JP5823285B2 - 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 description 123
- 239000000446 fuel Substances 0.000 title claims description 34
- 239000005518 polymer electrolyte Substances 0.000 title claims description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 134
- 229910052697 platinum Inorganic materials 0.000 claims description 67
- 238000001179 sorption measurement Methods 0.000 claims description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000002245 particle Substances 0.000 claims description 30
- 230000001590 oxidative effect Effects 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 14
- 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- 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 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 125000000686 lactone group Chemical group 0.000 claims description 4
- 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
- 238000011282 treatment Methods 0.000 description 39
- 239000000243 solution Substances 0.000 description 34
- 238000000137 annealing Methods 0.000 description 23
- 238000010248 power generation Methods 0.000 description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 230000006872 improvement Effects 0.000 description 12
- 238000000034 method Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 8
- 230000000977 initiatory effect Effects 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000006866 deterioration Effects 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000002585 base Substances 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 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 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- IXSUHTFXKKBBJP-UHFFFAOYSA-L azanide;platinum(2+);dinitrite Chemical compound [NH2-].[NH2-].[Pt+2].[O-]N=O.[O-]N=O IXSUHTFXKKBBJP-UHFFFAOYSA-L 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000003411 electrode reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 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
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
- Y02E60/50—Fuel cells
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- Fuel Cell (AREA)
- Catalysts (AREA)
- Inert Electrodes (AREA)
Description
上記工程により製造した白金触媒を100%水素ガス中で、1時間、900℃に保持することにより行った。
そして上記の熱処理を行った白金触媒につき、水分吸着能の改良処のための酸化性溶液処理を行った。熱処理した触媒を1.0mol/Lの硝酸水溶液(溶存酸素量0.01cm3/cm3(STP換算))中80℃にて2時間処理した後、濾過、乾燥した。
電極面積:25cm2
設定利用効率:40%
温度:80℃
圧力:大気圧
アノードガス:純水素
カソードガス:酸素
加湿条件:アノード 湿度100%
カソード 加湿なし
Claims (6)
- 炭素粉末担体上に、白金からなる触媒粒子が担持されてなる固体高分子形燃料電池用触媒において、
前記炭素粉末担体は、25℃で測定される水蒸気吸着等温線における最大水蒸気吸着量が、触媒質量基準で150〜250cm 3 /g(STP換算)であり、
前記白金粒子は、平均粒径3.5〜8.0nmであり、CO吸着による白金比表面積(COMSA)が40〜100m2/gであることを特徴とする固体高分子形燃料電池用触媒。 - 炭素粉末担体は、更に、0.7〜3.0mmol/g(担体重量基準)の親水基が結合された請求項1記載の固体高分子形燃料電池用触媒。
- 親水基は、少なくともヒドロキシル基、ラクトン基、カルボキシル基のいずれかである請求項2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〜請求項3のいずれか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4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を600〜1180℃で1時間以下熱処理する工程と、
前記熱処理後の白金触媒を少なくとも1回酸化性溶液に接触させ、担体表面の水分の吸着能を改良する工程と、を備え、
前記酸化性溶液は、その溶存酸素量が0.01〜0.02cm3/cm3(STP換算)である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、過マンガン酸カリウム、過酸化水素、塩酸、塩素酸、次亜塩素酸、クロム酸である請求項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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Families Citing this family (7)
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CA2910237C (en) | 2013-04-25 | 2019-01-15 | Nissan Motor Co., Ltd. | Catalyst and manufacturing method thereof, and electrode catalyst layer using the catalyst |
EP2990116B1 (en) | 2013-04-25 | 2018-06-06 | Nissan Motor Co., Ltd | Catalyst, electrode catalyst layer using said catalyst, membrane electrode assembly, and fuel cell |
US9947934B2 (en) | 2013-04-25 | 2018-04-17 | Nissan Motor Co., Ltd. | Catalyst and electrode catalyst layer, membrane electrode assembly, and fuel cell using the catalyst |
JP2015090851A (ja) * | 2013-11-07 | 2015-05-11 | 凸版印刷株式会社 | 固体高分子形燃料電池用電極触媒層を形成する触媒インクの製造方法、固体高分子形燃料電池の製造方法、固体高分子形燃料電池用電極触媒層が含む白金担持炭素粒子 |
WO2016067878A1 (ja) | 2014-10-29 | 2016-05-06 | 日産自動車株式会社 | 燃料電池用電極触媒層、その製造方法ならびに当該触媒層を用いる膜電極接合体および燃料電池 |
CN110537277B (zh) | 2017-04-18 | 2022-08-09 | 田中贵金属工业株式会社 | 固体高分子型燃料电池用催化剂及其制造方法 |
CN113328108A (zh) * | 2021-06-23 | 2021-08-31 | 大连交通大学 | 一种高稳定、高活性铂纳米线催化剂及其制备方法 |
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JP2005251455A (ja) * | 2004-03-02 | 2005-09-15 | Matsushita Electric Ind Co Ltd | 燃料電池用触媒およびその製造方法、電極、ならびに直接メタノール型燃料電池 |
WO2006088194A1 (ja) * | 2005-02-21 | 2006-08-24 | Nissan Motor Co., Ltd. | 電極触媒およびその製造方法 |
JP2006294306A (ja) * | 2005-04-06 | 2006-10-26 | Mitsubishi Chemicals Corp | プロトン伝導材料およびそれを用いた燃料電池 |
JP5458801B2 (ja) * | 2008-10-22 | 2014-04-02 | 新日鐵住金株式会社 | 燃料電池 |
JP2010123504A (ja) * | 2008-11-21 | 2010-06-03 | Toyota Motor Corp | 燃料電池用電極触媒の製造方法、及び燃料電池用電極触媒 |
JP5297786B2 (ja) * | 2008-12-16 | 2013-09-25 | 株式会社キャタラー | 固体高分子型燃料電池のアノード触媒層 |
JP5397241B2 (ja) * | 2009-01-26 | 2014-01-22 | 新日鐵住金株式会社 | 固体高分子型燃料電池用触媒及びこれを用いた固体高分子型燃料電池用電極 |
JP5375623B2 (ja) * | 2010-01-18 | 2013-12-25 | 新日鐵住金株式会社 | 固体高分子型燃料電池用触媒及びこれを用いた固体高分子型燃料電池用電極 |
JP4880064B1 (ja) * | 2010-12-08 | 2012-02-22 | 田中貴金属工業株式会社 | 固体高分子形燃料電池用触媒及びその製造方法 |
EP2734822A1 (en) * | 2011-07-18 | 2014-05-28 | Michael J. Grassi | Torque sensor |
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