CN109569594A - A kind of titanate supports noble metal base analysis oxygen elctro-catalyst and preparation method thereof - Google Patents
A kind of titanate supports noble metal base analysis oxygen elctro-catalyst and preparation method thereof Download PDFInfo
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- CN109569594A CN109569594A CN201811451186.7A CN201811451186A CN109569594A CN 109569594 A CN109569594 A CN 109569594A CN 201811451186 A CN201811451186 A CN 201811451186A CN 109569594 A CN109569594 A CN 109569594A
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- titanate
- catalyst
- noble metal
- analysis oxygen
- elctro
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- 239000003054 catalyst Substances 0.000 title claims abstract description 112
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 70
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000001301 oxygen Substances 0.000 title claims abstract description 62
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 62
- 238000004458 analytical method Methods 0.000 title claims abstract description 53
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000002253 acid Substances 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 18
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229940005991 chloric acid Drugs 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 12
- 239000010970 precious metal Substances 0.000 claims abstract description 12
- 238000009938 salting Methods 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 77
- 230000001376 precipitating effect Effects 0.000 claims description 35
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 22
- 229910052712 strontium Inorganic materials 0.000 claims description 21
- 238000001354 calcination Methods 0.000 claims description 18
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 17
- 229910002113 barium titanate Inorganic materials 0.000 claims description 17
- 239000013078 crystal Substances 0.000 claims description 16
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical group O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 9
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 4
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- LFSBSHDDAGNCTM-UHFFFAOYSA-N cobalt(2+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[Ti+4].[Co+2] LFSBSHDDAGNCTM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- PHGMGTWRSNXLDV-UHFFFAOYSA-N diethyl furan-2,5-dicarboxylate Chemical compound CCOC(=O)C1=CC=C(C(=O)OCC)O1 PHGMGTWRSNXLDV-UHFFFAOYSA-N 0.000 claims description 2
- DGXKDBWJDQHNCI-UHFFFAOYSA-N dioxido(oxo)titanium nickel(2+) Chemical compound [Ni++].[O-][Ti]([O-])=O DGXKDBWJDQHNCI-UHFFFAOYSA-N 0.000 claims description 2
- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 150000001768 cations Chemical class 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 19
- 229910052741 iridium Inorganic materials 0.000 description 16
- 238000005119 centrifugation Methods 0.000 description 15
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 150000002500 ions Chemical class 0.000 description 15
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 15
- 239000000725 suspension Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 12
- 238000013112 stability test Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000005868 electrolysis reaction Methods 0.000 description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011258 core-shell material Substances 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052707 ruthenium Inorganic materials 0.000 description 4
- MAZOHJVAXBNBPX-UHFFFAOYSA-N ruthenium hydrochloride Chemical compound Cl.[Ru] MAZOHJVAXBNBPX-UHFFFAOYSA-N 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical class CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 2
- 239000007784 solid electrolyte Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- -1 Iridium ion Chemical class 0.000 description 1
- 239000013132 MOF-5 Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- IUJMNDNTFMJNEL-UHFFFAOYSA-K iridium(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[Ir+3] IUJMNDNTFMJNEL-UHFFFAOYSA-K 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- 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
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
-
- 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
- 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
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
-
- 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
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
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Abstract
The invention belongs to elctro-catalyst fields, and in particular to a kind of titanate supports noble metal base analysis oxygen elctro-catalyst and preparation method thereof.The present invention mixes metal chloric acid and metatitanic acid salting liquid, because metal chloric acid has acidity, and in acid condition, the metal-oxygen structure on titanate surface and acid reaction generate the cation dissolution of metal, leave the titanate of perovskite structure of the surface with lattice vacancy, metal oxide containing precious metals are synthesized in the material surface, titanate has just been obtained and has supported noble metal base analysis oxygen elctro-catalyst；Preparation method of the present invention is simple, high safety, low for equipment requirements, is suitble to large-scale production；The analysis oxygen elctro-catalyst stability of acquisition is good, and reaction site is more, and catalytic activity is high.
