JP5654115B2 - 金属酸化物のナノファイバーおよびその製造方法 - Google Patents
金属酸化物のナノファイバーおよびその製造方法 Download PDFInfo
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- JP5654115B2 JP5654115B2 JP2013501613A JP2013501613A JP5654115B2 JP 5654115 B2 JP5654115 B2 JP 5654115B2 JP 2013501613 A JP2013501613 A JP 2013501613A JP 2013501613 A JP2013501613 A JP 2013501613A JP 5654115 B2 JP5654115 B2 JP 5654115B2
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Description
本発明の一観点によると、Sc、Y、La、Ce、Pr、Nd、Sm、Gd、Dy、Ho、Yb、Zr、Sr、Ba、Mn、Fe、Co、MaおよびGaのうちから選択される少なくとも1種の金属の金属酸化物のナノファイバーの製造方法が提供されており、
a)上記金属の塩を含有する前駆体を紡糸して、前記金属の塩を含有する前駆体のナノファイバーを得ることが可能であることと、
b)上記金属の塩を含有する前駆体のナノファイバーを500〜800℃の温度範囲内で焼成し、金属酸化物のナノファイバーを得ることが可能であることと、を含む。
本発明の一観点によると、前記前駆体中に、高分子化合物を含んでよい。
本発明の一観点によると、電界紡糸または液中紡糸法を利用して前記金属酸化物の前駆体のナノファイバーを製造してよい。
本発明の一観点によると、上記固体電解質材料により製造されてよい燃料電池が提供されている。
本発明の一観点によると、上記固体電解質材料により製造されてよい酸素センサが提供されている。
ここにおいて、“金属酸化物”とは金属元素の酸化物を主な形態とする化合物を指す。前記金属酸化物中には1種または複数種の金属元素が含まれてよく、好適には1種から2種の金属元素が含まれる。前記金属元素は、スカンジウム、イットリウム、ランタン、セリウム、プラセオジム、ネオジム、サマリウム、ガドリニウム、ジスプロシウム、ホルミウム、イッテルビウムなどの希土類金属、およびジルコニウム、ストロンチウム、バリウム、マンガン、鉄、コバルト、マグネシウムおよびガリウムなどその他金属の少なくとも1種としてよい。好適には、スカンジウム、イットリウム、ランタン、セリウム、プラセオジム、ネオジム、サマリウムまたはガドリニウム元素の少なくとも1種であり、より好適には、スカンジウム、セリウム、プラセオジム、サマリウムおよびガドリニウム元素の少なくとも1種を含有する。その他、前記金属酸化物中に、その他の金属元素を含有してもよい。しかし、本発明において効果が最良である金属酸化物中の金属元素は、上記金属から選択される。
本発明の金属酸化物ナノファイバーの製造方法には、ナノファイバーの調製工程および焼成工程が含まれる。各工程について、以下の通り説明する。
この工程について、その目的は金属塩を含有する前駆体に対してナノファイバー紡糸過程を実施して、金属塩を含有するナノファイバーを形成することにある。ここにおいて、“前駆体”とは金属塩を含有するナノファイバーを形成するための物質を指す。ナノファイバーの形成過程において、前駆体の化学成分内には最終的に金属酸化物ナノファイバーを形成するために必須の金属塩が含まれていなければならず、さらに溶媒および複数種の化合物も含まれる。当該前駆体は通常はゾル状である。その場合、溶媒としての組成は特に限定されるわけではなく、有機溶媒としてよく、水またはアルコールとしてもよく、好適には水である。金属塩は前述の金属カチオンの塩としてよく、その組成は具体的に限定されず、具体的な金属カチオンによる塩の種類は、硝酸塩、硫酸塩、ハロゲン化物など各種の無機塩類、および当該カチオンを含む有機塩類としてよく、本発明において好適には硝酸イオンを含有する塩である。前駆体中の金属塩の濃度は、好適にはその質量百分率濃度が2〜10wt%の間である。
