JP5109872B2 - 積層セラミックコンデンサおよびその製造方法 - Google Patents
積層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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- JP5109872B2 JP5109872B2 JP2008217585A JP2008217585A JP5109872B2 JP 5109872 B2 JP5109872 B2 JP 5109872B2 JP 2008217585 A JP2008217585 A JP 2008217585A JP 2008217585 A JP2008217585 A JP 2008217585A JP 5109872 B2 JP5109872 B2 JP 5109872B2
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- dielectric ceramic
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- 239000003985 ceramic capacitor Substances 0.000 title claims description 39
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000000919 ceramic Substances 0.000 claims description 128
- 239000000843 powder Substances 0.000 claims description 34
- 239000003990 capacitor Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 238000010304 firing Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052689 Holmium Inorganic materials 0.000 claims description 4
- 229910052765 Lutetium Inorganic materials 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 229910052775 Thulium Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 238000010030 laminating Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000011575 calcium Substances 0.000 description 11
- 238000009826 distribution Methods 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 7
- 229910052744 lithium Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052916 barium silicate Inorganic materials 0.000 description 1
- HMOQPOVBDRFNIU-UHFFFAOYSA-N barium(2+);dioxido(oxo)silane Chemical compound [Ba+2].[O-][Si]([O-])=O HMOQPOVBDRFNIU-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
0.96≦m≦1.03、
0≦x≦0.2、
0.2≦a≦5.0、
0≦b≦2.0、
0.2≦c≦1.0、および
0.5≦d≦4.0
の各条件を満足する。
96≦m≦1.03、0≦x≦0.2、0.2≦a≦5.0、0≦b≦2.0、0.2≦c≦1.0、および0.5≦d≦4.0の各条件を満足するとき、寿命特性をさらに向上させることができる。
0.96≦m≦1.03、
0≦x≦0.2、
0.2≦a≦5.0、
0≦b≦2.0、
0.2≦c≦1.0、および
0.5≦d≦4.0
の各条件を満足するようにされることが好ましい。
実験例1では、グレインの粒度分布およびLi添加量が、寿命特性に与える影響を調べた。
まず、主成分の出発原料として、BaCO3およびTiO2を用いて、表1に示す平均粒子径(Rb)および標準偏差(σb)を有するBa1.007TiO3粉末を準備した。平均粒子径(Rb)および標準偏差(σb)は、FE−SEMにて観察し、300個の粒子から、平均円相当径として解析し、算出した。次に、副成分と混合するに先立って、出発原料のBa1.007TiO3粉末を秤量した後、水を媒体としてボールミルにより湿式混合し、凝集体を解砕した。
組成式:100Ba1.007TiO3+1.0DyO3/2+0.7MgO+0.3MnO+1.5SiO2+eLiO1/2
で表され、かつ上記組成式中の係数eが表1に示す「Li添加量e」となるように、上記Ba1.007TiO3粉末と配合し、水を媒体としてボールミルにより混合した。その後、蒸発乾燥により試料1〜18の各々に係る誘電体原料配合物を得た。なお、試料1〜9と試料10〜18とは、平均粒子径(Rb)および標準偏差(σb)ならびにLi添加量eの各々については互いに同じであるが、以下に進める積層セラミックコンデンサの作製工程において、セラミック層の厚みが異ならされた点で異なっている。
上記誘電体原料配合物に、ポリビニルブチラール系バインダおよびエタノールを加えて、ボールミルにより湿式混合し、セラミックスラリーを得た。このセラミックスラリーをリップコータによりシート成形し、セラミックグリーンシートを得た。このとき、後述するように、セラミックグリーンシートとして、焼成後の厚みが0.9μmとなるものと1.0μmとなるものとの2種類の厚みのものを作製した。
