JP2015071520A - セリア−ジルコニア系複合酸化物及びその製造方法、並びにそのセリア−ジルコニア系複合酸化物を用いた排ガス浄化用触媒 - Google Patents
セリア−ジルコニア系複合酸化物及びその製造方法、並びにそのセリア−ジルコニア系複合酸化物を用いた排ガス浄化用触媒 Download PDFInfo
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- JP2015071520A JP2015071520A JP2013209190A JP2013209190A JP2015071520A JP 2015071520 A JP2015071520 A JP 2015071520A JP 2013209190 A JP2013209190 A JP 2013209190A JP 2013209190 A JP2013209190 A JP 2013209190A JP 2015071520 A JP2015071520 A JP 2015071520A
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- Prior art keywords
- ceria
- composite oxide
- zirconia composite
- zirconia
- rare earth
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 305
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 238000000746 purification Methods 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 119
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 69
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 62
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000011164 primary particle Substances 0.000 claims abstract description 61
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 41
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000002245 particle Substances 0.000 claims abstract description 41
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 29
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 22
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 21
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims description 290
- 239000000843 powder Substances 0.000 claims description 65
- 238000000034 method Methods 0.000 claims description 55
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 28
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 66
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- 229910052760 oxygen Inorganic materials 0.000 abstract description 66
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- 229910000510 noble metal Inorganic materials 0.000 description 19
- 238000010521 absorption reaction Methods 0.000 description 18
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- 239000007864 aqueous solution Substances 0.000 description 16
- 238000001878 scanning electron micrograph Methods 0.000 description 15
- 230000009467 reduction Effects 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 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 9
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- 150000002910 rare earth metals Chemical class 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
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- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
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- 238000012423 maintenance Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000001629 suppression Effects 0.000 description 3
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000000703 Cerium Chemical class 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000002706 hydrostatic effect Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 101150082630 pdf-2 gene Proteins 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 229910052706 scandium Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 150000003754 zirconium Chemical class 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910052765 Lutetium Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052771 Terbium Inorganic materials 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
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- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 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
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- UJVRJBAUJYZFIX-UHFFFAOYSA-N nitric acid;oxozirconium Chemical compound [Zr]=O.O[N+]([O-])=O.O[N+]([O-])=O UJVRJBAUJYZFIX-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 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
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- GBNDTYKAOXLLID-UHFFFAOYSA-N zirconium(4+) ion Chemical compound [Zr+4] GBNDTYKAOXLLID-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
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- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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- B01J23/66—Silver or gold
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- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
