JP2005154237A - 誘電体磁器組成物、その製造方法及び電子部品 - Google Patents
誘電体磁器組成物、その製造方法及び電子部品 Download PDFInfo
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- JP2005154237A JP2005154237A JP2003399008A JP2003399008A JP2005154237A JP 2005154237 A JP2005154237 A JP 2005154237A JP 2003399008 A JP2003399008 A JP 2003399008A JP 2003399008 A JP2003399008 A JP 2003399008A JP 2005154237 A JP2005154237 A JP 2005154237A
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Abstract
【解決手段】特定組成の誘電体酸化物を含む主成分と、V酸化物を含む第1副成分と、Al酸化物を含む第2副成分と、Mn酸化物を含む第3副成分と、特定の焼結助剤を含む第4副成分とが特定割合で特定割合で含有されている誘電体磁器組成物を製造する方法であって、少なくとも第3副成分の原料及び第4副成分の原料の一方又は双方を除いたその他の副成分の原料の少なくとも一部を、主成分の原料を得るために準備された出発原料と混合し、反応前原料を準備する工程と、準備された反応前原料を反応させて反応済み原料を得る工程と、得られた反応済み原料に、反応前原料を準備する際に除いた副成分の原料を混合し、誘電体磁器組成物原料を得る工程とを、有する誘電体磁器組成物の製造方法。
【選択図】 なし
Description
組成式{(Ca1−x Mex )O}m ・(Zr1−y Tiy )O2 で示され、該組成式中の元素名を示す記号Meが、Sr、MgおよびBaの少なくとも一つであり、該組成式中の組成モル比を示す記号m、xおよびyが、0.8≦m≦1.3、0≦x≦1.00、0≦y≦1.00の関係にある誘電体酸化物を含む主成分と、
V酸化物を含む第1副成分と、
Al酸化物を含む第2副成分と、
Mn酸化物を含む第3副成分と、
SiO2 を主成分とし、MO(ただし、Mは、Ba、Ca、SrおよびMgから選ばれる少なくとも1種の元素)、Li2 OおよびB2 O3 から選ばれる少なくとも1種を含む酸化物を含む第4副成分とを、有し、
主成分100モルに対する各副成分の比率が、
第1副成分:0モル<第1副成分<7モル(ただし、V酸化物をV2 O5 に換算した値)、
第2副成分:0モル<第2副成分<15モル(ただし、Al酸化物をAl2 O3 に換算した値)、
第3副成分:0モル<第3副成分<5モル(ただし、Mn酸化物のMn元素に換算した値)、
第4副成分:0モル<第4副成分<20モル(ただし、酸化物に換算した値)、である誘電体磁器組成物を製造する方法であって、
少なくとも第3副成分の原料及び第4副成分の原料の一方又は双方を除いたその他の副成分の原料の少なくとも一部を、主成分の原料を得るために準備された出発原料と混合し、反応前原料を準備する工程と、
準備された反応前原料を反応させて反応済み原料を得る工程と、
得られた反応済み原料に、反応前原料を準備する際に除いた副成分の原料を混合し、誘電体磁器組成物原料を得る工程とを、有する誘電体磁器組成物の製造方法が提供される。
本発明により得られる誘電体磁器組成物を構成する誘電体粒子は、1μm以下の平均結晶粒径を持つ。この平均結晶粒径は、たとえばコード法などにより算出される。本発明者らは、得られる誘電体磁器組成物を構成する誘電体粒子の平均結晶粒径を制御することにより、絶縁抵抗の加速寿命を向上させることができ、その結果、この誘電体磁器組成物を用いて製造された積層セラミックコンデンサなどの電子部品の信頼性を改善できることを見出した。
図1は本発明の一実施形態に係る積層セラミックコンデンサの断面図、
図2は実施例1での試料3における第1〜4副成分原料の前添加により製造された誘電体層(誘電体磁器組成物)の断面状態を示すSEM写真、
図3は実施例1での試料3における第1〜4副成分原料の後添加により製造された誘電体層(誘電体磁器組成物)の断面状態を示すSEM写真、である。
この誘電体磁器組成物は、
組成式{(Ca1−x Mex )O}m ・(Zr1−y Tiy )O2 で示される誘電体酸化物を含む主成分と、
少なくとも、
V酸化物を含む第1副成分と、
Al酸化物を含む第2副成分と、
Mn酸化物を含む第3副成分と、
