JP5668572B2 - 誘電体磁器組成物およびセラミック電子部品 - Google Patents
誘電体磁器組成物およびセラミック電子部品 Download PDFInfo
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- JP5668572B2 JP5668572B2 JP2011073336A JP2011073336A JP5668572B2 JP 5668572 B2 JP5668572 B2 JP 5668572B2 JP 2011073336 A JP2011073336 A JP 2011073336A JP 2011073336 A JP2011073336 A JP 2011073336A JP 5668572 B2 JP5668572 B2 JP 5668572B2
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Description
チタン酸バリウムからなる主成分を含有し、
前記チタン酸バリウム100モルに対して、各酸化物換算で、
Mgの酸化物を1.00〜2.50モルと、
Mnおよび/またはCrの酸化物を0.01〜0.20モルと、
V、MoおよびWからなる群から選ばれる少なくとも1つの酸化物を0.03〜0.15モルと、
R1の酸化物(R1は、Y、およびHoからなる群から選ばれる少なくとも1つである)を0.20〜1.50モルと、
R2の酸化物(R2は、Eu、GdおよびTbからなる群から選ばれる少なくとも1つである)を0.20〜1.50モルと、
Siおよび/またはBの酸化物を0.30〜1.50モルと、を副成分として含有する誘電体磁器組成物であって、
前記R1の酸化物のR12 O3 換算での含有量をαモル、前記R2の酸化物のR22 O3 換算での含有量をβモルとすると、0.25≦β/(α+β)≦0.85である関係を満足し、
前記誘電体磁器組成物において、A(Aは、BaおよびCaから選ばれる少なくとも1つである)の含有量と、B(Bは、TiおよびZrから選ばれる少なくとも1つである)の含有量とが、1.000≦A/B≦1.006である関係を満足する。
図1に示すように、積層セラミック電子部品の一例としての積層セラミックコンデンサ1は、誘電体層2と、内部電極層3と、が交互に積層された構成のコンデンサ素子本体10を有する。内部電極層3は、各端面がコンデンサ素子本体10の対向する2端部の表面に交互に露出するように積層してある。一対の外部電極4は、コンデンサ素子本体10の両端部に形成され、交互に配置された内部電極層3の露出端面に接続されて、コンデンサ回路を構成する。
誘電体層2は、本実施形態に係る誘電体磁器組成物から構成されている。本実施形態に係る誘電体磁器組成物は、主成分として、チタン酸バリウムを有し、後述する副成分を含む。
内部電極層3に含有される導電材は特に限定されないが、誘電体層2を構成する材料が耐還元性を有するため、比較的安価な卑金属を用いることができる。導電材として用いる卑金属としては、NiまたはNi合金が好ましい。Ni合金としては、Mn,Cr,CoおよびAlから選択される1種以上の元素とNiとの合金が好ましく、合金中のNi含有量は95重量%以上であることが好ましい。なお、NiまたはNi合金中には、P等の各種微量成分が0.1重量%程度以下含まれていてもよい。内部電極層3の厚さは用途等に応じて適宜決定すればよいが、通常、0.4〜1.5μm、特に0.5〜1.0μm程度であることが好ましい。
外部電極4に含有される導電材は特に限定されないが、本発明では安価なNi,Cuや、これらの合金を用いることができる。外部電極4の厚さは用途等に応じて適宜決定すればよいが、通常、5〜50μm程度であることが好ましい。
本実施形態の積層セラミックコンデンサ1は、従来の積層セラミックコンデンサと同様に、ペーストを用いた通常の印刷法やシート法によりグリーンチップを作製し、これを焼成した後、外部電極を印刷または転写して焼成することにより製造される。
まず、主成分の原料粉体としてチタン酸バリウム粉末(BauTivO3 、u/v=0.998)を準備した。また、副成分の原料として、Y、Tb、Mg、Mn、V、Si、Ba、Caをそれぞれ酸化物で用意し、主成分および副成分の添加量は表1に示す値となるように秤量した。
主成分原料であるチタン酸バリウムのu/vを、0.998〜1.007の範囲で変化させ、表1のように誘電体磁器組成物におけるA/Bの比率を変えた以外は、試料1と同様の条件で、試料2〜8の積層セラミックコンデンサを作製した。
(誘電体磁器組成物のA/Bの評価)
得られた誘電体層用ペーストの一部をサンプリングし、500℃、大気中において、脱バイ処理を行い、評価用誘電体粉末サンプルを得た。得られた誘電体粉末サンプルを、蛍光X線分析装置(リガク(株)製、サイマルティック3530)を用いガラスビード法によって測定し、誘電体磁器組成物のA/Bの比率を算出した(単位なし)。誘電体層用ペーストにおけるA/Bの比率は、誘電体磁器組成物(誘電体層2)におけるA/Bの比率と実質的に同じである。結果を表1に示す。
誘電損失(tanδ)は、コンデンサ試料に対し、基準温度25℃において、デジタルLCRメータ(アジレントテクノロジー社製E4980A)にて、周波数1kHz,入力信号レベル(測定電圧)0.5Vrmsの条件下で測定した。誘電損失は低いほうが好ましく、本実施例では6.0%以下を良好とした。結果を表1に示す。
