JP7432391B2 - セラミック電子部品およびその製造方法 - Google Patents
セラミック電子部品およびその製造方法 Download PDFInfo
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- JP7432391B2 JP7432391B2 JP2020032929A JP2020032929A JP7432391B2 JP 7432391 B2 JP7432391 B2 JP 7432391B2 JP 2020032929 A JP2020032929 A JP 2020032929A JP 2020032929 A JP2020032929 A JP 2020032929A JP 7432391 B2 JP7432391 B2 JP 7432391B2
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- ceramic
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- 239000003990 capacitor Substances 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 29
- 230000007423 decrease Effects 0.000 claims description 15
- 238000010304 firing Methods 0.000 claims description 15
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical group [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 14
- 229910002113 barium titanate Inorganic materials 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 9
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- 238000003475 lamination Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
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- 238000002156 mixing Methods 0.000 claims description 2
- -1 or Lu Inorganic materials 0.000 claims description 2
- 238000005245 sintering Methods 0.000 description 55
- 238000000280 densification Methods 0.000 description 36
- 239000000463 material Substances 0.000 description 27
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- 239000000654 additive Substances 0.000 description 16
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- 239000011777 magnesium Substances 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
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- 229910052804 chromium Inorganic materials 0.000 description 3
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 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
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- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
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- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- AOWKSNWVBZGMTJ-UHFFFAOYSA-N calcium titanate Chemical compound [Ca+2].[O-][Ti]([O-])=O AOWKSNWVBZGMTJ-UHFFFAOYSA-N 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 1
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- 238000007646 gravure printing Methods 0.000 description 1
- KJZYNXUDTRRSPN-UHFFFAOYSA-N holmium atom Chemical compound [Ho] KJZYNXUDTRRSPN-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
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- 229910052744 lithium Inorganic materials 0.000 description 1
- OHSVLFRHMCKCQY-UHFFFAOYSA-N lutetium atom Chemical compound [Lu] OHSVLFRHMCKCQY-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
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- 238000005498 polishing Methods 0.000 description 1
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- 238000010405 reoxidation reaction Methods 0.000 description 1
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- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-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
- 238000003980 solgel method Methods 0.000 description 1
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- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- H01G4/00—Fixed capacitors; Processes of their manufacture
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- H01G4/018—Dielectrics
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- H01G4/08—Inorganic dielectrics
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- 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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- 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
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/462—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
