JP4095586B2 - 積層型セラミックコンデンサおよびその製造方法 - Google Patents
積層型セラミックコンデンサおよびその製造方法 Download PDFInfo
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- JP4095586B2 JP4095586B2 JP2004190912A JP2004190912A JP4095586B2 JP 4095586 B2 JP4095586 B2 JP 4095586B2 JP 2004190912 A JP2004190912 A JP 2004190912A JP 2004190912 A JP2004190912 A JP 2004190912A JP 4095586 B2 JP4095586 B2 JP 4095586B2
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- rare earth
- earth element
- ceramic capacitor
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- 239000003985 ceramic capacitor Substances 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 73
- 238000009792 diffusion process Methods 0.000 claims description 45
- 239000002245 particle Substances 0.000 claims description 44
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 17
- 229910002113 barium titanate Inorganic materials 0.000 claims description 17
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052788 barium Inorganic materials 0.000 claims description 9
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Description
前記誘電体層が、チタン酸バリウムを含む主成分と、MgO、CaO、BaO、およびSrOのグループから選択される少なくとも1種からなる第1副成分と、酸化シリコンを主成分として含有する第2副成分と、V2O5、MoO3およびWO3のグループから選択される少なくとも1種からなる第3副成分と、Sc、Er、Tm、YbおよびLuのグループから選択される少なくとも1種の第1の希土類元素(R1)の酸化物からなる第4副成分と、CaZrO3、またはCaOとZrO2の混合体(CaO+ZrO2)からなる第5副成分と、Y、Dy、Ho、Tb、GdおよびEuのグループから選択される少なくとも1種の第2の希土類元素(R2)の酸化物からなる第6副成分と、を有し、
チタン酸バリウムを含む主成分100モルに対する、
第1副成分の含有量(モル)をy1、
第2副成分の含有量(モル)をy2、
第3副成分の含有量(モル)をy3、
第4副成分の含有量(モル)をy4、および
第5副成分の含有量(モル)をy5とした場合、
第6副成分の含有量(モル)をy6とした場合、
y1の値が、0.1〜3.0モルの範囲内にあり、
y2の値が、2〜10モルの範囲内にあり、
y3の値が、0.01〜0.5モルの範囲内にあり、
y4の値が、0.5〜7モル(但し、このモル数はR1単独での比率である)の範囲内にあり、
y5の値が、5モル以下(零を含まない)の範囲内にあり、
y6の値が、2〜9モル(但し、このモル数はR2単独での比率である)の範囲内にあり、
前記誘電体層を構成する結晶粒子に第1の希土類元素(R1)および第2の希土類元素(R2)がそれぞれ拡散されており、平均粒径の結晶粒子において、第1の希土類元素(R1)の結晶粒子表面からの拡散層深さd1が結晶粒子の径Dに対して占める割合をX1(%)とし、第2の希土類元素(R2)の結晶粒子表面からの拡散層深さd2が結晶粒子の径Dに対して占める割合をX2(%)とした場合、第2の希土類元素(R2)の拡散層深さd2が第1の希土類元素(R1)の拡散層深さd1よりも深部に及んでおり、X1=10〜35%、かつX2>X1(d2>d1と同義)の関係が成立してなるように構成される。