比誘電率εは、コンデンサ試料に対し、基準温度25℃において、デジタルLCRメータ(アジレントテクノロジー社製E4980A)にて、周波数1kHz,入力信号レベル(測定電圧)0.5Vrmsの条件下で測定された静電容量から算出した(単位なし)。比誘電率は高いほうが好ましく、本実施例では、1500以上を良好とした。結果を表1に示す。
コンデンサ試料に対し、絶縁抵抗計(アドバンテスト社製R8340A)を用いて、25℃において6V/μmの直流電圧を、コンデンサ試料に30秒間印加した後の絶縁抵抗IRを測定した。CR積は、上記にて測定した静電容量C(単位はμF)と、絶縁抵抗IR(単位はMΩ)との積を求めることにより測定した。本実施例では、300以上を良好とした。結果を表1に示す。表では、CRPとして表記する。
コンデンサ試料に対し、85℃における静電容量を測定し、室温(25℃)における静電容量の変化率ΔCを算出した。85℃における変化率ΔCが、±15%以内であるか否かを評価した。結果を表1に示す。表では、TC85として表記する。
コンデンサ試料に対し、200℃にて、15V/μmの電界下で直流電圧の印加状態に保持し、寿命時間を測定することにより、高温負荷寿命を評価した。本実施例においては、印加開始から絶縁抵抗が一桁落ちるまでの時間を破壊時間し、これをワイブル解析することにより算出した平均故障時間(MTTF)を寿命と定義した。また、本実施例では、上記の評価を20個のコンデンサ試料について行い、その平均値を高温負荷寿命とした。評価基準は1.0時間以上を良好とした。結果を表1に示す。
誘電体原料において、各副成分とその含有量を表2〜9のように変化させ、試料1と同様の条件で、試料20〜97の積層セラミックコンデンサを作製し、同様な評価を行った。結果を表2〜9に示す。
また、R2がTbおよびGdである場合には(試料40および42)、Euである場合(試料43)に比べて、CR積および高温負荷寿命(HALT)の特性に優れ、特に、R2がTbである場合には、GdおよびEuである場合に比べて、比誘電率εおよび静電容量の温度特性(TC)の特性をより向上できることが確認された。なお、表4におけるR1およびR2(RE)の数値は、RE2 O3 換算(Tbなどに関しては、Tb2 O3.5 )での数値である。
さらに、Mnの酸化物を用いる場合には、Crの酸化物を用いる場合に比べて、CR積および高温負荷寿命(HALT)の特性をより向上できることが確認された。なお、表7において、Crの数値は、Cr2 O3 換算での数値である。
さらに、Vの酸化物を用いる場合には、MoおよびWの酸化物を用いる場合に比べて、高温負荷寿命(HALT)の特性をより向上できることが確認された。なお、MoおよびWの数値は、それぞれMoO3 、WO3 換算での数値である。
試料101では、前述した試料72に基づき、各副成分とその含有量を表10のように変化させ、しかも、BaOとCaOを、主成分とは別に添加することで、完成A/Bが試料72と同様に、1.004となるようにした以外は、試料72と同様にして積層セラミックコンデンサを作製し、信頼性の評価を行った。さらに、試料100、102、103では、層間厚みを、表10示すように変化させた以外は、試料101と同様にして、積層セラミックコンデンサを作製し、信頼性の評価を行った。結果を表10に示す。
2… 誘電体層
3… 内部電極層
4… 外部電極
10… コンデンサ素子本体
Claims (6)
- チタン酸バリウムからなる主成分を含有し、
前記チタン酸バリウム100モルに対して、各酸化物換算で、
Mgの酸化物を1.00〜2.50モルと、
Mnおよび/またはCrの酸化物を0.01〜0.20モルと、
V、MoおよびWからなる群から選ばれる少なくとも1つの酸化物を0.03〜0.15モルと、
R1の酸化物(R1は、Y、およびHoからなる群から選ばれる少なくとも1つである)を0.20〜1.50モルと、
R2の酸化物(R2は、Eu、GdおよびTbからなる群から選ばれる少なくとも1つである)を0.50〜1.20モルと、
Siおよび/またはBの酸化物を0.50〜1.00モルと、を副成分として含有する誘電体磁器組成物であって、
前記R1の酸化物のR12O3換算での含有量をαモル、前記R2の酸化物のR22O3換算での含有量をβモルとすると、0.50≦β/(α+β)≦0.85である関係を満足し、
前記誘電体磁器組成物において、A(Aは、BaおよびCaから選ばれる少なくとも1つである)の含有量と、B(Bは、TiおよびZrから選ばれる少なくとも1つである)の含有量とが、1.000≦A/B≦1.006である関係を満足することを特徴とする誘電体磁器組成物。 - 前記R2がGdまたはTbである請求項1に記載の誘電体磁器組成物。
- 前記R2がTbである請求項2に記載の誘電体磁器組成物。
- 請求項1〜3のいずれかに記載の誘電体磁器組成物から構成される誘電体層と、電極とを有するセラミック電子部品。
- 前記誘電体層の厚みが1.0μm以下となることを特徴とする請求項4に記載のセラミック電子部品。
- 前記誘電体層の誘電体粒子の平均粒子径が0.1〜0.3μmであることを特徴とする請求項4または5に記載のセラミック電子部品。
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TW200927698A (en) * | 2007-09-28 | 2009-07-01 | Tdk Corp | Dielectric ceramic composition and electronic device |
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