JP4561922B2 - 誘電体磁器組成物、電子部品およびこれらの製造方法 - Google Patents
誘電体磁器組成物、電子部品およびこれらの製造方法 Download PDFInfo
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- JP4561922B2 JP4561922B2 JP2009055284A JP2009055284A JP4561922B2 JP 4561922 B2 JP4561922 B2 JP 4561922B2 JP 2009055284 A JP2009055284 A JP 2009055284A JP 2009055284 A JP2009055284 A JP 2009055284A JP 4561922 B2 JP4561922 B2 JP 4561922B2
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- dielectric
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Description
「[(CaxSr1−x)O]m[(TiyZr1−y−zHfz)O2]で示される組成の誘電体酸化物を含む主成分と、
Mn酸化物および/またはAl酸化物を含む第1副成分と、
ガラス成分とを少なくとも含む誘電体磁器組成物であって、
前記主成分に含まれる式中の組成モル比を示す記号m、x、yおよびzが、
0.90≦m≦1.04
0.5≦x<1
0.01≦y≦0.10
0<z≦0.20の関係にあることを特徴とする誘電体磁器組成物」が開示されている。さらに、特許文献1の記載によれば、前記誘電体磁器組成物にはMn酸化物が添加されてもよく、その添加量は、主成分100モル%に対して、MnO2換算で0.2〜5モル%とされている。
かかる知見に基づき本発明者らは、下記発明を着想するに至った。
[1]〔(Ca1−xSrx)O〕m〔(Zr1−y−z−αTiyHfzMnα)O2〕 …(2)
(ただし、(2)式において、m、x、y、zおよびαは
0.991≦m≦1.010
0≦x≦1
0≦y≦0.1
0<z≦0.02
0.002<α≦0.05 を満たす)
で示される組成の誘電体酸化物を含む主成分と、
主成分100モル部に対して、
0.1〜0.5モル部のAl2O3、および
0.5〜5.0モル部のSiO2を含む誘電体磁器組成物。
〔(Ca1−xSrx)O〕m〔(Zr1−y−zTiyHfz)O2〕 …(1)
(ただし、(1)式において、m、x、yおよびzは
0.993≦m≦1.055
0≦x≦1
0≦y≦0.1
0<z≦0.02 を満たす)
第1混合粉末を1100〜1300℃で熱処理し、第1焼成物を得る第1熱処理工程;
得られた第1焼成物に、マンガン化合物を合計の組成が(2)式で表される誘電体酸化物の組成を満たす割合で準備し、かつ(2)式で表される誘電体酸化物100モル部に対し、
0.1〜0.5モル部のAl2O3、および
0.5〜5.0モル部のSiO2を準備し、これらを混合し、第2混合粉末を準備する工程;
〔(Ca1−xSrx)O〕m〔(Zr1−y−z−αTiyHfzMnα)O2〕 …(2)
(ただし、(2)式において、m、x、y、zおよびαは
0.991≦m≦1.010
0≦x≦1
0≦y≦0.1
0<z≦0.02
0.002<α≦0.05 を満たす)
第2混合粉末を1150〜1300℃で熱処理する第2熱処理工程を含む誘電体磁器組成物の製造方法。
図1に示すように、本発明の一実施形態に係る電子部品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。このコンデンサ素子本体10の両端部には、素子本体10の内部で交互に配置された内部電極層3と各々導通する一対の外部電極4が形成してある。コンデンサ素子本体10の形状に特に制限はないが、通常、直方体状とされる。また、その寸法にも特に制限はなく、用途に応じて適当な寸法とすればよいが、通常、(0.4〜5.6mm)×(0.2〜5.0mm)×(0.2〜1.9mm)程度である。
