JPWO2012035935A1 - 誘電体セラミック、積層セラミックコンデンサ、及びこれらの製造方法 - Google Patents
誘電体セラミック、積層セラミックコンデンサ、及びこれらの製造方法 Download PDFInfo
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- JPWO2012035935A1 JPWO2012035935A1 JP2012533926A JP2012533926A JPWO2012035935A1 JP WO2012035935 A1 JPWO2012035935 A1 JP WO2012035935A1 JP 2012533926 A JP2012533926 A JP 2012533926A JP 2012533926 A JP2012533926 A JP 2012533926A JP WO2012035935 A1 JPWO2012035935 A1 JP WO2012035935A1
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- 239000000919 ceramic Substances 0.000 title claims abstract description 51
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 7
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 7
- 229910052693 Europium Inorganic materials 0.000 claims abstract description 7
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 7
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 7
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 7
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 7
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 7
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 7
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 7
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 7
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 7
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 26
- 238000010304 firing Methods 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 description 9
- 230000005684 electric field Effects 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 239000011572 manganese Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 5
- 229910052788 barium Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
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- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 229910052789 astatine Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000010419 fine particle Substances 0.000 description 1
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- 229910052735 hafnium Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
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 (6)
- 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み、結晶粒子の平均粒径が20nm以上かつ150nm以下である誘電体セラミック。
- 前記平均粒径が20nm以上かつ100nm未満である、請求項1に記載の誘電体セラミック。
- 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、請求項1または2に記載の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150nm以下である誘電体セラミックを得る工程と、
を備える、誘電体セラミックの製造方法。 - 前記平均粒径が20nm以上かつ100nm未満である、請求項4に記載の誘電体セラミックの製造方法。
- 請求項4または5の誘電体セラミックの製造方法を備えることを特徴とする、積層セラミックコンデンサの製造方法。
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TWI240288B (en) * | 2003-01-31 | 2005-09-21 | Murata Manufacturing Co | Dielectric ceramic and the manufacturing method thereof, and the laminated ceramic condenser |
US6905649B2 (en) * | 2003-04-11 | 2005-06-14 | The Regents Of The University Of California | High-density barium titanate of high permittivity |
JP4782552B2 (ja) * | 2005-11-28 | 2011-09-28 | 京セラ株式会社 | 誘電体磁器 |
JP5039039B2 (ja) * | 2006-07-27 | 2012-10-03 | 京セラ株式会社 | 誘電体磁器およびコンデンサ |
JP5078307B2 (ja) * | 2006-09-27 | 2012-11-21 | 京セラ株式会社 | 誘電体磁器およびその製法、ならびにコンデンサ |
JP4931697B2 (ja) * | 2007-05-29 | 2012-05-16 | 京セラ株式会社 | 誘電体磁器およびコンデンサ |
JP5207675B2 (ja) * | 2007-07-02 | 2013-06-12 | 京セラ株式会社 | 誘電体磁器およびこれを用いた積層セラミックコンデンサ |
JP4992918B2 (ja) * | 2009-01-30 | 2012-08-08 | 株式会社村田製作所 | 誘電体セラミックおよび積層セラミックコンデンサ |
WO2010098033A1 (ja) * | 2009-02-27 | 2010-09-02 | 株式会社村田製作所 | 誘電体セラミックおよび積層セラミックコンデンサ |
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- 2011-08-23 CN CN2011800420021A patent/CN103080044A/zh active Pending
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WO2012035935A1 (ja) | 2012-03-22 |
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US9061944B2 (en) | 2015-06-23 |
US20130141838A1 (en) | 2013-06-06 |
CN103080044A (zh) | 2013-05-01 |
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