SiO2 を主成分とし、MO(ただし、Mは、Ba、Ca、SrおよびMgから選ばれる少なくとも1種の元素)、Li2 OおよびB2 O3 から選ばれる少なくとも1種を含む酸化物を含む第4副成分とを、有する。
この際、酸素(O)量は、上記式の化学量論組成から若干偏倚してもよい。
第2副成分原料としては、Al酸化物及び/又は焼成によりAl酸化物になる化合物が用いられる。
第3副成分原料としては、Mn酸化物及び/又は焼成によりMn酸化物になる化合物が用いられる。
第4副成分原料としては、SiO2 、BaO、CaO、SrO、MgO、Li2 O、B2 O3 、及び/又は焼成によりこれらの酸化物になる化合物が用いられる。
本実施例では、以下に示す手順で積層セラミックコンデンサのサンプルを作製した。
まず、それぞれ平均粒径0.1〜1μmの、主成分原料を製造するための出発原料(SrCO3 、CaCO3 、TiO2 、ZrO2 )と、第1〜第4副成分原料を用意した。本実施例では、MnOの原料には炭酸塩(第3副成分:MnCO3 )を用い、他の原料には酸化物(第1副成分:V2 O5 、第2副成分:Al2 O3 、第4副成分:(Ba0.6 Ca0.4 )SiO3 (表では、BCGと記載してある))を用いた。なお、(Ba0.6 Ca0.4 )SiO3 は、BaCO3 ,CaCO3 およびSiO2 をボールミルにより16時間湿式混合し、乾燥後、1000〜1300℃で空気中で焼成し、さらに、ボールミルにより100時間湿式粉砕することにより製造した。
次いで、上記誘電体層用ペーストを用いてPETフィルム上に、厚さ6μmのグリーンシートを形成し、この上に内部電極層用ペーストを印刷したのち、PETフィルムからグリーンシートを剥離した。
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1MHz,入力信号レベル(測定電圧)1Vrmsの条件下で、静電容量および誘電損失(tanδ、単位は%)を測定した。tanδについては、いずれのサンプルも0.01%以下の値を示した。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(ε、単位はなし)を算出した。比誘電率εについては、いずれのサンプルも45以上と良好であった。比抵抗(ρ、単位はΩcm)は、絶縁抵抗計(アドバンテスト社製R8340A)を用いて、25℃においてDC50Vを、コンデンササンプルに60秒間印加した後に測定した。比抵抗ρについては、いずれのサンプルも1×1012Ωcm以上と良好であった。なお、これら比誘電率ε、比抵抗ρおよび誘電損失tanδのそれぞれの値は、コンデンサの試料数n=10個を用いて測定した値の平均値から求めた。
コンデンサのサンプルに対し、LCRメータを用いて、1MHz、1Vの電圧での静電容量を測定し、基準温度を20℃としたとき、20〜85℃の温度範囲内で、温度に対する静電容量変化率が−3000〜0ppm/℃を満足するかどうかを調べた。その結果、いずれの試料も満足できることが確認された。
コンデンサのサンプルに対し、200℃で60V/μmの直流電圧の印加状態に保持することにより、高温負荷寿命を測定した。この高温負荷寿命は、10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1に示す。評価として、高温負荷寿命は、誘電体層を薄層化する際に特に重要となるものであり、印加開始から抵抗が一桁落ちるまでの時間を寿命と定義した。
コンデンサのサンプルに対し、誘電体層を構成する誘電体粒子の平均結晶粒径をコード法により算出した。コード法とは、SEM写真から、誘電体粒子の平均結晶粒径を算出する方法である。本実施例では、誘電体粒子の形状を便宜的に球と仮定して粒径を算出する。具体的には、まず、誘電体層の微細構造を示すSEM写真を用い、このSEM写真上に任意の直線を引き、この線が隣接する誘電体粒子同士の間に存在する粒界と交錯する点(交点)の数を求める。次に、求められた交点数から単位長さ当たりの粒界との交点の数PLを計算する。次に、得られたPLの値を用いて、コード長さL3を算出する。コード長さL3は1/PLで求められる。次に、得られたL3の値に1.5を乗じたL3×1.5により、誘電体粒子の平均結晶粒径を算出した。なお、用いたSEM写真の視野は23μm×30μmとし、1サンプルにつき5〜6枚の写真を用いて、それぞれの粒径を算出し、これらの平均値を平均結晶粒径とした。結果を表1に示す。後述の実施例2〜3も同様にして求めた。
なお、参考のために、試料3の組成での前添加のSEM写真を図2に、後添加のSEM写真を図3に、それぞれ示した。図3に示すように、図2の場合と比較して、誘電体粒子が微細化されていることが確認できる。すなわち、第1〜4副成分の後添加による微細構造の違いを確認できる。
