JP6741545B2 - 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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Description
まず、前駆体となる白金触媒を製造した。ジニトロジアンミン白金硝酸溶液と純水と粉砕容器内に投入し、ここに担体となる炭素微粉末(比表面積900m2/g)を粉砕しながら添加した。その後、還元剤として変性アルコール(95%メタノール+5%エタノール)を加え、混合溶液を約95℃で6時間還流反応させて白金を還元した。その後、濾過、乾燥(125℃ 15時間)して洗浄し、白金触媒を得た。この白金触媒は、白金担持率46.5質量%である。
上記で用意した白金触媒にコバルトと第3金属Mを担持した。塩化コバルトと金属Mの塩化物又は硫酸塩をイオン交換水100mLに溶解させた金属塩溶液を作製し、ここに上記の白金触媒10gを浸漬し、マグネティックスターラーにて攪拌した。そして、この溶液に濃度1質量%の水素化ホウ素ナトリウム(SBH)溶液400mLを滴下し攪拌して還元処理し、白金触媒にコバルト、金属Mを担持した。その後、ろ過・洗浄・乾燥した。本実施形態では、各金属の担持量の比率を、Pt:Co:M=3:2:1とした。
Pt、Co、金属Mの触媒金属を担持した触媒について、合金化のための熱処理を行った。本実施形態では、100%水素ガス中で熱処理温度を900℃として30分の熱処理を行った。
熱処理語の触媒に対して、酸性溶液処理を行った。酸性溶液処理では、まず、熱処理後の触媒を、0.2mol/Lの硫酸水溶液中80℃にて2時間処理した後、濾過・洗浄・乾燥した。そして、1.0mol/Lの硝酸水溶液中70℃にて2時間処理した後、濾過・洗浄・乾燥した。更に、硝酸水溶液に処理をもう一回行い、洗浄しPt−Co−Mの3元系触媒を製造した。尚、本実施形態では、上記で製造した白金触媒にコバルトのみを添加・合金化したPt−Co触媒も製造している(Pt:Co=3:2で担持)。
Claims (9)
- 白金とコバルトとジルコニウムとが合金化した触媒金属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、
前記炭素粉末担体上の白金、コバルト、ジルコニウムの担持量の比率が、モル比でPt:Co:Zr=3:0.5〜1.5:0.1〜3.0であることを特徴とする固体高分子形燃料電池用触媒。 - 炭素粉末担体上の白金、コバルト、ジルコニウムの担持量の比率が、モル比でPt:Co:Zr=3:0.5〜1.5:0.2〜1.8である請求項1記載の固体高分子形燃料電池用触媒。
- 触媒粒子についてのX線回折分析による回折パターンにおいて、2θ=40.0°以上42.0°以下の領域で現れるPt3Coのピーク位置が、2θ=41.10°以上42.00°以下である請求項1又は請求項2記載の固体高分子形燃料電池用触媒。
- 触媒粒子についてのX線回折分析による回折パターンにおいて、2θ=28.0°以上28.4°以下の領域で現れるZrO2のピーク強度(Io)と、2θ=40.0°以上42.0°以下の領域で現れるPt3Coのピーク強度(Ia)との比(Io/Ia)が1.3以下である請求項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触媒。
- 触媒金属は、その表面のコバルト濃度及びジルコニア濃度が、その中心部のコバルト濃度及びジルコニウム濃度よりも低い請求項1〜請求項4のいずれかに記載の固体高分子形燃料電池用触媒。
- 触媒金属の担持密度は、30質量%以上70質量%以下である請求項1〜請求項5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6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、コバルト及びジルコニウムを担持する工程、
前記担持工程によりコバルト及びジルコニウムが担持された白金触媒を900℃以上1200℃以下で熱処理する工程、
前記熱処理工程後の触媒を、少なくとも1回酸化性溶液に接触させ、担持されたコバルト及びジルコニウムの一部を溶出させる工程、
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、過ジルコニウム酸カリウム、過酸化水素、塩酸、塩素酸、次亜塩素酸、クロム酸である請求項7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℃以上90℃以下とし、接触時間を1時間以上10時間以下とする請求項7又は請求項8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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JP2016199601A JP6741545B2 (ja) | 2016-10-10 | 2016-10-10 | 固体高分子形燃料電池用の触媒及びその製造方法 |
PCT/JP2017/032228 WO2018070149A1 (ja) | 2016-10-10 | 2017-09-07 | 固体高分子形燃料電池用の触媒及びその製造方法 |
KR1020197006861A KR20190034333A (ko) | 2016-10-10 | 2017-09-07 | 고체 고분자형 연료 전지용 촉매 및 그 제조 방법 |
US16/329,362 US10998556B2 (en) | 2016-10-10 | 2017-09-07 | Catalyst for solid polymer fuel cell and method for producing same |
KR1020217018570A KR102339556B1 (ko) | 2016-10-10 | 2017-09-07 | 고체 고분자형 연료 전지용 촉매 및 그 제조 방법 |
CN201780058221.6A CN109792059B (zh) | 2016-10-10 | 2017-09-07 | 用于固体高分子型燃料电池的催化剂及其制造方法 |
EP17861146.3A EP3525272B1 (en) | 2016-10-10 | 2017-09-07 | Catalyst for solid polymer fuel cell and method for producing the same |
TW106132031A TWI639271B (zh) | 2016-10-10 | 2017-09-19 | 固體高分子形燃料電池用觸媒及其製造方法 |
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US20210328230A1 (en) * | 2018-08-22 | 2021-10-21 | Tanaka Kikinzoku Kogyo K.K. | Catalyst for solid polymer fuel cell and method for selecting catalyst for solid polymer fuel cell |
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CN113097503B (zh) * | 2021-03-31 | 2023-03-10 | 中国科学技术大学 | 质子交换膜燃料电池催化剂合成方法 |
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US10998556B2 (en) | 2021-05-04 |
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