特性評価として、誘電率、誘電損失(DF)、容量温度特性、および高温負荷寿命特性を評価した。
実験例2は、寿命特性向上にとって、より好ましい組成範囲を規定するために実施したものである。
まず、主成分の出発原料として、BaCO3、CaCO3およびTiO2の各粉末を準備し、これら粉末を、表3に示されたmおよびxをそれぞれ有する(Ba1-xCax)mTiO3の組成になるように秤量し、次いで、熱処理し、表3に示す平均粒子径(Rb)および標準偏差(σb)を有する(Ba1-xCax)mTiO3粉末を得た。次に、副成分と混合するに先立って、出発原料の(Ba1-xCax)mTiO3粉末を秤量した後、水を媒体としてボールミルにより湿式混合し、凝集体を解砕した。
組成式:100(Ba1-xCax)mTiO3+aRO3/2+bMgO+cMO+dSiO2+eLiO1/2
で表され、かつ表3にそれぞれ示す、M成分およびR成分をそれぞれ用いながら、係数a、b、c、dおよびeを有する組成となるように、上記(Ba1-xCax)mTiO3粉末と配合し、水を媒体としてボールミルにより混合した。その後、蒸発乾燥により試料101〜128の各々に係る誘電体原料配合物を得た。
実験例1の場合と同様の操作を経て、各試料に係る積層セラミックコンデンサを得た。誘電体セラミック層の厚みは、0.8μmとした。
実験例1の場合と同様の特性評価およびセラミック微構造観察を行なった。その結果が表4に示されている。
組成式:100(Ba1-xCax)mTiO3+aRO3/2+bMgO+cMO+dSiO2+eLiO1/2において、
0.96≦m≦1.03、
0≦x≦0.2、
0.2≦a≦5.0、
0≦b≦2.0、
0.2≦c≦1.0、および
0.5≦d≦4.0
の各条件を満足しており、その結果、比誘電率が1500以上であり、温度特性がX5R特性を満足し、平均故障時間が150時間以上であって寿命特性がより向上している。
実験例3は、平均グレイン径について、より好ましい範囲を求めようとするものである。
表5に示す平均粒子径(Rb)および標準偏差(σb)を有するBaTiO3系粉末を用いたことを除いて、実験例1における試料1に係る誘電体原料配合物の場合と同様にして、試料201および202の各々に係る誘電体原料配合物を得た。
実験例1の場合と同様の操作を経て、各試料に係る積層セラミックコンデンサを得た。誘電体セラミック層の厚みは、0.9μmとした。
実験例1の場合と同様の特性評価およびセラミック微構造観察を行なった。特性評価の結果が表6に示されている。
2 誘電体セラミック層
3,4 内部電極
5 コンデンサ本体
6,7 外部電極
Claims (4)
- 積層された複数の誘電体セラミック層、および前記誘電体セラミック層間の特定の界面に沿って形成された複数の内部電極をもって構成される、コンデンサ本体と、
前記コンデンサ本体の外表面上の互いに異なる位置に形成され、かつ前記内部電極の特定のものに電気的に接続される、複数の外部電極と
を備え、
前記内部電極の積層方向に隣り合うものの間に位置する前記誘電体セラミック層の厚みは1μm未満であり、かつ、
前記誘電体セラミック層は、主成分がBaTiO3系である誘電体セラミックであって、副成分としてLiを含み、Li含有量e[モル部]が、主成分100モル部に対し、0.5≦e≦6.0であり、当該誘電体セラミックのグレインについて、グレイン径の平均値Rg[μm]が0.06<Rg<0.17であり、その標準偏差σg[μm]がσg<0.075である、誘電体セラミックからなる、
積層セラミックコンデンサ。 - 前記誘電体セラミックは、
組成式:100(Ba1-xCax)mTiO3+aRO3/2+bMgO+cMO+dSiO2+eLiO1/2 (m、a、b、c、dおよびeはモル比を示す。RはLa、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、LuおよびYから選ばれる少なくとも1種を含有する。Mは、MnおよびVの少なくとも一方を含有する。)で表され、かつ、
0.96≦m≦1.03、
0≦x≦0.2、
0.2≦a≦5.0、
0≦b≦2.0、
0.2≦c≦1.0、および
0.5≦d≦4.0
の各条件を満足する、請求項1に記載の積層セラミックコンデンサ。 - 前記誘電体セラミックは、グレイン径の平均値Rg[μm]が0.06<Rg<0.14であり、その標準偏差σg[μm]がσg<0.075である、請求項1または2に記載の積層セラミックコンデンサ。
- 焼成後に厚みが1μm未満の誘電体セラミック層となる複数のセラミックグリーンシートを用意する工程と、
前記セラミックグリーンシート上に、内部電極を形成する工程と、
複数の前記セラミックグリーンシートを積層することによって、生のコンデンサ本体を得る工程と、
前記生のコンデンサ本体を焼成することによって、焼結したコンデンサ本体を得る工程と、
前記内部電極と電気的に接続される外部電極を前記コンデンサ本体上に形成する工程と
を備え、
前記セラミックグリーンシートを用意する工程は、
BaTiO3系を主成分とするBaTiO3系セラミック粉末を用意する工程と、
Li化合物を含む副成分を用意する工程と、
前記BaTiO3系セラミック粉末に前記副成分を混合することによって、セラミック原料粉末を得る工程と、
前記セラミック原料粉末にバインダおよび有機溶剤を加えて混合することによって、セラミックスラリーを得る工程と、
前記セラミックスラリーをシート状に成形することによって、セラミックグリーンシートを得る工程と
を含み、
前記セラミック原料粉末において、Li含有量e[モル部]が、主成分100モル部に対し、0.5≦e≦6.0であり、
前記BaTiO3系セラミック粉末において、粒径の平均値Rb[μm]が0.06<Rb<0.17であり、その標準偏差σb[μm]がσb<0.065である、
積層セラミックコンデンサの製造方法。
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