Description
Technical field
The invention belongs to elctro-catalyst fields, and in particular to a kind of titanate support noble metal base analysis oxygen elctro-catalyst and its
Preparation method.
Background technique
Energy Conversion Technology is dissolved in renewable energy to play a significant role with storage, wherein solid polymer water electrolysis
It is more that (Solid polymer water electrolysis, SPE) technology has that high-efficient, small in size, start and stop are fast, the service life is long etc.
Kind advantage, gradually to be received both at home and abroad and being tentatively commercialized.
However since solid polymer water electrolysis technology needs to use noble metal as its catalyst, pile cost is more current
Universal lye electrolysis is higher, so limiting its application scale.Side is precipitated in hydrogen, can be used at present carbon-supported
Platinum catalyst reaches better performance under lower noble metal loadings.Hydrogen evolution reaction also only relates to 2 electricity
The overpotential of son, elctro-catalyst is relatively low.And be 4 electron reactions for oxygen evolution, the overpotential of elctro-catalyst is relatively
Height needs the catalyst using high noble metal (iridium/ruthenium) loading to reach preferable performance.However your gold is used merely
Belong to big as the consumption of catalyst, cost is excessively high, therefore generally can be added to carrier for noble metal as activity, and load is made
Type noble metal catalyst.Common carrier has TiO2、Al2O3、AC、SnO2With MOF etc., such as (Sun Liangliang, the Luo Ling such as Sun Liang is good
Rainbow, Shi Jijun, Cheng Liang, Liu Lili, Xu Xu have core-shell structure IrO2In research [J] of the electrolysis water oxygen-separating catalyst of@Ti
State's ceramics, 2017,53 (07): 36-40.) with H2IrCl6·nH2O and titanium valve are primary raw material, using sodium borohydride reduction
Prepare iridium package titanium (Ir@Ti) catalyst.By heating at different temperatures to Ir@Ti catalyst, IrO is prepared2
Wrap up Ti (IrO2@Ti) catalyst.Research shows that: the IrO of this method preparation2@Ti catalyst, nanoscale IrO2It is distributed in Ti
Grain surface, forms the coated catalytic layer with core-shell structure.The IrO handled at 500 DEG C2@Ti catalyst has highest
Oxygen evolution activity.Molar ratio according to Ir: Ti is the IrO of 1: 2,1: 6,1: 10 configurations2@Ti catalyst, with IrO2The increasing of content
Height forms IrO2Sheath configuration, IrO2Catalytic Layer, which is coated on, can be effectively reduced oxygen evolution potential.The wherein catalyst of 1:2
Oxygen best performance is analysed, under normal pressure, at 25 DEG C, electrolysis water electric current is 0.24Acm-2When decomposition voltage be 3V.Chinese patent
Application CN108546962A discloses a kind of preparation method of the electrolysis water oxygen-separating catalyst of high specific surface area porous carbon doped iridium,
Iridium ion is impregnated into using infusion process and obtains presoma in organic frame MOF-5 material and thus to prepare high-specific surface area more
Hole carbon doped iridium oxygen-separating catalyst, the preparation process improve corrosion resistance of the anode of electrolytic water catalyst in acidic electrolysis bath
With the stability of catalyst.But the step of this preparation method, is various, and needs more organic solvent, higher cost.
However, these researchs the problems such as that there are still catalyst activities is low, and preparation method is complicated, and consumption of organic solvent is big.This field skill
Art personnel have been devoted to find the carried noble metal analysis oxygen catalysis that a kind of preparation method is simple, at low cost, catalytic performance is good
Agent, and there is no the reports that titanate and noble metal base are combined as to analysis oxygen elctro-catalyst at present.