この過程は、上記工程で得られた金属塩を含有するナノファイバーを焼成することにより金属酸化物の焼成体形式のナノファイバーを得るものである。この工程により、金属は酸化されて金属酸化物を形成し、金属酸化物は結晶化し、凝集して、結晶体が長くなり、結晶粒寸法が比較的大きな金属酸化物結晶体を形成する。この過程において、焼成温度の範囲は500〜800℃であり、好適には550〜650℃の範囲内である。焼成時間は一般には2〜10時間以上であり、好適には2〜4時間である。この焼成過程は空気雰囲気中で実施してよいが、焼成を加速させるため、雰囲気中の酸素分圧を低下させ、例えば水素ガス雰囲気、窒素ガス雰囲気、真空または水素ガスとアルゴンガスとの混合雰囲気中で焼成してもよい。
Ce(NO3)3・6H2O(純度99.9%以上)
Gd(NO3)3・6H2O(純度99.9%以上)
Y(NO3)3・6H2O(純度99.9%以上)
ZrO(NO3)2・2H2O(純度99.9%以上)
ポリビニルアルコール(PVA、MW=80000)
以下の方法に基づき、Ce0.9Gd0.1O1.95(GDC)の前駆体溶液を調製した。
0.6gのPVA粒子を5.4gの脱イオン水中に溶解し、温度60℃下で加熱しながら3時間撹拌してPVA水溶液を得た。その後、0.48gのセリウムおよびガドリニウムを含有する金属硝酸塩(モル比はCe:Gd=9:1)を上記PVA水溶液に加えた。室温下で2時間撹拌した後に、ガドリニウムを含有する硝酸セリウム/PVAの透明ゾル状の前駆体溶液が得られた。
電気化学ワークステーション(Zahner、IM6、Germany)を採用し、空気雰囲気中でGDCおよびYSZナノファイバーの400〜650℃の温度範囲内における交流インピーダンススペクトルを測定して、GDCおよびYSZナノファイバーの結晶粒界、結晶粒子および総導電率を算出した。
102:固体電解質
103:カソード
104:アノード
110:外部回路
Claims (10)
- Sc、Y、La、Ce、Pr、Nd、Sm、Gd、Dy、Ho、Yb、Zr、Sr、Ba、Fe、Co、MgおよびGaのうちから選択される少なくとも1種の金属の金属酸化物のナノファイバーの製造方法であって、
a)前記金属の塩及び高分子化合物を含有する前駆体を電界紡糸して、前記金属の塩を含有する前駆体のナノファイバーを製造することと、
b)前記金属の塩及び高分子化合物を含有する前駆体のナノファイバーを550〜650℃の温度範囲内で2〜4時間焼成し、前記少なくとも1種の金属元素を含有する金属酸化物のナノファイバーを得ることと、を含み、
前記ナノファイバーの平均径が50〜100nmの範囲であり、前記ナノファイバー中の結晶体の平均結晶粒が2〜20nmの範囲である、金属酸化物のナノファイバーの製造方法。 - 前記金属酸化物は、Sc、Y、La、Ce、Pr、Nd、SmおよびGdから選択される少なくとも1種の金属の金属酸化物である、請求項1に記載の製造方法。
- 前記金属酸化物が、ガドリニウムドープセリア(GDC)またはイットリア安定化ジルコニア(YSZ)である、請求項1または2に記載の製造方法。
- 前記高分子化合物がポリビニルアルコールである、請求項1〜3のいずれか一項に記載の製造方法。
- 前記工程b)が、前記前駆体のナノファイバーを600℃で2時間焼成することで実施される、請求項1〜4のいずれか一項に記載の製造方法。
- Sc、Y、La、Ce、Pr、Nd、Sm、Gd、Dy、Ho、Yb、Zr、Sr、Ba、Fe、Co、MgおよびGaのうちから選択される少なくとも1種の金属元素を含有する金属酸化物のナノファイバーであって、前記ナノファイバーの平均径は50〜100nmの範囲であり、前記ナノファイバー中の結晶体の平均結晶粒は2〜20nmの範囲である、金属酸化物のナノファイバー。
- 前記金属酸化物が、ガドリニウムドープセリア(GDC)またはイットリア安定化ジルコニア(YSZ)である、請求項6に記載の金属酸化物のナノファイバー。
- 請求項6または7記載の金属酸化物のナノファイバーを含む、固体電解質材料。
- 請求項8記載の固体電解質材料から製造される、燃料電池。
- 請求項8記載の固体電解質材料から製造される、酸素センサ。
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2011
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- 2011-03-29 JP JP2013501613A patent/JP5654115B2/ja active Active
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