JP2007145672A - 複合金属酸化物用原料組成物 - Google Patents
複合金属酸化物用原料組成物 Download PDFInfo
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- JP2007145672A JP2007145672A JP2005344700A JP2005344700A JP2007145672A JP 2007145672 A JP2007145672 A JP 2007145672A JP 2005344700 A JP2005344700 A JP 2005344700A JP 2005344700 A JP2005344700 A JP 2005344700A JP 2007145672 A JP2007145672 A JP 2007145672A
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- raw material
- metal oxide
- composite metal
- material composition
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- 239000002994 raw material Substances 0.000 title claims abstract description 131
- 229910044991 metal oxide Inorganic materials 0.000 title claims abstract description 120
- 150000004706 metal oxides Chemical class 0.000 title claims abstract description 120
- 239000000203 mixture Substances 0.000 title claims abstract description 104
- 239000002253 acid Substances 0.000 claims abstract description 58
- 150000002902 organometallic compounds Chemical class 0.000 claims abstract description 36
- 150000002148 esters Chemical class 0.000 claims abstract description 34
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 19
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 6
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 5
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims description 109
- 239000010955 niobium Substances 0.000 claims description 81
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical group COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 claims description 39
- 238000009835 boiling Methods 0.000 claims description 24
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- -1 lead metal carboxylate Chemical class 0.000 claims description 14
- 238000006068 polycondensation reaction Methods 0.000 claims description 9
- 229910052732 germanium Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 5
- 150000001733 carboxylic acid esters Chemical class 0.000 claims description 4
- 230000036961 partial effect Effects 0.000 claims description 4
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 35
- 239000000126 substance Substances 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 150000007513 acids Chemical class 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 112
- 239000000243 solution Substances 0.000 description 109
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 78
- 239000010936 titanium Substances 0.000 description 44
- 239000012528 membrane Substances 0.000 description 34
- 239000013078 crystal Substances 0.000 description 31
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 30
- 238000002441 X-ray diffraction Methods 0.000 description 30
- 238000002425 crystallisation Methods 0.000 description 30
- 230000008025 crystallization Effects 0.000 description 30
- 229910052751 metal Inorganic materials 0.000 description 27
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 27
