JP5724708B2 - 誘電体薄膜形成用組成物、誘電体薄膜の形成方法及び該方法により形成された誘電体薄膜 - Google Patents
誘電体薄膜形成用組成物、誘電体薄膜の形成方法及び該方法により形成された誘電体薄膜 Download PDFInfo
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- JP5724708B2 JP5724708B2 JP2011158537A JP2011158537A JP5724708B2 JP 5724708 B2 JP5724708 B2 JP 5724708B2 JP 2011158537 A JP2011158537 A JP 2011158537A JP 2011158537 A JP2011158537 A JP 2011158537A JP 5724708 B2 JP5724708 B2 JP 5724708B2
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- Prior art keywords
- thin film
- copper
- dielectric thin
- composition
- capacitor
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- 239000010409 thin film Substances 0.000 title claims description 150
- 239000000203 mixture Substances 0.000 title claims description 74
- 238000000034 method Methods 0.000 title claims description 34
- 239000003990 capacitor Substances 0.000 claims description 75
- 239000010949 copper Substances 0.000 claims description 55
- 229910052751 metal Inorganic materials 0.000 claims description 42
- 239000002184 metal Substances 0.000 claims description 42
- 239000002131 composite material Substances 0.000 claims description 39
- 150000001875 compounds Chemical class 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 27
- 229910052802 copper Inorganic materials 0.000 claims description 27
- 229910044991 metal oxide Inorganic materials 0.000 claims description 21
- 150000004706 metal oxides Chemical class 0.000 claims description 21
- 229940120693 copper naphthenate Drugs 0.000 claims description 16
- SEVNKWFHTNVOLD-UHFFFAOYSA-L copper;3-(4-ethylcyclohexyl)propanoate;3-(3-ethylcyclopentyl)propanoate Chemical compound [Cu+2].CCC1CCC(CCC([O-])=O)C1.CCC1CCC(CCC([O-])=O)CC1 SEVNKWFHTNVOLD-UHFFFAOYSA-L 0.000 claims description 16
- 239000010408 film Substances 0.000 claims description 15
- 239000003381 stabilizer Substances 0.000 claims description 12
- 150000002902 organometallic compounds Chemical class 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 150000004703 alkoxides Chemical class 0.000 claims description 7
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 7
- GKJJZVUBNWHDLD-UHFFFAOYSA-L copper;2-ethylbutanoate Chemical compound [Cu+2].CCC(CC)C([O-])=O.CCC(CC)C([O-])=O GKJJZVUBNWHDLD-UHFFFAOYSA-L 0.000 claims description 7
- VNZQQAVATKSIBR-UHFFFAOYSA-L copper;octanoate Chemical compound [Cu+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O VNZQQAVATKSIBR-UHFFFAOYSA-L 0.000 claims description 7
- 150000002009 diols Chemical class 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 6
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 150000007942 carboxylates Chemical class 0.000 claims description 5
- LZJJVTQGPPWQFS-UHFFFAOYSA-L copper;propanoate Chemical compound [Cu+2].CCC([O-])=O.CCC([O-])=O LZJJVTQGPPWQFS-UHFFFAOYSA-L 0.000 claims description 5
- 239000012212 insulator Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 4
- 125000000962 organic group Chemical group 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 229940070710 valerate Drugs 0.000 claims description 4