前添加成分と後添加成分とを表2に示すように変化させた以外は、実施例1と同様にして、コンデンササンプルを作製し、同様の特性を評価した。その結果、いずれのサンプルについても、tanδが0.01%以下、比誘電率εが45以上、比抵抗ρが1×1012Ωcm以上、と良好であった。静電容量の温度特性についても、上記温度に対する静電容量変化率−3000〜0ppm/℃を満足していた。平均結晶粒径及び高温負荷寿命については、表2に示す。
なお、本実施例でいう前添加成分とは、主成分原料を含む仮焼き済み原料を製造する際に、主成分原料を製造するための出発原料に対して添加される副成分原料のことである。後添加成分とは、主成分原料を含む仮焼き済み原料に対して添加される副成分原料のことである。
後添加成分としての第1〜4副成分の添加量を表3に示すように変化させた以外は、実施例1と同様にして、コンデンササンプルを作製し、同様の特性を評価した。その結果、いずれのサンプルについても、tanδが0.01%以下、比誘電率εが45以上、比抵抗ρが1×1012Ωcm以上、と良好であった。静電容量の温度特性についても、上記温度に対する静電容量変化率−3000〜0ppm/℃を満足していた。平均結晶粒径及び高温負荷寿命については、表3に示す。
なお、本実施例でいう後添加成分とは、主成分原料を含む仮焼き済み原料に対して添加される副成分原料のことである。
なお、表3において、後添加成分の添加量が0(ゼロ)モル%の副成分(具体的には、試料21の第1副成分、試料27の第2副成分、試料33の第3副成分、試料37の第4副成分)については、これを前添加しているかもしれない、との疑義を生じるが、本実施例では前添加もしていない。すなわち、表3において、添加量が0(ゼロ)モル%の副成分は最終組成にも含まれていないことを意味する。
10… コンデンサ素子本体
2… 誘電体層
3… 内部電極層
4… 外部電極
Claims (9)
- 組成式{(Ca1−x Mex )O}m ・(Zr1−y Tiy )O2 で示され、該組成式中の元素名を示す記号Meが、Sr、MgおよびBaの少なくとも一つであり、該組成式中の組成モル比を示す記号m、xおよびyが、0.8≦m≦1.3、0≦x≦1.00、0≦y≦1.00の関係にある誘電体酸化物を含む主成分と、
V酸化物を含む第1副成分と、
Al酸化物を含む第2副成分と、
Mn酸化物を含む第3副成分と、
SiO2 を主成分とし、MO(ただし、Mは、Ba、Ca、SrおよびMgから選ばれる少なくとも1種の元素)、Li2 OおよびB2 O3 から選ばれる少なくとも1種を含む酸化物を含む第4副成分とを、有し、
主成分100モルに対する各副成分の比率が、
第1副成分:0モル<第1副成分<7モル(ただし、V酸化物をV2 O5 に換算した値)、
第2副成分:0モル<第2副成分<15モル(ただし、Al酸化物をAl2 O3 に換算した値)、
第3副成分:0モル<第3副成分<5モル(ただし、Mn酸化物のMn元素に換算した値)、
第4副成分:0モル<第4副成分<20モル(ただし、酸化物に換算した値)、である誘電体磁器組成物を製造する方法であって、
少なくとも第3副成分の原料及び第4副成分の原料の一方又は双方を除いたその他の副成分の原料の少なくとも一部を、主成分の原料を得るために準備された出発原料と混合し、反応前原料を準備する工程と、
準備された反応前原料を反応させて反応済み原料を得る工程と、
得られた反応済み原料に、反応前原料を準備する際に除いた副成分の原料を混合し、誘電体磁器組成物原料を得る工程とを、有する
誘電体磁器組成物の製造方法。 - 組成式{(Ca1−x Mex )O}m ・(Zr1−y Tiy )O2 で示され、該組成式中の元素名を示す記号Meが、Sr、MgおよびBaの少なくとも一つであり、該組成式中の組成モル比を示す記号m、xおよびyが、0.8≦m≦1.3、0≦x≦1.00、0≦y≦1.00の関係にある誘電体酸化物を含む主成分と、
V酸化物を含む第1副成分と、
Al酸化物を含む第2副成分と、
Mn酸化物を含む第3副成分と、
SiO2 を主成分とし、MO(ただし、Mは、Ba、Ca、SrおよびMgから選ばれる少なくとも1種の元素)、Li2 OおよびB2 O3 から選ばれる少なくとも1種を含む酸化物を含む第4副成分とを、有し、
主成分100モルに対する各副成分の比率が、
第1副成分:0モル<第1副成分<7モル(ただし、V酸化物をV2 O5 に換算した値)、
第2副成分:0モル<第2副成分<15モル(ただし、Al酸化物をAl2 O3 に換算した値)、
