JP4883110B2 - 積層セラミックコンデンサ - Google Patents
積層セラミックコンデンサ Download PDFInfo
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- JP4883110B2 JP4883110B2 JP2009041785A JP2009041785A JP4883110B2 JP 4883110 B2 JP4883110 B2 JP 4883110B2 JP 2009041785 A JP2009041785 A JP 2009041785A JP 2009041785 A JP2009041785 A JP 2009041785A JP 4883110 B2 JP4883110 B2 JP 4883110B2
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- dielectric ceramic
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- dielectric
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- 239000003985 ceramic capacitor Substances 0.000 title claims description 37
- 239000002245 particle Substances 0.000 claims description 128
- 239000000919 ceramic Substances 0.000 claims description 100
- 239000013078 crystal Substances 0.000 claims description 95
- 238000009826 distribution Methods 0.000 claims description 27
- 229910052712 strontium Inorganic materials 0.000 claims description 9
- 229910052735 hafnium Inorganic materials 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 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
- 229910052804 chromium Inorganic materials 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000000843 powder Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 14
- 238000009413 insulation Methods 0.000 description 13
- 239000002994 raw material Substances 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 10
- 239000003990 capacitor Substances 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 5
- 238000010292 electrical insulation Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- 239000011230 binding agent Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- 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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Description
(A)誘電体セラミック原料の作製
まず、主成分の出発原料として、BaCO3およびTiO2の各粉末を用意し、これら粉末を、BaTiO3の組成になるように秤量した後、ボールミルにより混合し、1150℃で熱処理し、BaTiO3粉末を得た。この粉末の平均粒径は0.15μmであり、Ba/Ti比は1.001であった。
上記誘電体セラミック原料粉末に、ポリビニルブチラール系バインダおよびエタノールなどの有機溶剤を加えて、ボールミルにより湿式混合し、セラミックスラリーを作製した。
各試料に係る積層セラミックコンデンサを断面研磨し、焼成温度よりも100℃低い温度を目安に、熱エッチング処理したものを電子顕微鏡で観察した。そして、この観察画像をもとに、200個以上の観察粒子について円相当径を求めた。このように求められた円相当径が、誘電体セラミック層の厚みの1/4(図3および図4に示した試料6および試料3では、0.2μm)以下のものを第2の結晶粒子と分類し、誘電体セラミック層の厚みの1/4よりも大きいものを第1の結晶粒子と分類し、第1および第2の結晶粒子の各々について、平均粒径を求めた。
得られた各試料に係る積層セラミックコンデンサにつき、誘電率および絶縁抵抗(log IR)を求めた。なお、誘電率は、温度25℃、1kHz、および0.5Vrmsの条件下で測定した。また、絶縁抵抗は、温度25℃において直流電圧6.3Vを180秒間印加した後に測定した。これらの結果が表2に示されている。
この発明に係る積層セラミックコンデンサの誘電体セラミック層を構成する誘電体セラミックの主成分であるABO3において、Aサイトは、Baを必ず含み、さらにBaの一部がCaおよびSrの少なくとも一方で置換されることがあり、Bサイトは、Tiを必ず含み、さらにTiの一部がZrおよびHfの少なくとも一方で置換されることがあるが、実験例2では、AサイトにおけるCaおよびSrの各置換量ならびにBサイトにおけるZrおよびHfの各置換量を変えて、電気特性を評価した。
まず、主成分の出発原料として、BaCO3、CaCO3、SrCO3、TiO2、ZrO2およびHfO2の各粉末を用意し、これら粉末を、表3に示すように秤量した後、ボールミルにより混合し、1100〜1200℃で熱処理し、BaTiO3系のABO3粉末を得た。この粉末の平均粒径は0.11〜0.17μmであった。