- PUHAKHQMSBQAKT-UHFFFAOYSA-L copper;butanoate Chemical compound [Cu+2].CCCC([O-])=O.CCCC([O-])=O PUHAKHQMSBQAKT-UHFFFAOYSA-L 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 description 21
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- -1 i-valeric acid Chemical compound 0.000 description 11
- 239000010936 titanium Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 229910052454 barium strontium titanate Inorganic materials 0.000 description 6
- CINXMKKDUHOADH-UHFFFAOYSA-N copper;octanoic acid Chemical compound [Cu].CCCCCCCC(O)=O CINXMKKDUHOADH-UHFFFAOYSA-N 0.000 description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- FWPJKASAXSYLKP-UHFFFAOYSA-L barium(2+);2-ethylbutanoate Chemical compound [Ba+2].CCC(CC)C([O-])=O.CCC(CC)C([O-])=O FWPJKASAXSYLKP-UHFFFAOYSA-L 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 3
- SEKCXMNFUDONGJ-UHFFFAOYSA-L copper;2-ethylhexanoate Chemical compound [Cu+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O SEKCXMNFUDONGJ-UHFFFAOYSA-L 0.000 description 3
- MLFHJEHSLIIPHL-UHFFFAOYSA-N isoamyl acetate Chemical compound CC(C)CCOC(C)=O MLFHJEHSLIIPHL-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- XKFQWWYUSWDWTF-UHFFFAOYSA-L strontium;2-ethylbutanoate Chemical compound [Sr+2].CCC(CC)C([O-])=O.CCC(CC)C([O-])=O XKFQWWYUSWDWTF-UHFFFAOYSA-L 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 2
- GQKZRWSUJHVIPE-UHFFFAOYSA-N 2-Pentanol acetate Chemical compound CCCC(C)OC(C)=O GQKZRWSUJHVIPE-UHFFFAOYSA-N 0.000 description 2
- WFRBDWRZVBPBDO-UHFFFAOYSA-N 2-methyl-2-pentanol Chemical compound CCCC(C)(C)O WFRBDWRZVBPBDO-UHFFFAOYSA-N 0.000 description 2
- ATUUSOSLBXVJKL-UHFFFAOYSA-N 3-ethylpentanoic acid Chemical compound CCC(CC)CC(O)=O ATUUSOSLBXVJKL-UHFFFAOYSA-N 0.000 description 2
- ROWKJAVDOGWPAT-UHFFFAOYSA-N Acetoin Chemical compound CC(O)C(C)=O ROWKJAVDOGWPAT-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 125000005907 alkyl ester group Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
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- 230000001590 oxidative effect Effects 0.000 description 2
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 description 2
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- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
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- 150000004072 triols Chemical class 0.000 description 2
- 229940005605 valeric acid Drugs 0.000 description 2
- IGIDLTISMCAULB-YFKPBYRVSA-N (3s)-3-methylpentanoic acid Chemical compound CC[C@H](C)CC(O)=O IGIDLTISMCAULB-YFKPBYRVSA-N 0.000 description 1
- SHXHPUAKLCCLDV-UHFFFAOYSA-N 1,1,1-trifluoropentane-2,4-dione Chemical compound CC(=O)CC(=O)C(F)(F)F SHXHPUAKLCCLDV-UHFFFAOYSA-N 0.000 description 1
- CVBUKMMMRLOKQR-UHFFFAOYSA-N 1-phenylbutane-1,3-dione Chemical compound CC(=O)CC(=O)C1=CC=CC=C1 CVBUKMMMRLOKQR-UHFFFAOYSA-N 0.000 description 1
