본 발명은 유전율이 작은 유전체 자기 조성물 및 이로 제조된 적층 세라믹 커패시터(Multi Layered Ceramic Capacitor; 이하, 'MLCC'라 한다.)에 관한 것이며, 보다 상세하게는 유전율이 작은 유전체 자기 조성물 및 이로 제조된 손실값 및 ESR이 감소되며 X8R의 온도특성을 만족하는 MLCC에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dielectric ceramic composition having a low dielectric constant and a multilayer ceramic capacitor (hereinafter referred to as 'MLCC') made thereof, and more particularly, to a dielectric ceramic composition having a low dielectric constant and a loss produced therefrom. The value and ESR are reduced and the MLCC satisfying the temperature characteristic of the X8R.
종래의 저유전율 적층세라믹 커패시터의 유전체로는 BaTiO3분말에 2종 이상의 첨가제를 첨가하여 입자가 강유전성을 띄는 BaTiO3(이하, 'BT'라 한다.)로 이루어진 코어영역과 그 표면이 첨가제로 치환되어 상유전성을 띄는 쉘 영역으로 둘러쌓인 미세한 입자가 사용되었다. 이와 같이, 유전율을 감소시키기 위해 쉘 영역을 증대시키거나, 평균입경이 0.5㎛이하인 미세한 분말로 형성하였으며 상기 유전체분말은 k=2500±500의 유전상수를 갖으며, X7R(-55∼125℃에서 용량 변화율 ±15%)의 온도특성을 충족하는 것이다.As a dielectric of a conventional low dielectric constant multilayer ceramic capacitor, a core region consisting of BaTiO3 (hereinafter referred to as 'BT') in which particles are ferroelectric by adding two or more additives to BaTiO3 powder and its surface is replaced with an additive. Fine particles surrounded by shell regions with homogeneous properties were used. As such, the shell area was increased to reduce the dielectric constant, or formed into a fine powder having an average particle diameter of 0.5 μm or less. The dielectric powder had a dielectric constant of k = 2500 ± 500 and was X7R (-55 to 125 ° C.). Capacity change rate of ± 15%).
그러나, 종래 이와 같은 유전체 분말은 비교적 높은 유전율을 갖음으로 저용량 적층세라믹 커패시터(MLCC)에 적용하는 경우, 인쇄층이 겹쳐지는 부분이 적어 얼라인먼트(alignment)에 의한 용량 편차가 커진다. 또한, 이와 같은 문제를 해결하고자 겹쳐지는 부분을 늘이면 적층수가 감소하고 또한 ESR이 증가한다.However, such a dielectric powder has a relatively high dielectric constant, and thus, when applied to a low capacitance multilayer ceramic capacitor (MLCC), a portion of the printed layer overlaps with each other, resulting in a large capacity variation due to alignment. In addition, increasing the overlapping portion to solve such a problem reduces the number of stacking and increases the ESR.
이에 본 발명의 목적은 저용량 MLCC 제작에 적합한 저유전율 유전체 자기 조성물을 제공하는 것이다.Accordingly, it is an object of the present invention to provide a low dielectric constant dielectric ceramic composition suitable for low capacity MLCC fabrication.
본 발명의 다른 목적은 손실값(DF) 및 ESR(Equivalent Series Resistance)이 낮은 전기적 특성 및 X8R의 온도특성을 만족하는 MLCC제조에 적합한 유전체 자기 조성물을 제공하는 것이다.It is another object of the present invention to provide a dielectric ceramic composition suitable for MLCC production that satisfies the electrical characteristics of low loss value (DF) and equivalent series resistance (ESR) and the temperature characteristic of X8R.
본 발명의 또 다른 목적은 낮은 손실값(DF) 및 ESR(Equivalent Series Resistance)이 낮고 X8R의 온도특성을 만족하는 MLCC를 제공하는 것이다.It is still another object of the present invention to provide an MLCC which has a low loss value (DF) and low ESR (Equivalent Series Resistance) and satisfies the temperature characteristics of X8R.