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- B01J37/04—Mixing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract
Description
I(14/29)値≧0.02
I(28/29)値≦0.08
を満たすものであることを特徴とするものである。
I(14/29)値≧0.02
I(28/29)値≦0.08
を満たすものである。
I(14/29)値≧0.02
I(28/29)値≦0.08
を満たすセリア−ジルコニア系複合酸化物を得ることができる。
セリウムとジルコニウムとの含有比率がモル比([セリウム]:[ジルコニウム])で46:54であるセリア−ジルコニア系固溶体粉末を以下のようにして調製した。すなわち、先ず、CeO2換算で28質量%の硝酸セリウム水溶液452gと、ZrO2換算で18質量%のオキシ硝酸ジルコニウム水溶液590gと、含有されるセリウムの1.1倍モル量の過酸化水素を含む200gとを、中和当量に対して1.2倍当量のアンモニアを含有する水溶液321gに添加し、共沈物を生成し、得られた共沈物を遠心分離、洗浄(イオン交換水)した。次に、得られた共沈物を大気中110℃で10時間以上乾燥した後、400℃で5時間大気中にて焼成してセリウムとジルコニウムとの固溶体(CeO2−ZrO2固溶体)を得た。その後、前記固溶体を粉砕機(アズワン社製の商品名「ワンダーブレンダー」)を用いて篩で粒径が75μm以下となるように粉砕して、前記セリア−ジルコニア固溶体粉末を得た。
得られたLa含有セリア−ジルコニア複合酸化物(La−CZ複合酸化物)を大気中1100℃、5時間の条件で熱処理し、高温耐久試験を行った<1100℃air>。
得られたLa含有セリア−ジルコニア複合酸化物(La−CZ複合酸化物)をモデルガス流通下において1050℃、5時間の条件で熱処理し、高温耐久試験を行った<1050℃RL>。なお、モデルガスの流通条件は、窒素中に8容量%のCOを含むリッチガス(R)と、窒素中に20容量%のO2を含むリーンガス(L)とを15分ごとに交互に供給する条件とした。
前記得られたLa含有セリア−ジルコニア複合酸化物で耐久試験を行わなかったLa−CZ複合酸化物(Fresh)、耐久試験1後のLa−CZ複合酸化物(1100℃air)、及び耐久試験2後のLa−CZ複合酸化物(1050℃RL)を用い、それぞれLa−CZ複合酸化物の結晶相をX線回折法により測定した。なお、X線回折装置として理学電機社製の商品名「RINT−2100」を用いてX線回折パターンを測定(条件:X線源:Cu−Kα線(λ=0.15418nm)、管電圧:40kV、管電流:30mA)し、I(14/29)値及びI(28/29)値を求めた。得られた結果を、それぞれ表1に示す。
前記得られたLa含有セリア−ジルコニア複合酸化物で耐久試験を行わなかったLa−CZ複合酸化物(Fresh)、耐久試験1後のLa−CZ複合酸化物(1100℃air)、及び耐久試験2後のLa−CZ複合酸化物(1050℃RL)を用い、それぞれLa−CZ複合酸化物3gと、Pd(0.25wt%)を担持したPd/Al2O3触媒1gとを乳鉢で物理混合し、加圧成形、粉砕して、直径0.5mm〜1mmのペレット状の排ガス浄化用触媒を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.5at%となるランタン(La)を含む硝酸ランタン水溶液を調製して用いた以外は、実施例1と同様にして粒子状のLa含有セリア−ジルコニア複合酸化物を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.5at%となるイットリウム(Y)を含む硝酸イットリウム水溶液を調製して用いた以外は、実施例1と同様にして粒子状のY含有セリア−ジルコニア複合酸化物を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.5at%となるプラセオジム(Pr)を含む硝酸プラセオジム水溶液を調製して用いた以外は、実施例1と同様にして粒子状のPr含有セリア−ジルコニア複合酸化物を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.5at%となるランタン(La)を含む硝酸ランタン水溶液を調製して用い、焼成工程における焼成温度を1100℃とした以外は、実施例1と同様にして粒子状のLa含有セリア−ジルコニア複合酸化物を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として1.0at%となるランタン(La)を含む硝酸ランタン水溶液を調製して用いた以外は、実施例1と同様にして粒子状のLa含有セリア−ジルコニア複合酸化物を得た。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として2.5at%となるランタン(La)を含む硝酸ランタン水溶液を調製して用いた以外は、実施例1と同様にして粒子状のLa含有セリア−ジルコニア複合酸化物を得た。
実施例1において得られたセリア−ジルコニア複合酸化物(ランタン担持及び焼成を行わないもの)を、比較用の粒子状のセリア−ジルコニア複合酸化物として準備した。
希土類元素担持工程においてセリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として5.0at%となるランタン(La)を含む硝酸ランタン水溶液を調製して用いた以外は、実施例1と同様にして粒子状のLa含有セリア−ジルコニア複合酸化物を得た。
希土類元素(ランタン)担持工程においてランタンの代わりに鉄を用い、セリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として2.5at%となる鉄(Fe)を含む硝酸鉄水溶液を調製して用いた以外は、実施例1と同様にして粒子状のFe含有セリア−ジルコニア複合酸化物を得た。
表1に示した実施例1〜実施例7の結果と比較例1〜比較例3の結果との比較から明らかなように、添加希土類元素の含有量が希土類含有セリア−ジルコニア複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.1〜4.0at%の範囲内にあるとともに、前記希土類含有セリア−ジルコニア複合酸化物の一次粒子の表面から50nm以内の表面近傍領域に前記希土類元素の全量のうちの90at%以上が含有されている場合には(実施例1〜実施例7)、十分に優れた酸素貯蔵能(OSC)と十分に高度な耐熱性とを併せ持ち、高温に長時間晒された後においても十分に優れた酸素貯蔵能(OSC)を発揮することが確認された。
Claims (3)
- セリア及びジルコニアの複合酸化物を含むセリア−ジルコニア系複合酸化物であって、
該セリア−ジルコニア系複合酸化物はランタン(La)、イットリウム(Y)及びプラセオジム(Pr)からなる群から選択される少なくとも一種の希土類元素を合計で、前記セリア−ジルコニア系複合酸化物中のセリウム及びジルコニウムの総量に対して元素として0.1〜4.0at%含有するとともに、前記セリア−ジルコニア系複合酸化物の一次粒子の表面から50nm以内の表面近傍領域に前記希土類元素の全量のうちの90at%以上が含有されており、
前記セリア−ジルコニア系複合酸化物におけるセリウムとジルコニウムとの含有比率がモル比([セリウム]:[ジルコニウム])で43:57〜48:52の範囲にあり、
前記セリア−ジルコニア系複合酸化物の一次粒子の平均粒子径が2.2〜4.5μmであり、かつ、
大気中、1100℃の温度条件で5時間加熱後のX線回折測定により得られるCuKαを用いたX線回折パターンから求められる2θ=14.5°の回折線と2θ=29°の回折線との強度比{I(14/29)値}及び2θ=28.5°の回折線と2θ=29°の回折線との強度比{I(28/29)値}がそれぞれ以下の条件:
I(14/29)値≧0.02
I(28/29)値≦0.08
を満たすものであることを特徴とするセリア−ジルコニア系複合酸化物。 - セリア及びジルコニアの複合酸化物を含むセリア−ジルコニア系複合酸化物の製造方法であって、
セリウムとジルコニウムとの含有比率がモル比([セリウム]:[ジルコニウム])で43:57〜48:52の範囲にあり、かつ一次粒子の平均粒子径が2.2〜4.5μmの範囲にあるセリア−ジルコニア系複合酸化物粉末を準備する工程と、
前記工程により得られた前記複合酸化物粉末にランタン(La)、イットリウム(Y)及びプラセオジム(Pr)からなる群から選択される少なくとも一種の希土類元素を担持せしめる工程と、
前記希土類元素が担持されたセリア−ジルコニア系複合酸化物粉末を600〜1200℃で焼成することにより請求項1に記載のセリア−ジルコニア系複合酸化物を得る工程と、
を含むことを特徴とするセリア−ジルコニア系複合酸化物の製造方法。 - 請求項1に記載のセリア−ジルコニア系複合酸化物を含有していることを特徴とする排ガス浄化用触媒。
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US10112180B2 (en) | 2018-10-30 |
US20160250620A1 (en) | 2016-09-01 |
CN105636687A (zh) | 2016-06-01 |
CN105636687B (zh) | 2017-10-13 |
WO2015049575A1 (en) | 2015-04-09 |
DE112014004568T5 (de) | 2016-06-30 |
JP5883425B2 (ja) | 2016-03-15 |
BR112016007140A2 (pt) | 2017-08-01 |
BR112016007140B1 (pt) | 2021-03-30 |
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