JP4541900B2 - ナノ粒子製造用金属供給システム - Google Patents
ナノ粒子製造用金属供給システム Download PDFInfo
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- JP4541900B2 JP4541900B2 JP2004572053A JP2004572053A JP4541900B2 JP 4541900 B2 JP4541900 B2 JP 4541900B2 JP 2004572053 A JP2004572053 A JP 2004572053A JP 2004572053 A JP2004572053 A JP 2004572053A JP 4541900 B2 JP4541900 B2 JP 4541900B2
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- Prior art keywords
- metal
- carboxylate
- oxide
- viscosity
- metals
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- 229910052751 metal Inorganic materials 0.000 title claims description 106
- 239000002184 metal Substances 0.000 title claims description 105
- 238000004519 manufacturing process Methods 0.000 title claims description 61
- 239000002105 nanoparticle Substances 0.000 title description 29
- 238000000034 method Methods 0.000 claims description 62
- 239000002243 precursor Substances 0.000 claims description 50
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 32
- 229910044991 metal oxide Inorganic materials 0.000 claims description 32
- 150000004706 metal oxides Chemical class 0.000 claims description 32
- 239000002904 solvent Substances 0.000 claims description 27
- 150000007942 carboxylates Chemical class 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 17
- 229910052726 zirconium Inorganic materials 0.000 claims description 17
- 229910052684 Cerium Inorganic materials 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 13
- 239000008096 xylene Substances 0.000 claims description 13
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 150000001340 alkali metals Chemical class 0.000 claims description 10
- 150000002739 metals Chemical class 0.000 claims description 10
- 150000007513 acids Chemical class 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- 239000001301 oxygen Substances 0.000 claims description 9
- 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 claims description 8
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 8
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 150000001735 carboxylic acids Chemical class 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 6
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 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 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 229910052723 transition metal Inorganic materials 0.000 claims description 5
- 150000003624 transition metals Chemical class 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052718 tin Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 150000003842 bromide salts Chemical class 0.000 claims description 3
- 150000001805 chlorine compounds Chemical class 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910001510 metal chloride Inorganic materials 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 229910052702 rhenium Inorganic materials 0.000 claims description 3
