JP4821357B2 - 電子部品、誘電体磁器組成物およびその製造方法 - Google Patents
電子部品、誘電体磁器組成物およびその製造方法 Download PDFInfo
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- JP4821357B2 JP4821357B2 JP2006037137A JP2006037137A JP4821357B2 JP 4821357 B2 JP4821357 B2 JP 4821357B2 JP 2006037137 A JP2006037137 A JP 2006037137A JP 2006037137 A JP2006037137 A JP 2006037137A JP 4821357 B2 JP4821357 B2 JP 4821357B2
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Description
チタン酸バリウムを含む主成分と、
MgOを含む第1副成分と、
SiO2系の焼結助剤を含む第2副成分と、
V2O5、MoO3 およびWO3 から選ばれる少なくとも1種を含む第3副成分と、
R1の酸化物(ただし、R1は、Y、Ho、Er、Tm、YbおよびLuから選ばれる少なくとも1種)を含む第4副成分と、
R2の酸化物(ただし、R2は、Dy、Tb、GdおよびEuから選ばれる少なくとも1種)を含む第5副成分と、
MnOおよびCr2 O3 の少なくとも1種を含む第6副成分とを有する誘電体磁器組成物であって、
前記主成分100モルに対する各副成分の比率が、
第1副成分:0.8〜2モル、
第2副成分:1.5〜5モル、
第3副成分:0.01〜0.1モル、
第4副成分:0.5〜2モル(ただし、第4副成分のモル数は、R1単独での比率)、
第5副成分:1.5〜4.5モル(ただし、第5副成分のモル数は、R2単独での比率)、
第6副成分:0.1〜0.2モルであり、
前記主成分100モルに対する第4副成分および第5副成分の合計モル数が、前記R1換算および前記R2換算で、2〜6モルであり、かつ、
主成分100モルに対する第4副成分および第5副成分の合計モル数に対する第5副成分の比率が、前記R1換算および前記R2換算で、0.5≦R2/(R1+R2)≦0.75の関係であることを特徴とする。
前記誘電体磁器組成物を製造する方法であって、
前記主成分の原料と、前記第1〜第6副成分の原料とを混合し、誘電体磁器組成物粉末を得る工程と、
前記誘電体磁器組成物粉末を焼成し、誘電体磁器組成物を得る工程と、を有し、前記主成分の原料として平均粒径が0.1〜0.3μmである原料を使用し、
焼成後の前記誘電体磁器組成物に含まれる誘電体粒子の平均結晶粒径が、前記主成分の原料の平均粒径の1.5倍以上2.0倍以下となるように焼成することを特徴とする。
図1に示すように、本発明の一実施形態に係る積層セラミックコンデンサ2は、誘電体層10および内部電極12が交互に積層された構成のコンデンサ素子4を有する。交互に積層される一方の内部電極層12は、コンデンサ素子4の第1端部4aの外側に形成してある外部電極6の内側に対して電気的に接続してある。また、交互に積層される他方の内部電極層12は、コンデンサ素子4の第2端部4bの外側に形成してある外部電極8の内側に対して電気的に接続してある。
誘電体層10は、本発明に係る誘電体磁器組成物を含有する。
本発明の誘電体磁器組成物は、チタン酸バリウムを含む主成分と、
MgOを含む第1副成分と、
SiO2系の焼結助剤を含む第2副成分と、
V2O5、MoO3 およびWO3 から選ばれる少なくとも1種を含む第3副成分と、
R1の酸化物(ただし、R1は、Y、Ho、Er、Tm、YbおよびLuから選ばれる少なくとも1種)を含む第4副成分と、
R2の酸化物(ただし、R2は、Dy、Tb、GdおよびEuから選ばれる少なくとも1種)を含む第5副成分と、
MnOおよびCr2 O3 の少なくとも1種を含む第6副成分とを有する。
第1副成分に含まれるMgOは、容量温度変化率を平坦化する効果を有する。主成分100モルに対する含有量は、0.8〜2モル、好ましくは、1〜1.5モルである。MgO以外の第1副成分としては、CaO、BaOおよびSrOから選ばれる少なくとも1種が含まれることが好ましい。これらの酸化物も、容量温度変化率を平坦化する効果を示す。第1副成分の含有量が少なすぎると、このような効果が得られなくなる傾向にあり、多すぎると、焼結性が悪くなり、比誘電率が低下する傾向にある。
