40 to 95% by mass. The range is particularly preferably from 70 to 95% by mass.
- the solvent for preparing the coating solution for forming the gas barrier layer is not particularly limited as long as it can dissolve the silicon compound, but water and reactive groups that easily react with the silicon compound (for example, hydroxy groups, Alternatively, an organic solvent that does not contain an amine group and is inert to the silicon compound is preferable, and an aprotic organic solvent is more preferable.
- the solvent is an aprotic solvent; for example, carbon such as aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons such as pentane, hexane, cyclohexane, toluene, xylene, solvesso, and turben.
- Hydrogen solvents Halogen hydrocarbon solvents such as methylene chloride and trichloroethane; Esters such as ethyl acetate and butyl acetate; Ketones such as acetone and methyl ethyl ketone; Aliphatic ethers such as dibutyl ether, dioxane and tetrahydrofuran; Alicyclic ethers and the like Ethers: Examples include tetrahydrofuran, dibutyl ether, mono- and polyalkylene glycol dialkyl ethers (diglymes), and the like.
- the above solvent is selected according to the purpose such as the solubility of the silicon compound and the evaporation rate of the solvent, and may be used alone or in the form of a mixture of two or more.
- the concentration of the silicon compound in the gas barrier layer forming coating solution is not particularly limited, and varies depending on the film thickness of the layer and the pot life of the coating solution, but is preferably 1 to 80% by mass, more preferably 5 to 50% by mass. Particularly preferred is 10 to 40% by mass.
- the coating solution for forming the gas barrier layer preferably contains an aluminum compound from the viewpoint of improving the heat resistance of the gas barrier layer.
- the aluminum compound include aluminum trimethoxide, aluminum triethoxide, and aluminum trioxide. n-propoxide, aluminum triisopropoxide, aluminum tri-n-butoxide, aluminum tri-sec-butoxide, aluminum tri-tert-butoxide, aluminum acetylacetonate, acetoalkoxyaluminum diisopropylate, aluminum ethyl acetoacetate / diisopropylate, Aluminum ethyl acetoacetate di n-butyrate, aluminum diethyl acetoacetate mono n-butyrate, aluminum diisopropylate monos c-butyrate, aluminum trisacetylacetonate, aluminum trisethylacetoacetate, bis (ethylacetoacetate) (2,4-pentanedionato) aluminum, aluminum alkylacetoacetate diis
- ком ⁇ онентs include, for example, AMD (aluminum diisopropylate monosec-butyrate), ASBD (aluminum secondary butyrate), ALCH (aluminum ethyl acetoacetate diisopropylate), ALCH-TR (aluminum tris).
- Ethyl acetoacetate aluminum chelate M (aluminum alkyl acetoacetate / diisopropylate), aluminum chelate D (aluminum bisethylacetoacetate / monoacetylacetonate), aluminum chelate A (W) (aluminum trisacetylacetonate) , Manufactured by Kawaken Fine Chemical Co., Ltd.), Preneact (registered trademark) AL-M (acetoalkoxyaluminum diisopropylate, manufactured by Ajinomoto Fine Chemical Co., Ltd.), Ruga Chicks series (manufactured by Matsumoto Fine Chemical Co., Ltd.) and the like.
- the content in the coating solution for forming the gas barrier layer is preferably 0.1 to 10% by mass, and more preferably 1 to 5% by mass.
- the formation method by the coating method of the above gas barrier layers is not particularly limited, and a known method can be applied. Specific examples include a spin coating method, a roll coating method, a flow coating method, an ink jet method, a spray coating method, a printing method, a dip coating method, a casting film forming method, a bar coating method, and a gravure printing method.
- a method of applying a coating solution for forming a gas barrier layer containing a silicon compound and, if necessary, a catalyst in an organic solvent by the above known coating method, evaporating and removing the solvent, and then performing a modification treatment is preferable. .
- the coating thickness can be appropriately set according to the purpose.
- the coating thickness per gas barrier layer is preferably about 10 nm to 10 ⁇ m after drying, more preferably 15 nm to 1 ⁇ m, and even more preferably 20 to 500 nm. If the film thickness is 10 nm or more, sufficient barrier properties can be obtained, and if it is 10 ⁇ m or less, stable coating properties can be obtained during layer formation, and high light transmittance can be realized.
- the coating film After applying the coating solution, it is preferable to dry the coating film.
- the organic solvent contained in the coating film can be removed. At this time, all of the organic solvent contained in the coating film may be dried or may be partially left. Even when a part of the organic solvent is left, a suitable gas barrier layer can be obtained. The remaining solvent can be removed later.
- the modification treatment of polysilazane in the present invention refers to a reaction that converts at least a part of polysilazane into silicon oxide or silicon oxynitride.
- vacuum ultraviolet light irradiation treatment In vacuum ultraviolet ray irradiation treatment in the present invention, it is preferable that the illuminance of the vacuum ultraviolet rays in the coating film surface for receiving the polysilazane coating film is in the range of 30 ⁇ 200mW / cm 2, in the range of 50 ⁇ 160mW / cm 2 It is more preferable. When it is 30 mW / cm 2 or more, there is no concern that the reforming efficiency is lowered, and when it is 200 mW / cm 2 or less, the coating film is not ablated and the substrate is not damaged.
- Irradiation energy amount of the VUV in the polysilazane coating film surface is preferably in the range of 200 ⁇ 10000mJ / cm 2, and more preferably in the range of 500 ⁇ 5000mJ / cm 2. Within this range, there are no cracks or thermal deformation of the substrate.
- a rare gas excimer lamp is preferably used as the vacuum ultraviolet light source.
- Atoms of noble gases such as Xe, Kr, Ar, and Ne are called inert gases because they are not chemically bonded to form molecules.
- the Xe excimer lamp emits ultraviolet light having a short wavelength of 172 nm at a single wavelength, and thus has excellent luminous efficiency. Since this light has a large oxygen absorption coefficient, it can generate radical oxygen atom species and ozone at a high concentration with a very small amount of oxygen.
- the energy of light having a short wavelength of 172 nm has a high ability to dissociate organic bonds. Due to the high energy of the active oxygen, ozone and ultraviolet radiation, the polysilazane layer can be modified in a short time.
- the oxygen concentration at the time of vacuum ultraviolet irradiation is preferably in the range of 10 to 10000 ppm, more preferably in the range of 50 to 5000 ppm, and still more preferably in the range of 1000 to 4500 ppm.
- the gas satisfying the irradiation atmosphere used at the time of irradiation with vacuum ultraviolet rays is preferably a dry inert gas, and particularly preferably dry nitrogen gas from the viewpoint of cost.
- the oxygen concentration can be adjusted by measuring the flow rate of oxygen gas and inert gas introduced into the irradiation chamber and changing the flow rate ratio.
- the gas barrier layer according to the present invention may have a laminated structure of two or more layers as long as a layer obtained by applying a modification treatment to a layer obtained by applying a coating liquid containing polysilazane is dried.
- a plurality of gas barrier layers having the same composition may be formed, or a plurality of layers having different compositions may be formed.
- a chemical vapor deposition method such as a vacuum plasma CVD method (Chemical Vapor Deposition), a sputtering method, etc.
- a combination with a gas barrier layer formed by a physical vapor deposition method may also be used.
- a preferable example is a vacuum plasma CVD method.
- a gas barrier layer is further formed on the base material by a plasma CVD method in which the base material is disposed on a pair of film forming rollers and discharges between the pair of film forming rollers to generate plasma. The method will be described below.
- the sealing film of the present invention is also referred to as a gas barrier film.
- the gas barrier layer preferably contains carbon, silicon, and oxygen as constituent elements.
- a more preferable form is a layer that satisfies the following requirements (i) to (iii).
- the silicon distribution curve, the oxygen distribution curve, the carbon distribution curve, and the oxygen carbon distribution curve are obtained by using X-ray photoelectron spectroscopy (XPS) measurement and rare gas ion sputtering such as argon in combination.
- XPS X-ray photoelectron spectroscopy
- rare gas ion sputtering such as argon in combination.
- XPS depth profile measurement in which surface composition analysis is sequentially performed while exposing the inside of the sample.
- a distribution curve obtained by such XPS depth profile measurement can be created, for example, with the vertical axis as the atomic ratio (unit: at%) of each element and the horizontal axis as the etching time (sputtering time).
- the etching time is generally correlated with the distance (L) from the surface of the gas barrier layer in the film thickness direction of the gas barrier layer in the film thickness direction. Therefore, as the “distance from the surface of the gas barrier layer in the thickness direction of the gas barrier layer”, the surface of the gas barrier layer calculated from the relationship between the etching rate and the etching time employed in the XPS depth profile measurement The distance from can be adopted.
- the silicon distribution curve, oxygen distribution curve, carbon distribution curve, and oxygen carbon distribution curve can be prepared under the following measurement conditions.
- Etching ion species Argon (Ar + ) Etching rate (SiO 2 thermal oxide equivalent value): 0.05 nm / sec Etching interval (SiO 2 equivalent value): 10 nm
- X-ray photoelectron spectrometer Model name “VG Theta Probe” manufactured by Thermo Fisher Scientific Irradiation X-ray: Single crystal spectroscopy AlK ⁇ X-ray spot and size: 800 ⁇ 400 ⁇ m oval.