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- 239000010948 rhodium Substances 0.000 claims description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052776 Thorium Inorganic materials 0.000 claims description 2
- 229910052770 Uranium Inorganic materials 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 229910052793 cadmium Inorganic materials 0.000 claims description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052792 caesium Inorganic materials 0.000 claims description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- 150000004673 fluoride salts Chemical class 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052701 rubidium Inorganic materials 0.000 claims description 2
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 2
- 229910052715 tantalum Inorganic materials 0.000 claims description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 125000001931 aliphatic group Chemical group 0.000 claims 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims 1
- 125000003118 aryl group Chemical group 0.000 claims 1
- 150000001734 carboxylic acid salts Chemical class 0.000 claims 1
- 229910001507 metal halide Inorganic materials 0.000 claims 1
- 150000005309 metal halides Chemical class 0.000 claims 1
- 229910000000 metal hydroxide Inorganic materials 0.000 claims 1
- 150000004692 metal hydroxides Chemical class 0.000 claims 1
- 125000003944 tolyl group Chemical group 0.000 claims 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 claims 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 63
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 46
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 46
- 239000007788 liquid Substances 0.000 description 29
- 238000002441 X-ray diffraction Methods 0.000 description 25
- 239000000344 soap Substances 0.000 description 23
- 239000000243 solution Substances 0.000 description 23
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 16
- 239000002245 particle Substances 0.000 description 16
- 239000000843 powder Substances 0.000 description 16
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 14
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 13
- 230000015572 biosynthetic process Effects 0.000 description 13
- 239000000919 ceramic Substances 0.000 description 13
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 12
- 238000010586 diagram Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 12
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- 239000003208 petroleum Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 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 8
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 7
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- 238000002360 preparation method Methods 0.000 description 7
- 238000005245 sintering Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