第1副成分の含有量(モル)をy1、
第2副成分の含有量(モル)をy2、
第3副成分の含有量(モル)をy3、
第4副成分の含有量(モル)をy4、および
第5副成分の含有量(モル)をy5とした場合、
第6副成分の含有量(モル)をy6とした場合、
y1の値が、0.1〜3.0モルの範囲内にあり、
y2の値が、2〜10モルの範囲内にあり、
y3の値が、0.01〜0.5モルの範囲内にあり、
y4の値が、0.5〜7モル(但し、このモル数はR1単独での比率である)の範囲内にあり、
y5の値が、5モル以下(零を含まない)の範囲内にあり、
y6の値が、2〜9モル(但し、このモル数はR2単独での比率である)の範囲内にあり、
前記誘電体層を構成する結晶粒子に第1の希土類元素(R1)および第2の希土類元素(R2)がそれぞれ拡散されており、平均粒径の結晶粒子において、第1の希土類元素(R1)の結晶粒子表面からの拡散層深さd1が結晶粒子の径Dに対して占める割合をX1(%)とし、第2の希土類元素(R2)の結晶粒子表面からの拡散層深さd2が結晶粒子の径Dに対して占める割合をX2(%)とした場合、第2の希土類元素(R2)の拡散層深さd2が第1の希土類元素(R1)の拡散層深さd1よりも深部に及んでおり、X1=10〜35%、かつX2>X1(d2>d1と同義)の関係が成立してなるように構成されているので、EIA規格のX8R特性を満足することはもとより、加速試験における抵抗変化率が小さく(IR平均寿命が長く)、信頼性に優れる誘電体磁器組成物を得ることができる。
本発明の電子部品の好適な一例として積層型セラミックコンデンサを取りあげて、構成部材である誘電体磁器組成物とともに説明する。
本発明の電子部品の好適な一例である積層型セラミックコンデンサの概略構成について、図1〜図3を参照しつつ説明する。図1は、積層型セラミックコンデンサの一実施形態を示す斜視図であり、図2は、図1に示される積層型セラミックコンデンサのA−A線矢視断面図であり、図3は、積層構造の形成過程を分かりやすく説明するための斜視図である。
誘電体層7は、チタン酸バリウムを含む主成分と、MgO、CaO、BaOおよびSrOのグループから選択される少なくとも1種からなる第1副成分と、酸化シリコンを主成分として含有する第2副成分と、V2O5、MoO3およびWO3のグループから選択される少なくとも1種からなる第3副成分と、Sc、Er、Tm、YbおよびLuのグループから選択される少なくとも1種の第1の希土類元素(R1)の酸化物からなる第4副成分と、CaZrO3、またはCaOとZrO2の混合体(CaO+ZrO2)からなる第5副成分と、Y、Dy、Ho、Tb、GdおよびEuのグループから選択される少なくとも1種の第2の希土類元素(R2)の酸化物からなる第6副成分と、を有する誘電体磁器組成物の結晶粒子で構成された焼結体からなっている。
チタン酸バリウムを含む主成分100モルに対する、
第1副成分の含有量(モル)をy1、
第2副成分の含有量(モル)をy2、
第3副成分の含有量(モル)をy3、
第4副成分の含有量(モル)をy4、
第5副成分の含有量(モル)をy5、および
第6副成分の含有量(モル)をy6とした場合、
y1の値は、0.1〜3.0モル、好ましくは0.5〜2.5モルの範囲内にあり、
y2の値は、2〜10モル、好ましくは2〜5モルの範囲内にあり、
y3の値は、0.01〜0.5モル、好ましくは0.1〜0.4モルの範囲内にあり、
y4の値は、0.5〜7モル、好ましくは0.5〜5モルの範囲内にあり、
y5の値は、5モル以下(零を含まない)、好ましくは0.5〜3モルの範囲内にあり、
y6の値は、2〜9モル、好ましくは2〜8モルの範囲内にあるように構成される。
なお、第4副成分の上記モル量および第6副成分の上記モル量は、それぞれ、第1の希土類元素(R1)の酸化物の酸化物のモル比ではなく、R1単独のモル量および第2の希土類元素(R2)の酸化物の酸化物のモル比ではなく、R2単独のモル量である。すなわち、例えば、第4副成分として、Ybの酸化物を用いた場合、第4副成分のモル量が1モルであることは、Yb2O3のモル量が1モルなのではなく、Ybのモル量が1モルであることを意味する。つまり、Yb2O3を1モル含有していれば、Ybは2モル含有となる。
