JP2018522424A - 水性環境中での鉛フリーの圧電セラミックの製造 - Google Patents
水性環境中での鉛フリーの圧電セラミックの製造 Download PDFInfo
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Abstract
Description
a) 原料の混合
b) 原料の粉砕
c) 粉砕された原料混合物の造粒、例えば噴霧凍結造粒
d) か焼
e) か焼物を含むスラリー製造
f) スラリーの造粒
g) 圧粉体製造
h) 結合剤除去および焼結
i) 金属化および分極
を含む。
この方法を、次の方法工程に基づき実施する:
1) Bi2O3−Na2CO3−TiO2懸濁液の製造
Bi2O3、Na2CO3、TiO2、水および粉砕ボールを容器内に秤量した。引き続き、この懸濁液を均質化または解凝集させた。
このセラミック懸濁液を、液体窒素で満たされたシャーレ内へ吹き付け、それにより急速凍結させた。スラリー供給は貯蔵容器を介したホース接続によって行った。生成物シャーレは、それぞれの吹付過程の開始に、液体窒素で満たされた。液体窒素の蒸発に基づき、スプレーユニット間の充填レベルを規則的に制御し、かつ場合により窒素を後充填した。これは、凍結された液滴が液体窒素で連続的に覆われることを保証し、ひいてはスラリーの再溶融を回避するために用いられる。吹付過程の後に、凍結されたスラリー液滴と液体窒素とを有する生成物シャーレを凍結乾燥装置に入れた。液体窒素が、僅かな残留物を除いて完全に蒸発すると同時に、凍結乾燥プロセスを開始した、つまり凍結乾燥装置内の圧力を低下させた。顆粒の主乾燥のために、約24時間の時間を規定した。後乾燥工程は省略した。
Bi2O3−Na2CO3−TiO2−BaTiO3粉末混合物のために、この噴霧凍結顆粒とBaTiO3粉末とを多様な割合(表1参照)で容器内に秤量した。均一な粉末混合物を作製するために、いくつかの粉砕ボールを添加した後に、容器をロール装置に設置し、かつ乾式で混合した。
Bi2O3−Na2CO3−TiO2−BaTiO3粉末混合物をシャーレ上に分配した。粉末混合物のBNT−BTへのか焼を900℃で行った。
か焼後に、このBNT−BT粉末を遊星型ボールミルを用いて粉砕した。粉砕ボールの分離後に、このスラリーに有機添加物を添加した。このスラリーをもう一回ロール装置で均質化した。
工程2)と同様
圧粉体の製造を、一軸プレス機を用いて約200MPaのプレス圧で行った。
グリーン成形品を800℃で結合剤除去した。引き続き、このプレス成形体をカプセル内に入れ、焼結した。
平面の研削により、焼結したタブレットの厚みを1mmに調節した。両面の金属化を、銀ペーストを用い、これをスクリーン印刷により塗布し、700〜900℃で焼き付けることにより行った。分極のために、台形型の電圧プロフィールを印加し、ここで最大電圧を2〜5kVの間で変化させた。
Claims (17)
- 圧電特性を有するセラミックの製造方法において、主に水性の懸濁剤を使用することを特徴とする、前記製造方法。
- 第1の方法工程で、原料を主に水性の懸濁剤中で混合し、かつ粉砕し、この際に、等方性の分布を有する懸濁液が生じることを特徴とする、請求項1記載の圧電特性を有するセラミックの製造方法。
- 前記懸濁液の等方性の分布を次の方法工程で固定することを特徴とする、請求項2記載の圧電特性を有するセラミックの製造方法。
- 前記等方性の分布の固定を前記懸濁液の凍結により行うことを特徴とする、請求項3記載の圧電特性を有するセラミックの製造方法。
- 前記凍結を、液体、固体または気体の凍結媒体中で行うことを特徴とする、請求項4記載の圧電特性を有するセラミックの製造方法。
- 前記凍結媒体の温度は、前記懸濁液の溶融温度を下回る、好ましくは前記溶融温度を遙かに下回ることを特徴とする、請求項5記載の圧電特性を有するセラミックの製造方法。
- 前記懸濁液を急速凍結することを特徴とする、請求項6記載の圧電特性を有するセラミックの製造方法。
- 前記凍結媒体は、液体窒素もしくは気体窒素、液体空気もしくは気体空気、液体酸素もしくは気体酸素、または他の液体のもしくは気体の有機媒体もしくは無機媒体からなる群から選択されることを特徴とする、請求項5から7までのいずれか1項記載の圧電特性を有するセラミックの製造方法。
- 凍結媒体中への吹き込みにより凍結を行い、それにより原顆粒が生じることを特徴とする、請求項4から7までのいずれか1項記載の圧電特性を有するセラミックの製造方法。
- 前記等方性の分布の固定を、圧力変化、固体媒体などのような物理学的方法により、ゲル化プロセスにより、分散液のフロキュレーションにより、または添加物の添加により行うことを特徴とする、請求項3記載の圧電特性を有するセラミックの製造方法。
- 前記懸濁剤を、毛管力を排除しながら、かつ液相を顕著に生じさせることなく除去することを特徴とする、請求項1から10までのいずれか1項記載の圧電特性を有するセラミックの製造方法。
- 前記懸濁剤の除去を昇華により行うことを特徴とする、請求項11記載の圧電特性を有するセラミックの製造方法。
- 固定された等方性の分布を、反応プロセスを用いて圧電材料に変換することを特徴とする、請求項3から12までのいずれか1項記載の圧電特性を有するセラミックの製造方法。
- 前記反応プロセスは熱処理(か焼)であり、それによりか焼物が得られることを特徴とする、請求項13記載の圧電特性を有するセラミックの製造方法。
- 前記か焼物から造粒法を用いて、圧縮可能な粉末を製造することを特徴とする、請求項14記載の圧電特性を有するセラミックの製造方法。
- 前記造粒法は噴霧乾燥または噴霧凍結造粒であることを特徴とする、請求項15記載の圧電特性を有するセラミックの製造方法。
- 前記懸濁液は、好ましくはチタン酸ビスマスナトリウム(BNT)セラミック、チタン酸ビスマスナトリウム−チタン酸バリウム(BNT−BT)セラミック、ニオブ酸カリウムナトリウム(KNN)セラミック、またはチタン酸ビスマスナトリウム−ニオブ酸カリウムナトリウム(BNT−KNN)セラミック、またはそれらの混合物から選択されるセラミック40〜60%、水40〜60%、および(有機)添加物<20%、好ましくは<5%を含むことを特徴とする、圧電特性を有するセラミックを製造するための懸濁液。
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