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- 239000003054 catalyst Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000000446 fuel Substances 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 229910003455 mixed metal oxide Inorganic materials 0.000 description 6
- 238000005498 polishing Methods 0.000 description 6
- WNKMTAQXMLAYHX-UHFFFAOYSA-N barium(2+);dioxido(oxo)titanium Chemical compound [Ba+2].[O-][Ti]([O-])=O WNKMTAQXMLAYHX-UHFFFAOYSA-N 0.000 description 5
- FXNONNRUNQPNLF-UHFFFAOYSA-N cerium;2-ethylhexanoic acid Chemical compound [Ce].CCCCC(CC)C(O)=O.CCCCC(CC)C(O)=O.CCCCC(CC)C(O)=O FXNONNRUNQPNLF-UHFFFAOYSA-N 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 5
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- 238000011020 pilot scale process Methods 0.000 description 5
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- 238000003860 storage Methods 0.000 description 5
- 239000005662 Paraffin oil Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 4
- 229910002113 barium titanate Inorganic materials 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- NDWWLJQHOLSEHX-UHFFFAOYSA-L calcium;octanoate Chemical compound [Ca+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O NDWWLJQHOLSEHX-UHFFFAOYSA-L 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- SGGOJYZMTYGPCH-UHFFFAOYSA-L manganese(2+);naphthalene-2-carboxylate Chemical compound [Mn+2].C1=CC=CC2=CC(C(=O)[O-])=CC=C21.C1=CC=CC2=CC(C(=O)[O-])=CC=C21 SGGOJYZMTYGPCH-UHFFFAOYSA-L 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- RQSNFKKPWDDEKE-UHFFFAOYSA-L octanoate;zirconium(2+) Chemical compound [Zr+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O RQSNFKKPWDDEKE-UHFFFAOYSA-L 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 229910002084 calcia-stabilized zirconia Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 210000004027 cell Anatomy 0.000 description 3
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 3
- 239000012776 electronic material Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910002607 Gd0.1Ce0.9O1.95 Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 150000001991 dicarboxylic acids Chemical class 0.000 description 2
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Description
本発明は特定種の金属酸化物を製造する方法および前記方法で得ることができる特定の特徴を持たせた金属酸化物、特にセリウム、ジルコニウム、ガドリニウム、鉄、マンガンの酸化物、混合酸化物、特にアルカリ土類のチタン酸塩、アルカリ金属のマンガン酸塩、安定化ジルコニアおよびセリアに関する。
金属酸化物、特に混合金属酸化物は幅広い範囲の用途、例えばセラミック、重合体用添加剤、充填材、顔料、反応性表面、触媒、貯蔵材料、研磨用添加剤、膜、燃料電池などの用途を有する。とりわけ最も重要な金属酸化物は酸化セリウム、セリウム−ジルコニウムおよび他の安定化ジルコニア混合酸化物、チタン酸塩、また以下にセラミック酸化物と呼ぶ他の混合酸化物である。そのような材料をナノ粒子(直径が200nm未満の粒子)として用いると、少しではあるが挙げると、それらは有利な特性、例えば高い触媒活性、向上した加工能力、低い焼結温度、良好な分散性などを示す。チタン酸塩は蓄電器用誘電体として用いられる。形状を小さくするには誘電体シートを薄くする必要があるが、そのように薄いシートの製造では好適に非常に小さな粒子、例えばナノ粒子などが用いられることから、ナノ粒子に非常に興味が持たれている。
従って、本発明の一般的目的は、向上した特性を持つことから、用途が広い金属酸化物を製造するに適した方法ばかりでなくそのような金属酸化物を提供することにある。
− 既知の有機金属化合物の種類の数が僅かであり、有機金属化合物は全部いくらか高価でありおよび/または他の望まれない元素、例えばハロゲンなどを含有する。
− 安価な前駆体は主に水溶性である。しかしながら、水を用いて必要な高温を達成しよとすると費用および装置集約的(プラズマ、レーザー、マイクロ波、高希釈度)であることから、水はFSPにとってあまり良くない基材である。
