JP5531125B1 - 固体高分子形燃料電池用の触媒及びその製造方法 - Google Patents
固体高分子形燃料電池用の触媒及びその製造方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 141
- 239000000446 fuel Substances 0.000 title claims abstract description 29
- 239000005518 polymer electrolyte Substances 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000011777 magnesium Substances 0.000 claims abstract description 57
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 53
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 50
- 239000010941 cobalt Substances 0.000 claims abstract description 45
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims description 2
- 229940005991 chloric acid Drugs 0.000 claims description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- SWHAQEYMVUEVNF-UHFFFAOYSA-N magnesium potassium Chemical compound [Mg].[K] SWHAQEYMVUEVNF-UHFFFAOYSA-N 0.000 claims 1
- 230000000977 initiatory effect Effects 0.000 abstract description 9
- 238000010248 power generation Methods 0.000 abstract description 3
- 229940091250 magnesium supplement Drugs 0.000 description 43
- 229910052751 metal Inorganic materials 0.000 description 31
- 239000002184 metal Substances 0.000 description 31
- 239000003426 co-catalyst Substances 0.000 description 21
- 230000000694 effects Effects 0.000 description 20
- 239000000243 solution Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 16
- 238000005275 alloying Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 9
- 239000012266 salt solution Substances 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 229910000531 Co alloy Inorganic materials 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229910018979 CoPt Inorganic materials 0.000 description 5
- 229910001260 Pt alloy Inorganic materials 0.000 description 5
- 229910000905 alloy phase Inorganic materials 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 230000006872 improvement Effects 0.000 description 5
- 229910020634 Co Mg Inorganic materials 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 150000001868 cobalt Chemical class 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910002058 ternary alloy Inorganic materials 0.000 description 3
- 229910020707 Co—Pt Inorganic materials 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 159000000003 magnesium salts Chemical class 0.000 description 2
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- IKZWTUJFVXRBEC-UHFFFAOYSA-N O.O.O.O.[Mg].C(C)(=O)O Chemical compound O.O.O.O.[Mg].C(C)(=O)O IKZWTUJFVXRBEC-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 229960002337 magnesium chloride Drugs 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 description 1
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 230000004660 morphological change Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 150000003057 platinum Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
- H01M8/1018—Polymeric electrolyte materials
-
- B01J35/33—
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M2004/8678—Inert electrodes with catalytic activity, e.g. for fuel cells characterised by the polarity
- H01M2004/8689—Positive electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M2008/1095—Fuel cells with polymeric electrolytes
-
- 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
- Y02E60/50—Fuel cells
Abstract
【解決手段】本発明は、白金、コバルト、マグネシウムからなる触媒粒子が炭素粉末担体上に担持されてなる固体高分子形燃料電池用触媒であって、前記触媒粒子の白金、コバルト、マグネシウムの構成比(モル比)が、Pt:Co:Mg=1:0.4〜0.5:0.00070〜0.00095である固体高分子形燃料電池用触媒である。この触媒は、白金触媒に、コバルトとマグネシウムを担持した後に、熱処理及び酸化性溶液に接触させる処理を経て製造するものであり、このようにして製造された触媒は、X線回折分析における2θ=40°〜42°の間で現れるメインピークのピーク位置に特徴があり、ピーク位置が41.0°〜41.5°にシフトしている。