- the gas barrier layer preferably has (ii) the carbon distribution curve has at least two extreme values.
- the gas barrier layer preferably has at least three extreme values in the carbon distribution curve, more preferably at least four extreme values, but may have five or more extreme values.
- the extreme value of the carbon distribution curve is one or less, the gas barrier property may be insufficient when the obtained gas barrier film is bent.
- the upper limit of the extreme value of the carbon distribution curve is not particularly limited, for example, it is preferably 30 or less, more preferably 25 or less, but the number of extreme values is also caused by the film thickness of the gas barrier layer. It cannot be stipulated in general.
- the absolute value of the difference in distance (L) is preferably 200 nm or less, more preferably 100 nm or less, and 75 nm or less. Is particularly preferred. If the distance is between such extreme values, the gas barrier layer has a portion with a high carbon atom ratio (maximum value) at an appropriate period, so that the gas barrier layer is provided with an appropriate flexibility, and the gas barrier Generation of cracks during bending of the conductive film can be more effectively suppressed / prevented.
- the “extreme value” refers to the maximum value or the minimum value of the atomic ratio of the element to the distance (L) from the surface of the gas barrier layer in the film thickness direction of the first gas barrier layer.
- the “maximum value” means that the value of the atomic ratio of an element (oxygen, silicon or carbon) changes from increasing to decreasing when the distance from the surface of the gas barrier layer is changed.
- the atomic ratio of the element at the position where the distance from the surface of the gas barrier layer in the thickness direction of the gas barrier layer from the point is further changed in the range of 4 to 20 nm, rather than the value of the atomic ratio of the element at that point. This is the point at which the value decreases by 3 at% or more.
- minimum value means that the value of the atomic ratio of an element (oxygen, silicon, or carbon) changes from decrease to increase when the distance from the surface of the gas barrier layer is changed. And the atom of the element at the position where the distance from the surface of the gas barrier layer in the thickness direction of the gas barrier layer from the point is further changed within the range of 4 to 20 nm, rather than the atomic ratio value of the element at that point This is the point where the ratio value increases by 3 at% or more.
- the atomic ratio value of the element when changing in the range of 4 to 20 nm, the atomic ratio value of the element only needs to increase by 3 at% or more in any range.
- the lower limit of the distance between the extreme values is because the smaller the distance between the extreme values, the higher the effect of suppressing / preventing crack generation when the gas barrier film is bent,
- it is preferably 10 nm or more, more preferably 30 nm or more in consideration of the flexibility of the gas barrier layer, the effect of suppressing / preventing cracks, thermal expansion, and the like.
- the gas barrier layer has (iii) an absolute value of a difference between the maximum value and the minimum value of the atomic ratio of carbon in the carbon distribution curve (hereinafter, also simply referred to as “C max ⁇ C min difference”) of 3 at% or more. It is preferable that When the absolute value is less than 3 at%, the gas barrier property may be insufficient when the obtained gas barrier film is bent.
- the C max -C min difference is preferably 5 at% or more, more preferably 7 at% or more, and particularly preferably 10 at% or more. By setting the difference C max ⁇ C min , the gas barrier property can be further improved.
- the “maximum value” is the atomic ratio of each element that is maximum in the distribution curve of each element, and is the highest value among the maximum values.
- the “minimum value” is the atomic ratio of each element that is the minimum in the distribution curve of each element, and is the lowest value among the minimum values.
- the upper limit of the C max -C min difference is not particularly limited, but it is preferably 50 at% or less in consideration of the effect of suppressing / preventing crack generation at the time of bending of the gas barrier film. The following is more preferable.
- the film thickness (dry film thickness) of the gas barrier layer formed by the above plasma CVD method is not particularly limited as long as the above (i) to (iii) are satisfied.
- the thickness of the gas barrier layer per layer is preferably 20 to 3000 nm, more preferably 50 to 2500 nm, and particularly preferably 100 to 1000 nm. With such a film thickness, the gas barrier film can exhibit excellent gas barrier properties and the effect of suppressing / preventing cracking during bending.
- each gas barrier layer has a film thickness as mentioned above.
- the gas barrier layer is substantially in the film surface direction (direction parallel to the surface of the gas barrier layer) from the viewpoint of forming a barrier layer having a uniform and excellent gas barrier property over the entire film surface. Preferably it is uniform.
- the gas barrier layer is substantially uniform in the film surface direction means that the oxygen distribution curve, the carbon distribution curve and the carbon distribution curve at any two measurement points on the film surface of the barrier layer by XPS depth profile measurement.
- the number of extreme values of the carbon distribution curve obtained at any two measurement points is the same, and the maximum value of the atomic ratio of carbon in each carbon distribution curve and The absolute value of the difference between the minimum values is the same as each other or within 5 at%.
- Formation method of other gas barrier layers by plasma CVD method As a method for forming another gas barrier layer on the surface of the substrate, it is preferable to employ a plasma CVD method from the viewpoint of gas barrier properties.
- FIG. 2 is a schematic view showing an example of a production apparatus that can be suitably used for producing a gas barrier layer by this production method.
- the same or corresponding elements are denoted by the same reference numerals, and redundant description is omitted.
- the manufacturing apparatus 31 shown in FIG. 2 includes a delivery roller 32, transport rollers 33, 34, 35, and 36, film formation rollers 39 and 40, a gas supply pipe 41, a plasma generation power source 42, and a film formation roller 39. And 40, and magnetic field generators 43 and 44 installed inside 40, and a take-up roller 45.
- a delivery roller 32 transport rollers 33, 34, 35, and 36
- film formation rollers 39 and 40 a gas supply pipe 41
- a plasma generation power source 42 and a film formation roller 39.
- And 40, and magnetic field generators 43 and 44 installed inside 40, and a take-up roller 45.
- at least the film forming rollers 39 and 40, the gas supply pipe 41, the plasma generating power source 42, and the magnetic field generating apparatuses 43 and 44 are arranged in a vacuum chamber (not shown).
- the vacuum chamber is connected to a vacuum pump (not shown), and the pressure in the vacuum chamber can be appropriately adjusted by the vacuum pump.
- the type of source gas, the power of the electrode drum of the plasma generator, the pressure in the vacuum chamber, the diameter of the film forming roller, and the conveyance of the film (base material) can be produced by appropriately adjusting the speed.
- a raw material gas, a reactive gas, a carrier gas, or a discharge gas can be used alone or in combination of two or more.
- the source gas in the film forming gas used for forming the gas barrier layer 1b can be appropriately selected and used according to the material of the gas barrier layer 1b to be formed.
- a source gas for example, an organic silicon compound containing silicon or an organic compound gas containing carbon can be used.
- organosilicon compounds examples include hexamethyldisiloxane (HMDSO), hexamethyldisilane (HMDS), 1,1,3,3-tetramethyldisiloxane, vinyltrimethylsilane, methyltrimethylsilane, hexamethyldisilane.
- HMDSO hexamethyldisiloxane
- HMDS hexamethyldisilane
- 1,1,3,3-tetramethyldisiloxane vinyltrimethylsilane
- methyltrimethylsilane hexamethyldisilane.
- Methylsilane dimethylsilane, trimethylsilane, diethylsilane, propylsilane, phenylsilane, vinyltriethoxysilane, vinyltrimethoxysilane, tetramethoxysilane (TMOS), tetraethoxysilane (TEOS), phenyltrimethoxysilane, methyltriethoxy
- TMOS tetramethoxysilane
- TEOS tetraethoxysilane
- Examples include silane and octamethylcyclotetrasiloxane.
- organosilicon compounds hexamethyldisiloxane and 11,3,3-tetramethyldisiloxane are preferable from the viewpoints of properties such as the handleability of the compound and the gas barrier property of the obtained first gas barrier layer.
- organosilicon compounds can be used alone or in combination of two or more.
- a reactive gas may be used in addition to the raw material gas.
- a gas that reacts with the raw material gas to become an inorganic compound such as an oxide or a nitride can be appropriately selected and used.
- a reaction gas for forming an oxide for example, oxygen or ozone can be used.
- the barrier layer according to the present invention is formed by a plasma CVD method using the plasma CVD apparatus (roll-to-roll method) having the counter roll electrode shown in FIG. It is characterized by forming a film.
- This is excellent in flexibility (flexibility) and mechanical strength, especially in roll-to-roll transportation, when mass-produced using a plasma CVD apparatus (roll-to-roll method) having a counter roll electrode. This is because it is possible to efficiently produce a gas barrier layer having both durability at the time and barrier performance.
- Such a manufacturing apparatus is also excellent in that it can inexpensively and easily mass-produce a gas barrier film that is required for durability against temperature changes used in solar cells and electronic components.
- a plastic film or a plastic sheet is preferably used as the substrate, and a film or sheet made of a colorless and transparent resin is more preferably used.