- YRAJNWYBUCUFBD-UHFFFAOYSA-N 2,2,6,6-tetramethylheptane-3,5-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(C)(C)C YRAJNWYBUCUFBD-UHFFFAOYSA-N 0.000 description 1
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- UWWDUVVCVCAPNU-UHFFFAOYSA-N 3-ethylhexanoic acid Chemical compound CCCC(CC)CC(O)=O UWWDUVVCVCAPNU-UHFFFAOYSA-N 0.000 description 1
- HXUIDZOMTRMIOE-UHFFFAOYSA-N 3-oxo-3-phenylpropionic acid Chemical compound OC(=O)CC(=O)C1=CC=CC=C1 HXUIDZOMTRMIOE-UHFFFAOYSA-N 0.000 description 1
- FHSUFDYFOHSYHI-UHFFFAOYSA-N 3-oxopentanoic acid Chemical compound CCC(=O)CC(O)=O FHSUFDYFOHSYHI-UHFFFAOYSA-N 0.000 description 1
- SQNZLBOJCWQLGQ-UHFFFAOYSA-N 6,6,7,7,8,8,8-heptafluoro-2,2-dimethyloctane-3,5-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(F)(F)C(F)(F)C(F)(F)F SQNZLBOJCWQLGQ-UHFFFAOYSA-N 0.000 description 1
- WDJHALXBUFZDSR-UHFFFAOYSA-N Acetoacetic acid Natural products CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical class O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 229910018921 CoO 3 Inorganic materials 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910019899 RuO Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910004121 SrRuO Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- ZRYCZAWRXHAAPZ-UHFFFAOYSA-N alpha,alpha-dimethyl valeric acid Chemical compound CCCC(C)(C)C(O)=O ZRYCZAWRXHAAPZ-UHFFFAOYSA-N 0.000 description 1
- BAZMYXGARXYAEQ-UHFFFAOYSA-N alpha-ethyl valeric acid Chemical compound CCCC(CC)C(O)=O BAZMYXGARXYAEQ-UHFFFAOYSA-N 0.000 description 1
- IGIDLTISMCAULB-UHFFFAOYSA-N anteisohexanoic acid Natural products CCC(C)CC(O)=O IGIDLTISMCAULB-UHFFFAOYSA-N 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- VJFFDDQGMMQGTQ-UHFFFAOYSA-L barium(2+);2-ethylhexanoate Chemical compound [Ba+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O VJFFDDQGMMQGTQ-UHFFFAOYSA-L 0.000 description 1
- TVSNZOUKUFGNLK-UHFFFAOYSA-N barium(2+);butan-1-olate Chemical compound [Ba+2].CCCC[O-].CCCC[O-] TVSNZOUKUFGNLK-UHFFFAOYSA-N 0.000 description 1
- CPUJSIVIXCTVEI-UHFFFAOYSA-N barium(2+);propan-2-olate Chemical compound [Ba+2].CC(C)[O-].CC(C)[O-] CPUJSIVIXCTVEI-UHFFFAOYSA-N 0.000 description 1
- UPURPFNAFBQPON-UHFFFAOYSA-N beta,beta-dimethyl valeric acid Chemical compound CCC(C)(C)CC(O)=O UPURPFNAFBQPON-UHFFFAOYSA-N 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- RMIKFWTVTCZVRL-UHFFFAOYSA-N butanoic acid;copper Chemical compound [Cu].CCCC(O)=O RMIKFWTVTCZVRL-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
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- 238000005234 chemical deposition Methods 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- NQDSPXCXIOLFGI-UHFFFAOYSA-L copper;heptanoate Chemical compound [Cu+2].CCCCCCC([O-])=O.CCCCCCC([O-])=O NQDSPXCXIOLFGI-UHFFFAOYSA-L 0.000 description 1
- SMNMOEIFYRALNM-UHFFFAOYSA-L copper;hexanoate Chemical compound [Cu+2].CCCCCC([O-])=O.CCCCCC([O-])=O SMNMOEIFYRALNM-UHFFFAOYSA-L 0.000 description 1