内部電極層12に含有される導電材は特に限定されないが、誘電体層10の構成材料が耐還元性を有するため、卑金属を用いることができる。導電材として用いる卑金属としては、NiまたはNi合金が好ましい。Ni合金としては、Mn,Cr,CoおよびAlから選択される1種以上の元素とNiとの合金が好ましく、合金中のNi含有量は95重量%以上であることが好ましい。なお、NiまたはNi合金中には、P等の各種微量成分が0.1重量%程度以下含まれていてもよい。内部電極層12の厚さは用途等に応じて適宜決定すればよいが、通常、0.5〜5μm、特に0.5〜2.5μm程度であることが好ましい。
外部電極6,8に含有される導電材は特に限定されないが、本発明では安価なNi,Cuや、これらの合金を用いることができる。外部電極6,8の厚さは用途等に応じて適宜決定されればよいが、通常、10〜50μm程度であることが好ましい。
本発明の誘電体磁器組成物を用いた積層セラミックコンデンサ2は、従来の積層セラミックコンデンサと同様に、ペーストを用いた通常の印刷法やシート法によりグリーンチップを作製し、これを焼成した後、外部電極を印刷または転写して焼成することにより製造される。以下、製造方法について具体的に説明する。
まず、主成分原料と副成分原料を用意した。主成分原料としては、平均粒径0.2μmのBaTiO3を用いた。副成分原料としては、MgCO3(第1副成分)、(Ba0.6 Ca0.4 )SiO3(第2副成分)、V2O5(第3副成分)、Y2O3(第4副成分)、Tb4O7(第5副成分)、MnCO3(第6副成分)を用いた。なお、MgCO3 およびMnCO3 は、焼成により酸化物となり、それぞれMgOおよびMnOとして誘電体磁器組成物に含まれることとなる。(Ba0.6 Ca0.4 )SiO3(以下、BCGともいう)については、下記に示す方法により製造した。
昇温速度:25°C/時間、
保持温度:260°C、
温度保持時間:8時間、
雰囲気:空気中。
昇温速度:200°C/時間、
保持温度:1200〜1260°C、
温度保持時間:2時間、
冷却速度:200°C/時間、
雰囲気:加湿したN2+H2混合ガス、
酸素分圧:10−12気圧。
昇温速度:200°C/時間、
保持温度:1050°C、
温度保持時間:2時間、
冷却速度:200°C/時間、
雰囲気:加湿したN2ガス、
酸素分圧:10−5気圧。
なお、焼成およびアニールの際の雰囲気ガスの加湿には、水温を20°Cとしたウェッターを用いた。
誘電体粒子の平均結晶粒径の測定方法としては、まず、得られたコンデンサ試料を内部電極に垂直な面で切断し、その切断面を研磨した。そして、その研磨面にケミカルエッチングを施し、その後、走査型電子顕微鏡(SEM)により観察を行い、コード法により誘電体粒子の形状を球と仮定して算出した。算出した値を、主成分の原料の平均粒径と比較し、誘電体粒子の平均結晶粒径が、主成分の原料の平均粒径の何倍となっているかを調べた。結果を表1に示す。
コンデンサ試料に対し、基準温度20°Cにおいて、デジタルLCRメータ(横河電機(株)製 YHP4274A)にて、周波数1kHz,入力信号レベル(測定電圧)0.25Vrms/μmの条件下で、静電容量Cを測定した。そして、得られた静電容量、積層セラミックコンデンサの誘電体厚みおよび内部電極同士の重なり面積から、比誘電率(単位なし)を算出した。比誘電率は、1800以上を良好とした。結果を表1に示す。
コンデンサ試料に対し、基準温度20°Cにおいて、デジタルLCRメータ(横河電機(株)製 YHP4274A)にて、周波数1kHz,入力信号レベル(測定電圧)0.25Vrms/μmの条件下で、誘電損失tanδを測定した。誘電損失は、小さいほど好ましい。結果を表1に示す。
まず、コンデンサ試料に対し、絶縁抵抗計(アドバンテスト社製R8340A)を用いて、20°Cにおいて4V/μmの直流電圧を、コンデンサ試料に1分間印加した後の絶縁抵抗IRを測定した。CR積は、上記にて測定した静電容量C(単位はμF)と、絶縁抵抗IR(単位はMΩ)との積を求めることにより測定した。CR積は、500以上を良好とした。結果を表1に示す。
高温負荷寿命(絶縁抵抗の加速寿命/HALT)は、得られた試料を、200°Cで50V/μmの直流電圧の印加状態に保持し、平均寿命時間を測定することにより評価した。本実施例においては、絶縁抵抗(IR)が2×105 Ω以下になるまでの時間(単位は時間)を寿命時間とした。また、この高温負荷寿命は、10個のコンデンサ試料について行った。高温負荷寿命は、3時間以上を良好とした。結果を表1に示す。
