JP5205545B1 - 積層セラミックコンデンサ及びその製造方法 - Google Patents
積層セラミックコンデンサ及びその製造方法 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002245 particle Substances 0.000 claims abstract description 96
- 238000010304 firing Methods 0.000 claims abstract description 21
- 230000001186 cumulative effect Effects 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 16
- 239000003989 dielectric material Substances 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 5
- 230000005684 electric field Effects 0.000 description 5
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 2
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- 230000007423 decrease Effects 0.000 description 2
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- 239000003960 organic solvent Substances 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
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- 238000005245 sintering Methods 0.000 description 2
- 230000005476 size effect Effects 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
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- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
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- 238000010191 image analysis Methods 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
【解決手段】誘電体層を構成する誘電体粒子の平均粒径ばらつきnd(累積存在率90%相当粒径D90を累積存在率10%相当粒径D10で除算した値(D90/D10))が4よりも小さい、積層セラミックコンデンサ。
【選択図】図1
Description
式(1)によれば、平均粒径ばらつきndが小さいほど誘電体粒子の粒径が均一であり、誘電体層12の表面が平坦であると評価できる。なお、粒径が均一であるほどndが1に近づく。
(1)誘電体原料粉末の調製
まず、誘電体の原料粉末として平均粒径が80〜280nmの高純度のBaTiO3粉末と、100molのBaTiO3に対し0.5molのHoO3/2、0.5molのSiO2、0.1molのMnCO3(焼成によりCO2が乖離してMnOとなる)、0.1molのV2O5、0.1molのZrO2、0〜0.04molのMgOの各化合物を秤量し誘電体の原料粉末として準備した。原料粉末の平均粒径は、チタン酸バリウムの粉末サンプルをSEM観察し、サンプル数500として、そのメジアン径をとることで求められる。そして、表1〜3に示す各試料の原料粉末を水で湿式混合し、乾燥、乾式粉砕して誘電体原料粉末を調製した。カバー層用の誘電体原料粉末も同様の組成化合物で準備した。
調製した誘電体原料粉末をポリビニルアセタール樹脂及び有機溶剤で湿式混合し、ドクターブレード法により1.0μm厚のセラミックグリーンシートを塗工して乾燥させた。カバー層用のセラミックカバーシートについては、厚みを10μmとした。誘電体層となるグリーンシート上にNi導電ペーストを所定パターンでスクリーン印刷することにより内部電極を配置した。電極パターンを配置したグリーンシートを101枚積層することで誘電体層の積層数nを100とした後、その積層体の上下に10μm厚のカバーシートを片側各々20枚ずつ圧着し、その後1.0×0.5mmにカットした。その後に外部電極となるNi導電ペーストを積層体の両側に塗布して乾燥させて、MLCC成型体の試料を得た。
MLCC成型体の試料をN2雰囲気中350℃で脱バインダした。その後、N2、H2、H2Oの混合ガス(酸素分圧が約1.0×10−11MPa)において1220〜1280℃で10分〜2時間焼成した。焼成の温度及び時間は、目標とするグレイン径が得られるように適宜調整した。焼成後、N2雰囲気中1000℃で1時間、誘電体の酸化処理を行った。
(1)グレイン径の評価方法
MLCCの一部断面を研磨することにより抽出し、走査型電子顕微鏡(SEM)で誘電体層の断面を撮影した写真に基づいて誘電体粒子のグレイン径を測定した。ここでは、サンプリングした500個の誘電体粒子について最大長さDgsをSEM写真に基づく画像解析により測定し、それらの平均値をグレイン径Dgとして評価した。なお、SEM写真における粒界の境界線を明瞭に撮影するために、予め焼成工程と同じ雰囲気(N2、H2、H2Oの混合ガス)中で1180℃、5分の熱処理を行い、粒子界面の熱エッチングを施した。
走査型電子顕微鏡(SEM)による誘電体層の断面写真からサンプリングした500個以上の誘電体粒子のグレイン径のデータから求めた累積存在率特性(図3参照)に基づいて、上記式(1)を用いて平均粒径ばらつきndを演算した。なお、サンプリングについては500個以上とし、1枚の断面写真で500個以上ある場合はその中の誘電体粒子全部についてサンプリングし、500個に満たない場合は別の部分の断面写真からサンプリングして500個以上とする。
焼成後酸化処理を行ったMLCCを150℃の恒温槽内に1時間静置し、更に室温25℃で24時間静置して条件を揃えた後に、インピーダンスアナライザを用いて静電容量Cmを測定した。測定のための電圧印加条件を、1kHz、1.0Vrmsとした。測定された静電容量Cmから下記の式(2)を用いて比誘電率εを求めた。
ここで、ε0は真空の誘電率であり、n、S、tは、それぞれ、誘電体層の積層数、内部電極層の面積、誘電体層の1層の厚さである。
焼成後酸化処理を行ったMLCCを150℃の恒温槽内に1時間静置し条件を揃えた後に、引続き恒温槽内温度150℃、電界強度8.5V/μm(誘電体層厚が0.7μmに対しDC電圧6V)の環境下に置いた。MLCCのリーク電流が初期の100倍になるまでの時間の平均を加速寿命時間と定義し、その時間を基準に寿命特性を評価した。
以上の条件で作製したMLCCの誘電体層に対する評価結果を表1〜3を参照しながら説明する。
10 セラミック焼結体
11 積層体
12 誘電体層
13 内部電極層
15 カバー層
20 外部電極
Claims (5)
- 誘電体層と内部電極層とが交互に積層されてなる積層セラミックコンデンサであって、
前記誘電体層を構成する誘電体粒子の平均粒径ばらつきnd(累積存在率90%相当粒径D90を累積存在率10%相当粒径D10で除算した値(D90/D10))が4よりも小さく、
前記誘電体粒子の平均粒径が300nmよりも大きく1000nmよりも小さい、積層セラミックコンデンサ。 - 前記誘電体層の100molのBaTiO3に対して0.03mol以下のMgを含有する、請求項1に記載の積層セラミックコンデンサ。
- 前記誘電体層の100molのBaTiO3に対して0.01mol以上、0.03mol以下のMgを含有する、請求項2に記載の積層セラミックコンデンサ。
- 100molのBaTiO 3 に対して0.03mol以下のMgを含有する、誘電体原料粉末を調製する工程と、
前記誘電体層を構成する誘電体粒子の平均粒径ばらつきnd(累積存在率90%相当粒径D90を累積存在率10%相当粒径D10で除算した値(D90/D10))が4よりも小さく、かつ、前記誘電体粒子の平均粒径が300nmよりも大きく1000nmよりも小さくなるように前記誘電体原料粉末を焼成する工程と、を含む積層セラミックコンデンサの製造方法。 - 前記誘電体原料粉末の平均粒径が80nm以上、200nm以下である、請求項4に記載の積層セラミックコンデンサの製造方法。
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