본 발명의 일 견지에 의하면,According to one aspect of the invention,
화학식 a BaTiO3-bMgCO3-cMnO2-dY2O3-eCr2O3-f Pe-gBaxCa(1-x)SiO3로 나타내어지며, 식중 Pe는 SrZrO3, SrTiO3, CaTiO3및 CaZrO3로 구성되는 그룹으로 부터 선택된 최소 하나의 상유전체이며, BaTiO3100mol당(즉, a=100) 0.2≤b≤6.0, 0.05≤c≤1.5, 0.05≤d≤2.0, 0.05≤e≤0.5, 5≤f≤30, 0.5≤g≤3 그리고 x는 0.4∼0.5인 저유전율 유전체 자기 조성물의 제공된다.Formulaa BaTiO 3 -bMgCO 3 -cMnO 2 -dY 2 O 3 -eCr 2 O 3 is represented by-f Pe-gBa x Ca (1 -x) SiO 3, wherein Pe is SrZrO3, SrTiO3, CaTiO3, and At least one dielectric material selected from the group consisting of CaZrO3 , 0.2 ≦ b ≦ 6.0, 0.05 ≦ c ≦ 1.5, 0.05 ≦ d ≦ 2.0, 0.05 ≦ e ≦ 0.5 per 100 mol of BaTiO3 (ie, a = 100) And 5 ≦ f ≦ 30, 0.5 ≦ g ≦ 3, and x are from 0.4 to 0.5.
본 발명의 다른 견지에 의하면,According to another aspect of the present invention,
화학식 a BaTiO3-bMgCO3-cMnO2-dY2O3-eCr2O3-f Pe-gBaxCa(1-x)SiO3로 나타내어지며, 식중 Pe는 SrZrO3, SrTiO3, CaTiO3및 CaZrO3로 구성되는 그룹으로 부터 선택된 최소 하나의 상유전체이며, BaTiO3100mol당(즉, a=100), 0.2≤b≤6.0, 0.05≤c≤1.5, 0.05≤d≤2.0, 0.05≤e≤0.5, 5≤f≤30, 0.5≤g≤3 그리고 x는 0.4∼0.5인 유전체 자기 조성물로 제조된 적층세라믹 커패시터가 제공된다.Formulaa BaTiO 3 -bMgCO 3 -cMnO 2 -dY 2 O 3 -eCr 2 O 3 is represented by-f Pe-gBa x Ca (1 -x) SiO 3, wherein Pe is SrZrO3, SrTiO3, CaTiO3, and At least one dielectric material selected from the group consisting of CaZrO3 , per 100 mol of BaTiO3 (ie a = 100), 0.2 ≦ b ≦ 6.0, 0.05 ≦ c ≦ 1.5, 0.05 ≦ d ≦ 2.0, 0.05 ≦ e ≦ There are provided multilayer ceramic capacitors made of a dielectric ceramic composition wherein 0.5, 5 ≦ f ≦ 30, 0.5 ≦ g ≦ 3 and x are 0.4 to 0.5.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에서는 BT 분말에 상유전성 페로브스카이트(perovskite)구조의 페로브스카이트 "c"축 길이를 감소시킴으로써 유전율을 낮추고, 이에 따라 유전손실이 낮아진다.In the present invention, the permittivity is lowered by reducing the perovskite "c" axis length of the peroelectric perovskite structure in the BT powder, thereby lowering the dielectric loss.
상유전체(Pe)로는 SrZrO3, SrTiO3, CaTiO3및 CaZrO3로 구성되는 그룹으로 부터 선택된 최소 하나의 상유전체가 BT분말에 첨가된다. 상유전체는 BT 분말 100mol당 5-30mol로 첨가된다. 상유전체를 30mol을 초과하여 첨가하면 큐리 포인트가 저온부로 이동하면서 온도 특성이 저하되고, 5mol미만으로 첨가하면 유전상수 감소효과가 적다. MgCO3, MnO2및 Cr2O3는 MLCC의 소성 분위기가 환원분위기임으로 내환원성을 부여하기 위하여 소량 첨가된다. 즉, BT 분말 100mol당 MgCO3는 0.2-6.0mol, MnO2는 0.05-1.5mol 그리고 Cr2O3는 0.05-0.5mol로 첨가된다. 이중 MnO2가 MgCO3,및 Cr2O3보다는 효과가 뛰어나나 IR 저하 및 신뢰성 불량을 유발함으로 소량 첨가한다.Paraelectric full (Pe) roneun SrZrO3, SrTiO3, CaTiO least one paraelectric total selected from the group consisting of3 and CaZrO3 is added to BT powder. The dielectric is added at 5-30 mol per 100 mol of BT powder. If more than 30 mol of dielectric material is added, the Curie point moves to the low temperature part, and the temperature characteristic is lowered. If it is added less than 5 mol, the dielectric constant decreases less. MgCO3 , MnO2 and Cr2 O3 are added in small amounts to impart reduction resistance because the firing atmosphere of MLCC is a reducing atmosphere. That is, MgCO3 is added at 0.2-6.0 mol, MnO2 is 0.05-1.5 mol, and Cr2 O3 is 0.05-0.5 mol per 100 mol of BT powder. MnO2 is more effective than MgCO3 and Cr2 O3, but is added in small amounts because it causes IR degradation and poor reliability.
