JP4877367B2 - 誘電体セラミックおよび積層セラミックコンデンサ - Google Patents
誘電体セラミックおよび積層セラミックコンデンサ Download PDFInfo
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- JP4877367B2 JP4877367B2 JP2009171010A JP2009171010A JP4877367B2 JP 4877367 B2 JP4877367 B2 JP 4877367B2 JP 2009171010 A JP2009171010 A JP 2009171010A JP 2009171010 A JP2009171010 A JP 2009171010A JP 4877367 B2 JP4877367 B2 JP 4877367B2
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- 239000000919 ceramic Substances 0.000 title claims description 111
- 239000003985 ceramic capacitor Substances 0.000 title claims description 41
- 239000002245 particle Substances 0.000 claims description 28
- 229910052748 manganese Inorganic materials 0.000 claims description 26
- 229910052791 calcium Inorganic materials 0.000 claims description 20
- 229910052788 barium Inorganic materials 0.000 claims description 19
- 239000003990 capacitor Substances 0.000 claims description 12
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052691 Erbium Inorganic materials 0.000 claims description 5
- 229910052765 Lutetium Inorganic materials 0.000 claims description 5
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 229910052775 Thulium Inorganic materials 0.000 claims description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 5
- 229910052804 chromium Inorganic materials 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052689 Holmium 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
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 description 33
- 238000012360 testing method Methods 0.000 description 28
- 239000002994 raw material Substances 0.000 description 25
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- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
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- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
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- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 229910052789 astatine Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
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- 239000011258 core-shell material Substances 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Classifications
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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
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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Description
実験例1では、主成分が(Ba,R)(Ti,Mn)O3系であり、M領域の面積を変化させた誘電体セラミックについて評価した。
まず、主成分の出発原料として、微粒のBaCO3、TiO2、Y2O3およびMnCO3の各粉末を用意し、これらを(Ba0.99Y0.01)(Ti0.995Mn0.005)O3となるよう秤量し、水を媒体としてボールミルにより8時間混合した。その後、蒸発乾燥し、1100℃の温度で2時間仮焼することによって、主成分粉末を得た。
上記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を加えて、ボールミルにより16時間湿式混合することによって、セラミックスラリーを作製した。このボールミルによる湿式混合工程において、試料101、102、103、104、105、106および107について、それぞれ、使用する玉石の径を2mm、1.5mm、1mm、0.8mm、0.6mm、0.5mmおよび0.3mmと変えることによって、後の焼成工程によって得られる焼結状態の誘電体セラミックにおける主成分粒子中でのM(=V)が固溶した領域の面積割合、すなわち、「M領域の面積割合」を表1に示すように変化させた。
得られた積層セラミックコンデンサについて、誘電体セラミック層の断面上でセラミック構造を観察し、分析した。この観察・分析では、粒子が20個前後入る視野でSTEMモードによるEDX元素マッピング分析を行ない、粒子中の後添加された副成分であるV(=M)成分の固溶面積割合を算出し、視野中において、当該固溶面積割合の平均値を求めた。その結果が、表1の「M領域の面積割合」の欄に示されている。なお、上記マッピング分析において、プローブ径を2nmとし、加速電圧を200kVとした。
