JP6631854B2 - 誘電体磁器組成物、積層セラミックコンデンサ、及び積層セラミックコンデンサの製造方法 - Google Patents
誘電体磁器組成物、積層セラミックコンデンサ、及び積層セラミックコンデンサの製造方法 Download PDFInfo
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- JP6631854B2 JP6631854B2 JP2017554200A JP2017554200A JP6631854B2 JP 6631854 B2 JP6631854 B2 JP 6631854B2 JP 2017554200 A JP2017554200 A JP 2017554200A JP 2017554200 A JP2017554200 A JP 2017554200A JP 6631854 B2 JP6631854 B2 JP 6631854B2
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- 238000000034 method Methods 0.000 title claims description 60
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- 239000002002 slurry Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000010953 base metal Substances 0.000 claims description 9
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- 238000001354 calcination Methods 0.000 claims description 7
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- 229910052802 copper Inorganic materials 0.000 claims description 5
- -1 rare earth compound Chemical class 0.000 claims description 5
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- 229910052688 Gadolinium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 150000003623 transition metal compounds Chemical class 0.000 claims description 3
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- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 30
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- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 5
- 229910002113 barium titanate Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910018054 Ni-Cu Inorganic materials 0.000 description 1
- 229910018481 Ni—Cu Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910007605 Zn—ZnO Inorganic materials 0.000 description 1
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- 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
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- 238000001027 hydrothermal synthesis Methods 0.000 description 1
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- 229910052738 indium Inorganic materials 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
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- 150000003624 transition metals Chemical class 0.000 description 1
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- 238000004876 x-ray fluorescence Methods 0.000 description 1
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Description
上述したようにBサイトに固溶する揮発性元素を主成分粉末の合成時にTiの一部と置換する形態で予め含有させ、還元性雰囲気下で焼成処理を行うことにより揮発性元素が揮発し、これにより高温で長時間連続駆動しても絶縁性能の経時的劣化を抑制することができ、信頼性の向上を図ることができる。
ペロブスカイト型化合物のBサイト元素に対するAサイト元素の比(A/B比)は、化学量論比は1.000であるが、化学量論比に限定されるものではない。
