JP2006228565A - 固体酸化物形燃料電池用電解質シートおよびその製法、並びに固体酸化物形燃料電池セル - Google Patents
固体酸化物形燃料電池用電解質シートおよびその製法、並びに固体酸化物形燃料電池セル Download PDFInfo
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Abstract
【解決手段】 ドクターブレード法または押出成形法によって成形され、ジルコニアに対し4〜6モル%のスカンジアが固溶したスカンジア部分安定化ジルコニアシートであって、結晶構造が正方晶を主体とし単斜晶を含む多結晶系であり、そのX線回折による回折ピーク強度から下記式(1)によって算出される単斜晶比率M(%)が1〜80%であり、かつ10を下回らないワイブル係数(m)を有する固体酸化物形燃料電池用電解質シートを開示する。
単斜晶比率(M:%)=[[monoclinic(1,1,1) + monoclinic(-1,1,1)]/[tetragonal and cubic(1,1,1) + monoclinic(1,1,1) + monoclinic(-1,1,1)]]×100……(1)
Description
単斜晶比率(M:%)=[[monoclinic(1,1,1) + monoclinic(-1,1,1)]/[tetragonal and cubic(1,1,1)+ monoclinic(1,1,1) + monoclinic(-1,1,1)]]×100……(1)
幅4mm×厚さ0.2mm×長さ40mmのシート状試験片20本を使用し、各試験片について表面粗さの調整や面取りなどはしないでJIS R1601の方法に準拠して3点曲げ強度を測定する。次いで、「耐火物」39−489,1987−No.9の尾崎義治「セラミックスの強度と信頼性予測」11頁右欄に記載された下記式(2)
InIn{1/(1−Pf)}=mIn(σf−σu)−mInσ0……(2)
(式中、Pfは破壊確率であり、Pf=n/(N+1)で定義される(ここで、Nはサンプル個数、nはn番目のサンプルである)、σfは破壊曲げ強度、mはワイブル係数、σ0は規格化因子、σuは、この破壊曲げ強度以下では0となる応力値である)に基づき、σfは上記3点曲げ強度の測定値とし、縦軸にInIn{1/(1−Pf)}を、横軸にIn(σf−σu)をとってグラフを描き、その傾きから(m)の値を最小自乗法によって求める(なお、−mInσ0はグラフの切片となる)。
1000℃で2時間仮焼した4モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「4ScSZ」、シリカ含有量80ppm)100質量部と高純度アルミナ粉末(大明化学社製:商品名「TM−D」、シリカ含有量15ppm)1質量部との混合粉末に対し、エチルアクリレート2質量%、2−エチルヘキシルアクリレート38質量%、メチルメタクリレート4.94質量%、シクロヘキシルメタクリレート25質量%およびアクリル酸0.06質量%の混合モノマーを、アゾビスイソブチロニトリルを重合開始剤としてトルエン中で共重合した(メタ)アクリル酸エステル共重合体からなるバインダー(分子量:90,000、ガラス転移温度:−36℃)を固形分換算で14質量部、可塑剤としてジブチルフタレート1質量部、分散媒としてトルエン/イソプロピルアルコール(質量比:3/2)の混合溶剤50質量部を、直径10mmのジルコニアボールが装入された内容積が100リットルのナイロン製ボールミルに入れ、45rpmで40時間混練してスラリーを調製した。
高温耐久性=(1000℃で500時間保持した後の強度)/(初期強度)
導電率の劣化率=[(初期導電率−所定時間保持後の導電率)/(初期導電率)]
×100(%)
900℃で2時間仮焼した4モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「4ScSZ」、シリカ含有量30ppm)100質量部と高純度アルミナ粉末(大明化学社製:商品名「TM−D」、シリカ含有量:15ppm)0.5質量部との混合粉末を使用した以外は、上記実施例1と同様にしてスラリーを調製した。
850℃で2時間仮焼した4.5モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「4.5ScSZ」、シリカ含有量70ppm)70質量部と高純度アルミナ粉末(大明化学社製:商品名「TM−D」、シリカ含有量:15ppm)0.8質量部との混合粉末を使用した以外は、前記実施例1と同様にしてスラリーを調製した。
800℃で2時間仮焼した5モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「5ScSZ」、シリカ含有量130ppm)70質量部と高純度アルミナ粉末(大明化学社製:商品名「TM−D」、シリカ含有量:15ppm)1.5質量部との混合粉末を使用した以外は、前記実施例1と同様にしてスラリーを調製した。
上記実施例4で用いた5モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「5ScSZ」、シリカ含有量:90ppm)に、360ppmに相当するエタノールシリケートのエタノール溶液を加えて撹拌し混合した後、ロータリーエバポレータでエタノールを留去し、100℃で乾燥してから800℃で2時間仮焼することにより、シリカ分散5モル%スカンジア部分安定化ジルコニア粉末を得た。
前記実施例1で使用した4モル%スカンジア部分安定化ジルコニア粉末100質量部と高純度アルミナ粉末1質量部との混合粉末に対し、ヒドロキシエチルセルロース(ダイセル社製、商品名「SP600」)6質量部、グリセリン4質量部、水18質量部を加え、ニーダーを用いて室温で2時間混練してスカンジア部分安定化ジルコニア系の混練物を得た。