内部電極層に含有される導電材は特に限定されるものではないが、上述のごとく誘電体層7の構成材料が耐還元性を有するために、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は、NiまたはNi合金が好ましい。Ni合金としては、Mn、Cr、Co、Al、W等のグループから選択される1種以上とNiとの合金が好ましい。Ni合金中のNi含有量は95重量%以上であることが好ましい。
外部電極に含有される導電材は特に限定されるものではないが、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。外部電極の厚さは用途に応じて適宜決定することができる。通常、その厚さは、10〜50μm程度とされる。
次に、本発明の積層型チップコンデンサの製造方法について説明する。
いわゆる印刷法を用いる場合、誘電体層形成用ペーストおよび内部電極層形成用ペーストが、ポリエチレンテレフタレート等の支持体上に順次、積層印刷される。このとき、第1内部電極層11および第2の内部電極層15は、それぞれ図2や図3に示されるように、誘電体層形成用ペーストの外枠に対して所定の形態が得られるように印刷される。誘電体層と内部電極層とが順次積層印刷された後、このものは所定形状に切断されチップ化され、しかる後、支持体から剥離されてチップ状積層体(素子本体の原型)が形成される。
また、いわゆるシート法を用いる場合、誘電体層形成用ペーストを用いて誘電体のグリーンシートが複数枚、形成される。それらのグリーンシートの上に内部電極層形成用ペーストが塗設され、図3に示されるようなシート体73,78が形成される。これらは順次積層され、所定の加熱・加圧操作を経た後、所定形状に切断されてチップ状積層体(素子本体の原型)が形成される。
誘電体層形成用ペーストとしては、誘電体原料と有機ビヒクルとを混練分散したものが使用される。
内部電極層形成用ペーストは、上述の各種導電性金属や合金と、上記有機ビヒクルとを混練分散して調製される。
上記のようにして作製されたチップ状積層体は、焼成される前に、脱バインダ処理が施されることが好ましい。この脱バインダ処理の条件は、使用した材料等を考慮して適宜設定することができ、例えば、内部電極層の導電材にNiやNi合金等の卑金属を用いる場合、下記の条件で行うことが特に好ましい。
昇温速度 :5〜300℃/時間、特に10〜100℃/時間
保持温度 :180〜400℃、特に200〜300℃
温度保持時間:0.5〜24時間、特に5〜20時間
雰囲気 :空気中
本発明におけるチップ状積層体の焼成時の雰囲気は、内部電極層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。導電材として、NiやNi合金等の卑金属を用いる場合、焼成雰囲気中の酸素分圧は、10-9〜10-4Paとすることが好ましい。酸素分圧が前記10-9Pa未満であると、内部電極層の導電材が異常焼結を起こし、内部電極層が途切れてしまうことがある。また、酸素分圧が10-4Paを超えると、内部電極が酸化してしまう傾向がある。
還元雰囲気で焼成した場合、焼成後の積層体にはアニールを施すことが好ましい。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の加速寿命を著しく長くすることができる。
上記のように作製したチップ状積層体(素子本体の原型)の対向する両端面側に外部電極形成用ペーストを印刷あるいは転写する。その後、焼成して、外部電極を形成する。また、ディッピングにより塗布後、焼成して、形成することもできる。
外部電極形成用ペーストとしては、導電材としてPd、Ag、Au、Cu、Pt、Rh、Ru、Ir等の金属の少なくとも1種、あるいは、これらの合金が使用され、上記の内部電極層用ペーストと同様にして調製される。
(実施例1)
誘電体材料を作製するための出発原料として、それぞれの平均粒径が0.1〜1.0μmに含まれる主成分原料(BaTiO3)、および第1副成分〜第7副成分の原料を用意した。
第2副成分の原料として(Ba0.6Ca0.4)SiO3を用い、
第3副成分の原料としてV2O5を用い、
第4副成分(R1)の原料としてYb2O3を用い、
第5副成分の原料としてCaZrO3を用い、
第6副成分(R2)の原料としてY2O3を用い、
第7副成分の原料として、MnCO3を用いた。
なお、第2副成分の原料である(Ba0.6Ca0.4)SiO3は、BaCO3、CaCO3およびSiO2をボールミルに入れて16時間湿式混合した後、これを乾燥し、1150℃で空気中で焼成し、さらに、ボールミルに入れて100時間湿式粉砕することにより製造した。
