JP2013518710A - 触媒の製造方法及び触媒 - Google Patents
触媒の製造方法及び触媒 Download PDFInfo
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- JP2013518710A JP2013518710A JP2012551724A JP2012551724A JP2013518710A JP 2013518710 A JP2013518710 A JP 2013518710A JP 2012551724 A JP2012551724 A JP 2012551724A JP 2012551724 A JP2012551724 A JP 2012551724A JP 2013518710 A JP2013518710 A JP 2013518710A
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Abstract
さらに、本発明はこの方法により製造された触媒であって、炭素含有担体及び触媒活性物質を含み、この炭素含有担体が金属炭化物層を含有し、且つその触媒活性物質が金属炭化物層を備えた炭素含有担体に施された触媒を提供する。
【選択図】なし
Description
(a)金属塩溶液に炭素含有担体を含浸させる工程、
(b)この金属塩溶液が含浸した炭素含有担体を、少なくとも1200℃の温度に加熱して金属炭化物層を形成する工程、
(c)金属炭化物層を備えた炭素含有担体に触媒活性物質を施す工程
を含む方法により達成される。
炭素含有担体が含浸される金属塩溶液として、タングステン酸アンモニウム溶液等の、タングステン酸塩溶液等を用いることができる。
DenkaBlackカーボンブラックの表面を改質するために、22gのアンモニウムヘプタタングステン酸塩を580gの水に溶解し、そこに15gのDenkaBlackカーボンブラックを加えた。混合物を30分間8000rpmでUltra−Turraxを用いて均質化した。カーボンブラック懸濁液をロータリーエバポレーターで濃縮し、窒素下において1500℃で6時間、400℃1時間の中間温度工程をはさみつつ管状炉中で加熱した。
カーボンブラックC2(AT325 from Evonik Degussa GmbH)の表面を改質するために、5.9gのアンモニウムヘプタタングステン酸塩を580gの水に溶解し、16gのカーボンブラックC2をそこに添加した;全体を8000rpmで30分間Ultra−Turraxを用いて均質化した。カーボンブラック懸濁液をロータリーエバポレーターで濃縮し、窒素下において1500℃で6時間、400℃1時間の中間温度工程をはさみつつ管状炉中で加熱した。
7.0gのカーボンブラックC1(XMB206 from Evonik Degussa GmbH)を500mlの水に分散し、15分間8000rpmでUltra−Turraxを用いて均質化した。5.13gの白金硝酸を100mlの水に溶解し、ゆっくりとカーボンブラック分散液に添加した。その後、200mlの水と800mlのエタノールを混合物に添加し、混合物を6時間還流した。一晩冷却した後、懸濁液を濾過し、固体を熱水2lで洗浄して硝酸塩を無くし、減圧下で乾燥させた。白金担持は27.1%であり、XRDにおける平均結晶子サイズは3.4nmであった。
調整はカーボンブラック担体を除いては、比較例1に記載した方法と同様の方法で行った。カーボンブラックC2をカーボンブラックC1の代わりに使用した。白金担持は27.4%であり、XRDにおける平均結晶子サイズは3.1nmであった。
表面の改質を実施例2に記載した方法と同様の方法で行なったが、カーバイド化工程を(WO2006/002228と類似の)850℃の温度で6時間、400℃で1時間の中間温度工程をはさみつつ実施した。タングステン担持は7%であった。計算値20%であった、すなわち、タングステンを定量的に付着させることができなかった。タングステンカーバイド相はXRDにおいて観察されず、H2WO4*H2Oのみが観察された。
調製をWO2006/002228に記載された方法と類似の方法で行った。この目的のために、8gのVulcan XC72を1000gの水に懸濁し、8000rpmで30分間、Ultra−Turraxを用いて均質化した。3.2gのタングステン酸アンモニウムを200mlの水に溶解し、ゆっくりと懸濁液に添加した。さらに750mlの水を混合物に添加し、混合物を4時間還流した。その後、30.4gのNaBH4を100mlの水に溶解し、気体の活発な放出と共に1時間に亘って滴下し、混合物をさらに20分間還流した。反応混合物を濾過し、固形物を2lの水で洗浄した。まだ湿った濾過ケーキを管状炉で、最初に100℃で1時間、次いで900℃で1時間加熱した。
調整はカーボンブラック担体を除いて、比較例1に記載した方法と類似の方法で行った。カーボンブラックXC72をカーボンブラックC1の代わりに使用した。白金担持は27.7%であり、XRDにおける平均結晶子サイズは1.9nmであった。