Summary of the invention
Therefore, in the prior art noble metal oxygen is supported without titanate the technical problem to be solved in the present invention is that overcoming
Compound prepares the defect of oxygen-separating catalyst, to provide a kind of preparation method simple, at low cost, good catalyst activity titanate
Support the analysis oxygen elctro-catalyst and preparation method thereof of noble metal base.
For this purpose, technical scheme is as follows:
A kind of titanate supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that including titanate, has crystal lattice vacancy
Titanate and metal oxide containing precious metals；The titanate is selected from strontium titanates, barium titanate, magnesium titanate, calcium titanate, iron titanate, metatitanic acid
One of copper, nickel titanate, cobalt titanate, metatitanic acid yttrium, zinc titanate, manganese titanate, metatitanic acid molybdenum, metatitanic acid silver.
Further, the metal oxide containing precious metals are yttrium oxide or ruthenium-oxide.
Further, the titanate is one of strontium titanates, barium titanate, calcium titanate.
Further, the titanate is strontium titanates.
Further, the titanate with crystal lattice vacancy, which is reacted by titanate with H+, is made.
Further, the mass ratio of the titanate and metal oxide containing precious metals is 10-99:1-90.
Further, the mass ratio of the titanate and metal oxide containing precious metals is 50-99:1-50.
Further, the analysis oxygen elctro-catalyst, it is described multiple including titanate nucleome and the composite layer for being coated on titanate
Closing layer includes the titanate and metal oxide containing precious metals with crystal lattice vacancy.
Further, the composite layer includes the titanate layer and noble metal oxide layer with crystal lattice vacancy；Or,
The composite layer includes the titanate layer with crystal lattice vacancy, noble metal oxide layer and by with crystal lattice vacancy
The mixed layer that the mixture of titanate and metal oxide containing precious metals is formed；Or,
The composite layer includes the mixing formed by the mixture of titanate and metal oxide containing precious metals with crystal lattice vacancy
Layer.
The present invention also provides the preparation methods that a kind of titanate supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that
The following steps are included:
(1) nano barium titanate salting liquid is mixed to form mixed solution with metal chloric acid, sodium hydroxide respectively；
(2) mixed solution for obtaining step (1) is centrifuged, and takes precipitating；
(3) the precipitating calcining obtained step (2) is to get analysis oxygen elctro-catalyst.
Further, in the step (1), after nano barium titanate salting liquid is first mixed with metal chloric acid, hydrogen is added
Sodium oxide molybdena forms the mixed solution that pH value is 5-11.
Further, in the step (1), after nano barium titanate salting liquid is mixed with sodium hydroxide, metal is added
Chloric acid forms mixed solution, and adjusts pH value less than 7.
Further, in the step (1), after nano barium titanate salting liquid is mixed with sodium hydroxide, metal is added
Chloric acid forms mixed solution, and adjusts pH value less than 7；It continuously adds acid or alkaline solution and pH value is adjusted to 5-11.
Further, the acid solution is hydrochloric acid, sulfuric acid or nitric acid.
Further, the metal chloric acid is chloro-iridic acid or ruthenium hydrochloride.
Further, in the step (1), the molar ratio of Nano titanate and metal chloric acid is 1:0.1-10.
Further, in the step (1), the incorporation time of nano barium titanate salting liquid and metal chloric acid is 5-20min.
Further, in the step (1), the concentration of nano barium titanate salting liquid is 0.01-1mol/L.
Further, in the step (1), the concentration of sodium hydroxide is 0.1-5mol/L.
It further, further include that gained is precipitated into the process repeatedly rinsed in the step (2).
Further, in the step (3), calcination temperature is 300-800 DEG C, calcines 1-4h.
Technical solution of the present invention has the advantages that
1, the present invention provides the preparation method that a kind of titanate supports noble metal base analysis oxygen elctro-catalyst, and metal chloric acid has
Acidity, and the metal-oxygen structure on titanate surface and acid reaction generate the cation dissolution of metal in acid condition, leave
Surface has the titanate of the perovskite structure of lattice vacancy, synthesizes yttrium oxide/ruthenium-oxide in the material surface, is just had
There is the high performance surface metal of more active sites that the titanate-yttrium oxide/ruthenium-oxide core-shell structure electro-catalysis to form vacancy is precipitated
Agent；Preparation method is simple, high safety, low for equipment requirements, is suitble to large-scale production.