次いで、平均粒径0.4μmのNi粒子100重量部と、有機ビヒクル(エチルセルロース8重量部をブチルカルビトール92重量部に溶解させたもの)40重量部と、ブチルカルビトール10重量部とを3本ロールにより混練してペースト化し、内部電極層用のペーストを得た。
作製された各積層型セラミックコンデンサのサンプルについて、(1)容量温度特性、および(2)平均寿命を評価した。
コンデンササンプルに対し、−55〜150℃の温度範囲で最も容量温度特性が悪くなる150℃の温度環境下での静電容量の変化率(%)を測定することにより評価した。
静電容量の測定にはLCRメータを用い、周波数1kHz、入力信号レベル1Vrmsの条件下で測定した。測定結果に対しては、X8R特性(−55〜150℃、ΔC=±15%以内)を満足するか否かで評価した。満足するものを「○」、満足しないものを「×」表示した。
コンデンササンプルに対し、200℃の温度条件下で、10.0V/μmの直流電圧を印加する加速試験状態で、抵抗が1桁変化するまでの時間(hr)を測定した。測定対象のサンプル個数は10個とし、各サンプルに対し、抵抗が1桁変化するまでの時間(hr)の平均値を求め、この値を平均寿命とした。
なお、第1の希土類元素(R1)の拡散層深さd1および第2の希土類元素(R2)の拡散層深さd2は、上記した要領で透過型電子顕微鏡でR1およびR2の分布を測定することにより求めた。表1に記載されているR1拡散領域X1(%)およびR2拡散領域X2(%)の値は、それぞれ、平均粒径Dの結晶粒子におけるR1の拡散層深さd1の割合(d1/D×100)、およびR2の拡散層深さd2の割合(d2/D×100)を示している。
2…素子本体
7…誘電体層
11,15…外部電極
23,28…内部電極層
Claims (7)
- 誘電体層と内部電極層が交互に積層された積層体の構造を備える積層型セラミックコンデンサであって、
前記誘電体層が、
チタン酸バリウムを含む主成分と、
MgO、CaO、BaO、およびSrOのグループから選択される少なくとも1種からなる第1副成分と、
酸化シリコンを主成分として含有する第2副成分と、
V2O5、MoO3およびWO3のグループから選択される少なくとも1種からなる第3副成分と、
Sc、Er、Tm、YbおよびLuのグループから選択される少なくとも1種の第1の希土類元素(R1)の酸化物からなる第4副成分と、
CaZrO3、またはCaOとZrO2の混合体(CaO+ZrO2)からなる第5副成分と、
Y、Dy、Ho、Tb、GdおよびEuのグループから選択される少なくとも1種の第2の希土類元素(R2)の酸化物からなる第6副成分と、を有し、
チタン酸バリウムを含む主成分100モルに対する、
第1副成分の含有量(モル)をy1、
第2副成分の含有量(モル)をy2、
第3副成分の含有量(モル)をy3、
第4副成分の含有量(モル)をy4、および
第5副成分の含有量(モル)をy5とした場合、
第6副成分の含有量(モル)をy6とした場合、
y1の値が、0.1〜3.0モルの範囲内にあり、
y2の値が、2〜10モルの範囲内にあり、
y3の値が、0.01〜0.5モルの範囲内にあり、
y4の値が、0.5〜7モル(但し、このモル数はR1単独での比率である)の範囲内にあり、
y5の値が、5モル以下(零を含まない)の範囲内にあり、
y6の値が、2〜9モル(但し、このモル数はR2単独での比率である)の範囲内にあり、
前記誘電体層を構成する結晶粒子に第1の希土類元素(R1)および第2の希土類元素(R2)がそれぞれ拡散されており、平均粒径の結晶粒子において、第1の希土類元素(R1)の結晶粒子表面からの拡散層深さd1が結晶粒子の径Dに対して占める割合をX1(%)とし、第2の希土類元素(R2)の結晶粒子表面からの拡散層深さd2が結晶粒子の径Dに対して占める割合をX2(%)とした場合、第2の希土類元素(R2)の拡散層深さd2が第1の希土類元素(R1)の拡散層深さd1よりも深部に及んでおり、
X1=10〜35%、かつX2>X1(d2>d1と同義)の関係が成立してなることを特徴とする積層型セラミックコンデンサ。 - 前記第1の希土類元素(R1)の拡散層深さd1が結晶粒子の径Dに対して占める割合であるX1(%)と、前記第2の希土類元素(R2)の拡散層深さd2が結晶粒子の径Dに対して占める割合であるX2(%)との関係において、X2とX1との差である(X2−X1)の値が少なくとも3%以上である請求項1に記載の積層型セラミックコンデンサ。
- 前記誘電体層を構成する結晶粒子の平均粒径が0.2〜0.55μmである請求項1または請求項2に記載の積層型セラミックコンデンサ。