調整はカーボンブラック担体を除いて、比較例1に記載した方法と類似の方法で行った。 DenkaBlackカーボンブラックをカーボンブラックC1の代わりに使用した。白金担持は27.7%であり、XRDにおける平均結晶子サイズは3.7nmであった。
図1は、電気化学プロセスへの暴露前の比較例1による触媒を示しており、
図2は、電気化学プロセスへの暴露後の比較例1による触媒を示しており、
図3は、電気化学プロセスへの暴露前の例1による触媒を示しており、
図4は、電気化学プロセスへの暴露後の例1による触媒を示している。
図中、被覆されていない担体が符号1で示され、炭化物で被覆された担体が符号3で示され、白金粒子が符号2で示されている。
Claims (16)
- 触媒活性物質及び炭素含有担体を含む触媒の製造方法であって、
以下の工程:
(a)金属塩溶液に炭素含有担体を含浸させる工程、
(b)金属塩溶液が含浸した炭素含有担体を、不活性雰囲気中で1200℃の温度に加熱して金属炭化物層を形成する工程、
(c)金属炭化物層を備えた炭素含有担体に触媒活性物質を施す工程
を含む方法。 - 炭素含有担体を含浸させる金属塩溶液が化学量論量で添加される請求項1に記載の方法。
- 前記金属塩溶液の金属が、タングステン、モリブデン、又はこれらの金属の少なくとも1種を含む混合物若しくは合金である請求項1又は2に記載の方法。
- 前記金属塩溶液が、タングステン酸塩溶液である請求項1〜3のいずれかに記載の方法。
- 工程(b)における加熱が、不活性雰囲気中で実施される請求項1〜4のいずれかに記載の方法。
- 触媒活性金属が、白金属の金属であるか、或いは白金属の少なくとも1種の金属を含有する合金である請求項1〜5の何れかに記載の方法。
- 白金族の少なくとも1種の金属を含む合金が、PtNi、PtFe、PtV、PtCr、PtTi、PtCu、PtPd、PtRu、PdNi、PdFe、PdCr、PdTi、PdCu及びPdRuからなる群から選択される請求項6に記載の方法。
- 白金族の金属が、白金又はパラジウムである請求項6に記載の方法。
- 触媒活性物質を、還元析出により、又はH2/N2ガス混合物中での分解及び還元により、金属炭化物層を備える炭素含有担体に施す請求項1〜8に記載の方法。
- 炭素含有担体が250m2/g以下のBET表面積を有する請求項1〜9の何れかに記載の方法。
- 請求項1〜10の何れかに記載の方法により製造された触媒であって、
炭素含有担体と触媒活性物質を含有し、
該炭素含有担体は、金属炭化物層を有し、
前記触媒活性物質は、該金属炭化物層を備える炭素含有担体に施されていることを特徴とする触媒。 - 炭素含有担体が、250m2/g以下のBET表面積を有する請求項11に記載の触媒。
- 触媒活性物質が白金属の金属であるか、又は白金属の少なくとも1種の金属を含有する合金である請求項11又は12に記載の触媒。
- 白金族の少なくとも1種の金属を含む合金が、PtNi、PtFe、PtV、PtCr、PtTi、PtCu、PtPd、PtRu、PdNi、PdFe、PdCr、PdTi、PdCu及びPdRuからなる群から選択される請求項13に記載の触媒。
- 金属炭化物層の金属が、タングステン及び/又はモリブデンを含む請求項11〜14の何れかに記載の触媒。
- 燃料電池の電気触媒として請求項11〜15の何れかに記載の触媒を使用する方法。
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WO2015141595A1 (ja) * | 2014-03-20 | 2015-09-24 | 国立大学法人九州大学 | 燃料電池用電極材料およびその製造方法、並びに燃料電池用電極、膜電極接合体及び固体高分子形燃料電池 |
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KR20170095407A (ko) | 2014-08-28 | 2017-08-22 | 엔.이. 켐캣 가부시키가이샤 | 전극용 촉매, 가스확산 전극 형성용 조성물, 가스확산 전극, 막-전극 접합체, 연료전지 스택 |
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- 2011-02-03 CN CN201180009060.4A patent/CN102762297B/zh not_active Expired - Fee Related
- 2011-02-03 EP EP11739479.1A patent/EP2531295A4/en not_active Withdrawn
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JP2013531554A (ja) * | 2010-05-10 | 2013-08-08 | ユーティーシー パワー コーポレイション | 支持触媒 |
