KR0174719B1 - Dielectric ceramic composition - Google Patents
Dielectric ceramic composition Download PDFInfo
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- KR0174719B1 KR0174719B1 KR1019960046375A KR19960046375A KR0174719B1 KR 0174719 B1 KR0174719 B1 KR 0174719B1 KR 1019960046375 A KR1019960046375 A KR 1019960046375A KR 19960046375 A KR19960046375 A KR 19960046375A KR 0174719 B1 KR0174719 B1 KR 0174719B1
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Abstract
본 발명은 티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5∼4.5mol%,산화사마륨(Sm2O3) 2.5∼4.5mol%, 산화티탄(TiO2) 3∼9mol%, 산화코발트(Co2O3) 0.05∼0.1mol%, 산화안티몬(Sb2O3) 0.05∼0.1mol%를 기본 구성물로 갖는 고유전율 유전체 자기조성물에 관한 것으로서, 상기 고유전율 유전체 자기조성물의 유전변화율이 -20∼80℃의 범위 내에서 25℃에서 유전율을 기준으로 -82% 내지 +22%를 나타내는 EIA(Electronic Industry Association)규격의 Y5V 온도특성을 만족하고, 상온에서 안정한 온도특성을 갖으며, 적층 세라믹 콘덴서의 재료로 사용되는 고유전율 유전체 자기 조성물에 관한 것이다.The present invention, barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 2.5~4.5mol%, samarium (Sm 2 O 3) oxide 2.5~4.5mol%, titanium (TiO 2) 3~9mol% oxide, The present invention relates to a high dielectric constant dielectric ceramic composition having a basic constitution of 0.05 to 0.1 mol% of cobalt (Co 2 O 3 ) and 0.05 to 0.1 mol% of antimony oxide (Sb 2 O 3 ) Satisfies the EIA (Electronic Industry Association) standard Y5V temperature characteristic indicating -82% to + 22% based on the dielectric constant at 25 DEG C within a range of -20 to 80 DEG C, has a stable temperature characteristic at room temperature, To a high dielectric constant dielectric ceramic composition used as a material for a ceramic capacitor.
Description
본 발명은 고유전율 유전체 자기조성물에 관한 것으로서, 특히 적층 세라믹 콘덴서의 재료로 사용되는 고유전율 유전체 자기조성물에 관한 것이다.The present invention relates to a high dielectric constant dielectric ceramic composition, and more particularly, to a high dielectric constant dielectric ceramic composition used as a material for a multilayer ceramic capacitor.
상기 고유전체 자기조성물이라 함은 -20∼80℃에서 25℃의 유전율을 기준으로 유전변화율 -82% 내지 +22%인 EIA(Electronic Industry Association)규격의 Y5V 온도특성을 갖는 물질이다.The high dielectric ceramic composition is a material having a Y5V temperature characteristic of EIA (Electronic Industry Association) standard with a dielectric change rate of -82% to + 22% based on a dielectric constant at 25 占 폚 at -20 to 80 占 폚.
종래의 고유전율 유전체 자기 조성물은 티탄산 바륨(BaTiO3)을 주성분으로 하여 지르콘산 칼슘(CaZrO3), 지르콘산 바륨(BaZrO3), 티탄산 칼슘(CaTiO3), 티탄산 마그네슘(MgTiO3) 등의 산화물이 첨가된 유전체가 사용되었다.A conventional high-permittivity dielectric ceramic composition zirconate calcium to as a main component barium titanate (BaTiO 3) (CaZrO 3) , zirconate, barium (BaZrO 3), calcium titanate (CaTiO 3), magnesium titanate (MgTiO 3) oxides such as The added dielectric was used.
그러나, 상기와 같이 조성된 종래의 유전체 자기 조성물들은 상온에서 높은 유전율을 갖는 반면, 절연 파괴전압이 낮고, 1,350℃ 이상의 높은 소결온도를 갖는다는 문제점이 있었다.However, the conventional dielectric ceramic compositions as described above have a high dielectric constant at room temperature, a low dielectric breakdown voltage, and a high sintering temperature of 1,350 캜 or more.