Y2O3는 도너(Donor)로서 내환원제로 사용되는 원소에 의한 산소 공급을 감소시켜 주는 전하 보상 역할을 한다. 이러한 첨가제는 서로 전하 보상의 역할을 하고, 과량 첨가시에는 고용되지 않는 2차상이 형성되어 신뢰성 저하를 유발할 수 있음으로, BT 분말 100mol당 Y2O3는 0.05-2.0mol로 첨가된다.Y2 O3 serves as a charge compensation to reduce the oxygen supply by the element used as a reducing agent as a donor. These additives play a role of charge compensation with each other, and when excessively added, a secondary phase, which is not dissolved, may be formed, thereby causing a decrease in reliability. Thus, Y2 O3 per 100 mol of BT powder is added at 0.05-2.0 mol.
나아가, V2O5, R2O3또는 이들의 혼합물이 부가적으로 저유전율 유전체 자기 조성물에 첨가될 수 있다. 다만, R2O3에서 R은 Er, Yb, La 및 Dy로 구성되는 그룹으로 부터 선택된 최소 하나의 희토류 원소이다.Furthermore, V2 O5 , R2 O3, or mixtures thereof may additionally be added to the low dielectric constant ceramic composition. In R2 O3 , R is at least one rare earth element selected from the group consisting of Er, Yb, La, and Dy.
V2O5첨가시 이는 BaTiO3100mol(즉, a=100)당 최대 2mol로 첨가된다. R2O3는 첨가되는 경우, BaTiO3100mol(즉, a=100)당 최대 10mol로 첨가된다When V2 O5 is added it is added up to 2 mol per 100 mol of BaTiO3 (ie a = 100). If R2 O3 is added, at most 10 mol per 100 mol of BaTiO3 (ie a = 100) is added
V2O5는 Y2O3와 마찬가지로 도너(Donor)로서 내환원제로 사용되는 원소에 의한 산소 공급을 감소시켜 주는 전하 보상 역할을 한다. 이러한 첨가제는 서로 전하 보상의 역할을 하고, 과량 첨가시에는 고용되지 않는 2차상이 형성되어 신뢰성 저하를 유발할 수 있다. R2O3는 큐리 포인트를 높이는 작용을 하며 10mol을 초과하는 과량으로 사용되면 이차상이 형성되고 신뢰성이 저하된다.V2 O5 , like Y2 O3 , serves as a charge compensation to reduce the oxygen supply by the element used as a reducing agent as a donor. These additives play a role of charge compensation with each other, and when excessively added, a secondary phase that is not dissolved may be formed, which may cause a decrease in reliability. R2 O3 acts to increase the Curie point and when used in excess of 10 mol, secondary phases are formed and reliability is lowered.
BaxCa(1-x)SiO3는 MLCC 특성에는 별다른 기여를 하지 않고, 소결 소제 즉, 저온에서 소결이 일어나면서 입자가 성장되지 않도록 도와주는 역할을 한다. x값은 0.4∼0.5범위이다.Bax Ca(1-x) SiO3 does not contribute much to the MLCC properties, and helps to prevent the particles from growing as the sintering agent, that is, sintering at low temperature. The x value is in the range of 0.4 to 0.5.
상기 본 발명의 유전체 자기 조성물은 종래 BT의 유전율의 약 60%에 해당하는 낮은 유전율을 갖는다. 예를들어, 종래 BT의 유전상수가 2500인 경우, 본 발명에 의한 유전체 가지 조성물의 유전율은 약 1500이다. 따라서, 본 발명의 유전율이 낮은 유전체 자기 조성물로 제조된 MLCC는 k=1500±200의 유전상수를 갖으며, 1%이하의 손실값 및 200±50MHz에서 500mΩ이하의 ESR을 충족하는 전기적 특성을 갖으며 . 또한, X8R(-55∼150℃에서의 용량 변화율이 ±15%이내)를 충족한다.The dielectric ceramic composition of the present invention has a low dielectric constant corresponding to about 60% of the dielectric constant of conventional BT. For example, when the dielectric constant of conventional BT is 2500, the dielectric constant of the dielectric branch composition according to the present invention is about 1500. Therefore, the MLCC prepared from the low dielectric constant ceramic composition of the present invention has a dielectric constant of k = 1500 ± 200, has a loss value of less than 1% and an electrical property satisfying an ESR of less than 500 mΩ at 200 ± 50 MHz. And. In addition, it satisfies X8R (the rate of change of capacity at -55 to 150 ° C is within ± 15%).