以下に行う本発明の詳細な説明を考慮に入れることで本発明がより良好に理解されかつこの上に挙げた目的以外の目的も明らかになるであろう。そのような説明を添付図を参照にして行う。
本発明の金属酸化物は、少なくとも1種の金属カルボン酸塩(「金属石鹸」)を純粋または溶解した状態で用い次にその液を液滴にし、そしてそれに酸化を高温環境、特に炎内で受けさせる方法を用いて得ることができる。
一般的手順
実験室規模の組み立て[Maedler他(2002A)、図1]またはパイロット規模の石油バーナー[SYSTHERM、CH−8105 Regensdorf、Typ NS1、Ausfuehrung 1.1、1988、Nr.20940;制御装置(Satronic Type ZT801およびMMD870);Flicker検出器(Satronic IRP 1010);バーナー管の長さ:0.23m、直径:0.0825m;分散用ガスとして空気を1時間当たり720 l、液体を1時間当たり3リットル、図1および図2]を用いたフレーム溶射熱分解で混合酸化物粉末を製造した。§以下に標準的調製を後で記述する時、それを(3/3)として示す。金属含有液をシリンジポンプ(Inotech IR−232)で炎の中に3ml/分で入れた。前記炎を中心の噴霧供給、円形の予混合支持炎(直径6mm、スリット幅150μm)および円形のシートガス供給(焼結金属の管、内径11mm、外径18mm、1分当たり5 lの酸素)で構成させる。あらゆる実験で酸素(Pan Gas、99.8%)を分散用ガスとして用いて、それを3 l/分で供給した。メタン(1.5 l/分、Pan Gas、99%)と酸素(3.2 l/分)の混合物を内部スリットに供給することで、予混合炎を生じさせた。あらゆるガス流量を較正を受けさせておいた質量流量制御装置(Bronkhorst EL−Flow F201)で制御した。
キシレン、トルエン、石油、軽質パラフィン油または他の適切な溶媒に金属石鹸を相当する量で溶解させる。場合により、ある種のカルボン酸を加える。特定の物質を用いた一連の調製を以下に示す。
酸化鉄。 10mlのナフテン酸鉄(Strem Chemicals、CAS no.[1338−14−3]、LOT no.138222−S、ミネラルスピリット中80%、鉄が12質量%)を10mlのキシレンと混合する結果として暗赤色の溶液を生じさせる。この前駆体を3ml/分(セリア/ジルコニア実験の場合と同じ実験パラメーター)でメタン/酸素スプレー炎の中に噴霧すると、結果として、BET比表面積が71m2/gの酸化鉄ナノ粒子がもたらされる。生産速度:前駆体液1リットル当たり85gの酸化鉄。
カルシア安定化ジルコニアの製造
実験室規模。 3.5mlのオクタン酸ジルコニウム(IV)(工業品質、SocTech SA、ブカレスト、ルーマニア、CAS no.[18312−04−4]、ジルコニウムが16質量%)と8.5mlの2−エチルヘキサン酸と5.5mlのトルエンと0.5mlのオクタン酸カルシウム(工業品質、SocTech SA、ブカレスト、ルーマニア、CAS no.[242−197−8]、カルシウムが5.2質量%)を混合した後、標準的なパラメーターを用いて噴霧した。生じたままの粉末が示した比表面積は62m2/gであったが、空気中で焼結(700℃で16時間、5℃/分で上昇)後にそれは19m2/gまで低下する。
オクタン酸ジルコニウム(IV)(工業品質、SocTech SA、ブカレスト、ルーマニア、CAS no.[18312−04−4]、ジルコニウムが16質量%)が2kgで軽質パラフィン油が0.66リットルでオクタン酸カルシウム(工業品質、SocTech SA、ブカレスト、ルーマニア、CAS no.[242−197−8]、カルシウムが5.2質量%)が0.225リットルの混合物を大きい方のバーナー(一般的手順を参照)の中に3kg/時で噴霧すると結果として24.5m2/gの均一な白色粉末が生じる。生産速度:前駆体1リットル当たり180g。
実験室規模。 セリアの場合、10.5mlのオクタン酸セリウム(III)(SocTech SA、ブカレスト、ルーマニア、工業品質、CAS no.[56797−01−4]、セリウムが10.2質量%、Naを0.14質量%含有)を5.5mlのトルエンおよび2mlの2−エチルヘキサン酸で希釈する。標準的なパラメーターを用いた噴霧を行うと結果として67m2/gそして空気中で焼結(700℃で16時間、5℃/分で上昇)後に10m2/gがもたらされる。高品質の前駆体を噴霧すると結果として結果部分で考察するように安定性がずっとより高くなる。
オクタン酸セリウム(III)(SocTech SA、ブカレスト、ルーマニア、工業品質、CAS no.[56797−01−4]、セリウムが10.2質量%、Naを0.14質量%含有)が0.75kgで軽質パラフィン油が0.275リットルの混合物を大きい方のバーナー(一般的手順を参照)の中に3kg/時で噴霧すると結果として18m2/gの若干黄色がかった均一な粉末が生じ、空気中で焼結(700℃で16時間、5℃/分で上昇)後は4m2/gである。生産速度:前駆体1リットル当たり90g。
オクタン酸セリウム(III)(SocTech SA、ブカレスト、ルーマニア、工業品質、CAS no.[56797−01−4]、セリウムが10.2質量%、Naを0.14質量%含有)が2.5kgでオクタン酸ジルコニウム(IV)(SocTech SA、ブカレスト、ルーマニア、CAS no.[18312−04−4]、ジルコニウムが16質量%)が0.833kgでトルエンが0.833 lの混合物を大きい方のバーナー(一般的手順を参照)の中に3kg/時で噴霧すると結果として21m2/gの若干黄色がかった均一な粉末が生じ、空気中で焼結(700℃で16時間、5℃/分で上昇)後は14m2/gである。生産速度:前駆体1リットル当たり125g。
粘度の重要性
金属担体液を噴霧中に分散させて小さい液滴にする時の粘度は良好な液体分散が起こるに充分なほど低くなければならない。以下の第1表にフレーム溶射合成に適した液体粘度の範囲を示す。
材料の純度が熱安定性に対して示す重要性
金属カルボン酸塩の製造工程でナトリウムまたは塩化物が追加的元素として存在すると最終的生成物の安定性が大きな影響を受けるが、高純度の前駆体(金属含有量が>99%)と工業品質の前駆体(金属が99%未満、塩化物および主にナトリウムを含有)の比較を示す。ナトリウムが工業用前駆体に入っていると焼結後に安定性が大きく低下するが、その度合はセリアの場合が最大であり、それによって焼結速度が速くなる。高純度のオクタン酸セリウムを用いた実験と追加的にナトリウムを1質量%用いた実験の相互実験の結果としてもたらされた比表面積の損失は工業品質の前駆体の場合と同様であった。その結果を以下の第2表に示す。
