JPH1149565A - セラミック粉末の製造方法 - Google Patents

セラミック粉末の製造方法

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Publication number
JPH1149565A
JPH1149565A JP9219982A JP21998297A JPH1149565A JP H1149565 A JPH1149565 A JP H1149565A JP 9219982 A JP9219982 A JP 9219982A JP 21998297 A JP21998297 A JP 21998297A JP H1149565 A JPH1149565 A JP H1149565A
Authority
JP
Japan
Prior art keywords
ceramic powder
water
powder
core
ceramic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP9219982A
Other languages
English (en)
Other versions
JP3302627B2 (ja
Inventor
Yasuhisa Kono
泰久 河野
Kenji Saito
賢二 斎藤
Yoichi Mizuno
洋一 水野
Koichi Chazono
広一 茶園
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Taiyo Yuden Co Ltd
Original Assignee
Taiyo Yuden Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Taiyo Yuden Co Ltd filed Critical Taiyo Yuden Co Ltd
Priority to JP21998297A priority Critical patent/JP3302627B2/ja
Priority to US09/118,820 priority patent/US6007870A/en
Priority to MYPI98003496A priority patent/MY122242A/en
Priority to DE69808569T priority patent/DE69808569T2/de
Priority to EP98114290A priority patent/EP0894779B1/en
Publication of JPH1149565A publication Critical patent/JPH1149565A/ja
Priority to US09/436,346 priority patent/US6254991B1/en
Application granted granted Critical
Publication of JP3302627B2 publication Critical patent/JP3302627B2/ja
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

(57)【要約】 【課題】 結晶性の高いセラミック粉末を用いてコア−
シェル構造のセラミック粉末を得ようとした場合、結晶
性の高いセラミック粉末は反応性が低いので、かなり高
温で焼成しなければならず、コスト高になる。また、結
晶性の低いセラミック粉末を用いてコア−シェル構造の
セラミック粉末を得ようとした場合、結晶性の低いセラ
ミック粉末によって作られたセラミック電子部品は電気
的特性や機械的特性が悪くなる。 【解決手段】 この発明に係るセラミック粉末の製造方
法は、結晶質のセラミック粉末を水とともに加熱して該
セラミック粉末を該水にコア部を残すようにして溶解さ
せる溶解工程と、該溶解工程を経た該セラミック粉末と
該水を徐冷して該水に溶解させた該セラミック粉末の成
分を該水から該コア部の周囲に析出物として析出させる
析出工程と、該析出工程を経た該セラミック粉末に添加
物を添加して混合し、これらを高温で焼成して該析出物
と該添加物とを固相反応させて該コア部の周囲にシェル
部を形成させる焼成工程とを備えている。

