JP2011251901A - スカンジア安定化ジルコニア焼結粉末 - Google Patents
スカンジア安定化ジルコニア焼結粉末 Download PDFInfo
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- JP2011251901A JP2011251901A JP2011164770A JP2011164770A JP2011251901A JP 2011251901 A JP2011251901 A JP 2011251901A JP 2011164770 A JP2011164770 A JP 2011164770A JP 2011164770 A JP2011164770 A JP 2011164770A JP 2011251901 A JP2011251901 A JP 2011251901A
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- scandia
- stabilized zirconia
- powder
- zirconia
- sheet
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
- H01M8/124—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte
- H01M8/1246—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides
- H01M8/1253—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the process of manufacturing or by the material of the electrolyte the electrolyte consisting of oxides the electrolyte containing zirconium oxide
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Abstract
【解決手段】本発明に係るスカンジア安定化ジルコニア焼結粉末は、透過型電子顕微鏡で測定される平均粒子径(De)が0.3μm超、1.5μm以下、レーザー散乱法で測定される平均粒子径(Dr)が0.3μm超、3.0μm以下、且つ透過型電子顕微鏡で測定される平均粒子径に対するレーザー散乱法で測定される平均粒子径の比(Dr/De)が1.0以上、2.5以下であることを特徴とする。
【選択図】なし
Description
本発明方法では、原料としてスカンジア安定化ジルコニアの焼結体を用いる。
本発明に係るスカンジア安定化ジルコニアシートの製造方法では、本発明に係る上記スカンジア安定化ジルコニア焼結粉末とジルコニア未焼結粉末を含むスラリーであって、スラリー中におけるスカンジア安定化ジルコニア焼結粉末とジルコニア未焼結粉末の合計に対するスカンジア安定化ジルコニア焼結粉末の割合が2質量%以上、40質量%以下であるスラリーを調製する。当該割合としては、3質量%以上、30質量%以下がより好ましく、5質量%以上、25質量%以下がさらに好ましい。スラリーの調製条件としては、常法を用いることができる。例えば、上記原料ジルコニア粉末、溶媒、バインダー、分散剤、可塑剤等を混合する。
次に、得られたスラリーをシート状に成形する。成形方法は特に制限されないが、ドクターブレード法や押出成形法を用いて、適切な厚さのシートとすることが好ましい。なお、本発明におけるシート状とは、シートを丸めた円筒状や、リング状も含むものとする。
以上、2000cm2以下程度にすることができる。
次いで、得られたシート状成形体を焼結する。焼結の条件としては、常法を用いることができる。
.1μm以上、3μm以下が好ましく、より好ましくは0.3μm以上、2μm以下であり、さらに好ましくは0.5μm以上、1.5μm以下である。
O3安定化ジルコニアからなるサーメットである。これら燃料極材料を、エチルセルロー
ス等のバインダー、α−テルピネオール等の溶剤とともに混練して燃料極ペーストとするか、或いはミリングして燃料極スラリーとし、これをスクリーン印刷法、コーティング法などで被覆・乾燥・焼成することで燃料極を形成することができる。
ブスカイト型構造酸化物、さらには、これらペロブスカイト構造酸化物に安定化ジルコニアおよび/またはセリア酸化物が添加された混合物を挙げることができる。特に好ましくは、La0.6Sr0.4Co0.2Fe0.8O3またはLaNi0.6Fe0.4O3に9〜12モル%
Sc2O3安定化ジルコニアを加えた混合物が好適に使用される。上記燃料極の場合と同様に、空気極ペーストあるいは空気極スラリーを調製し、電解質シートの燃料極と反対の面に、スクリーン印刷法、コーティング法などで被覆・乾燥・焼成することで空気極を形成することができる。
銅メッシュにコロジオン膜を張り、乾燥後、カーボン蒸着することにより親水化処理した。別途、ジルコニア焼結粉末を水に分散し、懸濁液とした。前記銅メッシュの上に当該懸濁液を載せ、乾燥させることにより、測定用試料を得た。
