WO1983000869A1 - Lead-containing composite metal oxide precursor composition, and process for its preparation - Google Patents
Lead-containing composite metal oxide precursor composition, and process for its preparation Download PDFInfo
- Publication number
- WO1983000869A1 WO1983000869A1 PCT/JP1982/000353 JP8200353W WO8300869A1 WO 1983000869 A1 WO1983000869 A1 WO 1983000869A1 JP 8200353 W JP8200353 W JP 8200353W WO 8300869 A1 WO8300869 A1 WO 8300869A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- lead
- metal oxide
- composite metal
- containing composite
- oxide precursor
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000012702 metal oxide precursor Substances 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 4
- 239000011651 chromium Substances 0.000 claims abstract description 4
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 4
- 239000011777 magnesium Substances 0.000 claims abstract description 4
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 239000011701 zinc Substances 0.000 claims abstract description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000010936 titanium Substances 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 150000003609 titanium compounds Chemical class 0.000 claims description 5
- 150000002611 lead compounds Chemical class 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 2
- BLMLUAPGAFJNBS-UHFFFAOYSA-N C(C)C(C[Ti])CCCC Chemical compound C(C)C(C[Ti])CCCC BLMLUAPGAFJNBS-UHFFFAOYSA-N 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910017060 Fe Cr Inorganic materials 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000011572 manganese Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 18
- 150000004706 metal oxides Chemical class 0.000 abstract description 17
- -1 organic acid salt Chemical class 0.000 abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000010955 niobium Substances 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 229910052793 cadmium Inorganic materials 0.000 abstract description 3
- 150000004703 alkoxides Chemical class 0.000 abstract description 2
- 229910052715 tantalum Inorganic materials 0.000 abstract description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 229910052758 niobium Inorganic materials 0.000 abstract 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 16
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 15
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 14
- 238000000921 elemental analysis Methods 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- KKEBXNMGHUCPEZ-UHFFFAOYSA-N 4-phenyl-1-(2-sulfanylethyl)imidazolidin-2-one Chemical compound N1C(=O)N(CCS)CC1C1=CC=CC=C1 KKEBXNMGHUCPEZ-UHFFFAOYSA-N 0.000 description 8
- QJWDYDSKKWMXSO-UHFFFAOYSA-N lanthanum Chemical compound [La].[La] QJWDYDSKKWMXSO-UHFFFAOYSA-N 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000002243 precursor Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 4
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- 150000001298 alcohols Chemical class 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 150000002736 metal compounds Chemical class 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- KVNYFPKFSJIPBJ-UHFFFAOYSA-N 1,2-diethylbenzene Chemical compound CCC1=CC=CC=C1CC KVNYFPKFSJIPBJ-UHFFFAOYSA-N 0.000 description 2
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229940043232 butyl acetate Drugs 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- VJPLIHZPOJDHLB-UHFFFAOYSA-N lead titanium Chemical compound [Ti].[Pb] VJPLIHZPOJDHLB-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- PGMYKACGEOXYJE-UHFFFAOYSA-N pentyl acetate Chemical compound CCCCCOC(C)=O PGMYKACGEOXYJE-UHFFFAOYSA-N 0.000 description 2
- 239000003495 polar organic solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- OGYSYXDNLPNNPW-UHFFFAOYSA-N 4-butoxy-4-oxobutanoic acid Chemical compound CCCCOC(=O)CCC(O)=O OGYSYXDNLPNNPW-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 101100194706 Mus musculus Arhgap32 gene Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 241000287463 Phalacrocorax Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 241000705989 Tetrax Species 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 101100194707 Xenopus laevis arhgap32 gene Proteins 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- ZFBGUXUJXUFOLU-UHFFFAOYSA-L butanoate;lead(2+) Chemical compound [Pb+2].CCCC([O-])=O.CCCC([O-])=O ZFBGUXUJXUFOLU-UHFFFAOYSA-L 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
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
Definitions
- the present invention relates to the production of a composite metal oxide, and more particularly, to a lead-containing composite metal oxide precursor composition and a method for producing the same.
- Background art :
- Lead-containing composite metal oxides for example, lead-titanium, lead zirconate, titan-colcone (hereinafter referred to as “"), lanthanum-containing titanium -Lead solconate (hereinafter referred to as “PLZT”) is also an important material for electronics due to its excellent dielectric properties, piezoelectricity, and light transmission. It is.
- a solid-phase method in which an oxide of each metal component is used as a starting material and a high-temperature solid-state reaction is used, and various metals are used. It is known that a solution method is produced from a combined aqueous solution of the nitrates of the components by a method such as evaporation to dryness, freeze drying, spray pyrolysis, or the like.
