KR19990056619A - High dielectric constant magnetic composition for MC - Google Patents
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Abstract
본 발명은 100BaTiO3+aNb2O5+bCeO2+ cNiO +dMnO2+ eSiO2+ fZnO (1.60≤a≤2.00mol%, 0.30≤b≤0.50mol%, 0.50≤c≤0.60mol%, 0.05≤d≤0.10mol%, 0.10≤e≤0.50mol%, 0.10≤f≤0.50mol%)로 조성된 유전체 자기 조성물에 관한 것으로서, 유전율이 3700이상이며, 1280℃이하의 비교적 낮은 온도에서 소결이 가능하고 절연저항1013Ωcm이상이므로, X7R 온도특성을 만족하는 적층세라믹 커패시터등에 적용될 수 있는 자기 조성물에 관한 것이다.100 BaTiO 3 + aNb 2 O 5 + bCeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (1.60≤a≤2.00mol%, 0.30≤b≤0.50mol%, 0.50≤c≤0.60mol%, 0.05≤ The dielectric ceramic composition is composed of d≤0.10mol%, 0.10≤e≤0.50mol%, 0.10≤f≤0.50mol%), and has a dielectric constant of 3700 or more and can be sintered at a relatively low temperature below 1280 ° C. Since the insulation resistance is 10 13 Ωcm or more, the present invention relates to a magnetic composition that can be applied to a multilayer ceramic capacitor that satisfies the X7R temperature characteristic.
Description
본 발명은 티탄산바륨(BaTiO3)을 주성분으로 하는 자기 조성물에 관한 것으로, 특히 유전율이 3700이상이고, EIA(Electronic Industry Association)규격의 X7R 온도 특성을 만족하는 동시에 1280℃이하의 온도에서 소결이 가능하며 1013Ωcm의 절연저항을 가져, 세라믹 커패시퍼(Ceramic Capacitor)와 같은 각종 부품에 적용할 수 있는 유전체 자기조성물에 관한 것이다.The present invention relates to a magnetic composition comprising barium titanate (BaTiO 3 ) as a main component, and in particular, has a dielectric constant of 3700 or more, and satisfies the X7R temperature characteristic of the Electronic Industry Association (EIA) standard and can be sintered at a temperature of 1280 ° C or lower. And it has a dielectric resistance of 10 13 Ωcm, and relates to a dielectric magnetic composition that can be applied to various components such as ceramic capacitor (Ceramic Capacitor).
종래의 X7R을 만족하는 유전체 자기조성물은 (BaTiO3+Nb2O5)을 기본물질로 하여 티탄산칼슘(CaTiO3), 산화니켈(NiO), 산화코발트(CoO), 산화마그네슘(MgO), 산화비스무스(Bi2O3), 산화셀륨(CeO2), 산화주석(MnO2), 산화아연(ZnO) 같은 전이금속산화물, 회토류산화물 등의 세라믹 부성분이 치환되거나 첨가되어 조성되었다. 그러나 상기의 조성물중 산화비스무스(Bi2O3)를 포함한 조성물은 소결성 및 유전율의 온도안전성은 우수하지만, 고온에서 팔라듐(Pd)전극과 반응한다는 문제점을 안고 있다. 또한 부성분으로 산화마그네슘(MgO) 및 산화셀륨(CeO2)이 첨가된 조성물(일본 특허 공보 소61-99207호)과 산화코발트(Co2O3), 산화망간(MnO2), 산화셀륨(CeO2)이 첨가된 조성물(일본 특허 공보 소62-22905호)은 유전율이 3000이상으로 높은 반면, 절연저항이 1011Ωcm정도로 낮고 유전율의 온도특성(TCC) 또한 조성에 따라 불규칙적으로 변하가 때문에 안정하지 못하며, 소결온도도 1300℃이상으로 비교적 높다. 이는 넓은 온도범위에서 안정된 온도특성이 요구되는 유전체 특성에 부적합한 것으며 특히 -55℃ ~ +125℃의 온도범위내에서는 ±15%이하의 용량변화량을 갖도록 규정되어진 EIA(Electronic Industry Association)규격의 X7R온도특성을 만족하는 자기조성물로 적용되어지기에 문제점이 있다.Conventional X7R-based dielectric ceramic compositions are based on (BaTiO 3 + Nb 2 O 5 ) as calcium carbonate (CaTiO 3 ), nickel oxide (NiO), cobalt oxide (CoO), magnesium oxide (MgO), and oxidation Ceramic subcomponents such as bismuth (Bi 2 O 3 ), cerium oxide (CeO 2 ), tin oxide (MnO 2 ), zinc oxide (ZnO), and rare earth oxides were substituted or added. However, although the composition including bismuth oxide (Bi 2 O 3 ) in the composition