JP7476477B2 - セラミック原料粉末、積層セラミックコンデンサ、および積層セラミックコンデンサの製造方法 - Google Patents
セラミック原料粉末、積層セラミックコンデンサ、および積層セラミックコンデンサの製造方法 Download PDFInfo
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- JP7476477B2 JP7476477B2 JP2018232703A JP2018232703A JP7476477B2 JP 7476477 B2 JP7476477 B2 JP 7476477B2 JP 2018232703 A JP2018232703 A JP 2018232703A JP 2018232703 A JP2018232703 A JP 2018232703A JP 7476477 B2 JP7476477 B2 JP 7476477B2
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- 239000000919 ceramic Substances 0.000 title claims description 60
- 239000000843 powder Substances 0.000 title claims description 55
- 239000002994 raw material Substances 0.000 title claims description 54
- 239000003985 ceramic capacitor Substances 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 238000000034 method Methods 0.000 title description 24
- 239000002245 particle Substances 0.000 claims description 22
- 230000007423 decrease Effects 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 9
- 229910002113 barium titanate Inorganic materials 0.000 claims description 8
- 239000006104 solid solution Substances 0.000 claims description 6
- 230000005484 gravity Effects 0.000 claims description 5
- 239000000370 acceptor Substances 0.000 description 44
- 230000009471 action Effects 0.000 description 16
- 229910010293 ceramic material Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- 230000007547 defect Effects 0.000 description 7
- 238000009413 insulation Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
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- 239000011572 manganese Substances 0.000 description 6
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- 239000000463 material Substances 0.000 description 5
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- 239000011230 binding agent Substances 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 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
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- 238000010586 diagram Methods 0.000 description 3
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- 238000007254 oxidation reaction Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
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- 238000005245 sintering Methods 0.000 description 3
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- 229910052692 Dysprosium Inorganic materials 0.000 description 2
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- 229910052689 Holmium Inorganic materials 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
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- 230000006866 deterioration Effects 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 238000010438 heat treatment Methods 0.000 description 2
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- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
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- 239000010955 niobium Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
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- 239000011734 sodium Substances 0.000 description 2
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- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical compound N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- 239000013078 crystal Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 238000007646 gravure printing Methods 0.000 description 1
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- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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- 238000010405 reoxidation reaction Methods 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
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- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Description
図1は、実施形態に係る積層セラミックコンデンサ100の部分断面斜視図である。図1で例示するように、積層セラミックコンデンサ100は、略直方体形状を有する積層チップ10と、積層チップ10のいずれかの対向する2端面に設けられた外部電極20a,20bとを備える。なお、積層チップ10の当該2端面以外の4面のうち、積層方向の上面および下面以外の2面を側面と称する。外部電極20a,20bは、積層チップ10の積層方向の上面、下面および2側面に延在している。ただし、外部電極20a,20bは、互いに離間している。
・中心部:(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)<(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数) (1)
・外縁部:(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)>(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数) (2)
まず、一般式ABO3で表されるペロブスカイト構造を主相とし、上記式(1)および上記式(2)を満たすように、Bサイトにドナーとして機能する元素およびアクセプタとして機能する元素の両方が置換固溶したセラミック原料粉末を用意する。当該セラミック原料粉末の合成方法としては、従来種々の方法が知られており、例えば固相合成法、ゾル-ゲル合成法、水熱合成法等が知られている。例えば、BaTiO3のTiサイトにMoおよびMnを置換固溶させる場合には、BaTiO3の合成時に、BaCO3、TiO2およびMnCO3の混合分散粉にてMn固溶BaTiO3を作製したのち、Mo化合物を添加し、粒成長させればよい。例えば、セラミック原料粉末の平均粒子径は、誘電体層11の薄層化の観点から、好ましくは50~150nmである。
次に、得られたセラミック材料に、ポリビニルブチラール(PVB)樹脂等のバインダと、エタノール、トルエン等の有機溶剤と、可塑剤とを加えて湿式混合する。得られたスラリを使用して、例えばダイコータ法やドクターブレード法により、基材上に例えば厚み3μm~10μmの帯状の誘電体グリーンシートを塗工して乾燥させる。
このようにして得られた成型体を、250~500℃のN2雰囲気中で脱バインダ処理した後に、酸素分圧10-5~10-8atmの還元雰囲気中で1100~1300℃で10分~2時間焼成することで、成型体の各粒子が焼結する。このようにして、セラミック積層体が得られる。
その後、N2ガス雰囲気中で600℃~1000℃で再酸化処理を行う。この工程により、酸素欠陥濃度が減少する。
その後、外部電極20a,20bの下地層上に、めっき処理により、Cu,Ni,Sn等の金属コーティングを行う。以上の行程により、積層セラミックコンデンサ100が完成する。
11 誘電体層
12 内部電極層
13 カバー層
20a,20b 外部電極
100 積層セラミックコンデンサ
Claims (7)
- ペロブスカイト構造を主相とするセラミック原料粉末であって、
前記ペロブスカイト構造のBサイトに、4価よりも大きい価数を有することでドナーとして機能する元素および4価よりも小さい価数を有することでアクセプタとして機能する元素の両方が置換固溶し、
前記セラミック原料粉末の各粒子の幾何学的な重心では、(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)<(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数)の関係が成立し、
前記セラミック原料粉末の各粒子の外縁では、(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)>(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数)の関係が成立し、
(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)は、前記外縁から前記重心にかけて徐々にまたは段階的に低下する勾配を有することを特徴とするセラミック原料粉末。 - 前記ペロブスカイト構造の主相は、BaTiO3であることを特徴とする請求項1記載のセラミック原料粉末。
- 前記ドナーとして機能する元素は、Moであり、
前記アクセプタとして機能する元素は、Mnであることを特徴とする請求項1または2に記載のセラミック原料粉末。 - ペロブスカイト構造を主相とするセラミック原料粉末を含むグリーンシートを作成する工程と、
前記グリーンシートと、内部電極形成用導電ペーストと、を交互に積層することで積層体を形成する工程と、
前記積層体を焼成する工程と、を含み、
前記ペロブスカイト構造のBサイトには、4価よりも大きい価数を有することでドナーとして機能する元素および4価よりも小さい価数を有することでアクセプタとして機能する元素の両方が置換固溶され、
前記セラミック原料粉末の各粒子の幾何学的な重心では、(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)<(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数)の関係が成立し、
前記セラミック原料粉末の各粒子の外縁では、(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)>(アクセプタとして機能する元素の濃度)×(4-アクセプタとして機能する元素の価数)の関係が成立し、
(ドナーとして機能する元素の濃度)×(ドナーとして機能する元素の価数-4)は、前記外縁から前記重心にかけて徐々にまたは段階的に低下する勾配を有することを特徴とする積層セラミックコンデンサの製造方法。 - 前記ペロブスカイト構造の主相は、BaTiO3であることを特徴とする請求項4記載の積層セラミックコンデンサの製造方法。
- 前記ドナーとして機能する元素は、Moであり、
前記アクセプタとして機能する元素は、Mnであることを特徴とする請求項4または5に記載の積層セラミックコンデンサの製造方法。 - 複数の誘電体層と、
複数の内部電極層と、を備え、
前記複数の誘電体層と前記複数の内部電極層とは、交互に積層され、
前記複数の誘電体層は、請求項1~3のいずれか一項に記載のセラミック原料粉末を焼成することによって得られたものであ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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