- 前記誘電体層を構成する結晶粒子の平均粒径が0.2〜0.35μmである請求項1または請求項2に記載の積層型セラミックコンデンサ。
- 前記酸化シリコンを主成分として含有する第2副成分が、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)、Li2OおよびB2O3から選ばれる少なくとも1種の元素を含んでなる複合酸化物である請求項1ないし請求項4のいずれかに記載の積層型セラミックコンデンサ。
- 前記酸化シリコンを主成分として含有する第2副成分が、(Ba,Ca)xSiO2+x(ただし、x=0.7〜1.2)である請求項1ないし請求項5のいずれかに記載の積層型セラミックコンデンサ。
- 前記誘電体層の厚さが2〜7μmである請求項1ないし請求項6のいずれかに記載の積層型セラミックコンデンサ。
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CN102320826B (zh) * | 2011-05-31 | 2013-07-17 | 武汉理工大学 | 多壳层结构x8r电容器介电陶瓷及其制备方法 |
DE102012217168A1 (de) * | 2012-09-24 | 2014-04-17 | Siemens Aktiengesellschaft | Verfahren zum Herstellen eines Kondensators und Kondensator |
WO2014207900A1 (ja) * | 2013-06-28 | 2014-12-31 | Tdk株式会社 | 誘電体磁器組成物および積層セラミックコンデンサ |
CN105236944A (zh) * | 2015-09-15 | 2016-01-13 | 中国建材国际工程集团有限公司 | 钡钙硅系复合纳米陶瓷粉体及其制备方法 |
US10431388B2 (en) | 2015-12-08 | 2019-10-01 | Avx Corporation | Voltage tunable multilayer capacitor |
CN116313521A (zh) * | 2017-09-08 | 2023-06-23 | 京瓷Avx元器件公司 | 高压可调多层电容器 |
CN116666112A (zh) | 2017-10-02 | 2023-08-29 | 京瓷Avx元器件公司 | 高电容可调多层电容器和阵列 |
CN113196428B (zh) | 2018-12-26 | 2022-12-13 | 京瓷Avx元器件公司 | 用于控制电压可调多层电容器的***和方法 |
CN109678495B (zh) * | 2019-01-15 | 2021-09-07 | 陕西科技大学 | 一种BaTiO3-Sr2CoMoO6磁电复合陶瓷及其制备方法 |
KR20230078335A (ko) | 2021-11-26 | 2023-06-02 | 삼성전기주식회사 | 적층형 전자 부품 |
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CN1092391C (zh) * | 1994-10-19 | 2002-10-09 | Tdk株式会社 | 多层瓷介片状电容器 |
JP3282520B2 (ja) * | 1996-07-05 | 2002-05-13 | 株式会社村田製作所 | 積層セラミックコンデンサ |
JP3039409B2 (ja) * | 1997-01-08 | 2000-05-08 | 株式会社村田製作所 | 積層セラミックコンデンサ |
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EP1036777B1 (en) * | 1999-03-16 | 2003-06-04 | TDK Corporation | Composition of dielectric ceramics and producing method therefor |
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TWI274356B (en) | 2007-02-21 |
KR100723305B1 (ko) | 2007-05-30 |
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