Description

【発明の詳細な説明】
【０００１】
【発明の属する技術分野】この発明はコア−シェル構造
を有するセラミック粉末の製造方法に関するものであ
る。
【０００２】
【従来の技術】セラミック電子部品は小型化と高性能化
が進められ、種々の材料が開発されているが、そのよう
な背景の下で、コア−シェル構造のセラミック粉末がセ
ラミック電子部品の材料として注目されている。
【０００３】このコア−シェル構造の粉末は、結晶性の
高いコア部の周囲にコア部とは異なる成分組成のシェル
部が形成されているものである。かかる構造を採るセラ
ミック粉末を誘電体材料として使用した場合、磁器コン
デンサの温度特性を平滑にすることができる。
【０００４】コア−シェル構造のセラミック粉末は、例
えば、セラミック粉末と添加物とを混合し、これを高温
で焼成してセラミック粉末の表面と添加物とを固相反応
させることによって得ることができる。
【０００５】
【発明が解決しようとする課題】ところで、結晶性の高
いセラミック粉末は誘電率等の電気的特性が良好なの
で、これを用いてコア−シェル構造のセラミック粉末を
作ることができれば好都合である。しかし、結晶性の高
いセラミック粉末は反応性が低いので、固相反応を生じ
させるためにはかなり高温で焼成しなければならず、コ
スト高になるという欠点がある。
【０００６】これに対し、結晶性の低いセラミック粉末
を用いてコア−シェル構造のセラミック粉末を作った場
合、低温で焼成しても容易に固相反応を生じさせること
ができる。しかし、結晶性の低いセラミック粉末によっ
て作られたセラミック電子部品は電気的特性や機械的特
性が悪いという欠点がある。
【０００７】この発明は、電気的、機械的特性の良いコ
ア−シェル構造のセラミック粉末を低温の焼成で得るこ
とができるようにしたセラミック粉末の製造方法を提供
することを目的とする。
【０００８】
【課題を解決するための手段】この発明に係るセラミッ
ク粉末の製造方法は、結晶質のセラミック粉末を水とと
もに加熱して該セラミック粉末を該水にコア部を残すよ
うにして溶解させる溶解工程と、該溶解工程を経た該セ
ラミック粉末と該水を徐冷して該水に溶解させた該セラ
ミック粉末の成分を該水から該コア部の周囲に析出物と
して析出させる析出工程と、該析出工程を経た該セラミ
ック粉末に添加物を添加して混合し、これらを高温で焼
成して該析出物と該添加物とを固相反応させて該コア部
の周囲にシェル部を形成させる焼成工程とを備えたこと
を特徴とするものである。
【０００９】ここで、前記セラミック粉末としては、例
えばチタン酸バリウム粉末、チタン酸ジルコン酸バリウ
ム粉末、チタン酸ジルコン酸鉛粉末又はチタン酸鉛粉末
を使用することができるが、これら以外の化合物を排除
するものではない。
【００１０】また、前記結晶質のセラミック粉末は、例
えば水熱法によって合成されたものを使用することがで
きるが、結晶質のものであれば他の方法によって得られ
たセラミック粉末を使用してもよい。
【００１１】また、前記セラミック粉末と水との加熱温
度は８０〜１２０℃が好ましい。この場合、前記セラミ
ック粉末を水とともに加圧下で加熱すれば、セラミック
粉末の溶解速度が早くなる。また、この加熱処理の時間
はシェル部の厚さに影響があり、加熱処理の時間を長く
すればシェル部の厚さを増加させることができる。
【００１２】また、徐冷速度は２〜２０℃／ｈが好まし
い。徐冷速度が２℃／ｈ未満では時間がかかり過ぎ、ま
た２０℃／ｈを超えると析出物がコア部の周囲にうまく
析出できないからである。なお、前記析出物は水酸基、
水分又はポアからなる欠陥を有しているので添加物との
反応性が高くなっていると考えられる。
【００１３】更に、前記添加物としては例えばＮｂ2 Ｏ
5 、Ｃｏ3 Ｏ4 、ＭｎＯ2 ，Ｔａ2Ｏ5 又はＶＯ5 を使
用することができるが、これら以外の化合物を排除する
ものではない。
【００１４】
【実施例】
実施例１ 水熱法で合成した結晶性の高い粒径０．５μｍのチタン
酸バリウム粉末１００ｇと純水２００ｍｌをオートクレ
ーブ中に入れて密閉し、これを表１のサンプルＡ〜Ｄに
示すように、８０〜１００℃で５〜１０時間保ち、チタ
ン酸バリウム粉末の粒子表面を純水中に徐々に溶解させ
た。
【００１５】次に、このオートクレーブを同表に示すよ
うに、２〜２０℃／ｈの降温速度で５０℃以下になるま
で徐冷した。
【００１６】次に、５０℃で得られたチタン酸バリウム
粉末のスラリーにＮｂ2 Ｏ5 １．１４ｇを添加し、５ｍ
ｍφＺｒＯ2 ビーズで１時間混合した。
【００１７】次に、このスラリーをろ過し、ケーキを１
１０℃で２４時間乾燥し、これを大気中において１１０
０℃で３時間焼成し、セラミック粉末を得た。
【００１８】次に、ＸＲＤでこのセラミック粉末を分析
したところ、チタン酸バリウムへのＮｂの固溶の程度を
示す、４５．２６°（ＣｕＫα）のピークのシフトは表
１に示す通りであった。
【００１９】また、得られたセラミック粉末の誘電率を
測定したところ、同表のサンプルＡ〜Ｄに示す通りであ
った。
【００２０】比較例１ 実施例１で使用した粒径０．５μｍのチタン酸バリウム
粉末１００ｇとＮｂ2Ｏ5 ０．５ｇをこのまま混合して
１１００℃で３時間焼成し、得られたセラミック粉末を
ＸＤＲで分析したところ、ピークシフトは、同表に示す
ように４５．２６°（通常の固体反応）であった。ま
た、得られたセラミック粉末の誘電率は、同表に示すよ
うに２３１０であった。
【００２１】
【表１】
【００２２】以上の結果から、比較例１によって得られ
たセラミック粉末と比較して、実施例１によって得られ
たセラミック粉末は、４５．２６°（ＣｕＫα）のピー
クのシフトの程度から考えて、結晶性の高いコア部の周
囲にシェル部が厚く形成されていることがわかる。
【００２３】また、比較例１によって得られたセラミッ
ク粉末は、誘電率が２３１０であるのに対し、実施例１
によって得られたセラミック粉末の誘電率は２７５５〜
２９０３と、かなり高くなることがわかる。
【００２４】なお、セラミック粉末としてチタン酸ジル
コン酸バリウム粉末、チタン酸ジルコン酸鉛粉末又はチ
タン酸鉛粉末を用い、実施例１と同様の実験をしたとこ
ろ、実施例１と同様の結果が得られた。
【００２５】また、添加物としてＭｎＯ2 、Ｔａ2 Ｏ5
又はＶＯ5 を用い、実施例１と同様の実験をしたとこ
ろ、実施例１と同様の結果が得られた。
【００２６】
【発明の効果】この発明によれば、理想的なコア−シェ
ル構造のセラミック粉末、従って、電気的、機械的特
性、特に温度特性の良好なセラミック粉末を、比較的低
い温度で、すなわち低コストで製造することができると
いう効果がある。
フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ０１Ｇ 35/00 Ｃ０１Ｇ 35/00 Ｄ 45/04 45/04 51/04 51/04 Ｃ０４Ｂ 35/626 Ｃ０４Ｂ 35/00 Ａ (72)発明者 茶園 広一 東京都台東区上野６丁目16番20号 太陽誘 電株式会社内