【選択図】図1
Description
白金触媒を製造しこれにコバルト、マグネシウムを担持した。白金触媒は、炭素微粉末(比表面積約900m2/g)を担体とする白金担持率46.5質量%の白金触媒を5g(白金換算で2.325g(11.92mmol)用意した。そして、塩化コバルト(CoCl2・6H2O)1.89gと、塩化マグネシウム(MgCl2・6H2O)1.61gをイオン交換水100mLに溶解させたコバルト塩とマグネシウム塩の混合溶液を製造し、この混合溶液を上記白金触媒に含浸した。その後、還元剤として水素化ホウ素ナトリウムを添加してコバルト、マグネシウムを担持した。
Claims (6)
- 白金、コバルト、マグネシウムからなる触媒粒子が炭素粉末担体上に担持されてなる固体高分子形燃料電池用触媒であって、
前記触媒粒子の白金、コバルト、マグネシウムの構成比(モル比)が、Pt:Co:Mg=1:0.4〜0.5:0.00070〜0.00095である固体高分子形燃料電池用触媒。 - 触媒粒子についてのX線回折分析において、2θ=40°〜42°の間で現れるメインピークのピーク位置が41.0°〜41.5°である請求項1記載の固体高分子形燃料電池用触媒。
- 触媒粒子の担持密度は、30〜70%である請求項1又は請求項2に記載の固体高分子形燃料電池用の触媒。
- 請求項1〜請求項3のいずれか1項に記載の固体高分子形燃料電池用触媒の製造方法であって、
炭素粉末担体上に白金粒子が担持されてなる白金触媒に、コバルトとマグネシウムを担持する工程と、
コバルト及びマグネシウムが担持された白金触媒を700〜1100℃で熱処理する工程と、
前記熱処理後の触媒を少なくとも1回、酸化性溶液に接触させる工程と、を含む固体高分子形燃料電池用触媒の製造方法。 - 酸化性溶液は、硫酸、硝酸、亜リン酸、過マグネシウム酸カリウム、過酸化水素、塩酸、塩素酸、次亜塩素酸、クロム酸の少なくともいずれかである請求項4記載の固体高分子形燃料電池用触媒の製造方法。
- 酸化性溶液との接触処理は、処理温度を40〜110℃とし、接触時間を1〜30時間とする請求項4又は請求項5記載の固体高分子形燃料電池用触媒の製造方法。
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JP2013019304A JP5531125B1 (ja) | 2013-02-04 | 2013-02-04 | 固体高分子形燃料電池用の触媒及びその製造方法 |
CN201480007395.6A CN104969391B (zh) | 2013-02-04 | 2014-01-31 | 固体高分子型燃料电池用催化剂及其制造方法 |
KR1020157021648A KR101842332B1 (ko) | 2013-02-04 | 2014-01-31 | 고체 고분자형 연료 전지용의 촉매 및 그 제조 방법 |
PCT/JP2014/052209 WO2014119707A1 (ja) | 2013-02-04 | 2014-01-31 | 固体高分子形燃料電池用の触媒及びその製造方法 |
US14/764,247 US9905859B2 (en) | 2013-02-04 | 2014-01-31 | Catalyst for solid polymer fuel cell and method for manufacturing the same |
EP14746144.6A EP2953195B1 (en) | 2013-02-04 | 2014-01-31 | Catalyst for polymer fuel cell and method for manufacturing the same |
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Cited By (2)
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US11239473B2 (en) | 2017-04-19 | 2022-02-01 | Tanaka Kikinzoku Kogyo K.K. | Catalyst for solid polymer fuel cells and method for manufacturing the same |
WO2022138270A1 (ja) | 2020-12-22 | 2022-06-30 | 田中貴金属工業株式会社 | 酸素還元反応用のコアシェル触媒及び触媒の設計方法 |
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JP6969996B2 (ja) * | 2016-12-09 | 2021-11-24 | トヨタ自動車株式会社 | 燃料電池用電極触媒及びその製造方法 |
JP6846210B2 (ja) * | 2017-01-17 | 2021-03-24 | 日産自動車株式会社 | 電極触媒ならびに当該電極触媒を用いる膜電極接合体および燃料電池 |
US11145874B2 (en) | 2017-04-18 | 2021-10-12 | Tanaka Kikinzoku Kogyo K.K. | Catalyst for solid polymer fuel cells and method for producing same |
EP3843186A4 (en) * | 2018-08-22 | 2021-10-20 | Tanaka Kikinzoku Kogyo K.K. | SOLID POLYMER FUEL CELL CATALYST AND SOLID POLYMER FUEL CELL CATALYST SELECTION METHOD |
WO2020246491A1 (ja) * | 2019-06-03 | 2020-12-10 | 東洋炭素株式会社 | 白金担持触媒、燃料電池用カソード、燃料電池、および白金担持触媒の製造方法 |
KR20230063021A (ko) * | 2021-11-01 | 2023-05-09 | 재단법인대구경북과학기술원 | 백금-알칼리토금속 합금을 포함하는 복합체, 이를 포함하는 연료전지 및 수전해 전지 그리고 이의 제조방법 |
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US11239473B2 (en) | 2017-04-19 | 2022-02-01 | Tanaka Kikinzoku Kogyo K.K. | Catalyst for solid polymer fuel cells and method for manufacturing the same |
WO2022138270A1 (ja) | 2020-12-22 | 2022-06-30 | 田中貴金属工業株式会社 | 酸素還元反応用のコアシェル触媒及び触媒の設計方法 |
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WO2014119707A1 (ja) | 2014-08-07 |
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KR20150105449A (ko) | 2015-09-16 |
EP2953195A4 (en) | 2016-08-17 |
CN104969391A (zh) | 2015-10-07 |
EP2953195B1 (en) | 2018-03-07 |
KR101842332B1 (ko) | 2018-03-26 |
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