(誘電体磁器組成物)
誘電体層2は、本発明の誘電体磁器組成物を含有する。
本発明の誘電体磁器組成物は、
〔(Ca1−xSrx)O〕m〔(Zr1−y−z−αTiyHfzMnα)O2〕 …(2)
で示される組成の誘電体酸化物を含む主成分と、
Al2O3およびSiO2を含む。
0.991≦m≦1.010、好ましくは0.995≦m≦1.005
0≦x≦1、好ましくは0≦x≦0.5、
0≦y≦0.1、好ましくは0≦y≦0.05、
0<z≦0.02、好ましくは0<z≦0.01
0.002<α≦0.05、好ましくは0.005≦α≦0.03の関係にある。
本発明の誘電体磁器組成物は、
CaCO3、SrCO3、ZrO2、TiO2、HfO2を所定の比率で含有する第1混合粉末を1100〜1300℃で熱処理し、第1焼成物を得た後、第1焼成物に、マンガン化合物、Al2O3およびSiO2を所定の割合で混合し、第2混合粉末を得て、該第2混合粉末を1150〜1300℃で熱処理して得られる。
〔(Ca1−xSrx)O〕m〔(Zr1−y−zTiyHfz)O2〕 …(1)
ただし、(1)式において、m、x、yおよびzは
0.993≦m≦1.055、好ましくは、1.009≦m≦1.040、
0≦x≦1、好ましくは0≦x≦0.5、
0≦y≦0.1、好ましくは0≦y≦0.05、
0<z≦0.02、好ましくは0<z≦0.01 を満たす。
次いで得られた第1焼成物に、マンガン化合物、Al2O3およびSiO2を所定の割合で混合し、第2混合粉末を得る。
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の構成材料が耐還元性を有するため、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,Fe,Mg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。
外部電極4に含有される導電材は、特に限定されないが、通常、CuやCu合金あるいはNiやNi合金等を用いる。なお、AgやAg−Pd合金等も、もちろん使用可能である。なお、本実施形態では、安価なNi,Cuや、これらの合金を用いる。外部電極の厚さは用途等に応じて適宜決定されればよいが、通常、10〜50μm程度であることが好ましい。
本発明の誘電体磁器組成物を用いた積層セラミックコンデンサは、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。以下、製造方法について具体的に説明する。
誘電体層用ペーストは、誘電体原料と有機ビヒクルとを混練した有機系の塗料であってもよく、水系の塗料であってもよい。
内部電極用ペーストは、上述した各種導電性金属や合金からなる導電材料あるいは焼成後に上述した導電材料となる各種酸化物、有機金属化合物、レジネート等と、上述した有機ビヒクルとを混練して調製される。また、外部電極用ペーストも、この内部電極用ペーストと同様にして調製される。
脱バインダ処理は、通常の条件で行えばよいが、特に内部電極層の導電材としてNiやNi合金等の卑金属を用いる場合には、空気雰囲気において、昇温速度を5〜300℃/時間、より好ましくは10〜100℃/時間、保持温度を180〜400℃、より好ましくは200〜300℃、温度保持時間を0.5〜24時間、より好ましくは5〜20時間とする。
グリーンチップの焼成雰囲気は、内部電極層用ペースト中の導電材の種類に応じて適宜決定すればよいが、導電材としてNiやNi合金等の卑金属を用いる場合には、還元雰囲気とすることが好ましく、焼成雰囲気の酸素分圧を、好ましくは10−10〜1Paとし、より好ましくは10−7〜1Pa(10−12〜10−5atm)とする。焼成時の酸素分圧が低すぎると内部電極の導電材が異常焼結を起こして途切れてしまう傾向にあり、酸素分圧が高すぎると内部電極が酸化される傾向にある。
アニールは誘電体層を再酸化するための処理であり、これにより絶縁抵抗を増加させることができる。アニール雰囲気の酸素分圧は、好ましくは10−4Pa以上、より好ましくは1〜10−3Pa(10−5〜10−8atm)である。酸素分圧が低すぎると誘電体層2の再酸化が困難となる傾向にあり、酸素分圧が高すぎると内部電極層3が酸化される傾向にある。