2, the present invention provides the preparation method that a kind of titanate supports noble metal base analysis oxygen elctro-catalyst, by Nano titanate
Solution is mixed to form mixed solution with metal chloric acid, sodium hydroxide respectively, calcines after centrifuging and taking precipitating；It is first that metatitanic acid salting liquid is first
After mixing with metal chloric acid, sodium hydroxide processing step is added, it is vacant to be capable of forming relatively thick titanate lattice surface
Titanate layer.After first nano barium titanate salting liquid is mixed with sodium hydroxide, metal chloric acid is added, finally reaches PH less than 7
Processing step, be capable of forming the titanate layer of relatively thin titanate lattice surface omission.If solution in processing step
It is always alkalinity or neutral environment, then cannot obtains the titanate layer that surface has crystal lattice vacancy, be only capable of obtaining common metatitanic acid
Salt.
3, the present invention provides a kind of titanate and supports noble metal base analysis oxygen elctro-catalyst, with the high advantage of reactivity,
Common titanium oxide supports object poorly conductive, and metal incorporation can have an impact lattice, forms perovskite structure, increases
Catalyst performance is improved in catalyst reaction site, reduces noble metal loadings.
Detailed description of the invention
The XRD spectra for the analysis oxygen elctro-catalyst that Fig. 1 embodiment 1 is prepared；
The electronic structure of Fig. 2 strontium titanates and the dissolved variation of surface strontium；
Fig. 3 strontium titanates supports yttrium oxide core-shell structure elctro-catalyst SEM (a:5000X) (b:50000x) photo；
Fig. 4 is the oxygen evolution activity comparison of different catalysts.
Specific embodiment
There is provided following embodiments is to preferably further understand the present invention, it is not limited to the best embodiment party
Formula is not construed as limiting the contents of the present invention and protection scope, anyone under the inspiration of the present invention or by the present invention and its
The feature of his prior art is combined and any and identical or similar product of the present invention for obtaining, all falls within of the invention
Within protection scope.
Specific experiment step or condition person are not specified in embodiment, according to the literature in the art described routine experiment
The operation of step or condition can carry out.Reagents or instruments used without specified manufacturer, being can be by commercially available acquisition
Conventional reagent product.
The molecular formula of chloro-iridic acid and ruthenium hydrochloride used is Cl in embodiment6H2Ir·6H2O, Cl6H2Ru·6H2O；All buy
From lark prestige.Nano titanate partial size is 20-40nm, and nano-titanium dioxide partial size is 20-40nm.
Overpotential test method: overpotential test method: VA characteristic curve is measured using electrochemical workstation, in correspondence
Current density under decomposition voltage value, subtract the numerical value of voltage needed for kinetics (1.229V).Anode side catalyst load
Carrying capacity is 2mg/cm2。
Stability test condition: anode side catalyst loading is 2.5mg/cm2, select 115 film of Nafion (thickness 127
μm) as the solid electrolyte diaphragm in water electrolytic cell, select the Pt/C bought from Johnson Matthey company
(40wt%Pt) is used as cathode hydrogen evolution catalyst.Catalyst effective area is about 1cm2。
Embodiment 1
The preparation of strontium titanates supported iridium base analysis oxygen elctro-catalyst
0.23g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.5g is added
Chloro-iridic acid stirs 10min, and the sodium hydroxide solution of 2mol/L is added until pH is 9；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；550 DEG C of calcining 2h will be deposited in, 0.46g analysis oxygen elctro-catalyst is obtained.