- the produced lead-containing composite metal compound has a coarse particle size of several or more, has a wide particle size distribution, and is easily mixed, crushed, and sieved.
- a lead-containing composite metal oxide having a particle size of 1 or less and a narrow particle size distribution can be obtained.
- OMPI It is dried, freeze-dried or evaporated to dryness, and then calcined at a temperature of 550 to 950 TC for 16 to 32 hours to obtain a powder.
- the titanium nitrate generated in the middle of the reaction is unstable, it is difficult to store the above mixed aqueous solution.
- the powder obtained by this method tends to have a large particle size, and uses a powder of monoxide & as a lead source. Is inevitable and is obtained: The properties of the PLZT powder as a material for electoral openings are reduced.
- An object of the present invention is to provide an organic solvent-soluble ⁇ -containing composite metal oxide precursor composition which can improve the disadvantages of the above-mentioned method for producing a ⁇ -containing composite metal oxide by a known solution method. Target.
- the present inventors have conducted intensive studies to achieve the above-mentioned object, and as a result, they have reacted the alcohols of titanium or quinolecum with lead calcium carbonate.
- the resulting reaction composition is hydrolyzed and then sintered or directly decomposed to obtain a chemically and physically homogeneous lead-containing material with excellent electrical winding properties.
- the inventors have found that a composite metal oxide can be obtained, and have completed the present invention.
- the present invention is a.
- the lead-containing composite metal oxide precursor composition of the present invention which is a lead-containing composite metal oxide precursor composition represented by
- a precursor composition of titanium lead, 'black lead' or titanyl lead lead (PZT) can be obtained, and the composition formula can be obtained by conducting the reaction in the presence of organic peranthane.
- a precursor composition of lanthanum-containing titanzyl-cone lead (PLZT) represented by the following formula (I) is obtained. Magnesium, iron, chromium, and sub !! In the presence of &, manganese, nickel or nickel cadmium organic acid salts and / or niobate or titanium oxide Then, the composite metal oxide precursor composition represented by the composition formula [II] is obtained.
- the organic titanium compounds and organosilicon compounds represented by the general formula [ ⁇ ] are the same or different monovalent carbons in which ⁇ in the set formula [m] is the same or different.
- Tetraline Proboxitanium, Tetrabutoxytanium, Tetrax (2— Tetium, Tetraisoproboxil, and Tetrabutoxyl components are industrially available. It is particularly preferred for use as a raw material because it is produced and easy to work with.
- compounds having different substituents can be used. Considering the recovery of alcohols and esters formed by the reaction, it is preferable to use compounds having the same substituent.
- R ′ in the one-sided [IV] is the same or different monovalent hydrocarbon group, preferably, the number of carbon atoms
- titanium and / or -alkoxides of -cluconium as one of the starting compounds
- the lanthanum added as the third raw material or the metal represented by M ′ in the composition formula [II] is the same organic acid salt as lead, and is represented by
- the amount of the organic acid lanthanum is usually 25 mol or less of the lead compound.
- the organic acid salt of the metal represented by is less than 20 mol of the lead compound, and the metal represented by M is less than 20 mol.
- less than 40 mol of the compound (2) is added.
- the fifteen-containing composite oxide precursor composition of the present invention is sintered by hydrolysis or directly thermally decomposed.
- metal compounds such as barium and strontium, which can convert the electrical properties, optical properties, sinterability, etc. of the sintered body and thin film body of the obtained lead-containing composite metal oxide
- Alkaline earth metals such as titanium, and transition metals such as indium, antimony, tungsten, and yttrium. It can also react with the addition of organic clay.
- the reaction can proceed in the presence or absence of an organic solvent, but is preferably in the presence of an organic solvent having a boiling point of 100 X to 250 1 C, more preferably In the reaction
- Organic solvents include non-polar organic solvents such as toluene, xylene, diethylbenzene, tetralin, and decalin, and butanol.
- polar organic solvents such as hexanol, hexanol, 2-ethylhexanol, succinic acid butyl ester, dextran hexyl acid, and acid 2-ethylhexyl.
- c the reaction that can have a this to be used either substantially organic Ji data two U beam compounds of rows cormorants this and raw material in the absence of water pre-Z or organic 'Bruno Turkey - ⁇ It is preferable to prevent hydrolysis of the organic compound and the ⁇ -containing organic metal compound formed.