has excellent temperature stability of sinterability and dielectric constant, it has a problem of reacting with a palladium (Pd) electrode at high temperature. In addition, a composition containing magnesium oxide (MgO) and cerium oxide (CeO 2 ) as a secondary component (Japanese Patent Publication No. 61-99207), cobalt oxide (Co 2 O 3 ), manganese oxide (MnO 2 ), and cerium oxide (CeO) 2 ) The added composition (Japanese Patent Publication No. 62-22905) is stable because the dielectric constant is higher than 3000, while the insulation resistance is as low as 10 11 Ωcm and the temperature characteristic (TCC) of the dielectric constant varies irregularly with the composition. The sintering temperature is relatively high, above 1300 ℃. This is unsuitable for dielectric properties that require stable temperature characteristics over a wide temperature range, especially the X7R of the EIA (Electronic Industry Association) standard, which has a capacity change of ± 15% or less within the temperature range of -55 ° C to + 125 ° C. There is a problem in that it is applied to a magnetic composition that satisfies the temperature characteristics.
상기와 같은 문제점을 해결하기 위해 본 발명은 산화비스무스(Bi2O3)를 포함하지 않으며, 유전율이 3700이상이고 절연저항이 1013Ωcm이상인 동시에 1280℃이하의 온도에서 소결가능한 X7R온도특성을 만족하는 유전체 자기조성물을 제공하는데 그 목적이 있다.In order to solve the above problems, the present invention does not include bismuth oxide (Bi 2 O 3 ), satisfies the X7R temperature characteristics that can be sintered at a temperature of 1280 ℃ or less while the dielectric constant is more than 3700 and the insulation resistance is more than 10 13 Ωcm The purpose is to provide a dielectric magnetic composition.
상기의 목적을 실현하기 위한 본 발명의 유전체 자기조성물은 100BaTiO3＋aNb2O5＋bCeO2＋ cNiO ＋dMnO2＋ eSiO2＋ fZnO (1.60≤a≤2.00mol%, 0.30≤b≤0.50mol%, 0.50≤c≤0.60mol%, 0.05≤d≤0.10mol%, 0.10≤e≤0.50mol%, 0.10≤f≤0.50mol%)로 조성된 것을 특징으로 한다.The dielectric ceramic composition of the present invention for achieving the above object is 100BaTiO 3 + aNb 2 O 5 + bCeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (1.60≤a≤2.00mol%, 0.30≤b≤0.50mol%, 0.50≤ c≤0.60mol%, 0.05≤d≤0.10mol%, 0.10≤e≤0.50mol%, 0.10≤f≤0.50mol%).
상기에서 산화니오븀(Nb2O5)은 결정립의 성장을 제한하여 미세한 결정립을 가지도록 하며, 산화세슘(CeO2)은 액상을 형성하여 치밀한 조직을 갖게끔 한다. 또한, 산화망간(MnO2)과 산화니켈(NiO)은 소량 첨가되어 온도특성, 절연저항 등의 전기특성을 변화시키며, 산화규소(SiO2)와 산화아연(ZnO)은 소결온도를 낮추는 소결조제의 역할을 한다.In the above niobium oxide (Nb 2 O 5 ) is to limit the growth of the crystal grains to have a fine grain, cesium oxide (CeO 2 ) to form a liquid to have a dense structure. In addition, a small amount of manganese oxide (MnO 2 ) and nickel oxide (NiO) is added to change the electrical characteristics such as temperature characteristics, insulation resistance, and silicon oxide (SiO 2 ) and zinc oxide (ZnO) sintering aid to lower the sintering temperature Plays a role.
본 발명을 실현하는 실시예를 자세히 설명하면 다음과 같다.An embodiment of realizing the present invention will be described in detail as follows.