コンデンサのサンプルに対し、基準温度25℃でデジタルLCRメータ(YHP社製4274A)にて、周波数1kHz,入力信号レベル(測定電圧)1Vrmsの条件下で、静電容量を測定した。そして、得られた静電容量と、コンデンササンプルの電極寸法および電極間距離とから、比誘電率(単位なし)を算出した。
コンデンサのサンプルに対し、LCRメータを用いて、1kHz、1Vの電圧での静電容量を測定し、25℃での静電容量(C25)と、125℃での静電容量(C125)とから、下記式により静電容量の温度係数(τC)を算出した。結果を表2および表3に示す。
コンデンサのサンプルに対し、200℃で70V/μmの直流電圧の印加状態に保持し、絶縁抵抗(LogIR)が6以下になるまでの時間を、高温負荷寿命として測定した。この高温負荷寿命は、20個のコンデンササンプルについて行い、平均寿命時間を測定することにより評価した。結果を表2および表3に示す。
コンデンササンプルを切断し、その断面を研磨し、研磨面に化学エッチングまたは熱エッチング処理を施した後、断面を走査型電子顕微鏡で観察し、画像解析処理ソフトにて、誘電体層を構成する結晶グレインの平均粒径を算出した。結果を表2および表3に示す。
同じ組成のサンプル100個を外観観察し、クラック発生したサンプルの数をカウントした。結果を表2および表3に示す。
主成分組成および添加成分の添加量を表4に示し、結果を表5および表6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 (5)
- 〔(Ca1−xSrx)O〕m〔(Zr1−y−z−αTiyHfzMnα)O2〕 …(2)
(ただし、(2)式において、m、x、y、zおよびαは
0.991≦m≦1.010
0≦x≦1
0≦y≦0.1
0<z≦0.02
0.002<α≦0.05 を満たす)
で示される組成の誘電体酸化物を含む主成分と、
主成分100モル部に対して、
0.1〜0.5モル部のAl2O3、および
0.5〜5.0モル部のSiO2 (ガラス成分を除く)を含む誘電体磁器組成物。 - 請求項1に記載の誘電体磁器組成物を製造する方法であって、
CaCO3、SrCO3、ZrO2、TiO2、HfO2を合計の組成が(1)式を満たす割合で混合し、第1混合粉末を準備する工程;
〔(Ca1−xSrx)O〕m〔(Zr1−y−zTiyHfz)O2〕 …(1)
(ただし、(1)式において、m、x、yおよびzは
0.993≦m≦1.055
0≦x≦1
0≦y≦0.1
0<z≦0.02 を満たす)
第1混合粉末を1100〜1300℃で熱処理し、第1焼成物を得る第1熱処理工程;
得られた第1焼成物に、マンガン化合物を合計の組成が(2)式で表される誘電体酸化物の組成を満たす割合で準備し、かつ(2)式で表される誘電体酸化物100モル部に対し、
0.1〜0.5モル部のAl2O3、および
0.5〜5.0モル部のSiO2 (ガラス成分を除く)を準備し、これらを混合し、第2混合粉末を準備する工程;
〔(Ca1−xSrx)O〕m〔(Zr1−y−z−αTiyHfzMnα)O2〕 …(2)
(ただし、(2)式において、m、x、y、zおよびαは
0.991≦m≦1.010
0≦x≦1
0≦y≦0.1
0<z≦0.02
0.002<α≦0.05 を満たす)
第2混合粉末を1150〜1300℃で熱処理する第2熱処理工程を含む誘電体磁器組成物の製造方法。 - 誘電体層を有する電子部品であって、
前記誘電体層が、請求項1に記載の誘電体磁器組成物で構成してあることを特徴とする電子部品。 - 内部電極と誘電体層とが交互に積層してある電子部品であって、
前記誘電体層が、請求項1に記載の誘電体磁器組成物で構成してあることを特徴とする電子部品。 - 前記内部電極が少なくともニッケルを含有する請求項4に記載の電子部品。
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