JP7347926B2 - 積層セラミックコンデンサの製造方法及び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の製造方法及び積層セラミックコンデンサ Download PDFInfo
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- JP7347926B2 JP7347926B2 JP2018227053A JP2018227053A JP7347926B2 JP 7347926 B2 JP7347926 B2 JP 7347926B2 JP 2018227053 A JP2018227053 A JP 2018227053A JP 2018227053 A JP2018227053 A JP 2018227053A JP 7347926 B2 JP7347926 B2 JP 7347926B2
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- 239000003985 ceramic capacitor Substances 0.000 title claims description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 239000000919 ceramic Substances 0.000 claims description 81
- 239000000463 material Substances 0.000 claims description 44
- 229910052783 alkali metal Inorganic materials 0.000 claims description 32
- 150000001340 alkali metals Chemical class 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 16
- 238000010304 firing Methods 0.000 claims description 12
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- 238000003475 lamination Methods 0.000 claims description 9
- 229910007746 Zr—O Inorganic materials 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 229910002976 CaZrO3 Inorganic materials 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000010030 laminating Methods 0.000 claims description 2
- 239000010949 copper Substances 0.000 description 33
- 238000007747 plating Methods 0.000 description 18
- 238000010586 diagram Methods 0.000 description 17
- 229910010293 ceramic material Inorganic materials 0.000 description 16
- 239000002585 base Substances 0.000 description 14
- 230000008859 change Effects 0.000 description 13
- 239000011575 calcium Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004020 conductor Substances 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 9
- 239000000654 additive Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000996 additive effect Effects 0.000 description 6
- 229910001413 alkali metal ion Inorganic materials 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 230000005012 migration Effects 0.000 description 5
- 238000013508 migration Methods 0.000 description 5
- 239000011572 manganese Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 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 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 101100513612 Microdochium nivale MnCO gene Proteins 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 2
- 238000002042 time-of-flight secondary ion mass spectrometry Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-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
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 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
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000007598 dipping method Methods 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
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 230000012447 hatching Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 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
- 239000011265 semifinished product Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 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
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Description