- C04B35/465—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
- 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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- H01G4/30—Stacked capacitors
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
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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2は、図1のA-A線断面図である。図3は、図1のB-B線断面図である。図1~図3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。
まず、誘電体層11を形成するための誘電体材料を用意する。誘電体材料は、誘電体層11の主成分セラミックを含む。誘電体層11に含まれるAサイト元素およびBサイト元素は、通常はABO3の粒子の焼結体の形で誘電体層11に含まれる。例えば、BaTiO3は、ペロブスカイト構造を有する正方晶化合物であって、高い誘電率を示す。このBaTiO3は、一般的に、二酸化チタンなどのチタン原料と炭酸バリウムなどのバリウム原料とを反応させてチタン酸バリウムを合成することで得ることができる。誘電体層11の主成分セラミックの合成方法としては、従来種々の方法が知られており、例えば固相法、ゾル-ゲル法、水熱法等が知られている。本実施形態においては、これらのいずれも採用することができる。
次に、原料粉末作製工程で得られた誘電体材料に、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。得られたスラリーを使用して、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0.8μm以下の帯状の誘電体グリーンシート51を塗工して乾燥させる。
このようにして得られたセラミック積層体を、N2雰囲気で脱バインダ処理した後に外部電極20a,20bの下地となるNiペーストをディップ法で塗布し、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。このようにして、積層セラミックコンデンサ100が得られる。
その後、N2ガス雰囲気中で600℃~1000℃で再酸化処理を行ってもよい。
その後、めっき処理により、外部電極20a,20bに、Cu,Ni,Sn等の金属コーティングを行ってもよい。
チタン酸バリウム粉末に対して添加物を添加し、ボールミルで十分に湿式混合粉砕して誘電体材料を得た。チタン酸バリウム粉末に対して添加物を添加し、ボールミルで十分に湿式混合粉砕してマージン材料を得た。チタン酸バリウム粉末に対して添加物を添加し、ボールミルで十分に湿式混合粉砕してカバー材料を得た。
比較例1では、(サイドマージン16における第1希土類元素のイオン半径)/(容量部14における第1希土類元素のイオン半径)が1となるように、誘電体材料およびマージン材料にHoを添加した。その他の条件は、実施例1と同様とした。
比較例2では、マージン材料に希土類を添加しなかった。その他の条件は、実施例1と同様とした。
実施例および比較例1,2のサンプルについて、サイドマージン16の積層方向中央部分の相対密度を、気孔が含まれていない場合を100%と仮定して測定した。測定方法は、チップ中央部を断面研磨した後、SEM観察を行い、視野内のサイドマージン面積とポア面積を測定しその比率を相対密度とした。相対密度は、以下の式で表すことができる。画像処理ソフトとしては、ImageJを用いた。
ポア総面積/サイドマージン面積
実施例および比較例1,2に対して、温度125℃の環境下で8Vの電圧を印加し、投入個数100個のうちの50%が故障するまでの時間を測定した。上記の条件下で1mA以上の電流が流れた場合に「故障」と判定した。
実施例および比較例1,2に対して、温度=85℃、相対湿度85%の環境下で4Vを印加した状態で17時間保持し、その後に取り出して絶縁抵抗計で直流抵抗を計測し、1MΩ以下となったサンプルを不良としてカウントした。
11 誘電体層
12 内部電極層
13 カバー層
14 容量部
15 エンドマージン
16 サイドマージン
17 逆パターン層
20a,20b 外部電極
51 誘電体グリーンシート
52 第1パターン
53 第2パターン
54 カバーシート
100 積層セラミックコンデンサ
Claims (10)
- セラミックを主成分とする誘電体層と、内部電極層と、が交互に積層され、略直方体形状を有し、積層された複数の前記内部電極層が交互に対向する2端面に露出するように形成された積層構造を備え、
前記積層構造において積層された複数の前記内部電極層が前記2端面以外の2側面に延びた端部を覆うように設けられたサイドマージンに添加された希土類元素のうち最大配合量の希土類元素のイオン半径は、異なる端面に露出する内部電極層同士が対向する容量部に添加された希土類元素のうち最大配合量の希土類元素のイオン半径よりも小さく、
(前記容量部の最大配合量の希土類元素のイオン半径):(前記サイドマージンの最大配合量の希土類元素のイオン半径)は、「1」:「0.987以下」であることを特徴とするセラミック電子部品。 - (前記容量部の最大配合量の希土類元素のイオン半径):(前記サイドマージンの最大配合量の希土類元素のイオン半径)は、「1」:「0.96以下」であることを特徴とする請求項1に記載のセラミック電子部品。
- 前記サイドマージンにおいて、最大配合量の希土類元素の存在量を、Bサイト元素の存在量との比で0.001以上、0.05以下とすることを特徴とする請求項1または請求項2に記載のセラミック電子部品。
- 前記サイドマージンにおける最大配合量の希土類元素は、Er、YbまたはLuであり、前記容量部における最大配合量の希土類元素は、DyまたはHoであることを特徴とする請求項1から請求項3のいずれか一項に記載のセラミック電子部品。
- 前記サイドマージンにおける最大配合量の希土類元素は、Tb、Dy、Ho、Y、Er、YbまたはLuであり、前記容量部における最大配合量の希土類元素は、Euであることを特徴とする請求項1から請求項3のいずれか一項に記載のセラミック電子部品。
- 前記誘電体層の主成分セラミックは、チタン酸バリウムであることを特徴とする請求項1から請求項5のいずれか一項に記載のセラミック電子部品。
- 前記積層構造の積層方向の上面および下面の少なくとも一方に設けられたカバー層を備え、
前記カバー層に添加された希土類元素のうち最大配合量の希土類元素のイオン半径は、前記容量部に添加された希土類元素のうち最大配合量の希土類元素のイオン半径よりも小さいことを特徴とする請求項1から請求項6のいずれか一項に記載のセラミック電子部品。 - 前記容量部の最大配合量の希土類元素は、前記容量部の内側での濃度が高く、前記容量部と前記サイドマージンとの境界付近では前記容量部から前記サイドマージンに向かって濃度が徐々に低下し、前記サイドマージンの外側に向かって濃度がさらに低下し、
前記サイドマージンの最大配合量の希土類元素は、前記サイドマージンの内側での濃度が高く、前記サイドマージンと前記容量部との境界付近では前記サイドマージンから前記容量部に向かって濃度が徐々に低下し、前記容量部の内側に向かって濃度がさらに低下することを特徴とする請求項1から請求項7のいずれか一項に記載のセラミック電子部品。 - 前記サイドマージンにおける最大配合量の希土類元素はYであり、前記容量部における最大配合量の希土類元素はDyであることを特徴とする請求項1から請求項8のいずれか一項に記載のセラミック電子部品。
- セラミックを主成分とする粒子を有するシートと金属導電ペーストのパターンとが、前記金属導電ペーストが対向する2端面に露出するように交互に積層された積層部分と、前記積層部分の側面に配置されたサイドマージン領域と、を含むセラミック積層体を準備する工程と、
前記セラミック積層体を焼成する工程と、を含み、
前記サイドマージン領域に含まれる希土類元素のうち最大配合量の希土類元素のイオン半径は、前記積層部分に含まれる希土類元素のうち最大配合量の希土類元素のイオン半径よりも小さく、
(前記積層部分の最大配合量の希土類元素のイオン半径):(前記サイドマージン領域の最大配合量の希土類元素のイオン半径)は、「1」:「0.987以下」であることを特徴とするセラミック電子部品の製造方法。
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