セラミック素原料として、BaCO3、TiO2、ZnO、MgCO3を用意し、Ti100モル部に対するZn及びMgのモル部、及びTiに対するBaのモル比(以下、「Ba/Ti比」という。)が合成後に表1となるように、これらセラミック素原料を秤量した。そしてこれら秤量物をPSZボール及び純水と共にボールミルに投入し、十分に湿式で混合粉砕し、乾燥させた後、1050℃の温度で約2時間、大気雰囲気で仮焼し、これにより主成分粉末を作製した。
試料番号1〜19の各試料について、Zn(2)/Zn(1)値を求め、Znの揮発量を評価した。
(試料番号21〜25)
セラミック素原料として、BaCO3、TiO2、ZnOを用意し、Ti100モル部に対するZnのモル部、及びBa/Ti比が、合成後に表3となるように、これらセラミック素原料を秤量し、実施例1と同様の方法・手順で大気雰囲気下、900〜1100℃の温度で仮焼し、これにより主成分粉末を作製した。
セラミック素原料として、BaCO3、TiO2、及びZnOを用意し、Ti100モル部に対するZnのモル部、及びBa/Ti比が、合成後に表3となるように、これらセラミック素原料を秤量した。そしてこれら秤量物をPSZボール及び純水と共にボールミルに投入し、十分に湿式で混合粉砕し、乾燥させた後、1000℃の温度で約2時間、大気雰囲気で仮焼し、主成分粉末を得た。
試料番号21〜28の各試料について、Zn(2)/Zn(1)値を求め、Znの揮発量を評価した。尚、この実施例2では、主成分粉末合成後のZn含有量をZn(1)、熱処理後の主成分中のZn含有量をZn(2)で表示している。
セラミック素原料として、BaCO3、TiO2、ZrO2、ZnOを用意し、Ti及びZrの総計100モル部に対するZn及びZrのモル部、Ti及びZrの総計に対するBaのモル比(以下、「Ba/(Ti+Zr)比」という。)が、合成後に表4となるように、これらセラミック素原料を秤量した。そしてこれら秤量物をPSZボール及び純水と共にボールミルに投入し、十分に湿式で混合粉砕し、乾燥させた後、1050℃の温度で約2時間、大気雰囲気で仮焼し、これにより主成分粉末を作製した。
試料番号31〜33の各試料について、Zn(2)/Zn(1)値を求め、Znの揮発量を評価した。尚、この実施例3でも、合成後の主成分中のZn含有量をZn(1)、焼成後の主成分中のZn含有量をZn(2)で表示している。
2a〜2f 内部電極
6a〜6g 誘電体層
Claims (12)
- 主成分が、一般式ABO3で表されるペロブスカイト型化合物で形成されると共に、
前記ペロブスカイト型化合物は、少なくともTi及びBサイトに固溶する揮発性元素としてのZnを含有し、かつZrを含有してもよく、
前記Znの含有量が、前記Ti及び前記Zrの総計100モル部に対し、0モル部より大きくかつ0.2モル部以下であり、
前記Ti及び前記Zrの総計に対するAサイト元素の比率が、モル比換算で1.00以上1.04以下であることを特徴とする誘電体磁器組成物。 - 前記Aサイト元素は、Ba、Ca、及びSr中から選択された少なくとも1種以上を含むことを特徴とする請求項1記載の誘電体磁器組成物。
- 希土類元素、遷移金属元素、及びSiの中から選択された少なくとも1種以上が、副成分として含有されていることを特徴とする請求項1又は請求項2記載の誘電体磁器組成物。
- 前記希土類元素は、Gd、Dy、及びYの中から選択された少なくとも1種以上であることを特徴とする請求項3記載の誘電体磁器組成物。
- 前記遷移金属元素は、Mg、Al、Mn、Cu、Vの中から選択された少なくとも1種以上であることを特徴とする請求項3記載の誘電体磁器組成物。
- 誘電体層と内部電極とが交互に積層されたセラミック焼結体を有する積層セラミックコンデンサにおいて、
前記内部電極が、卑金属材料で形成されると共に、
前記誘電体層が、請求項1乃至請求項5のいずれかに記載の誘電体磁器組成物で形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。 - 少なくともTi化合物及び揮発性元素としてのZnを含有した化合物を含むセラミック素原料を準備し、Zr化合物を前記セラミック素原料に含ませることが可能な素原料準備工程と、
前記セラミック素原料を大気雰囲気で仮焼し、一般式ABO3で表されるペロブスカイト型化合物を合成し、前記Znが前記ペロブスカイト型化合物のBサイトに固溶した主成分粉末を作製する主成分粉末作製工程と、
前記主成分粉末からセラミックスラリーを作製するスラリー作製工程と、
前記セラミックスラリーに成形加工を施し、セラミックグリーンシートを作製するグリーンシート作製工程と、
卑金属材料を主成分とする導電性ペーストを使用し、前記セラミックグリーンシート上に所定パターンの導電膜を形成する導電膜形成工程と、
前記導電膜が形成されたセラミックグリーンシートを積層し、積層成形体を作製する成形体作製工程と、
前記積層成形体を還元性雰囲気で焼成し、主成分中の前記Znの含有量を前記Ti及び前記Zrの総計100モル部に対し0モル部より大きくかつ0.2モル部以下とし、前記Ti及び前記Zrの総計に対するAサイト元素の比率をモル比換算で1.00以上1.04以下としたセラミック焼結体を作製する焼成工程とを含んでい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。 - 前記主成分粉末中のZnに対する前記セラミック焼結体の主成分中のZnの比率がモル比換算で0.4以下であることを特徴とする請求項7記載の積層セラミックコンデンサの製造方法。
- 前記還元性雰囲気は、強還元性雰囲気であることを特徴とする請求項7又は請求項8記載の積層セラミックコンデンサの製造方法。
- 前記主成分粉末を還元性雰囲気下で熱処理する熱処理工程を含み、該熱処理工程は、前記焼成工程を実施する前に実施することを特徴とする請求項7又は請求項8記載の積層セラミックコンデンサの製造方法。
- 前記スラリー作製工程は、前記主成分粉末に副成分を添加し、スラリー化することを特徴とする請求項7乃至請求項10のいずれかに記載の積層セラミックコンデンサの製造方法。
- 前記副成分は、希土類化合物、遷移金属化合物、及びSi化合物のうちの少なくとも1種以上を含むことを特徴とする請求項11記載の積層セラミックコンデンサの製造方法。
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