본 발명은 상기한 바와 같은 문제점을 해결하기 위하여 안출된 것으로서, 유전율이 9,000 이상, 1,300℃ 이하의 온도에서 소결이 가능하고 -20∼80℃까지 25℃의 유전율을 기준으로 유전변화율 -82% 내지 +22%를 만족하는 Y5V 온도특성을 갖는 유전체 분말을 제조함에 그 목적이 있다.Disclosure of the Invention The present invention has been conceived to solve the problems as described above, and it is an object of the present invention to provide a method for producing a sintered body capable of sintering at a temperature of 9000 or more and 1,300 ° C or less, + 22%. The present invention is directed to a dielectric powder having a Y5V temperature characteristic.
본 발명은 티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5∼4.5mol%,산화사마륨(Sm2O3) 2.5∼4.5mol%, 산화티탄(TiO2) 3∼9mol%, 산화코발트(Co2O3) 0.05∼0.1mol%, 산화안티몬(Sb2O3) 0.05∼0.1mol%로 이루어진 고유전율 유전체 자기 조성물에 관한것이다.The present invention, barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 2.5~4.5mol%, samarium (Sm 2 O 3) oxide 2.5~4.5mol%, titanium (TiO 2) 3~9mol% oxide, 0.05 to 0.1 mol% of cobalt (Co 2 O 3 ), and 0.05 to 0.1 mol% of antimony oxide (Sb 2 O 3 ).
산화세슘(CeO2), 산화사마륨(Sm2O3)은 유전율을 촉진시키는 역할을 하고, 산화티탄(TiO2)은 소결을 촉진하는 역할을 하는데, 상기 범위 이외에서는 온도특성이 벗어나며, 낮은 유전율을 갖는다. 산화코발트(Co2O3)와 산화안티몬(Sb2O3)은 유전율을 증가시키면서 온도특성을 완화시키나 0.1mol% 이상이면 소결성이 악화되고 유전손실이 증가된다.Cerium oxide (CeO 2 ) and samarium oxide (Sm 2 O 3 ) serve to promote the dielectric constant, and titanium oxide (TiO 2 ) plays a role in promoting sintering. Respectively. Cobalt oxide (CO 2 O 3 ) and antimony oxide (Sb 2 O 3 ) relax the temperature characteristics while increasing the dielectric constant, but if it is more than 0.1 mol%, the sinterability deteriorates and the dielectric loss increases.
표 1을 참조하여 본 발명의 실시예를 설명하면 다음과 같다. 티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5∼4.5mol%,산화사마륨(Sm2O3) 2.5∼4.5mol%, 산화티탄(TiO2) 3∼9mol%, 산화코발트(Co2O3) 0.05∼0.1mol%, 산화안티몬(Sb2O3) 0.05∼0.1mol%를 각각의 범위 내에서 적절한 양을 탈이온수와 함께 혼합한다. 이때 혼합은 볼 밀링(Ball Milling) 방법을 이용하며, 산화 아르곤(ZrO2) 볼과 우레탄 용기를 사용한다. 건조된 분말을 결합체와 유발로 혼합하고, 금형 유압프레스를 사용해 직경 24.5mm, 두께 1.5mm의 원형 시편을 제작한다. 이렇게 제작한 시편을 ZrO2세터(setter)에 놓고 공기 압의 전기로 중에서 1,250∼1,300℃의 온도로 2시간 소결한다. 소결된 시편의 양면에 은전극을 프린팅 방법으로 19.5mm 직경의 원형으로 도포한 다음, 열처리하여 유전상수, 유전손실, 절연저항,유전율의 온도특성(TCC%)을 측정한 결과, 유전상수는 25℃에서 9,200∼11,500Khz, 유전손실은 0.7∼2.1%, 절연저항은 1.1×1012∼2.1×1012, 유전율의 온도특성(TCC)은 -20℃에서 -41∼-10%, 80℃에서 -75∼-58%인 특성을 나타냈다.An embodiment of the present invention will be described with reference to Table 1 below. Barium titanate (BaTiO 3) 100mol%, cesium (CeO 2) 2.5~4.5mol%, samarium oxide (Sm 2 O 3) 2.5~4.5mol% , titanium (TiO 2) 3~9mol% oxide, cobalt (Co oxide 2 O 3) 0.05~0.1mol%, and mixing antimony oxide (Sb 2 O 3) 0.05~0.1mol% the appropriate amount with deionized water in each range. At this time, the ball milling method is used for mixing, and an argon (ZrO 2 ) ball and a urethane container are used. The dried powder is mixed with the binder and induction, and a circular specimen having a diameter of 24.5 mm and a thickness of 1.5 mm is prepared by using a mold hydraulic press. The specimen thus prepared is placed in a ZrO 2 setter and sintered in an air furnace at a temperature of 1,250 to 1,300 ° C for 2 hours. The dielectric constant, dielectric loss, insulation resistance, and dielectric constant (TCC%) were measured by applying a silver electrode on both sides of the sintered specimen in a circular shape with a diameter of 19.5 mm by printing and then heat treatment. in ℃ 9,200~11,500Khz, 0.7~2.1% dielectric loss, insulation resistance of 1.1 × 10 12 ~2.1 × 10 12 , the temperature characteristic of the dielectric constant (TCC) at -41~-10% at 80 ℃ -20 ℃ -75 to-58%.
