JP5733313B2 - 積層セラミックコンデンサ、及びその製造方法 - Google Patents
積層セラミックコンデンサ、及びその製造方法 Download PDFInfo
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- JP5733313B2 JP5733313B2 JP2012533926A JP2012533926A JP5733313B2 JP 5733313 B2 JP5733313 B2 JP 5733313B2 JP 2012533926 A JP2012533926 A JP 2012533926A JP 2012533926 A JP2012533926 A JP 2012533926A JP 5733313 B2 JP5733313 B2 JP 5733313B2
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Description
(A)セラミック粉末の作製
出発原料として、微粒のBaCO3、CaCO3、TiO2、Re(ReはLa、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及びY)、M(MはMg、Mn、Al、Cr及びZn)の各粉末を用意した。Reの粉末としては、La2O3、Ce2O3、Pr2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、Tb2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3及びY2O3の各粉末を用意した。また、Mの粉末としては、MgCO3、MnCO3、Al2O3、Cr2O3、ZnOの各粉末を用意した。そして、これらの粉末を(Ba1-x-yCaxRey)(Ti1-zMz)O3の表1の組成となるように秤量した後、ボールミルで80時間混合した。その後、上記の混合粉末を1000℃の熱処理で仮焼合成することにより、(Ba1-x-yCaxRey)(Ti1-zMz)O3の主成分粉末を得た。その後、主成分粉末100モル部に対して、BaCO3を1.5モル部、SiO2を2モル部添加して、セラミック粉末を得た。
まず、誘電体層となるべきセラミックグリーンシートを形成した。具体的には、上述したセラミック粉末に、ポリビニルブチラール系バインダ及びエタノールを加えて、ボールミルにより24時間湿式混合した。その後、フィルターでフィルタリングを行い、所定の範囲内の粒径以外の粒径を有する粉末を排除したスラリーを作製した。そして、このスラリーをリップ方式によりシート上に成形して、セラミックグリーンシートを得た。セラミックグリーンシートの厚さは、後述するように、焼成後に表2の「誘電体層厚」に示す厚さになるようにした。
得られた積層セラミックコンデンサについて、各種特性を評価した。
平均粒径は以下のように算出した。まず、各試料に係る積層セラミックコンデンサを破断し、1000℃の温度でサーマルエッチングを行い、破断面を走査型顕微鏡を用いて観察した。そして、この観察像について画像解析を行い、結晶粒子の円相当径を粒径として、結晶粒子の粒径を測定した。そして、各試料につき、300個の結晶粒子の粒径を測定し、その平均値を平均粒径として算出した。
高温負荷寿命試験は、下記のように実施した。各試料に係る積層セラミックコンデンサに、温度125℃にて、6.3kV/mm及び12.6kV/mmの各電界強度となるようにDC電圧を印加した。そして、100個の試料で高温負荷寿命試験を実施し、1000時間経過するまでに、絶縁抵抗値が100kΩ以下になった試料を不良と判定し、試料100個中の不良個数を求めた。
試料番号1、10、14は(Ba,Re)(Ti,M)O3が主成分であり、DC電圧が6.3kV/μm、12.6kV/μm共に、良好な信頼性を示した。また、試料番号2〜9、11〜13、15〜17は(Ba,Ca,Re)(Ti,M)O3が主成分であり、DC電圧が6.3kV/μm、12.6kV/μm共に、良好な信頼性を示した。なお、試料番号1〜3、5、7、8、10〜14、16は平均粒径が20nm以上かつ100nm未満であり、DC電圧が12.6kV/μmの試験条件でも不良が発生せず、良好な信頼性を示した。
実験例2では、不純物の影響を評価した。積層セラミックコンデンサの原料作製工程等において、Sr、Zr、Hf、Zn、Na、Ag、Pd及びNi等が不純物として混入する可能性がある。これらは結晶粒子内及び結晶粒子間を占める結晶粒界に存在する可能性がある。また、積層セラミックコンデンサの焼成工程等において、内部電極成分が誘電体セラミック中の結晶粒界及び結晶粒子間を占める結晶粒界に拡散して存在する可能性がある。実験例2は、これらの不純物の影響を評価しようとするものである。
実験例1の試料番号13の組成に、表3に示した不純物成分を加えたことを除いて、実験例1と同様の方法でセラミック粉末を作製した。
上記セラミック粉末を用いて、実験例1と同様の方法で積層セラミックコンデンサを作製した。
得られた積層セラミックコンデンサについて、実験例1と同様の方法で各種特性を評価した。表4に高温負荷寿命試験の結果を示す。
表4から分かるように、不純物が混入した試料31〜40のいずれにおいても、電界強度が6.3kV/mm及び12.6kV/mmの双方において、高温負荷寿命試験での不良個数が0であり、高い信頼性を示した。また、試料31〜40のいずれにおいても、平均粒径は20nm以上かつ150nm以下であった。
2 誘電体層
3、4 内部電極
5 積層体
6、7 外部電極
Claims (2)
- 積層されている複数の誘電体層と、前記誘電体層間の界面に沿って形成されている複数の内部電極と、を有する積層体と、前記積層体の外表面に形成され、前記内部電極と電気的に接続されている複数の外部電極と、を備える積層セラミックコンデンサにおいて、
前記誘電体層は、一般式(Ba 1−x−y Ca x Re y )(Ti 1−z M z )O 3 (但し、ReはLa、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及びYの中から選択された少なくとも一種以上の元素、MはMg、Mn、Al、Cr及びZnの中から選択された少なくとも一種以上の元素)で表されると共に、0≦x≦0.2、0.002≦y≦0.1、0.001≦z≦0.05の範囲である化合物を主成分として含み、結晶粒子の平均粒径が20nm以上かつ100nm未満である誘電体セラミックからなることを特徴とする積層セラミックコンデンサ。 - 一般式(Ba1−x−yCaxRey)(Ti1−zMz)O3(但し、ReはLa、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu及びYの中から選択された少なくとも一種以上の元素、MはMg、Mn、Al、Cr及びZnの中から選択された少なくとも一種以上の元素)で表されると共に、0≦x≦0.2、0.002≦y≦0.1、0.001≦z≦0.05の範囲である化合物を主成分として含む、セラミック粉末を用意する工程と、
前記セラミック粉末を成形し、成形体を得る工程と、
前記成形体を焼成し、結晶粒子の平均粒径が20nm以上かつ100nm未満である誘電体セラミックを得る工程と、
を備える、前記誘電体セラミックからなる積層セラミックコンデンサの製造方法。
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