티탄산바륨(BaTiO3)에 산화니오븀(Nb2O5), 산화셀륨(CeO2), 산화니켈(NiO), 산화망간(MnO2), 산화규소(SiO2), 산화아연(ZnO)을 상기의 중량비의 범위내에서 평량하여 혼합시킨 후 100℃에서 건조시켜 혼합분말을 만든다. 그 후 상기의 건조된 혼합분말에 압력을 가하여 성형시킨 다음 소결하여 은(Ag)전극으로 도포하고 전극을 소부하였다. 그 후, 본 발명이 속하는 기술분야에서 통상적으로 사용되는 방법으로 전극이 부착된 시편의 유전율, 유전손실, 유전율의 온도특성, 절연저항을 측정하여 다음과 같은 결과를 얻었다.Niobium oxide (Nb 2 O 5 ), cerium oxide (CeO 2 ), nickel oxide (NiO), manganese oxide (MnO 2 ), silicon oxide (SiO 2 ), and zinc oxide (ZnO) are added to barium titanate (BaTiO 3 ). After mixing in a basis weight within the range of the weight ratio of to dry at 100 ℃ to make a mixed powder. Then, the dried mixed powder was molded by applying pressure, sintered, coated with silver (Ag) electrodes, and baked. Then, the dielectric constant, dielectric loss, temperature characteristic of the dielectric constant and insulation resistance of the specimen attached to the electrode by a method commonly used in the art to which the present invention belongs to obtain the following results.
<실시예 1><Example 1>
100BaTiO3＋aNb2O5＋bCeO2＋ cNiO ＋dMnO2＋ eSiO2＋ fZnO (a=2.00mol%, b=0.30mol%, c=0.50mol%, d=0.10mol%, e=0.50mol%, f=0.10mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1280℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 4600, 유전손실은 25℃에서 1KHz를 걸어주었을 때 1.0, 절연저항은 1 × 1013Ωcm이며, 유전율의 온도특성(TCC)은 -55℃에서 -2%, ＋125℃에서 -7%였다.100 BaTiO 3 + aNb 2 O 5 + bCeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (a = 2.00mol%, b = 0.30mol%, c = 0.50mol%, d = 0.10mol%, e = 0.50mol%, f = 0.10 mol%) was prepared by the above method at a sintering temperature of 1280 ℃ to have a dielectric composition composed of 0.10 mol%), the dielectric constant is 4600 when 1KHz at 25 ℃, the dielectric loss is 1.0, when 1KHz at 25 ℃ The insulation resistance was 1 × 10 13 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -2% at -55 ° C and -7% at + 125 ° C.
<실시예 2><Example 2>
100BaTiO3＋aNb2O5＋bCeO2＋ cNiO ＋dMnO2＋ eSiO2＋ fZnO (a=2.00mol%, b=0.50mol%, c=0.50mol%, d=0.05mol%, e=0.40mol%, f=0.10mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1280℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 4450, 유전손실은 25℃에서 1KHz를 걸어주었을 때 1.0, 절연저항은 2 × 1013Ωcm이며, 유전율의 온도특성(TCC)은 -55℃에서 -5%, ＋125℃에서 -8%였다.100 BaTiO 3 + aNb 2 O 5 + bCeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (a = 2.00mol%, b = 0.50mol%, c = 0.50mol%, d = 0.05mol%, e = 0.40mol%, f = 0.10 mol%) was prepared by the above method at a sintering temperature of 1280 ℃ to have a dielectric composition composed of 4, when the dielectric constant is 1450 Hz at 1450Hz at 25 ℃, the dielectric loss is 1.0, when 1KHz at 25 ℃ The insulation resistance was 2 × 10 13 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -5% at -55 ° C and -8% at + 125 ° C.
<실시예 3><Example 3>
100BaTiO3+aNb2O5+bCeO2+ cNiO +dMnO2+ eSiO2+ fZnO (a=2.00mol%, b=0.50mol%, c=0.50mol%, d=0.05mol%, e=0.10mol%, f=0.50mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1260℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 4400, 유전손실은 25℃에서 1KHz를 걸어주었을 때 0.9, 절연저항은 4 × 1013Ωcm이며, 유전율의 온도특성(TCC)는 -55℃에서 +2%, +125℃에서 -11%였다.100 BaTiO 3 + aNb 2 O 5 + bCeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (a = 2.00mol%, b = 0.50mol%, c = 0.50mol%, d = 0.05mol%, e = 0.10mol% , f = 0.50mol%), which was prepared by the above method at the sintering temperature of 1260 ° C to have a dielectric composition of 1400Hz at a dielectric constant of 4400 and a dielectric loss of 1KHz at 25 ° C. At 0.9, the insulation resistance was 4 × 10 13 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was + 2% at -55 ° C and -11% at + 125 ° C.
