JP5058805B2 - 貴金属微粒子の製造方法 - Google Patents
貴金属微粒子の製造方法 Download PDFInfo
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- JP5058805B2 JP5058805B2 JP2007534369A JP2007534369A JP5058805B2 JP 5058805 B2 JP5058805 B2 JP 5058805B2 JP 2007534369 A JP2007534369 A JP 2007534369A JP 2007534369 A JP2007534369 A JP 2007534369A JP 5058805 B2 JP5058805 B2 JP 5058805B2
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- 239000010419 fine particle Substances 0.000 title claims description 110
- 229910000510 noble metal Inorganic materials 0.000 title claims description 68
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 128
- 229910052697 platinum Inorganic materials 0.000 claims description 62
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 40
- 229910052707 ruthenium Inorganic materials 0.000 claims description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 150000003057 platinum Chemical class 0.000 claims description 11
- 150000003303 ruthenium Chemical class 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000002923 metal particle Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 49
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 42
- 239000003054 catalyst Substances 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 230000003647 oxidation Effects 0.000 description 15
- 238000007254 oxidation reaction Methods 0.000 description 15
- 239000002253 acid Substances 0.000 description 14
- 238000009835 boiling Methods 0.000 description 14
- 239000003638 chemical reducing agent Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000446 fuel Substances 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000000084 colloidal system Substances 0.000 description 9
- 238000002484 cyclic voltammetry Methods 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- 238000010992 reflux Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 7
- 229910002091 carbon monoxide Inorganic materials 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 150000004687 hexahydrates Chemical class 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- CFQCIHVMOFOCGH-UHFFFAOYSA-N platinum ruthenium Chemical compound [Ru].[Pt] CFQCIHVMOFOCGH-UHFFFAOYSA-N 0.000 description 5
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 231100000572 poisoning Toxicity 0.000 description 4
- 230000000607 poisoning effect Effects 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000001509 sodium citrate Substances 0.000 description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 4
- 229910000929 Ru alloy Inorganic materials 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 229910021397 glassy carbon Inorganic materials 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000005518 polymer electrolyte Substances 0.000 description 2
- BIXNGBXQRRXPLM-UHFFFAOYSA-K ruthenium(3+);trichloride;hydrate Chemical compound O.Cl[Ru](Cl)Cl BIXNGBXQRRXPLM-UHFFFAOYSA-K 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000002336 sorption--desorption measurement 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
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229920000557 Nafion® Polymers 0.000 description 1
- 229910001260 Pt alloy Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
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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
- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
-
- 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
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
-
- 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
- B01J37/16—Reducing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
-
- 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
- H01M8/1009—Fuel cells with solid electrolytes with one of the reactants being liquid, solid or liquid-charged
- H01M8/1011—Direct alcohol fuel cells [DAFC], e.g. direct methanol fuel cells [DMFC]
-
- B01J35/23—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
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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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Description
