JP5033620B2 - 水素分離用混合プロトン/電子伝導性セラミック膜 - Google Patents
水素分離用混合プロトン/電子伝導性セラミック膜 Download PDFInfo
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/048—Composition of the impurity the impurity being an organic compound
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0495—Composition of the impurity the impurity being water
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Description
原材料の酸化物および炭酸塩の粉末(BaCO3,CeO2,Eu2O3)を化学量論的な量を加えてペロブスカイトBaCe0.8Eu0.2O2.9を形成することにより、化学量論的なペロブスカイト材料を調製した。これら粉末を24時間ボールミル粉砕したのに続き、1リットルのナルゲンボトルの中でジルコニウムミル粉砕媒体とともにペイントシェーカーの上で30分間混合した。次いで、十分に混合した粉末を1400℃で焼成して炭酸塩を分解し、粉を一緒に反応させて単相のペロブスカイト材料を形成した。次に、焼成した粉末をアセトン中で72時間ボールミルして、1−2ミクロンの粒径で表面積が1.5−3m2/gの微粉末を得た。
2相混合伝導性セラミック材料の2つの異なった組成物を、実施例1に記載の通り製造した。処方した2つの組成物は、(1)50質量%BaCe0.7Eu0.3O2.85+50質量%Ce0.8Eu0.2O2.9および(2)50質量%BaCe0.8Eu0.2O2.9+50質量%Ce0.8Y0.2O2.9である。2相複合材料の安定性を実証するために、H2OおよびCO2を含む還元的環境における熱重量分析(TGA)を行い、時間の関数として重量の変化を観測した。図2に示すように、TGA試験の間に重量変化は測定されず、このことは材料がこれらの温度およびガス組成の環境において安定であることを示す。図2は合成ガス中における熱重量分析のデータを描画しており、これはCO,CO2およびH2Oを含む還元的環境におけるペロブスカイト/酸化物複合体の極めて良好な安定性を示している。
原材料酸化物および炭酸塩の粉末(BaCO3,CeO2,EuO3)を非化学量論的量(バリウム欠陥)で添加してペロブスカイトBa0.92Ce0.8Eu0.2O2.82を形成することにより、非化学量論的ペロブスカイト材料を調製した。これら粉末を24時間ボールミル粉砕したのに引き続き、1リットルのナルゲンボトルでジルコニアミル媒体とともにペイントシェーカーの上で30分間混合した。その後、よく混合した粉末を1400℃で焼成して炭酸塩を分解し、粉末を一緒に反応させ単一相のペロブスカイト材料を形成した。次いで、焼成した粉末をアセトン中で72時間ボールミルして1−2ミクロンの粒径で表面積が1.5−3m2/gの微粉末を得た。
化学量論量のペロブスカイト/ドープしたセリアの複合体を実施例1に記載のとおり製造し、非化学量論量のペロブスカイト/ドープしたセリアの複合材料を実施例3に記載のとおり調製した。これら2つのサンプル材料を用いて、かかる2つの材料の安定性を900℃の合成ガス環境において比較した。図4は、化学量論および非化学量論のペロブスカイト相を有する複合体粉末のX線回折パターンの比較を示す。さらに具体的にいうと、図4は900℃で合成ガスに露曝した粉末のX線回折分析のデータを描画し、これは非化学量論のペロブスカイト/酸化物複合体粉末が、同一条件で露曝した化学量論的ペロブスカイト/酸化物複合体粉末と比較してほとんど炭酸塩を形成していないことを示している。図4中の矢印は主要な炭酸バリウムピークの位置を示す。非化学量論的なAサイト欠陥のペロブスカイトを有する複合体は、50容積%のBa0.92Ce0.8Eu0.2O2.82および50容積%のCe0.8Eu0.2O2.9を有し、化学量論的ペロブスカイト組成の複合体は50容積%のBaCe0.8Eu0.2O2.9および50容積%のCe0.8Eu0.2O2.9を有する。バリウム欠損組成の複合体は、著しく低い炭酸塩の形成により、また非化学量論的な組成物におけるAサイトの陽イオン(すなわち、本実施例におけるBa2+イオン)の一層低い活性により合成ガス中で優れた化学的安定性を示す。
二相複合セラミック粉末を実施例1に記載の通り調製した。次いで、多孔質基板によって支持された薄膜混合伝導体を製造するために、これら粉末を用いてテープ成型用スリップを調製した。緻密な構成部品用スリップを二つの厚さ、8ミルと1ミルに成形する一方、多孔質のスリップを8ミルのみに成形した。テープ成形品を、標準のセラミック加工処理を用いて乾燥し、膜パッケージ中の膜の薄層の露出表面積を最大化するように決めた形状および大きさに個々のテープを打ち抜く。膜の初期寸法を打ち抜くと、生成した断片をレーザーカッターを用いて切断し、膜の表面積を最大化しかつ膜支持体に付与するに必要な形体を得た。レーザー切断を完了すると、標準セラミック加工処理を用いてこれら断片を一緒に積層して基材及び膜支持体とともに膜パッケージを形成する。
Claims (4)
- 多相セラミック複合材料であって:
一般式:A1-x-αPXB1-yQyO3-δ[式中、Aは、バリウム(Ba)、ストロンチウム(Sr)、カルシウム(Ca)およびマグネシウム(Mg)並びにそれらの組み合わせからなる群より選択した二価の陽イオンであり、Pは、Pr、Sm、Erおよび周期律表のランタニド系列の元素からなる群より選択した陽イオンであるA−サイトドーパントであり、Bは、周期律表の第4族の元素および周期律表のランタニド系列の元素からなる群より選択した4価の陽イオンであり、Qは、周期律表の第3族の元素および周期律表のランタニド系列の元素からなる群より選択したB−サイトドーパントであり、αは、非化学量論的なA−サイト欠陥の数であり、δは、酸素欠陥の数であり、0<α≦0.1、0≦x≦0.5、0≦y≦0.3である]のドープした非化学量論的なペロブスカイト、