第3副成分:0モル<第3副成分<5モル(ただし、Mn酸化物のMn元素に換算した値)、
第4副成分:0モル<第4副成分<20モル(ただし、酸化物に換算した値)、である誘電体磁器組成物を製造する方法であって、
少なくとも第3副成分の原料及び第4副成分の原料を除いたその他の副成分の原料の少なくとも一部を、主成分の原料を得るために準備された出発原料と混合し、反応前原料を準備する工程と、
準備された反応前原料を反応させて反応済み原料を得る工程と、
得られた反応済み原料に、反応前原料を準備する際に除いた副成分の原料を混合し、誘電体磁器組成物原料を得る工程とを、有する
誘電体磁器組成物の製造方法。 - 組成式{(Ca1−x Mex )O}m ・(Zr1−y Tiy )O2 で示され、該組成式中の元素名を示す記号Meが、Sr、MgおよびBaの少なくとも一つであり、該組成式中の組成モル比を示す記号m、xおよびyが、0.8≦m≦1.3、0≦x≦1.00、0≦y≦1.00の関係にある誘電体酸化物を含む主成分と、
V酸化物を含む第1副成分と、
Al酸化物を含む第2副成分と、
Mn酸化物を含む第3副成分と、
SiO2 を主成分とし、MO(ただし、Mは、Ba、Ca、SrおよびMgから選ばれる少なくとも1種の元素)、Li2 OおよびB2 O3 から選ばれる少なくとも1種を含む酸化物を含む第4副成分とを、有し、
主成分100モルに対する各副成分の比率が、
第1副成分:0モル<第1副成分<7モル(ただし、V酸化物をV2 O5 に換算した値)、
第2副成分:0モル<第2副成分<15モル(ただし、Al酸化物をAl2 O3 に換算した値)、
第3副成分:0モル<第3副成分<5モル(ただし、Mn酸化物のMn元素に換算した値)、
第4副成分:0モル<第4副成分<20モル(ただし、酸化物に換算した値)、である誘電体磁器組成物を製造する方法であって、
第1〜4副成分の各原料を除いて、主成分の原料を得るために準備された出発原料を混合し、反応前原料を準備する工程と、
準備された反応前原料を反応させて反応済み原料を得る工程と、
得られた反応済み原料に、第1〜4副成分の各原料を混合し、誘電体磁器組成物原料を得る工程とを、有する
誘電体磁器組成物の製造方法。 - 第4副成分が、組成式{(Baz ,Ca1−z )O}v SiO2 で示され、該組成式中の組成モル比を示す記号zおよびvが、0≦z≦1および0.5≦v≦4.0の関係にある複合酸化物を含む、請求項1〜3のいずれかに記載の誘電体磁器組成物の製造方法。
- 反応前原料を反応させる方法としては、固相法を用いる、請求項1〜4のいずれかに記載の誘電体磁器組成物の製造方法。
- 得られた誘電体磁器組成物原料を1000〜1400℃で焼成する工程を有する、請求項1〜5のいずれかに記載の誘電体磁器組成物の製造方法。
- 請求項1〜6のいずれかに記載の方法により得られる1μm以下の平均結晶粒径を持つ誘電体粒子を有する誘電体磁器組成物。
- 請求項7に記載の誘電体磁器組成物で構成してある誘電体層を有する電子部品。
- 請求項7に記載の誘電体磁器組成物で構成してある誘電体層と、卑金属を主成分とする内部電極層とが交互に積層してある素子本体を有する積層セラミックコンデンサ。
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KR101389042B1 (ko) | 2010-10-01 | 2014-04-23 | 다이요 유덴 가부시키가이샤 | 적층 세라믹 콘덴서 |
US8995110B2 (en) | 2010-10-01 | 2015-03-31 | Taiyo Yuden Co., Ltd. | Laminated ceramic capacitor |
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TWI267497B (en) | 2006-12-01 |
KR20050052403A (ko) | 2005-06-02 |
CN100344578C (zh) | 2007-10-24 |
CN1778766A (zh) | 2006-05-31 |
US20050128683A1 (en) | 2005-06-16 |
JP3908723B2 (ja) | 2007-04-25 |
TW200526538A (en) | 2005-08-16 |
KR100683545B1 (ko) | 2007-02-15 |
US7157396B2 (en) | 2007-01-02 |
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