入手可能な材料の範囲
示した実施例は、40g/時を超える生産速度を維持しながら比表面積が60m2/gを超える単一種の遷移金属酸化物を生じさせることができることを示している。そのような材料は幅広い範囲の製品および工程で使用可能である。電子材料、電池、強誘電体、永久磁石、コイルおよび磁性流体が僅かの例である。
材料の均一性
マンガン酸リチウム、チタン酸カルシウムまたはセリア/ジルコニアの透過電子顕微鏡画像は、本明細書に記述する方法を用いて粒径の範囲が狭いナノ粒子を得ることができることを示している。このことは、更に、X線回折パターンによって大きな結晶子が生じたことが示されたことでも裏付けされる。比表面積によってTEMで観察したような粒径範囲が更に裏付けされる。このようなデータは、明らかに、本発明をナノ粒子の製造で用いることができることを示している。
本カルボキシ方法は、ナノ粒子を容易に得ることを可能にする生産方法を与えるものである。金属石鹸を主前駆体として用いると、ナノ粒子を合成する時に通常の石油バーナーでさえ使用することができる。とりわけ遷移金属酸化物、アルカリ金属、アルカリ土類金属、希土類金属および遷移金属系列の元素の混合酸化物の粒子を製造したが、このことは、本方法の多様性を示している。そのような金属石鹸が基になった液体は取り扱いと貯蔵と混合の適合性を有することに加えて高い生産速度をもたらす。ナノ粒子を前駆体液1リットル当たり200gを超える量で生産することができると同時にバーナーの種類にも分散用ガス系にも炎の種類にもあまり注意を払う必要がないことから、そのような前駆体はフレーム溶射合成で用いるに他の金属供給系のいずれよりも非常に有利である。
Claims (19)
- 金属酸化物の製造方法であって、カルボキシレート基1個当たりの平均炭素価が少なくとも5の金属カルボン酸塩である少なくとも1種の金属前駆体を液滴にしそしてそれに酸化を炎中で受けさせ、かつ前記金属カルボン酸塩が、置換されていない芳香族もしくは脂肪族の直鎖もしくは分枝炭化水素から成る群から選択した少なくとも1種の粘度低下用溶媒と混合される金属酸化物の製造方法。
- カルボキシレート基1個当たりの平均炭素価が5〜8の範囲である請求項1記載の方法。
- 液滴にする前の前記金属カルボン酸塩が示す粘度が高くて100mPa sである請求項1または2記載の方法。
- 液滴にする前の前記金属カルボン酸塩が示す粘度が高くて40mPa sである請求項1から3のいずれか1項記載の方法。
- 少なくとも1種の金属カルボン酸塩と少なくとも1種の粘度低下用溶媒の混合物の加熱を行なうことで前記粘度を得る請求項3または4記載の方法。
- 前記粘度低下用溶媒が含有する酸1種または2種以上が多くて40%質量/質量である請求項1記載の方法。
- 前記溶媒が酸を全く含有しない請求項6記載の方法。
- 前記溶媒がトルエン、キシレン、低級脂肪族炭化水素およびこれらの混合物から成る群から選択した少なくとも1種の非極性溶媒を含んで成る請求項5から7のいずれか1項記載の方法。
- 前記金属カルボン酸塩をC1〜C18−カルボン酸塩およびこれらの混合物から成る群から選択する請求項1から8のいずれか1項記載の方法。
- 前記金属もしくは金属の組み合わせをセリウム、ジルコニウム、全ての希土類金属、リチウム、ナトリウム、カリウム、ルビジウムまたはセシウム、マグネシウム、カルシウム、ストロンチウム、バリウム、アルミニウム、ホウ素、ガリウム、インジウム、錫、鉛、アンチモン、ビスマス、スカンジウム、イットリウム、ランタン、チタン、ハフニウム、バナジウム、ニオブ、タンタル、クロム、モリブデン、タングステン、マンガン、レニウム、鉄、ルテニウム、オスミウム、コバルト、ロジウム、イリジウム、ニッケル、パラジウム、白金、銅、銀、金、亜鉛、カドミウム、トリウム、ウランおよびケイ素から選択する請求項1から9のいずれか1項記載の方法。
- 前記炎による酸化をスプレーバーナーで実施する請求項1から10のいずれか1項記載の方法。
- 前記酸化を少なくとも600℃の温度で実施する請求項1から11のいずれか1項記載の方法。
- 前記金属カルボン酸塩を金属酸化物、金属水酸化物、金属炭酸塩、金属ハロゲン化物から出発して生じさせる請求項1から12のいずれか1項記載の方法。
- 前記金属カルボン酸塩もしくは前記金属カルボン酸塩含有溶液のエンタルピーが少なくとも13kJ/gである請求項1から13のいずれか1項記載の方法。
- 前記金属カルボン酸塩がアルカリ金属、アルカリ土類金属、遷移金属、希土類金属、塩化物、フッ化物、臭化物、燐酸塩、硫酸塩、ケイ素および主族金属を包含する群の1種以上の元素の不純物を含有していて、前記不純物が0.5〜5質量%の範囲内の量で存在する請求項1から14のいずれか1項記載の方法。
- 前記液滴となる溶液が金属を1リットル当たり少なくとも0.15モル含有し、結果としてノズル1個当たり1時間当たり少なくとも0.15モルの金属もしくは金属酸化物の生産速度をもたらす請求項1から15のいずれか1項記載の方法。
- 酸素量が完全な変換が起こるほどではない炎を用い、結果として化学量論以下の金属酸化物が生じる請求項1から16のいずれか1項記載の方法。
- 生じたままの金属酸化物を追加的処置で相当する非酸化物に変化させる請求項1から17のいずれか1項記載の方法。
- 前記金属カルボン酸塩として、水を含有しない1種以上の金属塩化物を金属源として用いて、前記金属源とカルボン酸を塩化水素が発生するように反応させて、前記塩化水素を除去することで得られる金属カルボン酸塩を用い、塩化物含有量0.1質量%未満の金属酸化物が製造されることを特徴とする請求項1から18のいずれか1項記載の方法。
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JP2006525930A (ja) | 2006-11-16 |
US20060229197A1 (en) | 2006-10-12 |
CN1787964A (zh) | 2006-06-14 |
CN100431946C (zh) | 2008-11-12 |
EP1626929B1 (en) | 2019-02-20 |
US8007758B2 (en) | 2011-08-30 |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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LAPS | Cancellation because of no payment of annual fees |