- the plastic film to be used is not particularly limited in material, thickness and the like as long as it can hold the gas barrier layer and the resin layer, and can be appropriately selected according to the purpose of use.
- Specific examples of the plastic film include polyester resin, methacrylic resin, methacrylic acid-maleic acid copolymer, polystyrene resin, transparent fluororesin, polyimide, fluorinated polyimide resin, polyamide resin, polyamideimide resin, and polyetherimide.
- Resin cellulose acylate resin, polyurethane resin, polyetheretherketone resin, polycarbonate resin, alicyclic polyolefin resin, polyarylate resin, polyethersulfone resin, polysulfone resin, cycloolefin copolymer, fluorene ring-modified polycarbonate resin, alicyclic ring
- thermoplastic resins such as modified polycarbonate resins, fluorene ring-modified polyester resins, and acryloyl compounds.
- the substrate is preferably transparent. That is, the light transmittance is usually 80% or more, preferably 85% or more, and more preferably 90% or more.
- the light transmittance is calculated by measuring the total light transmittance and the amount of scattered light using the method described in JISK105: 1981, that is, using an integrating sphere light transmittance measuring device, and subtracting the diffuse transmittance from the total light transmittance. be able to.
- the thickness of the substrate used for the sealing film of the present invention is appropriately selected depending on the application and is not particularly limited, but is typically 1 to 800 ⁇ m, preferably 10 to 200 ⁇ m.
- These plastic films may have functional layers such as a transparent conductive layer, a primer layer, and a clear hard coat layer.
- As the functional layer in addition to those described above, those described in paragraph numbers “0036” to “0038” of JP-A-2006-289627 can be preferably used.
- the substrate preferably has a high surface smoothness.
- the surface smoothness those having an average surface roughness (Ra) of 2 nm or less are preferable. Although there is no particular lower limit, it is practically 0.01 nm or more. If necessary, both surfaces of the substrate, at least the side on which the gas barrier layer is provided, may be polished to improve smoothness.
- the functional element specifically refers to a flexible electronic device such as an organic EL element or a solar cell element.
- a sealing film for organic EL elements since it is suitably used as a sealing film for organic EL elements, the sealing of organic EL elements will be described as an example.
- the organic EL element according to the present invention can take various configurations, and an example is shown in FIG.
- FIG. 3 illustrates the case where a resin substrate is used as the substrate used for the organic EL element.
- An organic EL element 100 is provided on a resin substrate 113, and an organic functional layer (light emission) configured using a first electrode (transparent electrode) 101, an organic material, and the like in order from the resin substrate 113 side.
- the functional layer 103 and the second electrode (counter electrode) 105a are stacked in this order.
- An extraction electrode 116 is provided at the end of the first electrode 101 (electrode layer 101b).
- the first electrode 101 and an external power source (not shown) are electrically connected via the extraction electrode 116.
- the organic EL element 100 is configured to extract the generated light (emitted light h) from at least the resin substrate 113 side.
- the layer structure of the organic EL element 100 is not limited and may be a general layer structure.
- the first electrode 101 functions as an anode (that is, an anode)
- the second electrode 105a functions as a cathode (that is, a cathode).
- the organic functional layer 103 has a configuration in which a hole injection layer 103a / a hole transport layer 103b / a light emitting layer 103c / an electron transport layer 103d / an electron injection layer 103e are stacked in this order from the first electrode 101 side that is an anode.
- the hole injection layer 103a and the hole transport layer 103b may be provided as a hole transport injection layer.
- the electron transport layer 103d and the electron injection layer 103e may be provided as an electron transport injection layer.
- the electron injection layer 103e may be made of an inorganic material.
- the organic functional layer 103 may have a hole blocking layer, an electron blocking layer, and the like laminated in necessary places in addition to these layers.
- the light-emitting layer 103c may have a structure in which each color light-emitting layer that generates light emitted in each wavelength region is stacked, and each color light-emitting layer is stacked via a non-light emitting intermediate layer.
- the intermediate layer may function as a hole blocking layer and an electron blocking layer.
- the second electrode 105a as the cathode may also have a laminated structure as necessary. In such a configuration, only a portion where the organic functional layer 103 is sandwiched between the first electrode 101 and the second electrode 105 a becomes a light emitting region in the organic EL element 100.
- the auxiliary electrode 115 may be provided in contact with the electrode layer 101b of the first electrode 101 for the purpose of reducing the resistance of the first electrode 101.
- the organic EL element 100 having the above configuration is sealed with the above-described sealing film 107 on the resin substrate 113 for the purpose of preventing the deterioration of the organic functional layer 103 formed using an organic material or the like. ing.
- the sealing film 107 is fixed to the resin substrate 113 side through a resin layer according to the present invention that functions as an adhesive.
- the terminal portions of the first electrode 101 (extraction electrode 116) and the second electrode 105a are provided on the resin substrate 113 in a state where they are exposed from the sealing film 107 while being insulated from each other by the organic functional layer 103. It is assumed that
- the manufacturing method of the organic EL element used for this invention has a lamination process which laminates
- a manufacturing method a conventionally well-known manufacturing method can be used.
- the measurement of the operation and physical properties is performed under the conditions of room temperature (20 to 25 ° C.) / Relative humidity 40 to 50%.
- the coating solution obtained above was formed into a film having a thickness of 300 nm on a PET base material (125 ⁇ m thick) provided with a clear hard coat manufactured by Kimoto Co., Ltd. with a spin coater, and allowed to stand for 2 minutes. A heat treatment was performed for 1 minute on an 80 ° C. hot plate to form a polysilazane coating film.
- a vacuum ultraviolet ray irradiation treatment of 6000 mJ / cm 2 was performed according to the following method to form a gas barrier layer A10.
- reference numeral 201 denotes an apparatus chamber, which supplies appropriate amounts of nitrogen and oxygen from a gas supply port (not shown) to the inside and exhausts gas from a gas discharge port (not shown), thereby substantially removing water vapor from the inside of the chamber.
- the oxygen concentration can be maintained at a predetermined concentration.
- Reference numeral 202 denotes an Xe excimer lamp having a double tube structure that irradiates vacuum ultraviolet rays of 172 nm
- reference numeral 203 denotes an excimer lamp holder that also serves as an external electrode.
- Reference numeral 204 denotes a sample stage. The sample stage 204 can be reciprocated horizontally at a predetermined speed in the apparatus chamber 201 by a moving means (not shown).
- the sample stage 204 can be maintained at a predetermined temperature by a heating means (not shown).
- Reference numeral 205 denotes a sample on which a polysilazane coating film is formed. When the sample stage moves horizontally, the height of the sample stage is adjusted so that the shortest distance between the surface of the sample coating layer and the excimer lamp tube surface is 3 mm.
- Reference numeral 206 denotes a light shielding plate, which prevents the vacuum ultraviolet light from being applied to the coating layer of the sample during the aging of the Xe excimer lamp 202.
- the energy irradiated on the coating film surface in the vacuum ultraviolet irradiation process was measured using a 172 nm sensor head using an ultraviolet integrated light meter manufactured by Hamamatsu Photonics Co., Ltd .: C8026 / H8025 UV POWER METER.
- the sensor head is installed in the center of the sample stage 204 so that the shortest distance between the Xe excimer lamp tube surface and the measurement surface of the sensor head is 3 mm, and the atmosphere in the apparatus chamber 201 is irradiated with vacuum ultraviolet rays. Nitrogen and oxygen were supplied so that the oxygen concentration was the same as in the process, and the sample stage 204 was moved at a speed of 0.5 m / min (V in FIG. 4) for measurement.
- an aging time of 10 minutes was provided after the Xe excimer lamp was turned on, and then the sample stage was moved to start the measurement.
- the irradiation speed was adjusted to 6000 mJ / cm 2 by adjusting the moving speed of the sample stage.
- the vacuum ultraviolet irradiation was performed after aging for 10 minutes, similar to the measurement of irradiation energy.
- NC3000 70 mass% solid content methyl ethyl ketone (MEK) solution 85 mass parts, phenoxy resin (Japan Epoxy Resin “YX6954”) 35 mass% MEK solution 60 Mix parts by mass with Ajihomo mixer Robomix type mixing stirrer (Primics Co.) 3 parts by mass of ionic liquid 1 (N-acetylglycine 1,1-dimethylpyrrolidinium salt), 15 parts by mass of solvent (MEK), and 20 parts by mass of solvent (acetone) are mixed with the mixture. Uniformly dispersed to obtain a varnish-like ionic liquid-containing coating solution.
- ionic liquid 1 N-acetylglycine 1,1-dimethylpyrrolidinium salt
- MEK solvent
- acetone 20 parts by mass of solvent
- the ionic liquid-containing coating solution is uniformly coated on the barrier layer A10 obtained above with an applicator so that the thickness of the thermosetting resin layer after drying is 40 ⁇ m, and dried at 60 to 80 ° C. for 6 minutes. By doing so, the sealing film 1 of the present invention was obtained.
- sealing film 2 Except for changing the ionic liquid to ionic liquid 2 (N-acetylglycine tetrabutylphosphonium salt), the sealing film 2 of the present invention was obtained in exactly the same manner as in “Production of sealing film 1”.