Claims (4)

    【特許請求の範囲】
  1. 【請求項１】 結晶質のセラミック粉末を水とともに加
    熱して該セラミック粉末を該水にコア部を残すようにし
    て溶解させる溶解工程と、該溶解工程を経た該セラミッ
    ク粉末と該水を徐冷して該水に溶解させた該セラミック
    粉末の成分を該水から該コア部の周囲に析出物として析
    出させる析出工程と、該析出工程を経た該セラミック粉
    末に添加物を添加して混合し、これらを高温で焼成して
    該析出物と該添加物とを固相反応させて該コア部の周囲
    にシェル部を形成させる焼成工程とを備えたことを特徴
    とするセラミック粉末の製造方法。
  2. 【請求項２】 前記セラミック粉末を水とともに加圧下
    で加熱することを特徴とする請求項１に記載のセラミッ
    ク粉末の製造方法。
  3. 【請求項３】 前記セラミック粉末がチタン酸バリウム
    粉末、チタン酸ジルコン酸バリウム粉末、チタン酸ジル
    コン酸鉛粉末又はチタン酸鉛粉末であることを特徴とす
    る請求項１又は２に記載のセラミック粉末の製造方法。
  4. 【請求項４】 前記添加物がＮｂ2 Ｏ5 、Ｃｏ3 Ｏ4 、
    ＭｎＯ2 ，Ｔａ2 Ｏ5 又はＶＯ5 であることを特徴とす
    る請求項１〜３のいずれかに記載のセラミック粉末の製
    造方法。
JP21998297A 1997-07-31 1997-07-31 セラミック粉末の製造方法 Expired - Fee Related JP3302627B2 (ja)

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JP21998297A JP3302627B2 (ja) 1997-07-31 1997-07-31 セラミック粉末の製造方法
US09/118,820 US6007870A (en) 1997-07-31 1998-07-20 Process for preparing ceramic powder
MYPI98003496A MY122242A (en) 1997-07-31 1998-07-30 Process for preparing ceramic powder
DE69808569T DE69808569T2 (de) 1997-07-31 1998-07-30 Verfahren zur Herstellung von keramischen Pulvern
EP98114290A EP0894779B1 (en) 1997-07-31 1998-07-30 Process for preparing ceramic powder
US09/436,346 US6254991B1 (en) 1997-07-31 1999-11-09 Prepared ceramic powder

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US6254991B1 (en) 2001-07-03
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