JP5313891B2 - カーボンに担持された白金・タングステン電極触媒およびその製造方法 - Google Patents
カーボンに担持された白金・タングステン電極触媒およびその製造方法 Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims description 201
- 229910052697 platinum Inorganic materials 0.000 title claims description 96
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims description 67
- 229910052721 tungsten Inorganic materials 0.000 title claims description 65
- 239000010937 tungsten Substances 0.000 title claims description 65
- 239000003054 catalyst Substances 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title description 25
- 229910052799 carbon Inorganic materials 0.000 title description 25
- 239000000203 mixture Substances 0.000 claims description 72
- 239000002245 particle Substances 0.000 claims description 37
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 25
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- FQNHWXHRAUXLFU-UHFFFAOYSA-N carbon monoxide;tungsten Chemical group [W].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-].[O+]#[C-] FQNHWXHRAUXLFU-UHFFFAOYSA-N 0.000 claims description 14
- ZONODCCBXBRQEZ-UHFFFAOYSA-N platinum tungsten Chemical compound [W].[Pt] ZONODCCBXBRQEZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000010411 electrocatalyst Substances 0.000 claims description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 9
- 239000000446 fuel Substances 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 229910001080 W alloy Inorganic materials 0.000 description 19
- 229910001260 Pt alloy Inorganic materials 0.000 description 16
- 238000002441 X-ray diffraction Methods 0.000 description 16
- 230000000694 effects Effects 0.000 description 15
- 239000000243 solution Substances 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 10
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000010287 polarization Effects 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- -1 platinum group metals Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 241000167854 Bourreria succulenta Species 0.000 description 1
- 244000122871 Caryocar villosum Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 239000012901 Milli-Q water Substances 0.000 description 1
- 241000218737 Mycobacterium phage Power Species 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 241001534066 Smithatris supraneanae Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000019693 cherries Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003273 ketjen black Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- 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
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/652—Chromium, molybdenum or tungsten
- B01J23/6527—Tungsten
-
- 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
-
- 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
-