- sealing film 3 Except for changing the ionic liquid to ionic liquid 3 (1-ethyl-3-methylimidazolium formate), the sealing film 3 of the present invention was obtained in exactly the same manner as in “Production of sealing film 1”.
- a gas barrier layer A11 was formed in the same manner as in [Formation of gas barrier layer A10] except that the thickness of the gas barrier layer was changed to 150 nm.
- a dibutyl ether solution containing 20% by mass of perhydropolysilazane (manufactured by AZ Electronic Materials Co., Ltd., Aquamica (registered trademark) NN120-20) is diluted to 5% by mass with dibutyl ether, and N, N, N is used as an amine catalyst.
- TDAH N'-tetramethyl-1,6-diaminohexane
- ALCH produced by Kawaken Fine Chemical Co., Ltd., aluminum ethyl acetoacetate diisopropyl Rate
- a 150 nm thick polysilazane coating film was formed on the gas barrier layer A11 obtained above using the coating solution, and then the first gas barrier was applied at a dew point of ⁇ 30 ° C. and an irradiation dose of 6000 mJ / cm 2.
- a vacuum ultraviolet ray irradiation treatment was performed in the same manner as the formation (application method) of the layer A10 to form a gas barrier layer A21.
- the sealing film 4 of the present invention was obtained by drying at 60 to 80 ° C. for 6 minutes.
- the sealing film 6 of the present invention was obtained by drying at 60 to 80 ° C. for 6 minutes.
- a film forming gas mixed gas of hexamethyldisiloxane (HMDSO) as a source gas and oxygen gas (also functioning as a discharge gas) as a source gas
- HMDSO hexamethyldisiloxane
- oxygen gas also functioning as a discharge gas
- a gas barrier layer C21 having a thickness of 150 nm was formed by a plasma CVD method, which is referred to as a CVD1 method.
- the film formation conditions were as follows.
- the carbon distribution curve has at least two extreme values.
- a gas barrier layer A11 was formed on the gas barrier layer C21 obtained above.
- the sealing film 7 of the present invention was obtained by drying at 60 to 80 ° C. for 6 minutes.
- a gas barrier layer C12 was formed in the same manner as in [Formation of gas barrier layer C11] except that the thickness of the gas barrier layer was changed to 100 nm.
- gas barrier layer A12 Except for changing the thickness of the gas barrier layer to 100 nm, the gas barrier layer A12 was formed on the gas barrier layer C12 in exactly the same manner as [Formation of the gas barrier layer A11].
- the ionic liquid-containing coating solution obtained in the “production of the sealing film 1” is uniformly applied with an applicator so that the thickness of the thermosetting resin layer after drying becomes 40 ⁇ m,
- the sealing film 9 of the present invention was obtained by drying at 60 to 80 ° C. for 6 minutes.
- the sealing film 10 of the present invention was obtained in exactly the same manner as in “Manufacture of the sealing film 9”.
- a gas barrier layer C23 having a thickness of 100 nm was formed by a plasma discharge method according to the conditions described below while conveying a PET base material (125 ⁇ m thick) having a clear hard coat manufactured by Kimoto Co., Ltd. This film forming method is referred to as a CVD2 method.
- the sealing film 11 of the present invention was obtained in exactly the same manner as in “Manufacture of the sealing film 10”.
- a gas barrier layer C10 was formed in exactly the same manner as [Formation of gas barrier layer C11] except that the thickness of the gas barrier layer was changed to 300 nm.
- a comparative sealing film 12 was obtained in exactly the same manner as in “Manufacture of sealing film 1” except that the gas barrier layer A10 was changed to the gas barrier layer C10.
- ITO Indium Tin Oxide
- the cleaning surface modification treatment of the glass substrate on which the first electrode is formed is performed using a low-pressure mercury lamp with a wavelength of 184.9 nm, an irradiation intensity of 15 mW / cm 2 , The distance was 10 mm.
- the charge removal treatment was performed using a static eliminator with weak X-rays.
- the following hole transport layer forming coating solution is applied by a spin coater in an environment of 25 ° C. and a relative humidity of 50% RH, Drying and heat treatment were performed under the following conditions to form a hole transport layer.
- the coating solution for forming the hole transport layer was applied so that the thickness after drying was 50 nm.
- PEDOT / PSS polystyrene sulfonate
- Baytron P AI 4083 manufactured by Bayer
- ⁇ Drying and heat treatment conditions After applying the hole transport layer forming coating solution, the solvent is removed at a height of 100 mm toward the film formation surface, a discharge air velocity of 1 m / s, a wide air velocity distribution of 5%, and a temperature of 100 ° C., followed by heat treatment.
- the back surface heat transfer type heat treatment was performed at a temperature of 150 ° C. using an apparatus to form a hole transport layer.
- the following coating solution for forming a white light emitting layer was applied with a spin coater under the following conditions, followed by drying and heat treatment under the following conditions to form a light emitting layer. .
- the white light emitting layer forming coating solution was applied so that the thickness after drying was 40 nm.
- ⁇ White luminescent layer forming coating solution> As a host material, 1.0 g of a compound represented by the following chemical formula HA, 100 mg of a compound represented by the following chemical formula DA as a dopant material, and 0.1 mg of a compound represented by the following chemical formula DB as a dopant material. 2 mg of a compound represented by the following chemical formula DC as a dopant material was dissolved in 0.2 mg and 100 g of toluene to prepare a white light emitting layer forming coating solution.
- the coating process was performed in an atmosphere having a nitrogen gas concentration of 99% or more, and the coating temperature was 25 ° C.
- ⁇ Drying and heat treatment conditions After applying the white light emitting layer forming coating solution, the solvent was removed at a height of 100 mm toward the film formation surface, a discharge wind speed of 1 m / s, a wide wind speed distribution of 5%, and a temperature of 60 ° C., and then a temperature of 130 ° C. A heat treatment was performed to form a light emitting layer.
- the following coating liquid for forming an electron transport layer was applied with a spin coater under the following conditions, and then dried and heated under the following conditions to form an electron transport layer.
- the coating solution for forming an electron transport layer was applied so that the thickness after drying was 30 nm.
- the coating process was performed in an atmosphere with a nitrogen gas concentration of 99% or more, and the coating temperature of the electron transport layer forming coating solution was 25 ° C.
- the electron transport layer was prepared by dissolving a compound represented by the following chemical formula EA in 2,2,3,3-tetrafluoro-1-propanol to obtain a 0.5 mass% solution as a coating solution for forming an electron transport layer.
- An electron injection layer was formed on the electron transport layer formed above.
- the substrate was put into a decompression chamber and decompressed to 5 ⁇ 10 ⁇ 4 Pa.
- cesium fluoride prepared in a tantalum vapor deposition boat was heated in a vacuum chamber to form an electron injection layer having a thickness of 3 nm.
- Formation of second electrode Using the aluminum as the second electrode forming material under the vacuum of 5 ⁇ 10 ⁇ 4 Pa on the portion of the electron injection layer formed above except for the portion that becomes the extraction electrode of the first electrode, the extraction is performed A mask pattern was formed by vapor deposition so as to have an electrode so that the emission area was 50 mm square, and a second electrode having a thickness of 100 nm was laminated.
- each laminated body on which the second electrode and so on were moved again to a nitrogen atmosphere, and was cut to a prescribed size using an ultraviolet laser to produce an organic EL element.
- Crimping conditions Crimping was performed at a temperature of 170 ° C. (ACF temperature 140 ° C. measured using a separate thermocouple), a pressure of 2 MPa, and 10 seconds.
- the resin layer of the sealing film is placed in a glove box having an oxygen concentration of 10 ppm or less and a moisture concentration of 10 ppm or less. Then, vacuum pressing was performed toward the organic EL element-formed glass substrate under the conditions of 80 ° C., 0.04 MPa load, reduced pressure (1 ⁇ 10 ⁇ 3 MPa or less) suction 20 seconds, and press 20 seconds.
- the sealing film of the present invention was thermally cured by heating on a hot plate at 110 ° C. for 30 minutes.
- the sealing film of the present invention does not deteriorate moisture permeation resistance even after performing accelerated deterioration treatment on the comparative example, and effectively suppresses the occurrence of dark spots (DS) in the organic EL element. I understand that I can do it.
- N-acetylglycine tetrabutylphosphonium salt and 1-ethyl-3-methylimidazolium formate as ionic liquids are superior to DS. I understand.
- sealing films 4, 5, and 9 to 11 containing an aluminum compound in the barrier layer are excellent in DS even when the ionic liquid 1 is used.
- the gas barrier layer is formed by a discharge plasma chemical vapor deposition method having a discharge space between a pair of rollers to which a magnetic field is applied. It can be seen that the encapsulating film 10 having formed a particularly excellent result.
- the sealing film 10 had the resistance to resistance before and after the bending test. It was found that the change in moisture permeability was small, and the carbon atoms had a distribution state satisfying the above (i) to (iii) in the thickness direction of the gas barrier layer, so that the flexibility was also excellent.