X7R特性については、コンデンサ試料に対し、基準温度を25°Cとした時に、デジタルLCRメータ(YHP社製4274A)にて、周波数1kHz、入力信号レベル(測定電圧)0.25Vrmsの条件下で、静電容量を測定し、−55〜125°Cの温度範囲内で、温度に対する静電容量変化率(ΔC/C)がEIAJ規格のX7R特性を満足する(±15%以内)試料を良好とした。−55°Cおよび125°Cにおける静電容量の変化率を、それぞれ表1に示す。
副成分の組成を表2に示す組成とした以外は、実施例1と同様にして、コンデンサ試料を作製し、実施例1と同様に特性評価を行った。結果を表2に示す。
4… コンデンサ素子
4a… 第1端部
4b… 第2端部
6,8… 外部電極
10… 誘電体層
12… 内部電極層
Claims (3)
- チタン酸バリウムを含む主成分と、
MgOを含む第1副成分と、
SiO2系の焼結助剤を含む第2副成分と、
V2O5、MoO3 およびWO3 から選ばれる少なくとも1種を含む第3副成分と、
R1の酸化物(ただし、R1は、Y、Ho、Er、Tm、YbおよびLuから選ばれる少なくとも1種)を含む第4副成分と、
R2の酸化物(ただし、R2は、Dy、Tb、GdおよびEuから選ばれる少なくとも1種)を含む第5副成分と、
MnOおよびCr2 O3 の少なくとも1種を含む第6副成分とを有する誘電体磁器組成物であって、
前記主成分100モルに対する各副成分の比率が、
第1副成分:0.8〜2モル、
第2副成分:1.5〜5モル、
第3副成分:0.01〜0.1モル、
第4副成分:0.5〜2モル(ただし、第4副成分のモル数は、R1単独での比率)、
第5副成分:1.5〜4.5モル(ただし、第5副成分のモル数は、R2単独での比率)、
第6副成分:0.1〜0.2モルであり、
前記主成分100モルに対する第4副成分および第5副成分の合計モル数が、前記R1換算および前記R2換算で、2〜6モルであり、かつ、
主成分100モルに対する第4副成分および第5副成分の合計モル数に対する第5副成分の比率が、前記R1換算および前記R2換算で、0.65≦R2/(R1+R2)≦0.75の関係であることを特徴とする誘電体磁器組成物。 - 請求項1に記載の誘電体磁器組成物から構成されている誘電体層を有する電子部品であって、前記誘電体層の1層あたりの厚みが、4μm以上7μm以下である電子部品。
- 請求項1に記載の誘電体磁器組成物を製造する方法であって、
前記主成分の原料と、前記第1〜第6副成分の原料とを混合し、誘電体磁器組成物粉末を得る工程と、
前記誘電体磁器組成物粉末を焼成し、誘電体磁器組成物を得る工程と、を有し、前記主成分の原料として平均粒径が0.1〜0.3μmである原料を使用し、
焼成後の前記誘電体磁器組成物に含まれる誘電体粒子の平均結晶粒径が、前記主成分の原料の平均粒径の1.5倍以上2.0倍以下となるように焼成することを特徴とする誘電体磁器組成物の製造方法。
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JP5668572B2 (ja) * | 2011-03-29 | 2015-02-12 | Tdk株式会社 | 誘電体磁器組成物およびセラミック電子部品 |
JP6089770B2 (ja) | 2013-02-25 | 2017-03-08 | Tdk株式会社 | 誘電体磁器組成物および電子部品 |
KR101792368B1 (ko) | 2015-12-24 | 2017-11-20 | 삼성전기주식회사 | 유전체 자기 조성물, 유전체 재료 및 이를 포함하는 적층 세라믹 커패시터 |
CN106977178A (zh) * | 2017-03-05 | 2017-07-25 | 临沂金成电子有限公司 | 一种微波陶瓷介质材料及制备方法 |
TWI766181B (zh) * | 2019-08-16 | 2022-06-01 | 興勤電子工業股份有限公司 | 陶瓷組成物用於熱敏電阻之用途、陶瓷燒結體用於熱敏電阻之用途、熱敏電阻及其製法 |
CN112408975B (zh) * | 2019-08-23 | 2022-11-04 | 兴勤电子工业股份有限公司 | 陶瓷组成物、陶瓷烧结体、叠层型陶瓷电子元件及其制法 |
CN110483035B (zh) * | 2019-09-24 | 2022-04-15 | 福建省德化县华瓷新材料科技有限公司 | 一种微波介质陶瓷材料及其制备方法和应用、一种滤波器陶瓷材料 |
JP2022122145A (ja) * | 2021-02-09 | 2022-08-22 | Tdk株式会社 | 誘電体組成物、電子部品および積層電子部品 |