- 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
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Inert Electrodes (AREA)
- Powder Metallurgy (AREA)
Description
白金カルボニル錯体は、Electrochim.Acta.Vol.47、p.3733、2002、A.J.Dickinson等の方法の変法により調製した。塩化白金酸をTHFに溶解し、常時撹拌しながら24時間CO(50cc/min)により溶液をパージした。COによりパージする間に、溶液の色はオレンジ色から暗緑色に徐々に変化した。24時間後、濃暗色の溶液が得られた。
THFに代えてメタノールを用いたことを除き、実施例1の反応条件と同じに行った。
白金カルボニル錯体を水中で調製したことを除き、実施例1の反応条件と同じに行った。
上記のように調製した白金・タングステン合金ナノ粒子の試料を、X線回折法(XRD)により分析した。Bruker粉末X線回折装置、D8 Discover型およびD8Advance型、Ge(Li)固体検出器(CuKα放射)を使用した。回折パターンは、2θ=25°〜90°、掃引速度0.02°/ステップ、5s/ポイントで記録した。平均粒子径は、Scherrer式を用いて回折ピーク幅の広がりから見積もった。
電気化学的分析は、0.5M硫酸溶液中、対極として白金メッシュを、参照電極として飽和甘汞電極(SCE)を、作用電極として回転ディスク電極(RDE)を用いる従来の三電極系によって行った。作用電極は、ピペット操作で触媒インクをRDEチップ表面上に均一に滴下し、終夜空気乾燥して調製した。触媒インクは、担持触媒20mg、Milli−Q水20mlおよび希釈Nafion溶液1ml(5重量%、Aldrich)を混合して調製した。電解質溶液は、高純度アルゴンガスで脱気した後に、掃引速度200mV/s、対SHE電位0.1Vから1V、100サイクルでサイクリックボルタモグラムをとって電気化学的に洗浄した。さらに、電極触媒の活性をスクリーニングする前に高純度酸素ガスで飽和処理を行った。作用電極の電位制御はSolartronポテンシオスタットによりSCE参照電極を基準として行った。全ての動圧的分極測定は、回転速度2000rpmおよび掃引速度5mV/sで行なった。標準白金触媒担持カーボンと対比させた相対活性度を求めるために、白金質量活性を使用した。
Claims (19)
- 白金含有カルボニル錯体と、タングステン含有カルボニル錯体とを製造する工程を有し、
前記白金カルボニル錯体と前記タングステンカルボニル錯体とを接触させて白金・タングステン含有錯体を形成する第一の工程と、
前記白金・タングステン含有錯体を担持素材と接触させて白金・タングステン含有担持組成物を製造する第二の工程とを有し、
前記担持組成物を500℃から800℃までの温度範囲で還元雰囲気下焼成することを特徴とする白金・タングステン含有担持組成物の製造方法。 - 前記タングステン含有カルボニル錯体がタングステンヘキサカルボニルからなることを特徴とする請求項1に記載の製造方法。
- 前記白金含有カルボニル錯体と前記タングステン含有カルボニル錯体を接触させる前記工程が、この二種類のカルボニル錯体を有機溶媒中にて混合することを特徴とする請求項1に記載の製造方法。
- 前記有機溶媒がアルコール、メタノール、エタノールおよびテトラヒドロフランからなる群から選ばれる少なくとも一種類の溶媒であることを特徴とする請求項3に記載の製造方法。
- 前記第一の接触工程中にCOによりパージすることをさらに特徴とする請求項1に記載の製造方法。
- 前記担持素材が高表面積カーボンブラック、アルミナ担持素材およびジルコニア担持素材からなる群から選ばれる少なくとも一種類の担持素材であることを特徴とする請求項1に記載の製造方法。
- 前記担持組成物を700℃で焼成することをさらに特徴とする請求項1に記載の製造方法。
- 焼成後の担持組成物が1ナノメートルから4ナノメートルの平均粒子径を持つ粒子からなることを特徴とする請求項1に記載の製造方法。
- 前記粒子が1.4ナノメートルから2.8ナノメートルの平均粒子径を持つことを特徴とする請求項8に記載の製造方法。
- 前記担持組成物が含有率20原子パーセントから95原子パーセントの白金と、含有率5原子パーセントから80原子パーセントのタングステンとからなることを特徴とする請求項1に記載の製造方法
- 前記担持組成物が含有率30原子パーセントから45原子パーセントの白金と、含有率55原子パーセントから70原子パーセントのタングステンとからなることを特徴とする請求項1に記載の製造方法
- 前記担持組成物が燃料電池のカソードを含むことを特徴とする請求項1に記載の製造方法。
- 白金およびタングステンを含む金属組成物よりなる電極触媒において、前記白金は白金カルボニル錯体由来の白金よりなり、前記タングステンはタングステンカルボニル錯体由来のタングステンよりなり、前記白金カルボニル錯体および前記タングステンカルボニル錯体を互いに接触させて混合物を形成し、この混合物に担持素材を加え、前記混合物および前記担持素材を焼成して白金・タングステン含有組成物を形成し、
前記金属組成物は1ナノメートルから4ナノメートルの平均粒子径を持つ粒子からなり、前記金属組成物は含有率30原子パーセントから45原子パーセントの白金と、含有率55原子パーセントから70原子パーセントのタングステンとからなり、前記混合物と前記担持素材は還元雰囲気下500℃から800℃の温度範囲で焼成することを特徴とする電極触媒。 - 前記タングステン含有カルボニル錯体はタングステンヘキサカルボニルを含むことを特徴とする請求項13に記載の電極触媒。
- 前記白金カルボニル錯体と前記タングステンカルボニル錯体とを有機溶媒中にて互いに接触させることを特徴とする請求項13に記載の電極触媒。
- 前記有機溶媒はアルコール、メタノール、エタノールおよびテトラヒドロフランからなる群から選ばれる少なくとも一種類の溶媒であることを特徴とする請求項15に記載の電極触媒。
- 前記担持素材は高表面積カーボンブラック、アルミナ担持素材およびジルコニア担持素材からなる群から選ばれる少なくとも一種類の担持素材であることを特徴とする請求項13に記載の電極触媒。
- 前記混合物と前記担持素材は700℃の温度で焼成されることを特徴とする請求項13に記載の電極触媒。