- the sealing film was repeatedly bent 100 times at an angle of 180 degrees so as to have a radius of curvature of 10 mm, and the water vapor permeability (WVTR) of the sealing film before and after the treatment was measured and compared.
- WVTR water vapor permeability
- the sealing film of the present invention is a sealing film having excellent moisture resistance even when used after being stored in a high humidity environment, and is an organic electroluminescence panel (organic EL panel), organic electroluminescence element (organic EL element) ), An organic photoelectric conversion element, a liquid crystal display element, and the like.
Landscapes
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Optics & Photonics (AREA)
- Electroluminescent Light Sources (AREA)
- Laminated Bodies (AREA)
- Photovoltaic Devices (AREA)
Abstract
Description
当該ガスバリアー層上に少なくともイオン液体を含有する樹脂層液を塗布、乾燥して樹脂層を形成する工程と、
を有することを特徴とする封止フィルムの製造方法。
本発明の封止フィルムは、基材と、前記基材の片方の表面上に形成されたガスバリアー層と樹脂層とをこの順に備える封止フィルムであって、前記ガスバリアー層は少なくともポリシラザンを含有する塗布液を塗布して乾燥した層に改質処理を施してなる層であり、かつ前記樹脂層は少なくともイオン液体を含有する層であることを特徴とする。
本発明に係る樹脂層は、少なくともイオン液体を含有する層であるが、当該イオン液体とともに少なくとも熱硬化性樹脂を含有し、機能素子を封止する際には接着層としての機能を併せ持つ層であることが好ましい。
本発明におけるイオン液体は、140℃以下(好ましくは120℃以下)の温度領域で融解しうる塩である。機能としては、吸湿剤のように水分を吸水すると同時に、ガスバリアー層中に残存する未反応部分のポリシラザンにその水分を供給する能力も有し、当該ポリシラザンの未反応部分の改質に寄与するものであることが好ましい。
(ただし、R-CO-は炭素数1~5の直鎖又は分岐鎖の脂肪酸より誘導されるアシル基、あるいは、置換又は無置換ベンゾイル基であり、-NH-CHX-CO2 -はアスパラギン酸、グルタミン酸等の酸性アミノ酸イオン、あるいはグリシン、アラニン、フェニルアラニン等の中性アミノ酸イオンである。)
また、アニオンは、一般式(1)で示されるN-アシルアミノ酸イオン又はカルボン酸系アニオンが好ましい。
樹脂層に含まれる樹脂は、熱硬化性樹脂であることが好ましく、当該熱可塑性樹脂は、特に制限はなく、具体的には、エポキシ樹脂、シアネートエステル樹脂、フェノール樹脂、ビスマレイミド-トリアジン樹脂、ポリイミド樹脂、アクリル樹脂、ビニルベンジル樹脂等の種々の熱硬化性樹脂が挙げられる。なかでも、低温硬化性や接着性等の観点から、エポキシ樹脂が好ましい。
本発明に係る樹脂層は、透湿性を調整する観点から吸湿性の金属酸化物を含有することも好ましい。
樹脂層を構成する樹脂組成物には、更にタルク、クレー、マイカ、ベーマイト等の粒子形態が平板状の充填材を含有させることができ、樹脂層の耐透湿性をより一層高めることができる。
本発明に係る樹脂層を構成する樹脂組成物においては、硬化温度、硬化時間等の調整のため、さらに硬化促進剤を含んでいても良い。硬化促進剤としてはテトラメチルアンモニウムブロマイド、テトラブチルアンモニウムブロマイド等の4級アンモニウム塩、テトラフェニルホスホニウムブロマイド、テトラブチルホスホニウムブロマイド等の4級スルホニウム塩、DBU(1,8-ジアザビシクロ(5.4.0)ウンデセン-7)、DBN(1,5-ジアザビシクロ(4.3.0)ノネン-5)、DBU-フェノール塩、DBU-オクチル酸塩、DBU-p-トルエンスルホン酸塩、DBU-ギ酸塩、DBU-フェノールノボラック樹脂塩等のジアザビシクロ化合物、1-ベンジル-2-メチルイミダゾール、1-ベンジル-2-フェニルイミダゾール、2-エチル-4-メチルイミダゾール等のイミダゾール化合物、トリス(ジメチルアミノメチル)フェノール、ベンジルジメチルアミン等の3級アミン、芳香族ジメチルウレア、脂肪族ジメチルウレア、芳香族ジメチルウレア等のジメチルウレア化合物等が挙げられる。
本発明に係る樹脂層は、当該樹脂層を構成する組成物を溶解したワニスを調製して、後述するガスバリアー層上に塗布、乾燥して形成することが好ましい。
本発明に係るガスバリアー層は、少なくともポリシラザンを含有する塗布液を塗布して乾燥した層に改質処理を施してなる層であり、ガスバリアー層が複数ある場合は、その最表面にあって、前記本発明に係る樹脂層に隣接する層である。隣接する層とは、直接ガスバリアー層が樹脂層に接している形態のみではなく、本発明に係るイオン液体の効果が発現する範囲内で他の薄膜層は間に介在してもよいことを意味する。
ポリシラザンとは、ケイ素-窒素結合を有するポリマーであり、Si-N、Si-H、N-H等の結合を有するSiO2、Si3N4、及び両方の中間固溶体SiOxNy等のセラミック前駆体無機ポリマーである。
ガスバリアー層形成用塗布液を調製するための溶媒としては、ケイ素化合物を溶解できるものであれば特に制限されないが、ケイ素化合物と容易に反応してしまう水及び反応性基(例えば、ヒドロキシ基、あるいはアミン基等)を含まず、ケイ素化合物に対して不活性の有機溶媒が好ましく、非プロトン性の有機溶媒がより好ましい。具体的には、溶媒としては、非プロトン性溶媒;例えば、ペンタン、ヘキサン、シクロヘキサン、トルエン、キシレン、ソルベッソ、ターベン等の、脂肪族炭化水素、脂環式炭化水素、芳香族炭化水素等の炭化水素溶媒;塩化メチレン、トリクロロエタン等のハロゲン炭化水素溶媒;酢酸エチル、酢酸ブチル等のエステル類;アセトン、メチルエチルケトン等のケトン類;ジブチルエーテル、ジオキサン、テトラヒドロフラン等の脂肪族エーテル、脂環式エーテル等のエーテル類:例えば、テトラヒドロフラン、ジブチルエーテル、モノ-及びポリアルキレングリコールジアルキルエーテル(ジグライム類)などを挙げることができる。
上記のようなガスバリアー層の塗布法による形成方法は、特に制限されず、公知の方法が適用できる。具体例としては、スピンコート法、ロールコート法、フローコート法、インクジェット法、スプレーコート法、プリント法、ディップコート法、流延成膜法、バーコート法、グラビア印刷法等が挙げられる。
本発明におけるポリシラザンの改質処理とは、少なくともポリシラザンの一部を、酸化ケイ素又は酸化窒化ケイ素へ転化させる反応をいう。
本発明における真空紫外線照射処理において、ポリシラザン層塗膜が受ける塗膜面での該真空紫外線の照度は30~200mW/cm2の範囲であることが好ましく、50~160mW/cm2の範囲であることがより好ましい。30mW/cm2以上では、改質効率が低下する懸念がなく、200mW/cm2以下では、塗膜にアブレーションを生じず、基材にダメージを与えないため好ましい。
本発明に係るガスバリアー層は、ポリシラザンを含有する塗布液を塗布して乾燥した層に改質処理を施してなる層が最表面にあれば、2層以上の積層構造であってもよい。同じ組成のガスバリアー層を複数層形成しても、異なる組成の層を複数形成してもよい。
(ii)前記炭素分布曲線が少なくとも二つの極値を有する;
(iii)前記炭素分布曲線における炭素の原子比の最大値及び最小値の差の絶対値
(以下、単に「Cmax-Cmin差」とも称する)が3at%以上である。
エッチングイオン種:アルゴン(Ar+)
エッチング速度(SiO2熱酸化膜換算値):0.05nm/sec
エッチング間隔(SiO2換算値):10nm
X線光電子分光装置:Thermo Fisher Scientific社製、機種名“VG Theta Probe”
照射X線:単結晶分光AlKα
X線のスポット及びそのサイズ:800×400μmの楕円形。
他のガスバリアー層を基材の表面上に形成させる方法としては、ガスバリアー性の観点から、プラズマCVD法を採用することが好ましい。
本発明の封止フィルムは、基材として、プラスチックフィルム又はプラスチックシートが好ましく用いられ、無色透明な樹脂からなるフィルム又はシートがより好ましく用いられる。用いられるプラスチックフィルムは、ガスバリアー層及び樹脂層を保持できるフィルムであれば材質、厚さ等に特に制限はなく、使用目的等に応じて適宜選択することができる。前記プラスチックフィルムとしては、具体的には、ポリエステル樹脂、メタクリル樹脂、メタクリル酸-マレイン酸共重合体、ポリスチレン樹脂、透明フッ素樹脂、ポリイミド、フッ素化ポリイミド樹脂、ポリアミド樹脂、ポリアミドイミド樹脂、ポリエーテルイミド樹脂、セルロースアシレート樹脂、ポリウレタン樹脂、ポリエーテルエーテルケトン樹脂、ポリカーボネート樹脂、脂環式ポリオレフィン樹脂、ポリアリレート樹脂、ポリエーテルスルホン樹脂、ポリスルホン樹脂、シクロオレフィルンコポリマー、フルオレン環変性ポリカーボネート樹脂、脂環変性ポリカーボネート樹脂、フルオレン環変性ポリエステル樹脂、アクリロイル化合物などの熱可塑性樹脂が挙げられる。
本発明の封止フィルムを用いて封止する機能素子について説明する。
本発明に係る有機EL素子は、種々の構成を採り得るが、一例を図3に示す。
本発明に用いられる有機EL素子の製造方法は、樹脂基板上に第一電極、有機機能層及び第二電極を積層して形成する積層工程を有する。製造方法については、従来公知の製造方法を用いることができる。