Fig. 1 is the XRD spectra for the analysis oxygen elctro-catalyst being prepared, and as can be seen from the figure the peak position of SrO embodies two
A, i.e., surface is different with the Sr-O plane in crystal；Fig. 2 is electronic structure and the dissolved variation of surface strontium of strontium titanates, table
The Sr with crystal lattice vacancy is formed after the dissolution of face strontium1-xTiO3-y；Fig. 3 the present embodiment analysis oxygen elctro-catalyst SEM (a:5000X) (b:
50000x) photo；It can be good core-shell structure to the catalyst from the photo of 50000x.The larger particles of ellipsoid are
Strontium titanates, 100 ~ 300nm of diameter are the core in nucleocapsid catalyst.Fine particle on surface is to be wrapped in core surface as shell
Yttrium oxide component, 20 ~ 40nm of diameter.Both ingredients are evenly distributed in photo, form hole (5000x photo) structure,
It is most typical nucleocapsid elctro-catalyst herein.
After tested, the catalyst is in 10mA/cm2Under current density, overpotential 0.23V, by the stability test of 1h
Afterwards, current attenuation rate is 4%.
Embodiment 2
The preparation of strontium titanates supported iridium base analysis oxygen elctro-catalyst
0.23g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 6；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.After tested, the catalyst
In 10mA/cm2Under current density, overpotential 0.31V, after the stability test of 1h, current attenuation rate is 5.2%.
Embodiment 3
The preparation of strontium titanates supported ruthenium base analysis oxygen elctro-catalyst
0.21g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.5g is added
Ruthenium hydrochloride stirs 10min, and the sodium hydroxide solution of 2mol/L is added until pH is 9；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；550 DEG C of calcining 2h will be deposited in, 0.42g analysis oxygen elctro-catalyst is obtained.After tested, should
Catalyst is in 10mA/cm2Under current density, overpotential 0.25V, after the stability test of 1h, current attenuation rate is
4.5%.
Embodiment 4
The preparation of strontium titanates supported ruthenium base analysis oxygen elctro-catalyst
0.21g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 5g chlorine is added
Ruthenic acid stirs 10min, and the sodium hydroxide solution of 2mol/L is added until pH is 10；10000rpm is centrifuged 1h, takes precipitating, repeatedly floats
Wash the ion in centrifugation removal precipitating；800 DEG C of calcining 1h will be deposited in get analysis oxygen elctro-catalyst.After tested, which exists
10mA/cm2Under current density, overpotential 0.23V, after the stability test of 1h, attenuation rate 4.8%.
Embodiment 5
The preparation of strontium titanates supported iridium base analysis oxygen elctro-catalyst
2.3g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 2mol/ is added
The sodium hydroxide solution 10mL of L mixes 10min；0.5g chloro-iridic acid is added and stirs 5min；Using 2mol/L titration with hydrochloric acid until pH
It is 5；10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；400 DEG C of calcining 3h will be deposited in, i.e.,
Oxygen elctro-catalyst must be analysed.After tested, the catalyst is in 10mA/cm2Under current density, overpotential 0.33V, by the stabilization of 1h
Property test after, attenuation rate 5.0%.
Embodiment 6
The preparation of strontium titanates supported iridium base analysis oxygen elctro-catalyst
1.5g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 4mol/ is added
The sodium hydroxide solution 5mL of L mixes 10min；0.5g chloro-iridic acid is added and stirs 15min；Using 4mol/L titration with hydrochloric acid until pH
It is 5.5；10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；600 DEG C of calcinings will be deposited in
1.5h is to get analysis oxygen elctro-catalyst.After tested, the catalyst is under 10mA/cm2 current density, overpotential 0.29V, passes through
After the stability test of 1h, attenuation rate 3.9%.