- 前記金属組成物は1.4ナノメートルから2.8ナノメートルの平均粒子径を持つ粒子からなることを特徴とする請求項13に記載の電極触媒。
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US11/483,102 | 2006-07-10 | ||
US11/483,102 US7871954B2 (en) | 2006-07-10 | 2006-07-10 | Synthesis of carbon supported platinum-tungsten electrocatalysts |
PCT/US2007/073104 WO2008008744A2 (en) | 2006-07-10 | 2007-07-10 | Synthesis of carbon supported platinum-tungsten electrocatalysts |
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JP2009117355A (ja) * | 2007-10-18 | 2009-05-28 | Toshiba Corp | 燃料極触媒、燃料極触媒の製造方法、燃料電池および燃料電池の製造方法 |
JP5436059B2 (ja) * | 2009-06-10 | 2014-03-05 | 公立大学法人大阪府立大学 | 白金粒子担持カーボンブラック触媒の製造方法 |
ES2713565T3 (es) | 2011-07-25 | 2019-05-22 | Ilika Tech Ltd | Catalizador de núcleo-cubierta económico con alta estabilidad electroquímica |
GB2517394A (en) | 2013-01-16 | 2015-02-25 | Ilika Technologies Ltd | Composite materials |
GB2509916A (en) | 2013-01-16 | 2014-07-23 | Ilika Technologies Ltd | A mixed metal oxide material of tantalum and titanium |
GB201300810D0 (en) | 2013-01-16 | 2013-02-27 | Llika Technologies Ltd | Composite Materials |
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US6967183B2 (en) * | 1998-08-27 | 2005-11-22 | Cabot Corporation | Electrocatalyst powders, methods for producing powders and devices fabricated from same |
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KR100358853B1 (ko) * | 2000-04-04 | 2002-10-31 | 광주과학기술원 | 무수 금속 염화물을 사용한 직접 메탄올 연료전지용 백금합금 전극촉매의 제조방법 |
US6656870B2 (en) * | 2000-09-29 | 2003-12-02 | Osram Sylvania Inc. | Tungsten-containing fuel cell catalyst and method of making same |
US6939640B2 (en) * | 2001-09-21 | 2005-09-06 | E. I. Dupont De Nemours And Company | Anode electrocatalysts for coated substrates used in fuel cells |
JP2004127814A (ja) * | 2002-10-04 | 2004-04-22 | Toyota Motor Corp | 燃料電池用電極触媒及びその製造方法 |
EP1632001B1 (en) * | 2003-06-06 | 2012-05-30 | Symyx Solutions, Inc. | Platinum-titanium-tungsten fuel cell catalyst |
JP2005034779A (ja) * | 2003-07-16 | 2005-02-10 | Nissan Motor Co Ltd | 電極触媒およびその製造方法 |
JP4290524B2 (ja) * | 2003-10-23 | 2009-07-08 | 株式会社キャタラー | 燃料電池用カソード触媒 |
US7718309B2 (en) * | 2004-12-06 | 2010-05-18 | Honda Motor Co., Ltd. | Platinum and tungsten containing electrocatalysts |
US7736790B2 (en) * | 2004-12-06 | 2010-06-15 | Honda Motor Co., Ltd. | Platinum and tungsten containing electrocatalysts |
US7435504B2 (en) * | 2005-08-25 | 2008-10-14 | Honda Motor Co., Ltd. | Platinum, tungsten, and nickel or zirconium containing electrocatalysts |
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WO2008008744A2 (en) | 2008-01-17 |
US7871954B2 (en) | 2011-01-18 |
US20110105312A1 (en) | 2011-05-05 |
US20080008924A1 (en) | 2008-01-10 |
WO2008008744A3 (en) | 2008-05-22 |
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