〔ガスバリアー層A10の形成〕
(ポリシラザン含有塗布液の調製)
無触媒のパーヒドロポリシラザンを20質量%含むジブチルエーテル溶液(AZエレクトロニックマテリアルズ株式会社製、アクアミカ(登録商標)NN120-20)と、アミン触媒(N,N,N′,N′-テトラメチル-1,6-ジアミノヘキサン(TMDAH))5質量%を含むパーヒドロポリシラザン20質量%のジブチルエーテル溶液(AZエレクトロニックマテリアルズ株式会社製、アクアミカ(登録商標)NAX120-20)とを、4:1の割合で混合し、さらにジブチルエーテルと2,2,4-トリメチルペンタンとの質量比が65:35となるように混合した溶媒で、塗布液の固形分が5質量%になるように、塗布液を希釈調製した。
真空紫外線照射は、図4に模式図で示した装置を用いて行った。
(イオン液体含有塗布液の調製)
液状ビスフェノールA型エポキシ樹脂(ジャパンエポキシレジン社製「828EL」)30質量部、オルソトルイジンジグリシジルアミン(日本化薬社製「GOT」)20質量部、アクリル系コアシェル樹脂(日本ゼオン社製「F351」)8質量部、固体分散型硬化剤(味の素ファインテクノ社製「VDH-J」)18質量部、固体分散型硬化剤(味の素ファインテクノ社製「PN40-J」)2質量部、ビフェニルアラルキル型エポキシ樹脂(日本化薬社製「NC3000」)の70質量%固形分のメチルエチルケトン(MEKという。)溶液85質量部、フェノキシ樹脂(ジャパンエポキシレジン社製「YX6954」)の35質量%MEK溶液60質量部をアジホモミキサーロボミックス型混合撹拌機(プライミクス社製)にて混合した混合物に、イオン液体1(N-アセチルグリシン1,1-ジメチルピロリジニウム塩)3質量部、溶媒(MEK)15質量部、溶媒(アセトン)20質量部とを混合し、高速回転ミキサーで均一に分散して、ワニス状のイオン液体含有塗布液を得た。該イオン液体含有塗布液を前記で得たバリアー層A10上に、乾燥後の熱硬化性樹脂層の厚さが40μmになるよう、アプリケーターにて均一に塗布し、60~80℃で6分間乾燥させることにより本発明の封止フィルム1を得た。
イオン液体をイオン液体2(N-アセチルグリシンテトラブチルホスホニウム塩)に変更する以外は「封止フィルム1の製造」と全く同様にして本発明の封止フィルム2を得た。
イオン液体をイオン液体3(ギ酸1-エチル-3-メチルイミダゾリウム塩)に変更する以外は「封止フィルム1の製造」と全く同様にして本発明の封止フィルム3を得た。
〔ガスバリアー層A11の形成〕
ガスバリアー層の厚さを150nmに変更する以外は、〔ガスバリアー層A10の形成〕と全く同様にして、ガスバリアー層A11を形成した。
パーヒドロポリシラザンを20質量%含むジブチルエーテル溶液(AZエレクトロニックマテリアルズ株式会社製、アクアミカ(登録商標)NN120-20)をジブチルエーテルで5質量%濃度まで希釈した後、アミン触媒としてN,N,N′,N′-テトラメチル-1,6-ジアミノヘキサン(TMDAH)をパーヒドロポリシラザンに対して1質量%となる量で加え、さらにALCH(川研ファインケミカル株式会社製、アルミニウムエチルアセトアセテート・ジイソプロピレート)をパーヒドロポリシラザンに対して1質量%となる量で加え、塗布液を調製した。該塗布液を用いて前記で得たガスバリアー層A11の上に厚さ150nmのポリシラザン塗膜を成膜し、その後、露点-30℃にて6000mJ/cm2の照射量で、上記第ガスバリアー層A10の形成(塗布法)と同様の方法で真空紫外線照射処理を施して、ガスバリアー層A21を形成した。
イオン液体をイオン液体2に変更する以外は「封止フィルム4の製造」と全く同様にして本発明の封止フィルム5を得た。
〔ガスバリアー層C11の形成(スパッタ法)〕
ハードコート層(中間層)付透明樹脂基材(きもと株式会社製、クリアハードコート層(CHC)付ポリエチレンテレフタレート(PET)フィルム)を、株式会社アルバック製スパッタ装置の真空槽内にセットし、10-4Pa台まで真空引きし、放電ガスとしてアルゴンを分圧で0.5Pa導入した。雰囲気圧力が安定したところで放電を開始し酸化ケイ素(SiOx)ターゲット上にプラズマを発生させ、スパッタリングプロセスを開始した。プロセスが安定したところでシャッターを開きフィルムへの酸化ケイ素膜(SiOx)形成を開始した。150nmの膜が堆積したところでシャッターを閉じて成膜を終了し、ガスバリアー層C11を形成した。
ガスバリアー層の厚さを150nmに変更する以外は、〔ガスバリアー層A10の形成〕と全く同様にして、ガスバリアー層C11の上にガスバリアー層A11を形成した。
〔ガスバリアー層のC21の形成(プラズマCVD1法)〕
株式会社きもと製のクリアハードコートを施したPET基材(125μm厚)を、図2に示されるような製造装置31にセットして、搬送させた。次いで、成膜ローラー39と成膜ローラー40との間に磁場を印加するとともに、成膜ローラー39と成膜ローラー40にそれぞれ電力を供給して、成膜ローラー39と成膜ローラー40との間に放電してプラズマを発生させた。次いで、形成された放電領域に、成膜ガス(原料ガスとしてヘキサメチルジシロキサン(HMDSO)と反応ガスとして酸素ガス(放電ガスとしても機能する)との混合ガスを供給し、基材上に、プラズマCVD法にて厚さ150nmのガスバリアー層C21を形成した。この成膜方法を、CVD1法という。
原料ガスの供給量:50sccm(Standard Cubic Centimeter per Minute、0℃、1気圧基準)
酸素ガスの供給量:500sccm(0℃、1気圧基準)
真空チャンバ内の真空度:3Pa
プラズマ発生用電源からの印加電力:0.8kW
プラズマ発生用電源の周波数:70kHz
フィルムの搬送速度:1.0m/min
ガスバリアー層C21は、前記XPSデプスプロファイル測定により、炭素分布曲線、ケイ素分布曲線及び酸素分布曲線を作成したところ、下記(i)~(iii)を満たすことを確認した。
前記で得られたガスバリアー層C21の上にガスバリアー層A11を形成した。
ガスバリアー層A11をガスバリアー層A21に変更する以外は「封止フィルム7の製造」と全く同様にして本発明の封止フィルム8を得た。
〔ガスバリアー層のC12の形成(スパッタ法)〕
ガスバリアー層の厚さを100nmに変更する以外は、〔ガスバリアー層C11の形成〕と全く同様にして、ガスバリアー層C12を形成した。
ガスバリアー層の厚さを100nmに変更する以外は、〔ガスバリアー層A11の形成〕と全く同様にして、ガスバリアー層C12の上にガスバリアー層A12を形成した。
ガスバリアー層の厚さを100nmに変更する以外は、〔ガスバリアー層A21の形成〕と全く同様にして、ガスバリアー層A12の上にガスバリアー層A22を形成した。
〔ガスバリアー層のC22の形成(プラズマCVD法)〕
ガスバリアー層の厚さを100nmに変更する以外は、〔ガスバリアー層C21の形成〕と全く同様にして、ガスバリアー層C22を形成した。
〔ガスバリアー層のC23の形成(プラズマCVD2法)〕
株式会社きもと製のクリアハードコートを施したPET基材(125μm厚)を搬送させながら、下記に記載の条件に従って、プラズマ放電方式により、厚さ100nmのガスバリアー層C23を形成した。この成膜方法を、CVD2法という。
〈ガスバリアー層C23形成用の混合ガス組成物〉
放電ガス:窒素ガス 94.9体積%
薄膜形成ガス:テトラエトキシシラン 0.5体積%
添加ガス:酸素ガス 5.0体積%
(ガスバリアー層の成膜条件)
第1電極側 電源種類 応用電機製 80kHz
周波数 80kHz
出力密度 8W/cm2
電極温度 120℃
第2電極側 電源種類 パール工業製 13.56MHz CF-5000-13M
周波数 13.56MHz
出力密度 10W/cm2
電極温度 90℃
ガスバリアー層C23は、XPSデプスプロファイル測定により、炭素分布曲線、ケイ素分布曲線及び酸素分布曲線を作成したところ、それぞれ膜厚方向で分布が一定であり、前記(i)~(iii)を満たさないことを確認した。
〔ガスバリアー層C10の形成〕
ガスバリアー層の厚さを300nmに変更する以外は、〔ガスバリアー層C11の形成〕と全く同様にして、ガスバリアー層C10を形成した。
イオン液体を用いない以外は「封止フィルム1の製造」と全く同様にして比較の封止フィルム13を得た。
本発明の封止フィルムを用いて、有機薄膜電子デバイスである有機EL素子を作製した。
(ガラス基板の洗浄)
ガラス基板の洗浄は、それぞれ、クラス10000のクリーンルーム内と、クラス100のクリーンブース内にて行った。洗浄溶媒は半導体洗浄用洗剤及び超純水(18MΩ以上、全有機炭素(TOC):10ppb未満)を用い、超音波洗浄機とUV洗浄機を用いた。
ガラス基板上に、厚さ150nmのITO(酸化インジウム・スズ(Indiumu Tin Oxide:ITO))をスパッタ法により成膜し、フォトリソグラフィー法によりパターニングを行い、第一電極を形成した。なお、パターンは発光面積が50mm平方になるようなパターンとした。
正孔輸送層形成用塗布液を塗布する前に、第一電極が形成されたガラス基板の洗浄表面改質処理を、波長184.9nmの低圧水銀ランプを使用し、照射強度15mW/cm2、距離10mmで実施した。帯電除去処理は、微弱X線による除電器を使用し行った。
ポリエチレンジオキシチオフェン・ポリスチレンスルホネート(PEDOT/PSS、Bayer社製 Bytron P AI 4083)を純水で65%、メタノール5%で希釈した溶液を正孔輸送層形成用塗布液として準備した。
正孔輸送層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度100℃で溶媒を除去した後、引き続き、加熱処理装置を用い温度150℃で裏面伝熱方式の熱処理を行い、正孔輸送層を形成した。
上記で形成した正孔輸送層上に、以下に示す白色発光層形成用塗布液を、下記の条件によりスピンコーターで塗布した後、下記の条件で乾燥及び加熱処理を行い、発光層を形成した。白色発光層形成用塗布液は乾燥後の厚さが40nmになるように塗布した。
ホスト材として下記化学式H-Aで表される化合物1.0gと、ドーパント材として下記化学式D-Aで表される化合物を100mg、ドーパント材として下記化学式D-Bで表される化合物を0.2mg、ドーパント材として下記化学式D-Cで表される化合物を0.2mg、100gのトルエンに溶解し白色発光層形成用塗布液として準備した。