<실시예 4><Example 4>
100BaTiO3+aNb2O5+bCeO2+ cNiO +dMnO2+ eSiO2+ fZnO (a=1.80mol%, b=0.40mol%, c=0.60mol%, d=0.10mol%, e=0.30mol%, f=0.20mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1260℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 4100, 유전손실은 25℃에서 1KHz를 걸어주었을 때 0.9, 절연저항은 2 × 1013Ωcm이며, 유전율의 온도특성(TCC)은 -55℃에서 +5%, +125℃에서 -9%였다.100 BaTiO 3 + aNb 2 O 5 + b CeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (a = 1.80 mol%, b = 0.40 mol%, c = 0.60 mol%, d = 0.10 mol%, e = 0.30 mol%) , f = 0.20mol%), which was prepared by the above method at the sintering temperature of 1260 ° C. The dielectric constant was 1100Hz at 4100 and the dielectric loss was 1KHz at 25 ° C. At 0.9, the insulation resistance was 2 × 10 13 Ωcm, and the dielectric constant (TCC) was + 5% at -55 ° C and -9% at + 125 ° C.
<실시예 5>Example 5
100BaTiO3+aNb2O5+bCeO2+ cNiO +dMnO2+ eSiO2+ fZnO (a=1.80mol%, b=0.40mol%, c=0.60mol%, d=0.10mol%, e=0.10mol%, f=0.50mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1240℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 3980, 유전손실은 25℃에서 1KHz를 걸어주었을 때 0.8, 절연저항은 2 × 1013Ωcm이며, 유전율의 온도특성(TCC)은 -55℃에서 +2%, +125℃에서 -6%였다.100 BaTiO 3 + aNb 2 O 5 + b CeO 2 + cNiO + dMnO 2 + eSiO 2 + fZnO (a = 1.80 mol%, b = 0.40 mol%, c = 0.60 mol%, d = 0.10 mol%, e = 0.10 mol%) , f = 0.50mol%), which was prepared by the above method at the sintering temperature of 1240 ° C to have a dielectric constant of 3980 when 1KHz at 25 ° C and dielectric loss of 1KHz at 25 ° C. At 0.8, the insulation resistance was 2 × 10 13 Ωcm, and the dielectric constant (TCC) was + 2% at -55 ° C and -6% at + 125 ° C.
<실시예 6><Example 6>
b=0.40mol%, c=0.60mol%, d=0.10mol%, e=0.20mol%, f=0.30mol%)로 조성된 유전체 조성물을 가지도록 소결온도 1240℃에서 상기의 방법으로 제조한 결과, 유전율은 25℃에서 1KHz를 걸어주었을 때 3760, 유전손실은 25℃에서 1KHz를 걸어주었을 때 0.8, 절연저항은 1 × 1013Ωcm이며, 유전율의 온도특성(TCC)은 -55℃에서 -5%, +125℃에서 +3%였다.b = 0.40 mol%, c = 0.60 mol%, d = 0.10 mol%, e = 0.20 mol%, f = 0.30 mol%) to have a dielectric composition prepared by the above method at the sintering temperature of 1240 ° C. The dielectric constant is 3760 when the 1KHz is applied at 25 ℃, the dielectric loss is 0.8 when the 1KHz is applied at 25 ℃, the insulation resistance is 1 × 10 13 Ωcm, and the temperature characteristic (TCC) of the dielectric constant is -5 at -55 ℃. %, + 3% at + 125 ° C.
본 발명에 의한 상기 유전체 자기 조성물은 1280℃이하의 비교적 낮은 온도에서 소결이 가능하며 유전율이 높기 때문에 적층세라믹 커패시터등에 적용할 수 있다.The dielectric ceramic composition according to the present invention can be sintered at a relatively low temperature of 1280 ° C or less, and can be applied to a multilayer ceramic capacitor because of its high dielectric constant.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100351228B1 (en) * | 1999-12-15 | 2002-09-09 | 엠아르에이 라보레이토리스 | Improved high dielectric constant x7r ceramic capacitor and powder for making |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100351228B1 (en) * | 1999-12-15 | 2002-09-09 | 엠아르에이 라보레이토리스 | Improved high dielectric constant x7r ceramic capacitor and powder for making |
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