- NBPFTDFXKORRKN-UHFFFAOYSA-L copper;pentanoate Chemical compound [Cu+2].CCCCC([O-])=O.CCCCC([O-])=O NBPFTDFXKORRKN-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- GFAZHVHNLUBROE-UHFFFAOYSA-N hydroxymethyl propionaldehyde Natural products CCC(=O)CO GFAZHVHNLUBROE-UHFFFAOYSA-N 0.000 description 1
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- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- DLWBHRIWCMOQKI-UHFFFAOYSA-L strontium;2-ethylhexanoate Chemical compound [Sr+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O DLWBHRIWCMOQKI-UHFFFAOYSA-L 0.000 description 1
- XFZYNDKPEWGZNJ-UHFFFAOYSA-N strontium;butan-1-olate Chemical compound [Sr+2].CCCC[O-].CCCC[O-] XFZYNDKPEWGZNJ-UHFFFAOYSA-N 0.000 description 1
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 1
- OHULXNKDWPTSBI-UHFFFAOYSA-N strontium;propan-2-olate Chemical compound [Sr+2].CC(C)[O-].CC(C)[O-] OHULXNKDWPTSBI-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WMOVHXAZOJBABW-UHFFFAOYSA-N tert-butyl acetate Chemical compound CC(=O)OC(C)(C)C WMOVHXAZOJBABW-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- UAXOELSVPTZZQG-UHFFFAOYSA-N tiglic acid Natural products CC(C)=C(C)C(O)=O UAXOELSVPTZZQG-UHFFFAOYSA-N 0.000 description 1
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Description
Sr化合物: 2−エチル酪酸ストロンチウム
Ti化合物: チタニウムテトライソプロポキシド
Cu化合物: ナフテン酸銅、2−エチル酪酸銅、n−オクタン酸銅、2−エチルヘキサン酸銅、n−吉草酸銅、i−吉草酸銅、n−酪酸銅、i−酪酸銅、プロピオン酸銅、酢酸銅、硝酸銅
<実施例1>
有機溶媒として、十分に脱水処理した酢酸イソアミルを使用し、これにBa化合物及びSr化合物として、2−エチル酪酸バリウム及び2−エチル酪酸ストロンチウムを、Ba:Srのモル比が70:30となるように溶解させた。その後、得られた溶液にTi化合物として、チタニウムテトライソプロポキシドをBa:Sr:Tiのモル比が70:30:100となるように添加した。更にCu化合物としてナフテン酸銅を、BとAのモル比B/Aが0.02となるように添加して溶解させた。また、溶液安定化のため安定化剤(アセチルアセトン)を金属合計量に対して1倍モル加え、金属酸化物換算濃度が7質量%の薄膜形成用組成物を調製し、メンブランフィルターと加圧タンクを用いて濾過を行った。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.03となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.05となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.10となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりにジエタノールアミンを加えたこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりにトリエタノールアミンを加えたこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりにホルムアミドを加えたこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりに1−アミノ2−プロパノールを加えたこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりにプロピレングリコールを加えたこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりに1−アミノ2−プロパノールを加えたこと以外は、実施例2と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてナフテン酸銅の代わりに2−エチル酪酸銅を添加したこと以外は、実施例2と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、安定化剤としてアセチルアセトンの代わりにホルムアミドを加えたこと、及び乾燥雰囲気中で焼成を行ったこと以外は、実施例11と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物として2−エチル酪酸銅の代わりに硝酸銅を添加したこと、及び酸素雰囲気中で焼成を行ったこと以外は、実施例12と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.001となるように添加したこと以外は、実施例8と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.002となるように添加したこと以外は、実施例8と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.005となるように添加したこと以外は、実施例8と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.01となるように添加したこと以外は、実施例8と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてナフテン酸銅の代わりにn−オクタン酸銅を