塗布工程を窒素ガス濃度99%以上の雰囲気で、塗布温度を25℃とした。
白色発光層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度60℃で溶媒を除去した後、引き続き、温度130℃で加熱処理を行い、発光層を形成した。
上記で形成した発光層の上に、以下に示す電子輸送層形成用塗布液を下記の条件によりスピンコーターで塗布した後、下記の条件で乾燥及び加熱処理し、電子輸送層を形成した。電子輸送層形成用塗布液は、乾燥後の厚さが30nmになるように塗布した。
塗布工程は窒素ガス濃度99%以上の雰囲気で、電子輸送層形成用塗布液の塗布温度を25℃とした。
電子輸送層は下記化学式E-Aで表される化合物を2,2,3,3-テトラフルオロ-1-プロパノール中に溶解し0.5質量%溶液とし電子輸送層形成用塗布液とした。
電子輸送層形成用塗布液を塗布した後、成膜面に向け高さ100mm、吐出風速1m/s、幅手の風速分布5%、温度60℃で溶媒を除去した後、引き続き、加熱処理部で、温度200℃で加熱処理を行い、電子輸送層を形成した。
上記で形成した電子輸送層上に、電子注入層を形成した。まず、基板を減圧チャンバに投入し、5×10-4Paまで減圧した。あらかじめ、真空チャンバにタンタル製蒸着ボートに用意しておいたフッ化セシウムを加熱し、厚さ3nmの電子注入層を形成した。
上記で形成した電子注入層の上であって、第一電極の取り出し電極になる部分を除く部分に、5×10-4Paの真空下で、第二電極形成材料としてアルミニウムを使用し、取り出し電極を有するように蒸着法にて、発光面積が50mm平方になるようにマスクパターン成膜し、厚さ100nmの第二電極を積層した。
以上のように、第二電極までが形成された各積層体を、再び窒素雰囲気に移動し、規定の大きさに、紫外線レーザーを用いて裁断し、有機EL素子を作製した。
作製した有機EL素子に、ソニーケミカル&インフォメーションデバイス株式会社製の異方性導電フィルムDP3232S9を用いて、フレキシブルプリント基板(ベースフィルム:ポリイミド12.5μm、圧延銅箔18μm、カバーレイ:ポリイミド12.5μm、表面処理NiAuメッキ)を接続した。
本発明の封止フィルムを保管代用条件として環境温湿度40℃・80%RHで3日間保存したのちに、封止フィルムの樹脂層を、酸素濃度10ppm以下、水分濃度10ppm以下のグローブボックス内で、80℃、0.04MPa荷重下、減圧(1×10-3MPa以下)吸引20秒、プレス20秒の条件で、有機EL素子形成ガラス基板に向けて真空プレスした。
上記作製した有機EL素子について、下記の方法に従って、加速劣化処理を施した後のダークスポットの評価を行うことにより、耐久性の評価を行った。
(加速劣化処理)
上記作製した各有機EL素子を、85℃、85%RHの環境下で1000時間の加速劣化処理を施した後、下記のダークスポットに関する評価を行った。
加速劣化処理を施した有機EL素子に対し、1mA/cm2の電流を印加し、24時間連続発光させた後、100倍のマイクロスコープ(株式会社モリテックス製MS-804、レンズMP-ZE25-200)でパネルの一部分を拡大し、撮影を行った。撮影画像を2mm四方スケール相当に切り抜き、ダークスポットの発生面積比率を求め、下記の基準に従って耐久性を評価した。評価ランクが、△であれば実用的な特性、○であればより実用的な特性、◎であれば全く問題のない好ましい特性であると判定した。
○:ダークスポット発生率が、0.3%以上1.0%未満である
△:ダークスポット発生率が、1.0%以上2.0%未満である
×:ダークスポット発生率が、2.0%以上5.0%未満である
××:ダークスポット発生率が、5.0%以上である。
封止フィルムを、半径10mmの曲率になるように、180度の角度で100回屈曲を繰り返し処理し、処理前後の封止フィルムの水蒸気透過率(WVTR)を測定し、比較した。
1a 基材
1b ガスバリアー層
1c 樹脂層
31 製造装置
32 送り出しローラー
33、34、35、36 搬送ローラー
39、40 成膜ローラー
41 ガス供給管
42 プラズマ発生用電源
43、44 磁場発生装置
45 巻取りローラー
100 有機EL素子
101 第一電極
101a 下地層
101b 電極層
103 有機機能層
103a 正孔注入層
103b 正孔輸送層
103c 発光層
103d 電子輸送層
103e 電子注入層
105a 第二電極
107 封止フィルム(基材+ガスバリアー層)
109 樹脂層
113 樹脂基板(透明基板)
113a 光取り出し面
115 補助電極
116 取り出し電極
h 発光光
201 装置チャンバ
202 Xeエキシマランプ
203 ホルダー
204 試料ステージ
205 試料
206 遮光板
Claims (6)
- 基材と、前記基材の片方の表面上に形成されたガスバリアー層と樹脂層とをこの順に備える封止フィルムであって、前記ガスバリアー層は少なくともポリシラザンを含有する塗布液を塗布して乾燥した層に改質処理を施してなる層であり、かつ前記樹脂層は少なくともイオン液体を含有することを特徴とする封止フィルム。
- 前記ガスバリアー層が、さらにアルミニウム化合物を含有することを特徴とする請求項1に記載の封止フィルム。
- 前記樹脂層に含有されるイオン液体が、少なくともアンモニウム系カチオン又はホスホニウム系カチオンと、N-アシルアミノ酸イオン又はカルボン酸系アニオンとから構成されることを特徴とする請求項1又は請求項2に記載の封止フィルム。
- 前記基材と前記ガスバリアー層の間に、当該基材の表面上に有機ケイ素化合物を含む原料ガスと酸素ガスとを用いて、磁場を印加した一対のローラー間に放電空間を有する放電プラズマ化学気相成長法により、さらにガスバリアー層が形成されていることを特徴とする請求項1から請求項3までのいずれか一項に記載の封止フィルム。
- 基材の片方の表面上に、ガスバリアー層と樹脂層とをこの順に形成する封止フィルムの製造方法であって、少なくともポリシラザンを含有する塗布液を塗布、乾燥した層に改質処理を施してガスバリアー層を形成する工程と、
当該ガスバリアー層上に少なくともイオン液体を含有する樹脂層液を塗布、乾燥して樹脂層を形成する工程と、
を有することを特徴とする封止フィルムの製造方法。 - 請求項1から請求項4までのいずれか一項に記載の封止フィルムで、封止されていることを特徴とする機能素子。
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015514790A JPWO2014178254A1 (ja) | 2013-04-30 | 2014-04-01 | 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 |
US14/785,638 US20160072096A1 (en) | 2013-04-30 | 2014-04-01 | Sealing film, method for producing same and functional element sealed by sealing film |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013094926 | 2013-04-30 | ||
JP2013-094926 | 2013-04-30 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2014178254A1 true WO2014178254A1 (ja) | 2014-11-06 |
Family
ID=51843389
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2014/059623 WO2014178254A1 (ja) | 2013-04-30 | 2014-04-01 | 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 |
Country Status (3)
Country | Link |
---|---|
US (1) | US20160072096A1 (ja) |
JP (1) | JPWO2014178254A1 (ja) |
WO (1) | WO2014178254A1 (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020004336A1 (ja) | 2018-06-26 | 2020-01-02 | 東京応化工業株式会社 | 液状組成物、量子ドット含有膜、光学フィルム、発光表示素子パネル、及び発光表示装置 |
WO2021015005A1 (ja) | 2019-07-19 | 2021-01-28 | 東京応化工業株式会社 | 波長変換膜、波長変換膜形成用組成物、及びクラスター含有量子ドットの製造方法 |
DE102022206729A1 (de) | 2022-06-30 | 2024-01-04 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | System und entsprechendes Herstellungsverfahren |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3825120B1 (en) | 2018-08-16 | 2024-05-22 | LG Chem, Ltd. | Encapsulation film |
WO2020205917A1 (en) * | 2019-04-01 | 2020-10-08 | First Solar, Inc. | Photovoltaic devices with encapsulation layers and systems and methods for forming the same |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006321052A (ja) * | 2005-05-17 | 2006-11-30 | Kuraray Co Ltd | ガスバリア性積層体の製造方法 |
WO2011016408A1 (ja) * | 2009-08-05 | 2011-02-10 | 味の素株式会社 | フィルム |