JP2022122146A (ja) * | 2021-02-09 | 2022-08-22 | Tdk株式会社 | 誘電体組成物、電子部品および積層電子部品 |
CN113563065B (zh) * | 2021-07-15 | 2022-05-13 | 潮州三环(集团)股份有限公司 | 一种介电陶瓷组合物及其制备方法与应用 |
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US4764493A (en) * | 1986-06-16 | 1988-08-16 | Corning Glass Works | Method for the production of mono-size powders of barium titanate |
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JP3568030B2 (ja) * | 1999-02-26 | 2004-09-22 | Tdk株式会社 | 誘電体磁器組成物の製造方法と誘電体層含有電子部品の製造方法 |
JP3760364B2 (ja) * | 1999-07-21 | 2006-03-29 | Tdk株式会社 | 誘電体磁器組成物および電子部品 |
JP3340722B2 (ja) * | 1999-10-05 | 2002-11-05 | ティーディーケイ株式会社 | 誘電体磁器組成物の製造方法 |
JP2002020166A (ja) * | 2000-06-30 | 2002-01-23 | Taiyo Yuden Co Ltd | 誘電体磁器組成物及び磁器コンデンサ |
JP3417911B2 (ja) * | 2000-08-21 | 2003-06-16 | ティーディーケイ株式会社 | 誘電体磁器組成物の製造方法と誘電体層含有電子部品の製造方法 |
KR100514574B1 (ko) * | 2002-01-15 | 2005-09-13 | 티디케이가부시기가이샤 | 유전체 자기 조성물 및 전자 부품 |
JP4191496B2 (ja) * | 2002-01-15 | 2008-12-03 | Tdk株式会社 | 誘電体磁器組成物および電子部品 |
US6777363B2 (en) * | 2002-07-05 | 2004-08-17 | Samsung Electro-Mechanics Co., Ltd. | Non-reducable, low temperature dielectric ceramic composition, capacitor and method of preparing |
JP2005145791A (ja) * | 2003-11-19 | 2005-06-09 | Tdk Corp | 電子部品、誘電体磁器組成物およびその製造方法 |
TW200531955A (en) * | 2004-03-16 | 2005-10-01 | Tdk Corp | Dielectric ceramic composition, multilayer ceramic capacitor, and method for manufacturing the same |
JP2005335963A (ja) * | 2004-05-24 | 2005-12-08 | Matsushita Electric Ind Co Ltd | 誘電体磁器組成物およびそれを用いた積層セラミックコンデンサ |
JP2006027939A (ja) * | 2004-07-14 | 2006-02-02 | Tdk Corp | 誘電体磁器組成物の製造方法、電子部品及び積層セラミックコンデンサ |
JP4839913B2 (ja) * | 2006-03-23 | 2011-12-21 | Tdk株式会社 | 電子部品、誘電体磁器組成物およびその製造方法 |
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JP2007217205A (ja) | 2007-08-30 |
US20070191211A1 (en) | 2007-08-16 |
KR100889900B1 (ko) | 2009-03-20 |
EP1820784A1 (en) | 2007-08-22 |
KR20070082049A (ko) | 2007-08-20 |
CN101024572A (zh) | 2007-08-29 |
TW200735141A (en) | 2007-09-16 |
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