JP2009007209A - 誘電体磁器及びそれを用いた積層セラミックコンデンサ - Google Patents
誘電体磁器及びそれを用いた積層セラミックコンデンサ Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 23
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 28
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 3
- 239000003989 dielectric material Substances 0.000 claims 1
- 239000002075 main ingredient Substances 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 17
- 239000010949 copper Substances 0.000 description 16
- 239000002994 raw material Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- 238000010304 firing Methods 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910008290 Li—B Inorganic materials 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920005822 acrylic binder Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000007650 screen-printing 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】CaxZrO3+aMn+bLi+cB+dSiで表され、CaxZrO3(但し、1.00≦x≦1.10)100molに対して、0.5≦a≦4.0mol、6.0≦(b+c+d)≦15.0molを含有し、0.15≦(b/(c+d))≦0.55、0.20≦(d/c)≦3.30であることを特徴とする誘電体磁器である。また、それを用いた積層セラミックコンデンサである。
【選択図】なし
Description
このような要求を満たす誘電体磁器組成物の発明が公知であり(特許文献1及び2参照)、これらの発明には、誘電体磁器組成物を積層セラミックコンデンサに用いることが示されている。
(1)CaxZrO3+aMn+bLi+cB+dSiで表され、
CaxZrO3(但し、1.00≦x≦1.10)100molに対して、
0.5≦a≦4.0mol、
6.0≦(b+c+d)≦15.0molを含有し、
0.15≦(b/(c+d))≦0.55、
0.20≦(d/c)≦3.30
であることを特徴とする誘電体磁器である。
(2)前記CaxZrO3のCaの一部をSrで置換したことを特徴とする前記(1)の誘電体磁器である。
(3)前記CaxZrO3のZrの一部をTiで置換したことを特徴とする前記(1)又は(2)の誘電体磁器である。
(4)さらに、Mg及び/又はAlを含有することを特徴とする前記(1)〜(3)のいずれか一項の誘電体磁器である。
(5)複数の誘電体磁器層と、前記誘電体磁器層間に形成されたCu若しくはCu合金からなる内部電極と、前記内部電極に電気的に接続された外部電極とを備えた積層セラミックコンデンサにおいて、前記誘電体磁器層が、前記(1)〜(4)のいずれか一項の誘電体磁器で構成されていることを特徴とする積層セラミックコンデンサである。
また、Cu内部電極を用いるために、寿命を低下させないようにLi及びBの含有量を抑えた状態でも、CaZrO3系誘電体磁器が1000℃以下で緻密化するCa/Zr比やLi−B−Si組成比の条件を見出した。
また、誘電特性等を任意に設計するために、Mn、Li、B及びSiと共に、Mg、Al等の他の元素を追加することも可能である。
原料としてCaCO3、ZrO2、さらに、必要に応じて、SrCO3、TiO2等を準備し、これらの原料を、所定の組成が得られるように秤量する。その後、これらの原料を湿式混合し、乾燥した後、800〜1200℃にて仮焼し、CaxZrO3を得る。
上記のように合成したCaxZrO3に対して、Mn原料(酸化物、炭酸塩等)、Li原料(Li2CO3等)、B原料(B2O3等)、Si原料(SiO2等)、さらに、必要に応じて、Mg原料(MgO)、Al原料(Al2O3)等を所定組成が得られるように秤量する。その後、これらの原料を湿式混合し、乾燥することで、誘電体粉末を得る。
上記のようにして得た誘電体粉末にPVBバインダ(又はアクリルバインダ)、可塑剤、溶媒となる有機溶剤を適宜添加してスラリーを作製し、所定の厚み(5〜50μm)のグリーンシートを作製する。グリーンシートに内部電極用Cuペーストを印刷し、積層・圧着後、所定の形状に切り出す。その後、(Cuが酸化されない)不活性雰囲気下、300〜600℃で脱バインダ処理を行い、還元雰囲気下、900〜1050℃で1〜5時間、焼成を行う。得られた焼結体に端子電極としてCu外電ペーストを塗布した後、N2雰囲気で焼き付ける。