JP2011116124A (ja) * | 2009-10-30 | 2011-06-16 | Sumitomo Chemical Co Ltd | 積層フィルムの製造方法 |
WO2011102465A1 (ja) * | 2010-02-18 | 2011-08-25 | 三井化学東セロ株式会社 | 封止された機能素子 |
JP2012250181A (ja) * | 2011-06-03 | 2012-12-20 | Konica Minolta Holdings Inc | バリアーフィルムの製造方法及び電子機器 |
WO2013011872A1 (ja) * | 2011-07-15 | 2013-01-24 | コニカミノルタホールディングス株式会社 | ガスバリア性フィルム及びその製造方法 |
JP2013073810A (ja) * | 2011-09-28 | 2013-04-22 | Konica Minolta Holdings Inc | 透明電極およびその製造方法ならびに有機電子デバイス |
JP2013071390A (ja) * | 2011-09-29 | 2013-04-22 | Konica Minolta Advanced Layers Inc | バリアーフィルム及びバリアーフィルムの製造方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP3511325B2 (ja) * | 1995-04-19 | 2004-03-29 | 三井化学株式会社 | ガスバリヤー性フィルム |
JP2011018785A (ja) * | 2009-07-09 | 2011-01-27 | Konica Minolta Holdings Inc | 薄膜形成方法、ガスバリアフィルム、及び有機光電変換素子 |
JP2012082464A (ja) * | 2010-10-08 | 2012-04-26 | Sumitomo Chemical Co Ltd | プラズマcvd成膜装置、成膜方法、ガスバリア性積層フィルム |
KR101813171B1 (ko) * | 2011-09-01 | 2017-12-28 | 삼성전자주식회사 | 가스차단성 박막, 이를 포함하는 전자소자 및 이의 제조방법 |
-
2014
- 2014-04-01 JP JP2015514790A patent/JPWO2014178254A1/ja active Pending
- 2014-04-01 US US14/785,638 patent/US20160072096A1/en not_active Abandoned
- 2014-04-01 WO PCT/JP2014/059623 patent/WO2014178254A1/ja active Application Filing
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2006321052A (ja) * | 2005-05-17 | 2006-11-30 | Kuraray Co Ltd | ガスバリア性積層体の製造方法 |
WO2011016408A1 (ja) * | 2009-08-05 | 2011-02-10 | 味の素株式会社 | フィルム |
JP2011116124A (ja) * | 2009-10-30 | 2011-06-16 | Sumitomo Chemical Co Ltd | 積層フィルムの製造方法 |
WO2011102465A1 (ja) * | 2010-02-18 | 2011-08-25 | 三井化学東セロ株式会社 | 封止された機能素子 |
JP2012250181A (ja) * | 2011-06-03 | 2012-12-20 | Konica Minolta Holdings Inc | バリアーフィルムの製造方法及び電子機器 |
WO2013011872A1 (ja) * | 2011-07-15 | 2013-01-24 | コニカミノルタホールディングス株式会社 | ガスバリア性フィルム及びその製造方法 |
JP2013073810A (ja) * | 2011-09-28 | 2013-04-22 | Konica Minolta Holdings Inc | 透明電極およびその製造方法ならびに有機電子デバイス |
JP2013071390A (ja) * | 2011-09-29 | 2013-04-22 | Konica Minolta Advanced Layers Inc | バリアーフィルム及びバリアーフィルムの製造方法 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2020004336A1 (ja) | 2018-06-26 | 2020-01-02 | 東京応化工業株式会社 | 液状組成物、量子ドット含有膜、光学フィルム、発光表示素子パネル、及び発光表示装置 |
WO2021015005A1 (ja) | 2019-07-19 | 2021-01-28 | 東京応化工業株式会社 | 波長変換膜、波長変換膜形成用組成物、及びクラスター含有量子ドットの製造方法 |
DE102022206729A1 (de) | 2022-06-30 | 2024-01-04 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | System und entsprechendes Herstellungsverfahren |
WO2024002850A1 (de) | 2022-06-30 | 2024-01-04 | Deutsches Zentrum für Luft- und Raumfahrt e.V. | System und entsprechendes herstellungsverfahren |
Also Published As
Publication number | Publication date |
---|---|
JPWO2014178254A1 (ja) | 2017-02-23 |
US20160072096A1 (en) | 2016-03-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US9646940B2 (en) | Gas barrier film and electronic device | |
JP5888329B2 (ja) | ガスバリア性フィルム、ガスバリア性フィルムの製造方法、および電子デバイス | |
US9362524B2 (en) | Method for producing gas barrier film, gas barrier film, and electronic device | |
US20160153089A1 (en) | Gas barrier film, method for producing the same, and electronic device using the same | |
US20150364720A1 (en) | Gas barrier film | |
WO2014178254A1 (ja) | 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 | |
US20150284844A1 (en) | Electronic device and gas barrier film manufacturing method | |
WO2014123201A1 (ja) | ガスバリア性フィルム、およびその製造方法 | |
WO2014163062A1 (ja) | ガスバリアー性フィルムの製造方法、ガスバリアー性フィルム及び電子デバイス | |
WO2015182623A1 (ja) | ガスバリア性フィルムおよびそれを用いた電子デバイス | |
JP5987562B2 (ja) | ガスバリア性フィルムの製造方法及び電子デバイス | |
WO2016039237A1 (ja) | 機能素子及び機能素子の製造方法 | |
WO2015119260A1 (ja) | 変性ポリシラザン、当該変性ポリシラザンを含む塗布液および当該塗布液を用いて製造されるガスバリア性フィルム | |
WO2014119754A1 (ja) | ガスバリア性フィルムおよびその製造方法、ならびにこれを用いた電子デバイス | |
WO2016084791A1 (ja) | 封止フィルム、機能素子及び封止フィルムの製造方法 | |
JP2015080855A (ja) | 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 | |
JP6115297B2 (ja) | 封止フィルム、その製造方法及び封止フィルムで封止された機能素子 | |
WO2015083706A1 (ja) | ガスバリア性フィルム及びその製造方法 | |
WO2015146886A1 (ja) | ガスバリア性フィルムおよびその製造方法、ならびにこれを用いた電子デバイス | |
JPWO2015146886A6 (ja) | ガスバリア性フィルムおよびその製造方法、ならびにこれを用いた電子デバイス | |
WO2015053055A1 (ja) | 機能性膜 | |
WO2015029795A1 (ja) | ガスバリア性フィルムの製造方法 | |
JPWO2019230283A1 (ja) | ガスバリアー性基材、その製造方法、それを具備した電子デバイス | |
WO2014188981A1 (ja) | ガスバリア性フィルム |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 14792149 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 2015514790 Country of ref document: JP Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 14785638 Country of ref document: US |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 14792149 Country of ref document: EP Kind code of ref document: A1 |