[실시예 1][Example 1]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5mol%, 산화사마륨(Sm2O3) 2.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.1mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1280℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,600KHz, 유전손실은 0.7%, 절연저항은 2.0×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -30%와 -60%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 2.5mol%, samarium oxide (Sm 2 O 3) 2.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol%, and 0.1 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1280 ° C. by the above-mentioned method. As a result, the dielectric constant was 9,600 KHz at 25 ° C., 0.7%, the insulation resistance was 2.0 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -30% and -60% at -20 ° C and 80 ° C, respectively.
[실시예 2][Example 2]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5mol%, 산화사마륨(Sm2O3) 2.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.1mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1300℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 10,200KHz, 유전손실은 1.0%, 절연저항은 2.1×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -28%와 -62%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 2.5mol%, samarium oxide (Sm 2 O 3) 2.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) oxide 0.1 mol%, and 0.05 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1300 ° C. by the above-mentioned method. As a result, the dielectric constant was 10,200 KHz at 25 ° C., 1.0%, the insulation resistance was 2.1 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -28% and -62% at -20 ° C and 80 ° C, respectively.
[실시예 3][Example 3]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 2.5mol%, 산화사마륨(Sm2O3) 2.5mol%, 산화티탄(TiO2) 0.1mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1290℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 11,500KHz, 유전손실은 1.5%, 절연저항은 1.3×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -10%와 -58%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 2.5mol%, samarium oxide (Sm 2 O 3) 2.5mol% , titanium (TiO 2) 0.1mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol% and antimony oxide (Sb 2 O 3 ) as constituent components at a sintering temperature of 1290 ° C. The dielectric constant was 11,500 KHz at 25 ° C. and the dielectric loss was 1.5%, the insulation resistance was 1.3 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -10% and -58% at -20 ° C and 80 ° C, respectively.
[실시예 4][Example 4]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 3.5mol%, 산화사마륨(Sm2O3) 3.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.1mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1280℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,200KHz, 유전손실은 1.2%, 절연저항은 1.2×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -22%와 -70%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 3.5mol%, samarium oxide (Sm 2 O 3) 3.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol%, and 0.1 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1280 ° C. by the above-mentioned method. As a result, the dielectric constant was 9,200 KHz at 25 ° C., 1.2%, insulation resistance was 1.2 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -22% and -70% at -20 ° C and 80 ° C, respectively.
[실시예 5][Example 5]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 3.5mol%, 산화사마륨(Sm2O3) 3.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.1mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1290℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,800KHz, 유전손실은 2.1%, 절연저항은 1.4×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -36%와 -72%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 3.5mol%, samarium oxide (Sm 2 O 3) 3.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) oxide 0.1 mol%, and 0.05 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1290 ° C. by the above-mentioned method. As a result, the dielectric constant was found to be 9,800 KHz at 25 ° C., 2.1%, the insulation resistance was 1.4 × 10 12 Ωcm, and the temperature characteristics (TCC) of the dielectric constant were -36 ° C and -72 ° C at -20 ° C and 80 ° C, respectively.
[실시예 6][Example 6]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 3.5mol%, 산화사마륨(Sm2O3) 3.5mol%, 산화티탄(TiO2) 0.1mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1,300℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,900KHz, 유전손실은 1.5%, 절연저항은 1.2×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -41%와 -75%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 3.5mol%, samarium oxide (Sm 2 O 3) 3.5mol% , titanium (TiO 2) 0.1mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol%, and 0.05 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were manufactured at the sintering temperature of 1,300 ° C. by the above-mentioned method. As a result, the dielectric constant was 9,900 KHz at 25 ° C., 1.5%, the insulation resistance was 1.2 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -41% and -75% at -20 ° C and 80 ° C, respectively.