- 239000003990 capacitor Substances 0.000 description 24
- 239000000758 substrate Substances 0.000 description 22
- 239000002184 metal Substances 0.000 description 21
- 150000004703 alkoxides Chemical class 0.000 description 19
- 238000000576 coating method Methods 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 16
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 15
- 238000005238 degreasing Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 238000010304 firing Methods 0.000 description 13
- 229910052745 lead Inorganic materials 0.000 description 13
- 238000004151 rapid thermal annealing Methods 0.000 description 13
- 239000002904 solvent Substances 0.000 description 13
- YUXIBTJKHLUKBD-UHFFFAOYSA-N Dibutyl succinate Chemical compound CCCCOC(=O)CCC(=O)OCCCC YUXIBTJKHLUKBD-UHFFFAOYSA-N 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 12
- 229960002097 dibutylsuccinate Drugs 0.000 description 12
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 12
- 229910052697 platinum Inorganic materials 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 239000012071 phase Substances 0.000 description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000012298 atmosphere Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000470 constituent Substances 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 229910020684 PbZr Inorganic materials 0.000 description 8
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 description 8
- 238000000137 annealing Methods 0.000 description 8
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 description 8
- BEPAFCGSDWSTEL-UHFFFAOYSA-N dimethyl malonate Chemical compound COC(=O)CC(=O)OC BEPAFCGSDWSTEL-UHFFFAOYSA-N 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 8
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 8
- 238000004528 spin coating Methods 0.000 description 8
- 230000008859 change Effects 0.000 description 7
- 230000007246 mechanism Effects 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- NBTOZLQBSIZIKS-UHFFFAOYSA-N methoxide Chemical compound [O-]C NBTOZLQBSIZIKS-UHFFFAOYSA-N 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 4
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229940046892 lead acetate Drugs 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000015654 memory Effects 0.000 description 4
- UPSOBXZLFLJAKK-UHFFFAOYSA-N ozone;tetraethyl silicate Chemical compound [O-][O+]=O.CCO[Si](OCC)(OCC)OCC UPSOBXZLFLJAKK-UHFFFAOYSA-N 0.000 description 4
- 229960005235 piperonyl butoxide Drugs 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 238000005809 transesterification reaction Methods 0.000 description 4
- 238000005160 1H NMR spectroscopy Methods 0.000 description 3
- QPRQEDXDYOZYLA-UHFFFAOYSA-N 2-methylbutan-1-ol Chemical compound CCC(C)CO QPRQEDXDYOZYLA-UHFFFAOYSA-N 0.000 description 3