スカンジウム粉末とジルコニウム粉末を、スカンジアの固溶量が4モル%となる様に配合し、これを硝酸水に加えて加熱溶解することにより、スカンジウム硝酸塩とジルコニウム硝酸塩の混合溶液を調製した。
上記比較例1と同様にして得た正方晶単相の4モル%スカンジア部分安定化ジルコニア粉末(平均粒径:2μm、シリカ含有量:7ppm)70質量部と、高純度アルミナ粉末(大明化学社製:商品名「TM-D」、シリカ含有量:15ppm)1質量部との混合粉末、および前記実施例1で用いたのと同じバインダー16質量部を用いた以外は、前記実施例1と同様にしてスラリーを調製した。
前記実施例1で使用した4モル%スカンジア部分安定化ジルコニア粉末(第一稀元素化学社製:商品名「4ScSZ」、シリカ含有量80ppm)に、920ppmに相当するエタノールシリケートのエタノール溶液を加え、ロータリーエバポレータにより常温で30分間撹拌して混合した後、減圧しながら50℃に昇温してエタノールを留去し、更に80℃で乾燥した。これをエバーポレータから取り出して600℃で仮焼することにより、シリカ分散4モル%スカンジア部分安定化ジルコニア粉末を得た。
加熱焼成後の500℃から200℃までの冷却過程で、扇風機により強制冷却することによってこの間の時間を10分とした以外は比較例3と同様にして、1辺が約100mm角で厚さが200μmの4%スカンジア部分安定化ジルコニアシートを得た。
Claims (6)
- ドクターブレード法または押出成形法によって成形され、ジルコニアに対し4〜6モル%のスカンジアが固溶したスカンジア部分安定化ジルコニアシートであって、結晶構造が正方晶を主体とし単斜晶を含む多結晶系であり、そのX線回折による回折ピーク強度から下記式(1)によって算出される単斜晶比率(M)が1〜80%であり、且つ10を下回らないワイブル係数(m)を有することを特徴とする固体酸化物形燃料電池用電解質シート。
単斜晶比率(M:%)=[[monoclinic(111) + monoclinic(-1,1,1)]/[tetragonal and cubic(1,1,1) + monoclinic(1,1,1) + monoclinic(-1,1,1)]]×100……(1) - 前記電解質シートにおいて、走査型電子顕微鏡によって観察される電解質焼結体のグレインサイズの平均値が0.2〜0.8μm、最大径が0.4〜1.5μm、最小径が0.1〜0.3μmで、その変動係数が40%以下である請求項1に記載の固体酸化物形燃料電池用電解質シート。
- シリカが10〜500ppm含まれている請求項1または2に記載の固体酸化物形燃料電池用電解質シート。
- 面積が50cm2以上で、厚さが50〜800μmである請求項1〜3のいずれかに記載の固体酸化物形燃料電池用電解質シート。
- 請求項1〜4のいずれかに記載された固体酸化物形燃料電池用電解質シートを製造する方法であって、原料粉末として、800〜1200℃で仮焼されており、その結晶系の単斜晶比率が1〜80%で、ジルコニアに対し4〜6モル%のスカンジアが固溶されたスカンジア部分安定化ジルコニア粉末を使用し、該粉末を含むスラリー、ペーストまたは混練物を用いてドクターブレード法または押出成形法によりグリーンシートに成形し、該グリーンシートを所定形状に切断した後、棚板上に載置して1300〜1450℃で加熱し、加熱した該成形体を冷却する過程で、500℃から200℃に至るまでの時間を10〜90分間とすることを特徴とする固体酸化物形燃料電池用電解質シートの製法。
- 前記請求項1〜4のいずれかに記載された固体酸化物形燃料電池用電解質シートが組み込まれていることを特徴とする固体酸化物形燃料電池セル。
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WO2007013567A1 (ja) * | 2005-07-27 | 2007-02-01 | Nippon Shokubai Co., Ltd. | 固体電解質シートの製造方法および固体電解質シート |
JP2011082149A (ja) * | 2009-09-11 | 2011-04-21 | Nippon Shokubai Co Ltd | 固体酸化物形燃料電池用スカンジア安定化ジルコニアシートの製造方法および固体酸化物形燃料電池用スカンジア安定化ジルコニアシート |
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EP2492257B1 (en) * | 2009-10-23 | 2018-03-14 | Nippon Shokubai Co., Ltd. | Scandia-stabilised zirconia sintered powder, process for production of scandia-stabilized zirconia sintered powder, process for production of scandia-stabilized zirconia sheet |
CN104707591B (zh) * | 2015-02-06 | 2017-11-28 | 复旦大学 | 一种乙醇转化制异丁烯的氧化物催化剂及其制备方法 |
WO2017006945A1 (ja) * | 2015-07-07 | 2017-01-12 | 日本碍子株式会社 | 燃料電池スタック |
KR102586150B1 (ko) | 2016-12-21 | 2023-10-06 | 코닝 인코포레이티드 | 소결 시스템 및 소결된 물품 |
JP6879759B2 (ja) * | 2017-02-09 | 2021-06-02 | 株式会社日本触媒 | ジルコニア電解質およびその製造方法 |
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