나아가, 본 발명의 유전체 자기 조성물은 유전율이 낮음으로 MLCC제작시 겹쳐지는 영역 및 적층수의 증가에 따른 ESR 증대 효과가 최소화된다. 따라서, 겹쳐지는 영역이 많아지도록 MLCC를 제조함으로써 얼라인먼드에 의한 용량 편차를 최소화할 수 있다. X8R 온도특성을 충족함으로 고온에서 사용가능한 것으로 차량등에도 적용가능하다.Furthermore, the dielectric ceramic composition of the present invention has a low dielectric constant, thereby minimizing an ESR increase effect due to an increase in the number of overlapping regions and the number of stacked layers. Therefore, by producing the MLCC so that there is a lot of overlapping area, it is possible to minimize the capacity deviation caused by the alignment. It can be used at high temperature because it meets X8R temperature characteristic and can be applied to vehicles.
이하, 실시예를 통하여 본 발명에 대하여 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.
실시예Example
1. 슬러리 제조단계1. Slurry Manufacturing Step
비교재 및 발명재 1 내지 8의 유전체 자기 조성물을 다음과 같이 제조하였다. 각각 하기 표 1의 조성이 되도록 하기 표 1의 각 성분(각 성분의 총 중량은 400g이다.), 포스페이트계 분산제(RE 610) 0.8g 그리고 PVB 바인더 0 27.6g을 혼합하여 약 24시간동안 로드밀에서 75rpm으로 밀링하였다. 용매로는 에탄올과 톨루엔이 6:4중량비로 혼합된 용액을 그리고 상기 바인더로는 Solutia B-79 레진을 사용하였다.Dielectric ceramic compositions of Comparative Materials and Inventive Materials 1 to 8 were prepared as follows. Load mill for about 24 hours by mixing each component of Table 1 (total weight of each component is 400g), 0.8g of phosphate-based dispersant (RE 610) and 27.6g of PVB binder 0 so as to have the composition of Table 1, respectively. Milling at 75 rpm. As a solvent, a solution in which ethanol and toluene were mixed at a 6: 4 weight ratio was used, and Solutia B-79 resin was used as the binder.
밀링에 사용되는 Media 3ф지르코니아 볼 350g을 충진하였다. BT 분말로 비교재 1 및 발명재 1-6에서는 Sakai BT-04를 그리고 발명재 7,8 및 비교재 2에서는 Fuji사의 HPBT-1AF를 사용하였다. SrZrO3은 Sakai상의 SZ-03을 사용하였다. BT분말과 SrZrO3를 제외한 다른 성분들과 소결조제인 BCG를 배합하여 1차 하소처리하였다. 메쉬 필터로 제조된 슬러리에서 이물질을 제거한 후, 500㎖ 날진병에 담아 밀봉한후 약 6시간 동안 에이징하여 밀링시 생성된 기포를 제거하였다.350 g of Media 3 zirconia balls used for milling were filled. As BT powder, Sakai BT-04 was used in Comparative Material 1 and Inventive Material 1-6, and HPBT-1AF from Fuji Inc. was used in Inventive Material 7, 8 and Comparative Material 2. SrZrO3 used SZ-03 on Sakai. The first calcination process was carried out by blending other ingredients except BT powder and SrZrO3 with BCG, a sintering aid. After removing the foreign matter from the slurry prepared by the mesh filter, it was sealed in a 500ml dust bottle and then aged for about 6 hours to remove bubbles generated during milling.
2. 케이싱(Cassing) 단계2. Casing Step
제조된 슬러리를 Doctor Blade Belt Caster에서 25㎛두께로 성형하였다. 이때 좌우 편차는 ±1/8㎛로 하였다. 그 후 성형된 시이트를 2장씩 겹쳐서 총 두께가 50㎛가 되도록 하였다.The prepared slurry was molded to a thickness of 25 ㎛ in Doctor Blade Belt Caster. At this time, the left and right deviations were ± 1/8 μm. Thereafter, two sheets of molded sheets were piled up so that the total thickness was 50 m.
3. 그린 칩(Green Chip) 제조단계3. Green Chip Manufacturing Stage
상기 성형 시이트에 페이스트를 인쇄하고 그 위에 새로운 시이트를 올리고, 다시 인쇄하는 방법으로 총 9층(10회)인쇄하고 탑(top)/바닥(Bottom) 커버를 위아래 200㎛이상으로 덮어 MLCC 그린바를 완성하였다.A total of 9 layers (10 times) is printed by printing a paste on the molded sheet, a new sheet is placed on it, and printed again, and the MLCC green bar is completed by covering the top / bottom cover with 200 μm or more above and below. It was.