分散剤として0.2質量%のメタリン酸ナトリウムを添加した水溶液(約100cm3)に、スカンジア安定化ジルコニア焼結体を粉砕して得たジルコニア焼結粉末を0.01〜0.5質量%添加し、3分間超音波処理して分散させた。堀場製作所製のレーザー回折式粒度分布測定装置「LA−920」を用い、当該分散液における体積基準の粒度分布を測定した。当該平均粒子径とは、体積基準の粒度分布の測定結果において、累積グラフにおける50体積%での粒径、即ちD50とした。
吸着分子として窒素を用い、BET法によりジルコニア粉末の比表面積を測定した。測定機器としては、マウンテック社製のマックソーブHM−1210型を用いた。測定は一試料につき3点行い、その平均値を比表面積とした。
得られたジルコニアグリーンシートを長方形に切断し、1400℃で3時間焼成して、5mm×50mm角の強度測定用試料を20枚作製した。万能材料試験機(インストロン社製,4301型)を用い、JIS R1601に準拠して、スパン20mm、クロスヘッド速度0.5mm/分の条件で各試料の3点曲げ強度値を測定した。得られた測定値の平均値を、3点曲げ強度とした。
安息角測定器(アズワン社製,ASK−01)を用い、ジルコニア粉末の安息角を測定した。詳しくは、試料粉末を上記測定器のホッパーから下部の板上に落下させ、堆積した円錐の斜面の角度を分度器で測定した。測定は2回ずつ行い、平均値を測定値とした。
(1) 従来のスカンジア安定化ジルコニアシートの製造
市販のスカンジア安定化ジルコニア未焼結粉末(第一稀元素化学工業社製,製品名「10Sc1CeSZ」,以下、「10Sc1CeSZ未焼結粉末」という)の透過型電子顕微鏡で測定される平均粒子径(De)、レーザー散乱法で測定される平均粒子径(Dr)および比表面積を、上記試験例1〜3と同様の条件で測定した。また、X線回折により分析して結晶形を特定した。その結果、Deは0.09μm、Drは0.60μm、比表面積は10.8m2/gであった。また、当該粉末は立方晶を主体とするものであり、立方晶比率は99.9%であった。
上記製造例1(1)の10Sc1CeSZ方形焼結シートとφ20mmのジルコニアボールを50Lのボールミル(中央化工機社製,MR−50)へ投入し、回転数45rpmで2時間乾式粉砕し、レーザー散乱法で測定される平均粒子径(Dr)が1000μmの一次乾式粉砕ジルコニア焼結粉末を得た。得られた一次乾式粉砕ジルコニア焼結粉末とφ5mmのジルコニアボールを乾式ビーズミル(アシザワ・ファインテック社製,ドライスターSDA5)へ投入し、回転数660rpmで45分間乾式粉砕することにより、レーザー散乱法で測定される平均粒子径(Dr)が5.3μmの二次乾式粉砕ジルコニア焼結粉末を得た。次いで、得られた二次乾式粉砕ジルコニア焼結粉末、エタノールおよびφ0.3mmのジルコニアボールをビーズミル(アシザワ・ファインテック社製,湿式微粉砕分散機「スターミル」)へ投入し、回転数3800rpmで2時間30分間湿式粉砕した。粉砕後、スプレードライヤーで乾燥し、Deが0.41μm、Drが0.42μm、Dr/Deが1.02であるスカンジア安定化ジルコニア焼結粉末Aを得た。
10Sc1CeSZ未焼結粉末のみに代えて、当該ジルコニア未焼結粉末と上記製造例1(2)のスカンジア安定化ジルコニア焼結粉末A〜Jとの混合物、または上記製造例1(2)のスカンジア安定化ジルコニア焼結粉末Aのみを用いた以外は上記製造例1(1)と同様にして、10Sc1CeSZシート1000枚を製造した。
Claims (4)
- 透過型電子顕微鏡で測定される平均粒子径(De)が0.3μm超、1.5μm以下、レーザー散乱法で測定される平均粒子径(Dr)が0.3μm超、3.0μm以下、且つ透過型電子顕微鏡で測定される平均粒子径に対するレーザー散乱法で測定される平均粒子径の比(Dr/De)が1.0以上、2.5以下であることを特徴とするスカンジア安定化ジルコニア焼結粉末。
- 安定化剤としてSc2O3を3モル%以上、15モル%以下含む請求項1に記載の安定化ジルコニア焼結粉末。
- 立方晶系および/または菱面体晶系である請求項1または2に記載のスカンジア安定化ジルコニア焼結粉末。
- さらに、Sc2O3以外の安定化剤を0.01質量%以上、5質量%以下含む請求項1〜3のいずれかに記載の安定化ジルコニア焼結粉末。
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CN102471167A (zh) | 2012-05-23 |
US9601795B2 (en) | 2017-03-21 |
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WO2011049202A1 (ja) | 2011-04-28 |
EP2492257A1 (en) | 2012-08-29 |
US20120231368A1 (en) | 2012-09-13 |
CN102471167B (zh) | 2015-03-25 |
EP2492257A4 (en) | 2013-08-14 |
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