添加したこと、及びn−オクタン酸銅をBとAのモル比B/Aが0.01となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりに2−エチルヘキサン酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりにn−吉草酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりにi−吉草酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりにn−酪酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりにi−酪酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりにプロピオン酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、Cu化合物としてn−オクタン酸銅の代わりに酢酸銅を添加したこと以外は、実施例18と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.14となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
Cu化合物を添加しなかったこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.0005となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
次の表1に示すように、ナフテン酸銅をBとAのモル比B/Aが0.15となるように添加したこと以外は、実施例1と同様に、薄膜形成用組成物を調製し、薄膜キャパシタを得た。
実施例1〜26及び比較例1〜3で得られた薄膜キャパシタについて、リーク電流密度、チューナビリティー及び誘電率を評価した。また、実施例1〜26及び比較例1〜3で調製した誘電体薄膜形成用組成物に含まれる液中パーティクル数を測定し、組成物の保存安定性を評価した。これらの結果を次の表2に示す。
(3) 誘電率:厚さdで面積をSとする薄膜キャパシタのPt上部電極とPt下部電極間に、10MHzにてバイアス電圧0V印加のときの静電容量C0Vから、次の式(2)より誘電率εを算出した。真空の誘電率は8.854×10-12(F/m)を用いた。なお、静電容量C0Vは、インピーダンスマテリアルアナライザ(ヒューレット・パッカード社製:HP4291A)を用いて測定した。
(4) 保存安定性:調製した誘電体薄膜形成用組成物をメンブランフィルター(日本インテグリス株式会社製:孔径0.05μm)と加圧タンクを用いて濾過を行い、洗浄済みガラス製スクリュー管瓶(和歌山CIC研究所洗浄品)に移し、温度を7℃に保った状態で2ヶ月間保存した。濾過直後(2時間静置後)の組成物と2ヶ月経過後の保存後の組成物について0.5μm以上の液中パーティクル数(個/ml)を、パーティクルカウンター(リオン株式会社製:KS−42B)によりそれぞれ確認した。なお、表2中、保存後の組成物に含まれる液中パーティクル数が50個/ml未満の場合を「良」とし、50個/ml以上の場合を「不良」とした。
Claims (10)
- BST誘電体薄膜を形成するための誘電体薄膜形成用組成物において、
一般式:Ba1-xSrxTiyO3(式中0.2<x<0.6、0.9<y<1.1)で示される複合金属酸化物Aに、Cu(銅)を含む複合酸化物Bが混合した混合複合金属酸化物の形態をとる薄膜を形成するための液状組成物であり、
前記複合金属酸化物Aを構成するための原料及び前記複合酸化物Bを構成するための原料が、前記一般式で示される金属原子比を与えるような割合で、かつ前記Aと前記Bとのモル比B/Aが0.001≦B/A<0.15の範囲内となるように、有機溶媒中に溶解している有機金属化合物溶液からなり、
前記複合酸化物Bを構成するための原料が、ナフテン酸銅、n−オクタン酸銅、2−エチル酪酸銅、n−吉草酸銅、i−吉草酸銅、n−酪酸銅、i−酪酸銅又はプロピオン酸銅又は酢酸銅である
ことを特徴とする誘電体薄膜形成用組成物。 - 前記複合金属酸化物Aを構成するための原料が、有機基がその酸素又は窒素原子を介して金属元素と結合している化合物である請求項1記載の誘電体薄膜形成用組成物。
- 前記複合金属酸化物Aを構成するための原料が、金属アルコキシド、金属ジオール錯体、金属トリオール錯体、金属カルボン酸塩、金属β−ジケトネート錯体、金属β−ジケトエステル錯体、金属β−イミノケト錯体、及び金属アミノ錯体からなる群より選ばれた1種又は2種以上である請求項2記載の誘電体薄膜形成用組成物。
- β−ジケトン、β−ケトン酸、β−ケトエステル、オキシ酸、ジオール、トリオール、高級カルボン酸、アルカノールアミン及び多価アミンからなる群より選ばれた1種又は2種以上の安定化剤を、前記組成物中の金属合計量1モルに対して、0.2〜3モルの割合で更に含有する請求項1ないし3いずれか1項に記載の誘電体薄膜形成用組成物。
- BとAとのモル比B/Aが0.002≦B/A≦0.1である請求項1ないし4いずれか1項に記載の誘電体薄膜形成用組成物。
- 請求項1ないし5のいずれか1項に記載の誘電体薄膜形成用組成物を耐熱性基板に塗布し乾燥する工程を所望の厚さの膜が得られるまで繰返し行った後、空気中、酸化雰囲気中又は含水蒸気雰囲気中で該膜を結晶化温度以上で焼成することを特徴とする誘電体薄膜の形成方法。
- 請求項6記載の方法により形成されたCuを含むBST誘電体薄膜。
- 膜厚が100〜500nmの範囲にある誘電体薄膜を誘電体層として薄膜キャパシタを形成し、前記薄膜キャパシタの印加電圧を20Vとしたとき、リーク電流密度が3.0×10-6A/cm2以下、チューナビリティが70%以上となり、前記薄膜キャパシタの印加電圧を0Vとしたとき、誘電率が300以上となる請求項7記載のCuを含むBST誘電体薄膜。
- 請求項8記載の誘電体薄膜を有する薄膜コンデンサ、キャパシタ、IPD、DRAMメモリ用コンデンサ、積層コンデンサ、トランジスタのゲート絶縁体、不揮発性メモリ、焦電型赤外線検出素子、圧電素子、電気光学素子、アクチュエータ、共振子、超音波モータ、又はLCノイズフィルタ素子の複合電子部品。
- 請求項9に記載する100MHz以上の周波数帯域に対応した、誘電体薄膜を有する薄膜コンデンサ、キャパシタ、IPD、DRAMメモリ用コンデンサ、積層コンデンサ、トランジスタのゲート絶縁体、不揮発性メモリ、焦電型赤外線検出素子、圧電素子、電気光学素子、アクチュエータ、共振子、超音波モータ、又はLCノイズフィルタ素子の複合電子部品。
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