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005481 NMR spectroscopy Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 150000001298 alcohols Chemical class 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229960005335 propanol Drugs 0.000 description 3
- 230000002829 reductive effect Effects 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 239000001384 succinic acid Substances 0.000 description 3
- 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 3
- MXLMTQWGSQIYOW-UHFFFAOYSA-N 3-methyl-2-butanol Chemical compound CC(C)C(C)O MXLMTQWGSQIYOW-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- JKRZOJADNVOXPM-UHFFFAOYSA-N Oxalic acid dibutyl ester Chemical compound CCCCOC(=O)C(=O)OCCCC JKRZOJADNVOXPM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 238000000224 chemical solution deposition Methods 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 description 2
- AQIXEPGDORPWBJ-UHFFFAOYSA-N pentan-3-ol Chemical compound CCC(O)CC AQIXEPGDORPWBJ-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- CYIDZMCFTVVTJO-UHFFFAOYSA-N pyromellitic acid Chemical compound OC(=O)C1=CC(C(O)=O)=C(C(O)=O)C=C1C(O)=O CYIDZMCFTVVTJO-UHFFFAOYSA-N 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 2
- 229940044613 1-propanol Drugs 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- DKMROQRQHGEIOW-UHFFFAOYSA-N Diethyl succinate Chemical compound CCOC(=O)CCC(=O)OCC DKMROQRQHGEIOW-UHFFFAOYSA-N 0.000 description 1
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical class OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 238000007664 blowing Methods 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
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- WOSVXXBNNCUXMT-UHFFFAOYSA-N cyclopentane-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C1CC(C(O)=O)C(C(O)=O)C1C(O)=O WOSVXXBNNCUXMT-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- IEPRKVQEAMIZSS-AATRIKPKSA-N diethyl fumarate Chemical compound CCOC(=O)\C=C\C(=O)OCC IEPRKVQEAMIZSS-AATRIKPKSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- XWENCHGJOCJZQO-UHFFFAOYSA-N ethane-1,1,2,2-tetracarboxylic acid Chemical compound OC(=O)C(C(O)=O)C(C(O)=O)C(O)=O XWENCHGJOCJZQO-UHFFFAOYSA-N 0.000 description 1
- RWLDAJMGAVDXSH-UHFFFAOYSA-N ethane-1,1,2-tricarboxylic acid Chemical compound OC(=O)CC(C(O)=O)C(O)=O RWLDAJMGAVDXSH-UHFFFAOYSA-N 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 150000002688 maleic acid derivatives Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- KPSSIOMAKSHJJG-UHFFFAOYSA-N neopentyl alcohol Chemical compound CC(C)(C)CO KPSSIOMAKSHJJG-UHFFFAOYSA-N 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003900 succinic acid esters Chemical class 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- GTZCVFVGUGFEME-HNQUOIGGSA-N trans-aconitic acid Chemical compound OC(=O)C\C(C(O)=O)=C/C(O)=O GTZCVFVGUGFEME-HNQUOIGGSA-N 0.000 description 1
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
- C01G33/006—Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
- C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