白金の塩化物であるヘキサクロロ白金酸6水和物0.7gに、イオン交換および限外濾過した純水を5mL加えて、ヘキサクロロ白金酸水溶液を調製した。また、ルテニウムの塩化物である塩化ルテニウム水和物(RuCl3・3H2O)0.21gに、この純水5mLを加えて塩化ルテニウム水溶液を調製した。また、還元剤として働くクエン酸ナトリウムにこの純水を加えて、2種類の還元剤溶液を調製した。より具体的には、クエン酸ナトリウム1.1gにイオン交換および限外濾過した純水20mLを加えることにより第1還元剤溶液を調製し、また、クエン酸ナトリウム1.4gにイオン交換および限外濾過した純水20mLを加えることにより第2還元剤溶液を調製した。
ヘキサクロロ白金酸6水和物の量を0.7gから0.62gに変えて調製したヘキサクロロ白金酸水溶液を用いたこと、また、第1還元剤溶液および第2還元剤溶液に代えて、クエン酸ナトリウム2.9gにイオン交換および限外濾過した純水を40mL加えて調製した還元剤溶液を用いたこと以外は、実施例1と同様にして貴金属微粒子を得た。
貴金属微粒子における白金に対するルテニウムの割合が表1に示す割合となるように、ヘキサクロロ白金酸6水和物の添加量を調整したこと以外は、実施例3〜7、10および11は実施例1と同様にして、また、実施例8および9は実施例2と同様にして、貴金属微粒子を得た。
比較例1は、国際公開2005/030416号パンフレットの実施例1を追試した例である。
比較例2は、白金のみからなる貴金属微粒子を作製した例である。
貴金属微粒子における白金に対するルテニウムの割合が、モル比で示して、Pt:Ru=1:0.66となるように、ヘキサクロロ白金酸6水和物の添加量を調整したこと以外は、比較例1と同様にして貴金属微粒子を得た。
図1に示すような、後述するようにして作製した作用電極20と、参照電極(Ag/AgCl電極)30および対極40とが、電気化学アナライザー(ビー・エー・エス(BAS)社製)10に接続された電気化学測定装置1を用い、これらの電極を、ビーカー50内に収容した1MのCH3OHおよび0.5MのH2SO4からなる電解質溶液60に浸漬した状態でポテンシャルスイープを行うことにより、貴金属微粒子のメタノール酸化特性(詳しくは後述する)を評価した。
Claims (2)
- 白金微粒子と、前記白金微粒子の表面の一部のみに被着したルテニウム微粒子と、を有
する貴金属微粒子の製造方法であって、
白金の塩を含む溶液において、前記白金の塩を還元することにより白金微粒子を前記溶液中に析出させる工程と、
前記溶液中の前記白金の塩を実質的に還元し終わった後に、前記白金微粒子を含む前記溶液にルテニウムの塩を添加し、前記ルテニウムの塩を還元することにより、前記白金微粒子の表面の一部のみに被着するようにルテニウム微粒子を析出させる工程と、を含み、 前記白金微粒子を構成する白金に対する前記析出したルテニウム微粒子を構成するルテニウムの割合が、モル比で示して、0.15〜0.8の範囲となるように、前記ルテニウムの塩を添加し、還元する、貴金属微粒子の製造方法。 - 前記溶液または前記溶液の溶媒に溶存する酸素を低減させる工程をさらに含む、請求項
1に記載の貴金属微粒子の製造方法。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP2007534369A JP5058805B2 (ja) | 2005-09-08 | 2006-09-01 | 貴金属微粒子の製造方法 |
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JP2005260015 | 2005-09-08 | ||
JP2005260015 | 2005-09-08 | ||
JP2007534369A JP5058805B2 (ja) | 2005-09-08 | 2006-09-01 | 貴金属微粒子の製造方法 |
PCT/JP2006/317309 WO2007029607A1 (ja) | 2005-09-08 | 2006-09-01 | 貴金属微粒子およびその製造方法 |
Publications (2)
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JPWO2007029607A1 JPWO2007029607A1 (ja) | 2009-03-19 |
JP5058805B2 true JP5058805B2 (ja) | 2012-10-24 |
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Country | Link |
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US (1) | US7754644B2 (ja) |
EP (1) | EP1930103B1 (ja) |
JP (1) | JP5058805B2 (ja) |
KR (1) | KR20080044324A (ja) |
WO (1) | WO2007029607A1 (ja) |
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US8309489B2 (en) * | 2009-06-18 | 2012-11-13 | University Of Central Florida Research Foundation, Inc. | Thermally stable nanoparticles on supports |
US9287569B2 (en) * | 2009-12-14 | 2016-03-15 | GM Global Technology Operations LLC | Method of enhancing electrodes |
US9722257B2 (en) * | 2009-12-14 | 2017-08-01 | GM Global Technology Operations LLC | Method of enhancing electrodes |
JP5778129B2 (ja) * | 2010-03-02 | 2015-09-16 | 日本板硝子株式会社 | 貴金属微粒子担持触媒およびその製造方法、ならびに浄化触媒 |
Citations (1)
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JP2000000467A (ja) * | 1998-06-16 | 2000-01-07 | Tanaka Kikinzoku Kogyo Kk | 高分子固体電解質型燃料電池用触媒の製造方法 |
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JPH09153366A (ja) | 1995-11-29 | 1997-06-10 | Aisin Seiki Co Ltd | 複合触媒成形体の製造方法 |
US6339038B1 (en) | 1998-06-16 | 2002-01-15 | Tanaka Kikinzoku Kogyo K. K. | Catalyst for a fuel cell containing polymer solid electrolyte and method for producing catalyst thereof |
JP2002102699A (ja) | 2000-09-29 | 2002-04-09 | Toshiba Corp | アルコール改質用触媒およびそれを用いた燃料電池 |
JP2002231257A (ja) * | 2001-01-30 | 2002-08-16 | Matsushita Electric Ind Co Ltd | 燃料電池用電極触媒およびその製造方法 |
WO2004073090A2 (en) * | 2003-02-13 | 2004-08-26 | E.I. Du Pont De Nemours And Company | Electrocatalysts and processes for producing |
JP4815215B2 (ja) | 2003-09-29 | 2011-11-16 | 日本板硝子株式会社 | 合金コロイド粒子、合金コロイド溶液とその製造方法および合金コロイド粒子を定着させた担持体 |
JP4180531B2 (ja) * | 2004-02-19 | 2008-11-12 | 日本板硝子株式会社 | 金属コロイド粒子及びその製造方法 |
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JP2000000467A (ja) * | 1998-06-16 | 2000-01-07 | Tanaka Kikinzoku Kogyo Kk | 高分子固体電解質型燃料電池用触媒の製造方法 |
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EP1930103B1 (en) | 2011-06-29 |
JPWO2007029607A1 (ja) | 2009-03-19 |
WO2007029607A1 (ja) | 2007-03-15 |
US7754644B2 (en) | 2010-07-13 |
US20090156390A1 (en) | 2009-06-18 |
EP1930103A4 (en) | 2009-05-06 |
EP1930103A1 (en) | 2008-06-11 |
KR20080044324A (ko) | 2008-05-20 |
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