実験例2では、実験例1の場合と同様、主成分を(Ba,R)(Ti,Mn)O3系としながら、Mn量およびR量を変化させた誘電体セラミックについて評価した。
RとしてDyを用いながら、主成分粉末として、(Ba1−x/100Dyx/100)(Ti1−y/100Mny/100)O3の組成であって、(Ba,R)サイトにおけるRとしてのDyの含有比xおよび(Ti,Mn)サイトにおけるMnの含有比yが、それぞれ、表2の「x」および「y」の欄に示した値を有するように調整されたことを除いて、実験例1の場合と同様の要領で、誘電体セラミック原料粉末を得た。
上記誘電体セラミック原料粉末を用い、実験例1の場合と同様の要領で、各試料に係る積層セラミックコンデンサを作製した。なお、ボールミルによる湿式混合工程では、実験例1における試料102の場合と同様、径1.5mmの玉石を用いて、16時間混合した。
実験例1の場合と同様の要領で、セラミック構造分析を行なったところ、試料201〜210のいずれについても、「M領域の面積割合」が3.5%前後であった。
実験例3では、実験例1の場合と同様、主成分を(Ba,R)(Ti,Mn)O3系としながら、不純物の影響を評価した。
表3に示した不純物成分を、実験例1において得られた誘電体セラミック原料100モル部に対して、表3に示した含有量をもって加えたことを除いて、実験例1の場合と同様の要領で、誘電体セラミック原料粉末を得た。
上記誘電体セラミック原料粉末を用い、実験例1の場合と同様の要領で、各試料に係る積層セラミックコンデンサを作製した。なお、ボールミルによる湿式混合工程では、実験例1における試料102の場合と同様、径1.5mmの玉石を用いて、16時間混合した。
実験例1の場合と同様の要領で、セラミック構造分析を行なったところ、試料301〜310のいずれについても、「M領域の面積割合」が3.5%前後であった。
実験例4は、実験例1に対応するものである。実験例1では、主成分を(Ba,R)(Ti,Mn)O3系としたが、実験例4では、主成分を(Ba,Ca,R)(Ti,Mn)O3系とした。
まず、主成分の出発原料として、微粒のBaCO3、CaCO3、Gd2O3、TiO2およびMnCO3の各粉末を用意し、これらを(Ba0.98Ca0.01Gd0.01)(Ti0.995Mn0.005)O3となるよう秤量し、水を媒体としてボールミルにより8時間混合した。その後、蒸発乾燥し、1100℃の温度で2時間仮焼することによって、主成分粉末を得た。
上記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を加えて、ボールミルにより16時間湿式混合することによって、セラミックスラリーを作製した。このボールミルによる湿式混合工程において、試料401、402、403、404、405、406および407について、それぞれ、使用する玉石の径を2mm、1.5mm、1mm、0.8mm、0.6mm、0.5mmおよび0.3mmと変えることによって、後の焼成工程によって得られる焼結状態の誘電体セラミックにおける主成分粒子中での「M領域の面積割合」を表4に示すように変化させた。
得られた積層セラミックコンデンサについて、実験例1の場合と同様の要領で、「M領域の面積割合」を求めた。その結果が表4に示されている。
実験例5では、実験例4の場合と同様、主成分を(Ba,Ca,R)(Ti,Mn)O3系としながら、Ca量、R量およびMn量を変化させた誘電体セラミックについて評価した。
主成分粉末として、(Ba1−xーy/100Cax/100Hoy/100)(Ti1−z/100Mnz/100)O3の組成であって、(Ba,Ca,R)サイトにおけるCaの含有比xおよびRとしてのHoの含有比yが、それぞれ、表5の「x」および「y」の欄に示す値を有し、かつ(Ti,Mn)サイトにおけるMnの含有比zが表5の「z」の欄に示した値を有するように調整されたことを除いて、実験例4の場合と同様の要領で、誘電体セラミック原料粉末を得た。
上記誘電体セラミック原料粉末を用い、実験例4の場合と同様の要領で、各試料に係る積層セラミックコンデンサを作製した。なお、ボールミルによる湿式混合工程では、実験例4における試料402の場合と同様、径1.5mmの玉石を用いて、16時間混合した。
実験例4の場合と同様の要領で、セラミック構造分析を行なったところ、試料501〜513のいずれについても、「M領域の面積割合」が3.5%前後であった。
実験例6では、実験例4の場合と同様、主成分を(Ba,Ca,R)(Ti,Mn)O3系としながら、不純物の影響を評価した。実験例6は、前述した実験例3に対応している。
表6に示した不純物成分を、実験例4において得られた誘電体セラミック原料100モル部に対して、表6に示した含有量をもって加えたことを除いて、実験例4の場合と同様の要領で、誘電体セラミック原料粉末を得た。
上記誘電体セラミック原料粉末を用い、実験例4の場合と同様の要領で、各試料に係る積層セラミックコンデンサを作製した。なお、ボールミルによる湿式混合工程では、実験例4における試料402の場合と同様、径1.5mmの玉石を用いて、16時間混合した。
実験例4の場合と同様の要領で、セラミック構造分析を行なったところ、試料601〜610のいずれについても、「M領域の面積割合」が3.5%前後であった。
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
11 主成分粒子
12 Mが存在している領域(M領域)
Claims (5)
- 主成分が(Ba,R)(Ti,Mn)O3系または(Ba,Ca,R)(Ti,Mn)O3系(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)であり、
副成分として、M(Mは、Fe、Co、V、W、Cr、Mo、Cu、AlおよびMgから選ばれる少なくとも1種)と、Siとを含み、
各主成分粒子の断面上における、Mが存在している領域の面積割合が、平均値で10%以下である、
誘電体セラミック。 - Mnの含有比は、(Ti,Mn)サイト全体において、0.01〜1モル%である、請求項1に記載の誘電体セラミック。
- Rの含有比は、(Ba,R)サイトまたは(Ba,Ca,R)サイト全体において、0.01〜2モル%である、請求項1または2に記載の誘電体セラミック。
- Caの含有比は、(Ba,Ca,R)サイト全体において、15モル%以下である、請求項1ないし3のいずれかに記載の誘電体セラミック。
- 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、
前記誘電体セラミック層は、請求項1ないし4のいずれかに記載の誘電体セラミックからなる、
積層セラミックコンデンサ。
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