US9147884B2 (en) | 2010-05-10 | 2015-09-29 | Audi Ag | Fuel cell catalyst including carbon support particles with metal carbide layer and catalytic material and fuel cell using the same |
US9991523B2 (en) | 2010-05-10 | 2018-06-05 | Audi Ag | Fuel cell catalyst including carbon support particles with metal carbide layer and catalytic material and fuel cell using the same |
US9153823B2 (en) | 2011-11-14 | 2015-10-06 | Audi Ag | Carbide stabilized catalyst structures and method of making |
WO2015141595A1 (ja) * | 2014-03-20 | 2015-09-24 | 国立大学法人九州大学 | 燃料電池用電極材料およびその製造方法、並びに燃料電池用電極、膜電極接合体及び固体高分子形燃料電池 |
JPWO2015141595A1 (ja) * | 2014-03-20 | 2017-04-06 | 国立大学法人九州大学 | 燃料電池用電極材料およびその製造方法、並びに燃料電池用電極、膜電極接合体及び固体高分子形燃料電池 |
KR20170095406A (ko) | 2014-08-28 | 2017-08-22 | 엔.이. 켐캣 가부시키가이샤 | 전극용 촉매, 가스확산 전극 형성용 조성물, 가스확산 전극, 막-전극 접합체, 연료전지 스택 |
KR101786408B1 (ko) * | 2014-08-28 | 2017-10-17 | 엔.이. 켐캣 가부시키가이샤 | 전극용 촉매, 가스확산 전극 형성용 조성물, 가스확산 전극, 막-전극 접합체, 연료전지 스택 |
US9893365B2 (en) | 2014-08-28 | 2018-02-13 | N.E. Chemcat Corporation | Electrode catalyst, composition for forming gas diffusion electrode, gas diffusion elelctrode, membrane-electrode assembly, and fuel cell stack |
KR20170095407A (ko) | 2014-08-28 | 2017-08-22 | 엔.이. 켐캣 가부시키가이샤 | 전극용 촉매, 가스확산 전극 형성용 조성물, 가스확산 전극, 막-전극 접합체, 연료전지 스택 |
JP2018509735A (ja) * | 2015-02-05 | 2018-04-05 | プサン ナショナル ユニバーシティー インダストリー−ユニバーシティー コーオペレイション ファウンデーション | 燃料電池用アノード電極およびこれを含む燃料電池用膜−電極アセンブリー |
KR20210037799A (ko) * | 2019-09-27 | 2021-04-07 | 한국과학기술원 | 완전 분산과 환원된 금속 상태를 갖는 고내구성 금속 앙상블 촉매 |
KR102268466B1 (ko) | 2019-09-27 | 2021-06-24 | 한국과학기술원 | 완전 분산과 환원된 금속 상태를 갖는 고내구성 금속 앙상블 촉매 |
KR20210158118A (ko) * | 2020-06-23 | 2021-12-30 | 한국과학기술원 | 백금 단일 원자 촉매 및 이의 제조 방법 |
KR102391273B1 (ko) | 2020-06-23 | 2022-04-27 | 한국과학기술원 | 백금 단일 원자 촉매 및 이의 제조 방법 |
Also Published As
Publication number | Publication date |
---|---|
EP2531295A4 (en) | 2014-01-29 |
KR20120115559A (ko) | 2012-10-18 |
EP2531295A1 (en) | 2012-12-12 |
WO2011095943A1 (en) | 2011-08-11 |
CN102762297A (zh) | 2012-10-31 |
CN102762297B (zh) | 2015-06-10 |
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