原料としてCaCO3、ZrO2を準備する。これらの原料を秤量し、表1のようにCa/Zr比を0.98〜1.12の範囲で変化させた。その後、これらの原料をボールミルにて湿式混合し、乾燥した後、1000℃にて仮焼し、CaxZrO3(0.98≦x≦1.12)を得た。
上記のCaxZrO3(以下、「CaZrO3」と省略)に対して、MnCO3、Li2CO3、B2O3、SiO2を秤量し、表1のように、CaZrO3100molに対して、Mn含有量を、0〜5.0molの範囲で変化させ、Li/(B+Si)比を0.37、Si/B比を0.61で一定とし、Li+B+Siのトータル含有量を3.0〜18.0molの範囲で変化させた。その後、これらの原料をボールミルにて湿式混合し、乾燥することで、誘電体粉末を得た。
上記の誘電体粉末にPVBバインダ、可塑剤、溶媒となる有機溶剤を適宜添加してスラリーを作製し、ダイ・コーターにて12μm厚みのグリーンシートを作製した。グリーンシートにスクリーン印刷法にて内部電極用Cuペーストを印刷し、電極枚数11層(層間 10層)に積層・圧着後、4.0mm×2.0mmに切り出した。その後、不活性雰囲気下、300〜600℃で脱バインダ処理を行い、還元雰囲気下(窒素−水素混合ガス:水素比率1〜3%)、980℃、2hrで焼成を行った。その後、端子電極としてCuペーストを塗布し、N2雰囲気で焼き付けた。
以上のような工程で、積層セラミックコンデンサ(試料番号101〜114)を作製した。
焼結性:980℃で焼成した時の吸水率が0.1%以下を◎、その他を×とした。
信頼性:HALT試験(条件:30V/um,150℃)においてMTTFが100hr以上のものを◎、それ未満を×とした。
試料番号101〜114について、誘電体の組成とコンデンサの特性の評価を表1に示す。
Ca/Zr比が1.00のCaZrO3100molに対して、Mn含有量を0.5又は4.0molとし、Li+B+Siのトータル含有量を6.0又は15.0molとし、Li/(B+Si)比、Si/B比を表2のように変化させて混合したこと以外は、実施例1と同様にして誘電体粉末を得た。その後、実施例1と同様に、積層セラミックコンデンサ(試料番号201〜217)を作製し、特性について評価をした。
試料番号201〜217について、誘電体の組成とコンデンサの特性の評価を表2に示す。
Ca/Zr比が1.05のCaZrO3100molに対して、Mnを2.0mol、Li+B+Siのトータル含有量を12.0mol、Li/(B+Si)比を0.37、Si/B比を0.61で一定(Liを3.24mol、Bを5.45mol、Siを3.31mol)とし、さらに、それぞれ、Mg(MgO)を1.0mol、Mg(MgO)を2.0mol、Al(Al2O3)を0.5mol混合したこと以外は、実施例1と同様にして誘電体粉末を得た。その後、実施例1と同様に、積層セラミックコンデンサ(試料番号301〜303)を作製し、特性について評価をした。
また、CaZrO3のCaの一部をSrで置換した(Ca0.9Sr0.1)ZrO3又はZrの一部をTiで置換したCa(Zr0.9Ti0.1)O3を用い、(Ca+Sr)/Zr比又はCa/(Zr+Ti)比(A/B比)が1.05の(Ca0.9Sr0.1)ZrO3又はCa(Zr0.9Ti0.1)O3100molに対して、Mnを2.0mol、Li+B+Siのトータル含有量を12.0mol、Li/(B+Si)比を0.37、Si/B比を0.61で一定(Liを3.24mol、Bを5.45mol、Siを3.31mol)としたこと以外は、実施例1と同様にして誘電体粉末を得た。その後、実施例1と同様に、積層セラミックコンデンサ(試料番号304、305)を作製し、特性について評価をした。
Claims (5)
- CaxZrO3+aMn+bLi+cB+dSiで表され、
CaxZrO3(但し、1.00≦x≦1.10)100molに対して、
0.5≦a≦4.0mol、
6.0≦(b+c+d)≦15.0molを含有し、
0.15≦(b/(c+d))≦0.55、
0.20≦(d/c)≦3.30
であることを特徴とする誘電体磁器。 - 前記CaxZrO3のCaの一部をSrで置換したことを特徴とする請求項1に記載の誘電体磁器。
- 前記CaxZrO3のZrの一部をTiで置換したことを特徴とする請求項1又は2に記載の誘電体磁器。
- さらに、Mg及び/又はAlを含有することを特徴とする請求項1〜3のいずれか一項に記載の誘電体磁器。
- 複数の誘電体磁器層と、前記誘電体磁器層間に形成されたCu若しくはCu合金からなる内部電極と、前記内部電極に電気的に接続された外部電極とを備えた積層セラミックコンデンサにおいて、前記誘電体磁器層が、請求項1〜4のいずれか一項に記載の誘電体磁器で構成されていることを特徴とする積層セラミックコンデンサ。
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