Embodiment 7
The preparation of strontium titanates supported ruthenium base analysis oxygen elctro-catalyst
10g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 1mol/L is added
Sodium hydroxide solution 15mL, mix 10min, be added 2g ruthenium hydrochloride stir 10min, using 4mol/L titration with hydrochloric acid until pH be
6；10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；450 DEG C of calcining 2.5h will be deposited in, i.e.,
Oxygen elctro-catalyst must be analysed.After tested, the catalyst is under 10mA/cm2 current density, overpotential 0.28V, by the stabilization of 1h
Property test after, attenuation rate 5.4%.
Embodiment 8
The preparation of barium titanate supported iridium base analysis oxygen elctro-catalyst
0.23g nano barium carbonate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 6；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.
Embodiment 9
The preparation of zinc titanate supported iridium base analysis oxygen elctro-catalyst
0.23g nano barium titanate zinc powder body is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 6；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.
Embodiment 10
The preparation of calcium titanate supported iridium base analysis oxygen elctro-catalyst
0.23g nano barium titanate calcium powder body is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 6；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.
Embodiment 11
The preparation of metatitanic acid yttrium supported iridium base analysis oxygen elctro-catalyst
0.23g nano barium titanate yttrium powder body is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 6；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.
Comparative example 1
The yttrium oxide elctro-catalyst that titanium oxide supports:
0.23g nano-titanium dioxide (partial size: 20nm, specific surface area: 30m/g) powder is weighed, 40mL deionized water is added,
It stirs 30min and forms suspension, 0.5g chloro-iridic acid is added and stirs 10min, the sodium hydroxide solution of 2mol/L is added until pH is
9；10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；550 DEG C of calcining 2h will be deposited in, will be obtained
The yttrium oxide elctro-catalyst that titanium oxide supports.After tested, the catalyst is under 10mA/cm2 current density, overpotential 0.42V,
After the stability test of 1h, attenuation rate 10.4%.
Comparative example 2
The yttrium oxide elctro-catalyst that gold-plated titanium oxide supports:
0.23g plating metal/titanic oxide (gold 1% is attached to titanium dioxide) powder is weighed, 40mL deionized water, stirring is added
30min forms suspension, and 0.5g chloro-iridic acid is added and stirs 10min, and the sodium hydroxide solution of 2mol/L is added until pH is 9；
10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；550 DEG C of calcining 2h will be deposited in, will be plated
The yttrium oxide elctro-catalyst that golden titanium oxide supports.After tested, under 10mA/cm2 current density, overpotential is the catalyst
0.40V, after the stability test of 1h, attenuation rate 8.6%.
Comparative example 3
After 0.23g nano strontium titanate powder and 0.267g hydroxide iridium are mixed, in 550 DEG C of calcining 2h, oxygen electricity must be analysed and urged
Agent；After tested, the catalyst is in 10mA/cm2Under current density, overpotential 0.51V, after the stability test of 1h,
Current attenuation rate is 19%.
Comparative example 4
The preparation of metatitanic acid yttrium supported iridium base analysis oxygen elctro-catalyst
0.23g nano barium titanate yttrium powder body is weighed, 40mL deionized water is added, stirring 30min forms suspension, 0.1g is added
Chloro-iridic acid stirs 5min, and the sodium hydroxide solution of 0.1mol/L is added until pH is 2；10000rpm is centrifuged 1h, takes precipitating, repeatedly
Ion in rinsing centrifugation removal precipitating；300 DEG C of calcining 4h will be deposited in get analysis oxygen elctro-catalyst.After tested, the catalyst
In 10mA/cm2Under current density, overpotential 0.38V, after the stability test of 1h, current attenuation rate is 7.1%.
Comparative example 5
The preparation of strontium titanates supported iridium base analysis oxygen elctro-catalyst
0.23g nano strontium titanate powder is weighed, 40mL deionized water is added, stirring 30min forms suspension, is added
The sodium hydroxide solution 20mL of 1mol/L mixes 10min, and 0.5g chloro-iridic acid is added and stirs 10min, uses 4mol/L titration with hydrochloric acid
Until pH is 10；10000rpm is centrifuged 1h, takes precipitating, repeatedly the ion in rinsing centrifugation removal precipitating；450 DEG C will be deposited in forge
2.5h is burnt to get analysis oxygen elctro-catalyst.After tested, the catalyst is under 10mA/cm2 current density, overpotential 0.55V, warp
After crossing the stability test of 1h, attenuation rate 15.7%.