まず、積層セラミックコンデンサについて説明する。図1は、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セラミック積層体10と、セラミック積層体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。ここで、略直方体形状とは、稜部にRがついている場合を含む。なお、セラミック積層体10の当該2端面以外の4面を側面と称する。外部電極20a,20bは、4つの側面に延在している。ただし、外部電極20a,20bは、4つの側面において互いに離間している。
まず、セラミック誘電体層11の主成分であるセラミック材料の粉末に、目的に応じて所定の添加化合物を添加する。セラミック材料としては、CaZrO3を用いることができる。添加化合物としては、Mg(マグネシウム),Mn(マンガン),V(バナジウム),Cr(クロム),希土類元素(Y(イットリウム),Sm(サマリウム),Eu(ユウロピウム),Gd(ガドリニウム),Tb(テルビウム),Dy(ジスプロシウム),Ho(ホロミウム),Er(エルビウム),Tm(ツリウム)およびYb(イッテルビウム))の酸化物、並びに、Co,Ni,Li(リチウム),B,Na(ナトリウム),K(カリウム)およびSiの酸化物もしくはガラスが挙げられる。例えば、まず、セラミック材料の粉末に添加化合物を含む化合物を混合して仮焼を行う。続いて、得られたセラミック材料の粒子を添加化合物とともに湿式混合し、乾燥および粉砕してセラミック材料の粉末を調製する。
次に、誘電体グリーンシートの表面に、内部電極層形成用導電ペーストをスクリーン印刷、グラビア印刷等により印刷することで、内部電極層12のパターンを配置する。内部電極層形成用導電ペーストは、内部電極層12の主成分金属の粉末と、共材と、バインダと、溶剤と、必要に応じてその他助剤とを含んでいる。共材、バインダ、溶剤、及びその他助剤は、アルカリ金属を含まない。共材としては、セラミック誘電体層11の主成分であるセラミック材料(CaZrO3)を用いることができる。主成分金属としては、Cuを用いることができる。
次に、外部電極形成用金属ペーストが塗布されたセラミック積層体を、例えば、H2が1.5体積%程度の還元雰囲気中において、900℃~1050℃程度の温度で2時間程度焼成する。それにより、セラミック誘電体層11および内部電極層12の焼成と、下地導体層21の焼き付けとを同時に行うことができ、積層セラミックコンデンサ100の半製品を得ることができる。
次に、下地導体層21上に、めっき処理により、第1めっき層22を形成する。さらに、第1めっき層22上に、めっき処理により、第2めっき層23を形成する。
図8に示すように、セラミック誘電体層11の主成分のセラミック材料として、CaZrO3を用いた。なお、Zrに対するCaのモル比率(Ca/Zr)を1.05とした。セラミック誘電体層11に、BN(3.5mol%)、SiO2(3.5mol%)、Li2CO3(1.75mol%)、およびMnCO3(3.5mol%)を添加材として添加した。なお、いずれの添加材の「mol%」も、主成分のCaZrO3を100mol%とした場合の数値である。内部電極層12の主成分として、Cuを用い、共材としてCaZrO3を10部含ませた。なお、内部電極層12は、アルカリ金属を含む焼結助剤及び添加材は含まない。外部電極20a,20bの下地導体層21の主成分としてCuを用い、共材としてCaZrO3を6部含ませた。焼成工程の焼成条件として、H2が1.5体積%程度の還元雰囲気、980℃の焼成温度とした。第1めっき層22には、Niを用いた。第2めっき層23には、Snを用いた。
比較例1~10では、内部電極層12に共材を含ませなかった。その他の条件は、実施例1~10とそれぞれ同様とした。
実施例1~5及び比較例1~5について、それぞれ図9(A)に示す電界強度の電圧を150℃で1000時間印加する前後の静電容量を測定し、静電容量変化率を求めた。図9(A)及び図9(B)に示すように、実施例1~5のいずれにおいても、容量変化率は0.0%であった。一方、比較例1及び2では、容量変化率が0.0%であるものの、比較例3~5では静電容量変化率が、4%を超えており、信頼性規格である3%未満を満足しなかった。
11 セラミック誘電体層
12 内部電極層
20a,20b 外部電極
21 下地導体層
22 第1めっき層
23 第2めっき層
100 積層セラミックコンデンサ
Claims (7)
- Ca、Zr、Oを主成分とし、アルカリ金属を含むグリーンシートと、Cuを主成分とし、Ca-Zr-O系の材料からなるセラミックの共材を含み、アルカリ金属を含まない内部電極層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積層工程と、
前記積層体を焼成することで、Ca、Zr、Oを主成分とし、アルカリ金属を含むセラミック誘電体層と、Cuを主成分とし、Ca-Zr-O系の材料からなりアルカリ金属を含まない共材を含む内部電極層と、が交互に積層されたセラミック積層体を得る焼成工程と、を含み、
前記セラミック誘電体層と前記内部電極層が交互に積層される位置において、前記セラミック誘電体層と前記内部電極層との積層方向に平行な断面を見た場合、前記セラミック誘電体層が前記内部電極層に接する位置から前記セラミック誘電体層側に1.2μmの範囲における前記アルカリ金属の濃度は、前記セラミック誘電体層のその他の範囲における前記アルカリ金属の濃度よりも低い、
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。 - 前記グリーンシートの主成分は、CaZrO3であり、
前記Ca-Zr-O系の材料は、CaZrO3である、
ことを特徴とする請求項1記載の積層セラミックコンデンサの製造方法。 - Ca、Zr、Oを主成分とし、アルカリ金属を含むセラミック誘電体層と、Cuを主成分とし、Ca-Zr-O系の材料からなりアルカリ金属を含まない共材を含む内部電極層と、が交互に積層された略直方体形状を有するセラミック積層体と、
前記セラミック積層体の端面に引き出された複数の前記内部電極層と接続する少なくとも2つの外部電極と、
を備え、
前記セラミック誘電体層と前記内部電極層が交互に積層される位置において、前記セラミック誘電体層と前記内部電極層との積層方向に平行な断面を見た場合、前記セラミック誘電体層が前記内部電極層に接する位置から前記セラミック誘電体層側に1.2μmの範囲における前記アルカリ金属の濃度は、前記セラミック誘電体層のその他の範囲における前記アルカリ金属の濃度よりも低い、
る積層セラミックコンデンサ。 - 前記アルカリ金属は、Liである、
請求項3記載の積層セラミックコンデンサ。 - 前記セラミック誘電体層は、B、Si、及びMnを含む、
請求項3または請求項4に記載の積層セラミックコンデンサ。 - 前記セラミック誘電体層の主成分はCaZrO3である、
請求項3から請求項5のいずれか一項記載の積層セラミックコンデンサ。 - 前記共材の主成分はCaZrO3である、
請求項3から請求項6のいずれか一項記載の積層セラミックコンデンサ。
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