[실시예 7][Example 7]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 4.5mol%, 산화사마륨(Sm2O3) 4.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.1mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1,300℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 10,100KHz, 유전손실은 0.8%, 절연저항은 1.1×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -32%와 -64%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 4.5mol%, samarium oxide (Sm 2 O 3) 4.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol%, and 0.1 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1,300 ° C. by the above-mentioned method. As a result, the dielectric constant was 10,100 KHz at 25 ° C., 0.8%, the insulation resistance was 1.1 × 10 12 Ωcm, and the temperature characteristic (TCC) of the dielectric constant was -32% and -64% at -20 ° C and 80 ° C, respectively.
[실시예 8][Example 8]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 4.5mol%, 산화사마륨(Sm2O3) 4.5mol%, 산화티탄(TiO2) 0.05mol%, 산화코발트(Co2O3) 0.1mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1,270℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,600KHz, 유전손실은 1.0%, 절연저항은 1.3×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -35%와 -70%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 4.5mol%, samarium oxide (Sm 2 O 3) 4.5mol% , titanium (TiO 2) 0.05mol%, cobalt oxide (Co 2 O 3) oxide 0.1 mol%, and 0.05 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1,270 ° C. by the above-mentioned method. As a result, the dielectric constant was 9,600 KHz at 25 ° C., 1.0%, the insulation resistance was 1.3 × 10 12 Ωcm, and the temperature characteristics (TCC) of the dielectric constant were -35 ° C and -70 ° C at -20 ° C and 80 ° C, respectively.
[실시예 9][Example 9]
티탄산 바륨(BaTiO3) 100mol%, 산화세슘(CeO2) 4.5mol%, 산화사마륨(Sm2O3) 4.5mol%, 산화티탄(TiO2) 0.1mol%, 산화코발트(Co2O3) 0.05mol%, 산화안티몬(Sb2O3) 0.05mol%를 구성 성분으로 갖는 고유전율 유전체 자기조성물을 소결온도 1,280℃에서 상기의 방법으로 제조한 결과, 유전상수는 25℃에서 9,200KHz, 유전손실은 1.2%, 절연저항은 2.1×1012Ωcm, 유전율의 온도 특성(TCC)은 -20℃와 80℃에서 각각 -32%와 -65%인 특성을 나타냈다.Barium titanate (BaTiO 3) 100mol%, cesium oxide (CeO 2) 4.5mol%, samarium oxide (Sm 2 O 3) 4.5mol% , titanium (TiO 2) 0.1mol%, cobalt oxide (Co 2 O 3) 0.05 oxide mol%, and 0.05 mol% of antimony oxide (Sb 2 O 3 ) as constituent components were produced at the sintering temperature of 1,280 ° C. by the above-mentioned method. As a result, the dielectric constant was 9,200 KHz at 25 ° C., 1.2%, the insulation resistance was 2.1 × 10 12 Ωcm, and the temperature characteristics (TCC) of the dielectric constant were -32 ° C and -65 ° C at -20 ° C and 80 ° C, respectively.
본 발명에 의한 상기 고유전율 유전체 자기조성물은 9,000KHz 이상의 고유전율을 갖고, 1×1012Ωcm 이상의 절연저항과, 1,300℃ 이하의 소결온도를 갖고 있으며, 유전변화율이 -20∼80℃의 범위 내에서 25℃에서 유전율을 기준으로 -82% 내지 +22%를 나타내는 EIA(Electronic Industry Association)규격의 Y5V 온도특성을 만족하므로 고신뢰성의 적층 세라믹 콘덴서의 제조를 가능하게 하는 효과가 있다.The high dielectric constant dielectric ceramic composition according to the present invention has a high dielectric constant of 9,000 KHz or more, an insulation resistance of 1 x 10 12 ? Cm or more, a sintering temperature of 1,300 ° C or less and a dielectric constant within a range of -20 to 80 ° C And the Y5V temperature characteristic of EIA (Electronic Industry Association) standard indicating -82% to + 22% based on the dielectric constant at 25 DEG C is satisfied. Thus, it is possible to manufacture a multilayer ceramic capacitor of high reliability.
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| KR100489887B1 (en) * | 2002-06-22 | 2005-05-27 | 주식회사 지믹스 | Microwave dielectric ceramic compositions and prepartion method thereof |
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