のプロトン伝導性セラミック相;および
酸化セリウムまたはドープした酸化セリウムの電子伝導性セラミック相を備えた多相セラミック複合材料。 - 電子伝導性のセラミック相が、材料を用いて製造した膜の水素ガス分離のための運転条件下でプロトン伝導相と少なくとも一つのガスとの間の反応の少なくとも一つの生成物と構造的および化学的に同一である請求項1記載の材料。
- 電子伝導性セラミック相はCe1−xBxO2−εの式を有し、Bはイットリウムの一つおよび周期律表中のランタニド系列に属する元素を表し、εは酸素欠陥の数である請求項1記載の材料。
- 電子伝導性セラミック相がCe1−xBxO2−εの式を有し、Bはイットリウム及び周期律表中のランタニド系列に属する元素の一つで、εは酸素欠陥の数である請求項2記載の材料。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/708,475 US7258820B2 (en) | 2004-03-05 | 2004-03-05 | Ceramic mixed protonic/electronic conducting membranes for hydrogen separation |
US10/708,475 | 2004-03-05 | ||
PCT/US2005/007124 WO2005086704A2 (en) | 2004-03-05 | 2005-03-03 | Ceramic mixed protonic/electronic conducting membranes for hydrogen separation |
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JP2007527356A JP2007527356A (ja) | 2007-09-27 |
JP5033620B2 true JP5033620B2 (ja) | 2012-09-26 |
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US (1) | US7258820B2 (ja) |
EP (2) | EP1730749A4 (ja) |
JP (1) | JP5033620B2 (ja) |
WO (1) | WO2005086704A2 (ja) |
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JP4018797B2 (ja) * | 1998-03-16 | 2007-12-05 | 新日本製鐵株式会社 | 電子伝導性セラミックス |
JP4608047B2 (ja) * | 1999-02-17 | 2011-01-05 | パナソニック株式会社 | 混合イオン伝導体およびこれを用いたデバイス |
US6235417B1 (en) * | 1999-04-30 | 2001-05-22 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Natural Resources | Two-phase hydrogen permeation membrane |
US6296687B2 (en) * | 1999-04-30 | 2001-10-02 | Her Majesty The Queen In Right Of Canada, As Represented By The Minister Of Natural Resources | Hydrogen permeation through mixed protonic-electronic conducting materials |
US6569226B1 (en) * | 2001-09-28 | 2003-05-27 | The United States Of America As Represented By The United States Department Of Energy | Metal/ceramic composites with high hydrogen permeability |
NO325218B1 (no) * | 2001-10-31 | 2008-02-25 | Norsk Hydro As | En fast flerkomponent blandet proton- og elektronledende membran og anvendelse derav |
EP1598325B1 (en) * | 2003-02-24 | 2014-04-09 | TYK Corporation | Proton-conductive and electron-conductive ceramic |
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2004
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US20050194571A1 (en) | 2005-09-08 |
WO2005086704A3 (en) | 2006-09-14 |
JP2007527356A (ja) | 2007-09-27 |
WO2005086704A2 (en) | 2005-09-22 |
US7258820B2 (en) | 2007-08-21 |
EP1730749A4 (en) | 2008-12-03 |
EP2457635A1 (en) | 2012-05-30 |
EP2457635B1 (en) | 2015-09-30 |
EP1730749A2 (en) | 2006-12-13 |
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