- C04B35/493—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT containing also other lead compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
【解決手段】複合金属酸化物用原料組成物は、複合金属酸化物を形成するための原料組成物であって、前記複合金属酸化物は、一般式AB1−xCxO3で示され、A元素は少なくともPbからなり、B元素はZr、Ti、V、WおよびHfの少なくとも一つからなり、C元素は、NbおよびTaの少なくとも一つからなり、前記原料組成物は、前記A元素、前記B元素または前記C元素を含む熱分解性有機金属化合物、前記A元素、前記B元素または前記C元素を含む加水分解性有機金属化合物、その部分加水分解物および/または重縮合物の少なくとも1種と、ポリカルボン酸およびポリカルボン酸エステルの少なくとも1種と、有機溶媒と、を含む。
【選択図】なし
Description
複合金属酸化物を形成するための原料組成物であって、
前記複合金属酸化物は、一般式AB1−xCxO3で示され、
A元素は少なくともPbからなり、
B元素はZr、Ti、V、WおよびHfの少なくとも一つからなり、
C元素は、NbおよびTaの少なくとも一つからなり、
前記原料組成物は、
前記A元素、前記B元素または前記C元素を含む熱分解性有機金属化合物、前記A元素、前記B元素または前記C元素を含む加水分解性有機金属化合物、その部分加水分解物および/または重縮合物の少なくとも1種と、
ポリカルボン酸およびポリカルボン酸エステルの少なくとも1種と、
有機溶媒と、を含む。
本実施形態にかかる複合金属酸化物用原料組成物(以下、「原料組成物」という)は、複合金属酸化物の成膜に用いられる。ここで、複合金属酸化物は、一般式AB1−xCxO3で示され、A元素は少なくともPbからなり、B元素はZr、Ti、V、WおよびHfの少なくとも一つからなり、C元素は、NbおよびTaの少なくとも一つからなることができる。
プロパノール(プロピルアルコール)として、1−プロパノール(沸点97.4℃)、2−プロパノール(沸点82.7℃)、
ブタノール(ブチルアルコール)として、1−ブタノール(沸点117℃)、2−ブタノール(沸点100℃)、2−メチル−1−プロパノール(沸点108℃)、2−メチル−2−プロパノール(融点25.4℃,沸点83℃)、
ペンタノール(アミルアルコール)として、1−ペンタノール(沸点137℃)、3−メチル−1−ブタノール(沸点131℃)、2−メチル−1−ブタノール(沸点128℃)、2,2ジメチル−1−プロパノール(沸点113℃)、2−ペンタノール(沸点119℃)、3−メチル−2−ブタノール(沸点112.5℃)、3−ペンタノール(沸点117℃)、2−メチル−2−ブタノール(沸点102℃)、
多価アルコール類;
エチレングリコール(融点−11.5℃,沸点197.5℃)、グリセリン(融点17℃,沸点290℃)。
複合金属酸化物膜の製造方法は、上述した本実施形態にかかる原料組成物を、基体上に塗布した後、熱処理することにより得られる。
以下、本発明の実施例について説明する。
(A)本実施例では、PZTN複合金属酸化物の原料組成物を調製した。有機金属化合物としては、Pb、Zr、Ti、およびNbの有機金属化合物をn−ブタノールに溶解した溶液を用いた。具体的には、酢酸鉛、ジルコニウムアルコキシド、チタンアルコキシドおよびオクチル酸ニオブを用いた。これらと、ポリカルボン酸エステルとしてのコハク酸ジメチルと、有機溶媒としてのn−ブタノールとを混合した。
本実施例では、溶液を調製する際に加熱する点で、実施例1と異なる。溶液の組成は実施例1と同様である。すなわち、原料組成物として、実施例1で用いられたPbZr0.2Ti0.8Nb0.2O3(PZTN)用溶液にシリコンアルコキシドを2モル%の割合で添加して原料組成物を得た。この原料組成物を80℃で60分間加熱した。
本実施例では、本願発明により得られたPZTNと従来のPZTとを比較する。成膜に用いられる溶液は、実施例2と同様にして、原料組成物を調製した。原料組成物の組成は以下のようである。
本実施例では、PZTN複合金属酸化物膜において、Nb添加量を0、5、10、20、30、40モル%と変化させて強誘電特性を比較した。全ての試料においてPbSiO3シリケートを5モル%添加している。溶液(原料組成物)は、実施例2と同様に調製され、コハク酸ジメチルおよび有機溶媒としてn−ブタノールを用いた。
比較のため、実施例2で用いたコハク酸ジメチルの代わりにモノカルボン酸エステルを用いた。
本実施例では、ポリカルボン酸エステルとして、コハク酸ジメチル、マレイン酸ジメチル、およびマロン酸ジメチルを用いて原料溶液を調製し、各原料溶液を用いて実施例2と同様にしてサンプルを形成した。
本実施例では、Nbの代わりにTaを含む酸化物を用いて原料溶液を調製し、実施例2と同様にしてサンプルを形成した。
本実施例では、結晶化温度を変えた他は、実施例1と同様にしてサンプルを形成した。
実施例7で用いたn−ブタノールの代わりに、有機溶媒としてアルカンであるn−オクタンを用いたほかは実施例7と同様にしてサンプルを得た。
本実施例では、有機溶媒としてn−ブタノールの代わりにエチレングリコールを用いた点で、実施例1と異なる。すなわち、本実施例では、PZTN複合金属酸化物膜は、Pb、Zr、TiおよびNbの少なくともいずれかを含む第1ないし第3の原料溶液と、ポリカルボン酸としてのコハク酸ジメチルと、有機溶媒としてのエチレングリコール(C2H6O2:二価アルコール)とを混合し、これらの混合液に含まれる酸化物を熱処理等により結晶化させて得られた。混合液は、原料溶液とコハク酸ジメチルとを1:1の割合でエチレングリコールに溶解したものである。
溶液):(第3の原料溶液)=2:6:2の比で混合する。さらに、複合金属酸化物膜の結晶化温度を低下させる目的で、第4の原料溶液として、PbSiO3結晶を形成するための縮重合体をエチレングリコールに無水状態で溶解した溶液を、1.5モル%の割合で上記混合溶液中に添加した。すなわち、原料組成物として上記第1、第2、第3および第4の原料溶液の混合溶液を用いることで、PZTNの結晶化温度を650℃で結晶化させることが可能となる。
本実施例では、PZTN複合金属酸化物膜は、Pb、Zr、Ti、およびNbの少なくともいずれかを含む第1ないし第3の原料溶液と、ポリカルボン酸としては、コハク酸ジメチル、マレイン酸ジメチル、マロン酸ジメチル、およびクエン酸トリブチルのいずれかと、有機溶媒としてのn−ブタノールとをそれぞれ混合し、これらの混合液に含まれる酸化物を熱処理等により結晶化させて得られた。混合液は、ゾルゲル原料とコハク酸ジメチル、マレイン酸ジメチル、マロン酸ジメチル、またはクエン酸トリブチルのそれぞれとを1:1の割合でn−ブタノールに溶解したものである。