実験例1における試料6の場合と同様の操作を経て、試料に係る積層セラミックコンデンサを得た。
実験例1の場合と同様に実施した。その結果、試料101〜109のいずれについても、実験例1における試料6とほぼ同等の結果が得られた。すなわち、結晶粒子の粒度分布が少なくとも2つのピークを有し、第1の結晶粒子と第2の結晶粒子とのそれぞれが粒度分布のピークを持ち、第1の結晶粒子の面積比率が41〜69%の範囲内にあるという条件を満たしていた。
実験例1の場合と同様に実施した。その結果が表4に示されている。
実験例3では、誘電体セラミックの組成を組成式:[100AmBO3]+aRO3/2+bMO+cSiO2で表わしたとき、Rを、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種の間で変え、Mを、Mn、Ni、Co、Fe、Cr、Cu、Mg、Li、Al、Mo、WおよびVから選ばれる少なくとも1種の間で変え、さらに、m、a、bおよびcを種々に変えて、電気特性を評価した。
組成式:[100AmBO3]+aRO3/2+bMO+cSiO2において、表5に示すような組成が得られるように、出発原料粉末を用意し、これら粉末を秤量した後、ボールミルにより混合し、実験例1における試料6の場合と同様の操作を経て、上記組成式で表わされる組成の誘電体セラミック原料を得た。
実験例1における試料6の場合と同様の操作を経て、試料に係る積層セラミックコンデンサを得た。
実験例1の場合と同様に実施した。その結果、試料301〜317のいずれについても、実験例1における試料6とほぼ同等の結果が得られた。すなわち、結晶粒子の粒度分布が少なくとも2つのピークを有し、第1の結晶粒子と第2の結晶粒子とのそれぞれが粒度分布のピークを持ち、第1の結晶粒子の面積比率が41〜69%の範囲内にあるという条件を満たしていた。
実験例1の場合と同様に実施した。その結果が表6に示されている。
実験例4は、不純物の影響を評価したものである。すなわち、原料作製等、積層セラミックコンデンサの製造工程において、Sr、Zr、Hf、Zn、Na、Ag、Ni、B、Y、AlおよびPdの少なくとも1種が不純物として混入する可能性があり、これらが、結晶粒子内および結晶粒子間を占める結晶粒界に存在する可能性がある。また、積層セラミックコンデンサの焼成工程などにおいて、内部電極成分が結晶粒子内および結晶粒子間を占める結晶粒界に拡散し存在する可能性がある。
実験例2における試料101の組成に、表7に示す不純物を加えたことを除いて、実験例2の場合と同様の操作を経て、各試料に係る誘電体セラミック原料を得た。
実験例2における試料101の場合と同様の操作を経て、試料に係る積層セラミックコンデンサを得た。
実験例2の場合と同様に実施した。その結果、試料401〜409のいずれについても、実験例2における試料101とほぼ同等の結果が得られた。すなわち、結晶粒子の粒度分布が少なくとも2つのピークを有し、第1の結晶粒子と第2の結晶粒子とのそれぞれが粒度分布のピークを持ち、第1の結晶粒子の面積比率が41〜69%の範囲内にあるという条件を満たしていた。
実験例2の場合と同様に実施した。その結果が表8に示されている。
実験例5では、Si含有する焼結助剤として種々の組成のものを用い、焼結助剤の種類の違いによる影響を調査した。
実験例1における試料6の組成中の焼結助剤成分としてのSiに代えて、表9に示す成分の焼結助剤を用いたことを除いて、実験例1における試料6の場合と同様の操作を経て、各試料に係る誘電体セラミック原料を得た。
実験例1における試料6の場合と同様の操作を経て、試料に係る積層セラミックコンデンサを得た。
実験例1の場合と同様に実施した。その結果、試料501〜509のいずれについても、実験例1における試料6とほぼ同等の結果が得られた。すなわち、結晶粒子の粒度分布が少なくとも2つのピークを有し、第1の結晶粒子と第2の結晶粒子とのそれぞれが粒度分布のピークを持ち、第1の結晶粒子の面積比率が41〜69%の範囲内にあるという条件を満たしていた。
実験例1の場合と同様に実施した。その結果が表10に示されている。
2 誘電体セラミック層
3,4 内部電極
17 誘電体セラミック
18 第1の結晶粒子
19 第2の結晶粒子
P1,P2 ピーク
Claims (3)
- 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備え、
前記誘電体セラミック層は、ABO3(Aは、Baを必ず含み、さらにCaおよびSrの少なくとも一方を含むことがある。Bは、Tiを必ず含み、さらにZrおよびHfの少なくとも一方を含むことがある。)で表わされるペロブスカイト型化合物を主成分とし、副成分として、R(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種である。)、M(Mは、Mn、Ni、Co、Fe、Cr、Cu、Mg、Li、Al、Mo、WおよびVから選ばれる少なくとも1種である。)およびSiを含む、誘電体セラミックからなり、
前記誘電体セラミックに含まれる結晶粒子を、前記誘電体セラミック層の厚みの1/4より大きい粒径を有する第1の結晶粒子と、前記誘電体セラミック層の厚みの1/4以下の粒径を有する第2の結晶粒子とに分類したとき、前記第1の結晶粒子と前記第2の結晶粒子とのそれぞれが粒度分布のピークを持ち、前記誘電体セラミック層の断面上での前記第1の結晶粒子の面積比率が41〜69%である、
積層セラミックコンデンサ。 - 前記誘電体セラミックの主成分としてのABO3において、Aは、Baを78〜100モル%、Srを0〜2モル%、Caを0〜20モル%含み、Bは、Tiを96〜100モル%、Zrを0〜2モル%、Hfを0〜2モル%含む、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の副成分としてのR、MおよびSiの各濃度は、ABO3100モルに対して、それぞれ、元素として、0.1〜3.0モル、0.2〜5モルおよび0.1〜3.5モルの各範囲にあり、かつABO3におけるA/Bの比が0.96〜1.030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。
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