Experimental example 1
Catalyst activity test
Anode side catalyst loading is 2mg/cm2, select 115 film of Nafion (127 μm of thickness) as in water electrolytic cell
Solid electrolyte diaphragm, select the Pt/C (40wt%Pt) that buy from Johnson Matthey company as cathode analysis
Hydrogen catalyst.Catalyst effective area is about 1cm2.The oxygen evolution activities (LCV) of different catalysts is as shown in Figure 1, can be with from Fig. 4
Find out, the yttrium oxide elctro-catalyst that strontium titanates supports, current density is more than 10mA/cm at 1.4Vsce2, it is gold-plated titanium oxide
10 times of activity or so (1mA/cm of the yttrium oxide elctro-catalyst supported2), for the work for the yttrium oxide elctro-catalyst that titanium oxide supports
20 times or more (< 0.5mA/cm of property2).In the noble metal electrocatalyst of three kinds of base metals dispersion, oxidation that strontium titanates supports
Iridium catalyst performance is best.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of titanate supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that including titanate, with crystal lattice vacancy
Titanate and metal oxide containing precious metals；The titanate be selected from strontium titanates, barium titanate, magnesium titanate, calcium titanate, iron titanate, copper titanate,
One of nickel titanate, cobalt titanate, metatitanic acid yttrium, zinc titanate, manganese titanate, metatitanic acid molybdenum, metatitanic acid silver.
2. titanate according to claim 1 supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that the noble metal
Oxide is yttrium oxide or ruthenium-oxide.
3. titanate according to claim 1 or 2 supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that the titanium
Hydrochlorate is strontium titanates.
4. titanate according to claim 3 supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that described that there is crystalline substance
The titanate of lattice omission, which is reacted by titanate with H+, to be made.
5. titanate according to claim 1 to 4 supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that institute
The mass ratio for stating titanate and metal oxide containing precious metals is 10-99:1-90.
6. -5 any titanates support noble metal base analysis oxygen elctro-catalyst according to claim 1, which is characterized in that packet
Titanate nucleome and the composite layer for being coated on titanate are included, the composite layer includes the titanate and noble metal with crystal lattice vacancy
Oxide.
7. titanate according to claim 6 supports noble metal base analysis oxygen elctro-catalyst, which is characterized in that the composite layer
Including titanate layer and noble metal oxide layer with crystal lattice vacancy；Or,
The composite layer includes the titanate layer with crystal lattice vacancy, noble metal oxide layer and by the metatitanic acid with crystal lattice vacancy
The mixed layer that the mixture of salt and metal oxide containing precious metals is formed；Or,
The composite layer includes the mixed layer formed by the mixture of titanate and metal oxide containing precious metals with crystal lattice vacancy.
8. the preparation method that a kind of titanate supports noble metal base analysis oxygen elctro-catalyst, which comprises the following steps:
(1) nano barium titanate salting liquid is mixed to form mixed solution with metal chloric acid, sodium hydroxide respectively；
(2) mixed solution for obtaining step (1) is centrifuged, and takes precipitating；
(3) the precipitating calcining obtained step (2) is to get analysis oxygen elctro-catalyst.
9. preparation method according to claim 8, which is characterized in that in the step (1), by nano barium titanate salting liquid
After first being mixed with metal chloric acid, adds sodium hydroxide and form the mixed solution that pH value is 5-11.
10. preparation method according to claim 8, which is characterized in that in the step (1), Nano titanate is molten
After liquid is mixed with sodium hydroxide, adds metal chloric acid and form mixed solution, and adjust pH value less than 7.
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