JP4796656B2 - スカンジア安定化ジルコニアシートの製造方法、および当該製造方法により得られるスカンジア安定化ジルコニアシート - Google Patents
スカンジア安定化ジルコニアシートの製造方法、および当該製造方法により得られるスカンジア安定化ジルコニアシート Download PDFInfo
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- JP4796656B2 JP4796656B2 JP2010237985A JP2010237985A JP4796656B2 JP 4796656 B2 JP4796656 B2 JP 4796656B2 JP 2010237985 A JP2010237985 A JP 2010237985A JP 2010237985 A JP2010237985 A JP 2010237985A JP 4796656 B2 JP4796656 B2 JP 4796656B2
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- 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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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。
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。
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 (18)
- スカンジア安定化ジルコニアシートを製造するための方法であって、
スカンジア安定化ジルコニアの焼結体を粉砕して、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以下であるスカンジア安定化ジルコニア焼結粉末を得る工程;
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工程;
上記スラリーをシート状に成形する工程;および、
得られた成形体を焼結する工程
を含むことを特徴とする製造方法。 - スカンジア安定化ジルコニアが、安定化剤としてスカンジアを3モル%以上、15モル%以下含むものである請求項1に記載の製造方法。
- スカンジア安定化ジルコニアの焼結体が、厚さ1mm以下のシート状焼結体である請求項1または2に記載の製造方法。
- スカンジア安定化ジルコニアの焼結体として、不良を有するスカンジア安定化ジルコニア焼結体または破損したスカンジア安定化ジルコニア焼結体の少なくとも一方を用いる請求項1〜3のいずれかに記載の製造方法。
- スカンジア安定化ジルコニアの焼結体として、固体酸化物形燃料電池由来の電解質シートを用いる請求項1〜3のいずれかに記載の製造方法。
- 固体酸化物形燃料電池由来の電解質シートが、電極が形成されている単セルから電極を溶解した電解質シートである請求項5に記載の製造方法。
- 立方晶系スカンジア安定化ジルコニア焼結粉末および/または菱面体晶系スカンジア安定化ジルコニア焼結粉末を用いる請求項1〜6のいずれかに記載の製造方法。
- スカンジア安定化ジルコニアの焼結体を湿式で粉砕した後、スプレードライすることによりスカンジア安定化ジルコニア焼結粉末を得る請求項1〜7のいずれかに記載の製造方法。
- 請求項1〜8のいずれかに記載の方法で製造されたスカンジア安定化ジルコニアシートからな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。
- 請求項1〜8のいずれかに記載の方法で製造されたスカンジア安定化ジルコニアシートを電解質シートとして含むことを特徴とする固体酸化物形燃料電池。
- 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以下であるスカンジア安定化ジルコニア焼結粉末に由来する成分を、全体質量に対して実質的に1.9質量%以上、40質量%以下含むことを特徴とするスカンジア安定化ジルコニアシート。
- 上記スカンジア安定化ジルコニア焼結粉末が立方晶系および/または菱面体晶系である請求項11に記載のスカンジア安定化ジルコニアシート。
- ジルコニア未焼結粉末と、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以下であるスカンジア安定化ジルコニア焼結粉末から製造されたものであり、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%以下であることを特徴とするスカンジア安定化ジルコニアシート。
- 上記スカンジア安定化ジルコニア焼結粉末が立方晶系および/または菱面体晶系である請求項13に記載のスカンジア安定化ジルコニアシート。
- 3点曲げ強度が0.35GPa以上である請求項11〜14のいずれかに記載のスカンジア安定化ジルコニアシート。
- 相対密度が98%以上である請求項11〜15のいずれかに記載のスカンジア安定化ジルコニアシート。
- 請求項11〜16のいずれかに記載のスカンジア安定化ジルコニアシートからな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。
- 電解質シートとして請求項11〜16のいずれかに記載のスカンジア安定化ジルコニアシートを含むことを特徴とする固体酸化物形燃料電池。
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WO2016018106A1 (ko) * | 2014-07-30 | 2016-02-04 | 주식회사 엘지화학 | 치밀도가 향상된 무기 전해질막의 제조방법, 이를 위한 무기 전해질막 제조용 조성물 및 이를 통해 제조된 무기 전해질막 |
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