- reaction conditions of this reaction are preferably carried out in a dry atmosphere to avoid the hydrolysis, and the reaction rate and the reaction time are determined based on the types of raw materials and the use of solvents. It can be varied depending on the type and amount of the organic solvent, but generally 50 to 300 TC, preferably '100: to 250 ° C, for 0.5 to 60 hours, preferably 1 to 15 hours, and more preferably 1 to 8 hours under the flowing temperature of an organic solvent.
- the (containing metal complex precursor) composition of the present invention varies depending on the type of raw materials, the mixing ratio, the type of organic solvent, the reaction conditions, and the like, but the composition formula U]
- the lead-containing composite oxide precursor composition of the present invention is characterized in that the hydrolysis product is dried and calcined in an oxygen-containing gas stream at a temperature of 400 C or higher.]
- the hydrolysis product is dried and calcined in an oxygen-containing gas stream at a temperature of 400 C or higher.
- Fine crystals of 0.1 to 0.5 ⁇ of complex metal tympanic matter such as PLZT are easily formed.
- Cane-containing composite metal oxide coating can be formed.
- a high-concentration solution can be obtained, so that there is a great degree of freedom in selecting the following chemical and physical utilization means.
- substituent it may have a small amount of hydrolyzability, so it is preferable to store it in the air and under conditions that do not come into contact with moisture from other sources. Best form to:
- the reaction solution was heated up to the decal's dark point, and 4.4 r (60 m mot) of butanol and 8.0 r (69 m mo) of the ethyl acetate were distilled off.
- the solvent, decalin was distilled off under reduced pressure to obtain 21.6 fr of a pale yellow solid.
- the product was found to have acetyl and butyl groups by IR analysis.
- the molecular weight was 1920.
- Example 1 Obtained in Example 1. 10.8 r Decalin A solution of 15 ⁇ r is heated to 220 liters under normal pressure to remove most of the decalin, then completely decalated at 10 Terr, 100 "C, yellow A brown solid 10.6 was obtained.
- Example 5 6.8 r of the composition obtained in Example 5 was calcined for 2.5 hours at a temperature of 630 ° C. in an air stream to obtain PLZT powder 4.8.
- the benefit composition of the present invention has the following features.
- the metal atomic ratio is the same as the metal atomic ratio of the raw materials to be mixed. , And completely uniform, the metal atom ratio in the composition or the composite metal oxide obtained from the compound is the same as the metal atom ratio of the raw material to be blended. , And at the atomic level, a uniform distribution is obtained. An excellent ⁇ -containing composite metal oxide can be produced.
- the present invention provides a lead-containing composite metal oxide precursor composition that can be used for producing a lead-containing composite metal oxide and a method for producing the same.], And its industrial significance is extremely large. n
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP56/138877810903 | 1981-09-03 | ||
| JP56138877A JPS5841723A (ja) | 1981-09-03 | 1981-09-03 | 鉛含有複合有機金属化合物 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1983000869A1 true WO1983000869A1 (en) | 1983-03-17 |
Family
ID=15232196
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP1982/000353 WO1983000869A1 (en) | 1981-09-03 | 1982-09-03 | Lead-containing composite metal oxide precursor composition, and process for its preparation |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPS5841723A (enrdf_load_stackoverflow) |
| WO (1) | WO1983000869A1 (enrdf_load_stackoverflow) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60103031A (ja) * | 1983-11-10 | 1985-06-07 | Agency Of Ind Science & Technol | Ｐｌζｔ又はｐζｔの製造方法 |
| JPS6130183U (ja) * | 1984-07-27 | 1986-02-22 | 株式会社 高見沢サイバネテイツクス | ソフトウエア複写販売装置 |
| JP2016032007A (ja) * | 2014-07-28 | 2016-03-07 | 株式会社リコー | 圧電膜の製造方法、圧電素子の製造方法、液体吐出ヘッド及び画像形成装置 |
-
1981
- 1981-09-03 JP JP56138877A patent/JPS5841723A/ja active Granted
-
1982
- 1982-09-03 WO PCT/JP1982/000353 patent/WO1983000869A1/ja unknown
Non-Patent Citations (1)
| Title |
|---|
| Journal of the American Ceramic Society, Vol. 55, No. 11, (1972), L.M. BROWN, K.S. MAZDIYASNI, "Cold-Pressing and Low-Temperature Sintering of Alkoxy-Derived PLZT", p. 541-544. * |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0124796B2 (enrdf_load_stackoverflow) | 1989-05-15 |
| JPS5841723A (ja) | 1983-03-11 |
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