まず、室温にて、PZTN形成用原料組成物a,b,c,dを、それぞれスピン塗布法によって白金基板に塗布し、ホットプレートを用いて150℃で乾燥処理を行い、アルコールを除去した。その後、ホットプレートを用いて300℃で脱脂熱処理を行った。その後、上記塗布工程、乾燥処理工程および脱脂熱処理を3回行った後、酸素中で650℃、5分間の結晶化アニール(焼成)により、膜厚120nmの複合金属酸化物膜のサンプルa,b,c,dを得た。結晶化のための焼成は、酸素雰囲気中で120℃/秒の昇温速度のサーマルラピッドアニール(RTA)を用いて行った。さらに、白金からなる上部電極をスパッタ法により形成して、複合金属酸化物キャパシタサンプルa,b,c,dを得た。
本発明の原料組成物を用いた複合金属酸化物の形成における反応機構に関する考察を行う。
まず、アルコキシドの反応機構を単純化してみるために、チタンアルコキシドを含む溶液について行った1H−NMRの結果を検討する。
次に、PZTNS(Pb(Zn,Ti,Nb)O3にSiが添加された複合金属酸化物)用の原料組成物について、1H−NMR分析を行ったところ、図50に示す結果が得られた。図50において、(A)は、BuOHに、Pb、Zr、Ti、SiおよびNbの有機金属化合物とDMSを室温で混合した溶液(1)のチャートを示す。Pbの有機金属化合物としては酢酸鉛を用い、Zr、TiおよびSiの有機金属化合物としては、それぞれアルコキシドを用い、Nbの有機金属化合物としてはオクチル酸ニオブを用いた。溶液(1)では、各金属の合計モル数とDMSのモル数とを等しくしている。
以上のことから、本発明にかかる原料組成物によって基板上に形成された塗布膜では、以下の反応が生じていることが考えられる。
、上記金属メトキシドのゾル体はコハク酸ジブチル溶液として基板上に存在すると考えられる。この溶液は、高い沸点と良好な濡れ性を併せ持った溶媒効果を有することができる。
Claims (13)
- 複合金属酸化物を形成するための原料組成物であって、
前記複合金属酸化物は、一般式AB1−xCxO3で示され、
A元素は少なくともPbからなり、
B元素はZr、Ti、V、WおよびHfの少なくとも一つからなり、
C元素は、NbおよびTaの少なくとも一つからなり、
前記原料組成物は、
前記A元素、前記B元素または前記C元素を含む熱分解性有機金属化合物、前記A元素、前記B元素または前記C元素を含む加水分解性有機金属化合物、その部分加水分解物および/または重縮合物の少なくとも1種と、
ポリカルボン酸およびポリカルボン酸エステルの少なくとも1種と、
有機溶媒と、を含む、複合金属酸化物用原料組成物。 - 請求項1において、
前記B元素は、ZrおよびTiであり、
前記C元素は、Nbである、複合金属酸化物用原料組成物。 - 請求項1または2において、
前記有機溶媒は、アルコールである、複合金属酸化物用原料組成物。 - 請求項1ないし3のいずれかにおいて、
前記複合金属酸化物は、0.05≦x<1の範囲でNbを含む、複合金属酸化物用原料組成物。 - 請求項4において、
前記複合金属酸化物は、0.1≦x≦0.3の範囲でNbを含む、複合金属酸化物用原料組成物。 - 請求項1ないし5のいずれかにおいて、
前記複合金属酸化物は、0.05≦x<1の範囲でTaを含む、複合金属酸化物用原料組成物。 - 請求項1ないし6のいずれかにおいて、
さらに、前記複合金属酸化物は、0.5モル%以上のSi、あるいはSiおよびGeを含む、複合金属酸化物用原料組成物。 - 請求項7において、
前記複合金属酸化物は、0.5〜5モル%のSi、あるいはSiおよびGeを含む、複合金属酸化物用原料組成物。 - 請求項1〜8のいずれかにおいて、
前記ポリカルボン酸または前記ポリカルボン酸エステルは、2価のカルボン酸またはカルボン酸エステルである、複合金属酸化物用原料組成物。 - 請求項1ないし9のいずれかにおいて、
前記A元素を含む有機金属化合物は、鉛のカルボン酸塩である、複合金属酸化物用原料組成物。 - 請求項1ないし10のいずれかにおいて、
前記B元素を含む有機金属化合物は、ニオブのカルボン酸塩である、複合金属酸化物用原料組成物。 - 請求項1ないし11のいずれかにおいて、
前記ポリカルボン酸または前記ポリカルボン酸エステルは、前記有機溶媒より高い沸点を有する、複合金属酸化物用原料組成物。 - 請求項1ないし12のいずれかにおいて、
前記ポリカルボン酸エステルは、コハク酸ジメチルである、複合金属酸化物用原料組成物。
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- 2006-11-28 US US11/605,561 patent/US20070119343A1/en not_active Abandoned
- 2006-11-29 EP EP06024716A patent/EP1790622A1/en not_active Withdrawn
- 2006-11-29 KR KR1020060118831A patent/KR100803440B1/ko not_active IP Right Cessation
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JP2011201773A (ja) * | 2004-02-27 | 2011-10-13 | Canon Inc | 圧電体薄膜、これを用いた圧電体素子、圧電アクチュエータ、インクジェット記録ヘッド |
US8012449B2 (en) | 2006-06-28 | 2011-09-06 | Seiko Epson Corporation | Method of manufacturing complex metal oxide powder and amorphous complex metal oxide |
Also Published As
Publication number | Publication date |
---|---|
KR20070057016A (ko) | 2007-06-04 |
EP1790622A1 (en) | 2007-05-30 |
US20070119343A1 (en) | 2007-05-31 |
KR100803440B1 (ko) | 2008-02-13 |
CN1990419A (zh) | 2007-07-04 |
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