이때 내부전극으로는 니켈을 사용하였으며, 바 완성후 150kgf/㎠으로 약 1.5분간 가압착하였다. 가압착 후, 바를 박스 오븐에서 60-100℃의 프로파일(profile) 로 약 6시간 건조하여, 페이스트중의 잔류 용매를 건조시켰다. 건조된 바를 진공포장하여 ISO 프레싱하였다. ISO 프레스는 물탱크를 넣어 700kgf/㎠으로 약 15분간 실시하였으며 물의 온도는 82-84℃였다.At this time, nickel was used as the internal electrode, and pressurized for about 1.5 minutes at 150 kgf / cm 2 after completion of the bar. After press bonding, the bars were dried for about 6 hours in a box oven at a profile of 60-100 ° C. to dry the residual solvent in the paste. The dried bar was vacuum packed and ISO pressed. ISO press was carried out for about 15 minutes at 700kgf / ㎠ with a water tank and the water temperature was 82-84 ℃.
압착이 완료된 바를 칩으로 절단하였다. 이 때 사용된 칼날의 두께는 0.1㎜이었다. 칩의 크기는 실험에 따라서 1005(1.0㎜ｘ0.5㎜), 1608(1.06㎜ｘ0.8㎜), 3216(3.2㎜ｘ1.6㎜)등으로 하였다. 실험 목적상 K2시편은 700∼1000㎛의 두께로 제작하여 유전율들을 평가하기 위해 칩과 같이 소성하였다.After the compression was completed, the bar was cut into chips. The thickness of the blade used at this time was 0.1 mm. The size of the chip was 1005 (1.0 mm 0.5 mm), 1608 (1.06 mm 0.8 mm), 3216 (3.2 mm 1.6 mm) or the like according to the experiment. For the purpose of experiment, K2 specimens were fabricated to a thickness of 700-1000㎛ and fired together with chips to evaluate the dielectric constants.
4. 가소/소성 단계4. Plasticizing / firing step
그린 칩을 A1203에 지르코니아 코팅된 세터(setter)에 1단으로 적재하여 250℃에서 22시간동안 구워서(bake-out) 바인더를 제거하였다. 가소가 완료된 칩을 1250-1350℃에서 약 27시간의 프로파일로 소성하였다. 가소 및 소성은 환원분위기하에 실시하여 내부전극의 산화를 방지하였다.The green chip was loaded in one step into a zirconia coated setter in A1203 and baked for 22 hours at 250 ° C. to remove the binder. The calcined chip was fired at a profile of about 27 hours at 1250-1350 ° C. The calcination and firing were carried out under a reducing atmosphere to prevent oxidation of the internal electrodes.
5. 외부전극 소성 단계5. External electrode firing step
가소가 완료된 칩을 Planatary Mill에서 150rpm으로 1시간동안 연마하였다. 이때 연마제로는 SIC를 사용하였다. 연마 후, Cu Paste를 MLCC양 끝에 디핑한 후에 건조하여 다시 750℃, 산소분압 7ppm으로 외부전극 Cu를 소성하였다. 외부전극 소성이 완료된 칩은 Ni/Sn-Pb로 도금 처리하여 최종 MLCC를 얻었다.The calcined chip was polished for 1 hour at 150 rpm in the Planatary Mill. At this time, SIC was used as the abrasive. After polishing, Cu Paste was dipped at both ends of MLCC, dried, and calcined at 750 ° C. with an oxygen partial pressure of 7 ppm. The chip after the external electrode firing was completed was plated with Ni / Sn-Pb to obtain a final MLCC.
상기 표 1에서 알 수 있듯이, 발명재로 제조된 MLCC는 약 1500±200의 유전상수를 나타냈다.As can be seen in Table 1, the MLCC prepared by the invention exhibited a dielectric constant of about 1500 ± 200.
상기 표 2에서와 같이 본 발명재로된 MLCC는 전기용량, 손실값 및 절연저항등의 전기적 특성을 만족한다.As shown in Table 2, the MLCC made of the present invention satisfies electrical characteristics such as capacitance, loss value, and insulation resistance.
발명재로 제조된 MLCC는 표 3에서와 같이 500mΩ이하의 ESR을 충족하는 것이다.The MLCC manufactured by the invention meets the ESR of 500 mΩ or less as shown in Table 3.
저유전율 유전체의 사용으로 저용량 MLCC 제조시 적층수와 인쇄층 오버랩 부분을 증가시킬수 있으며 이로 인한 정전용량 향상 및 ESR 감소 효과를 볼 수 있다.The use of low dielectric constant dielectrics can increase the number of stacked layers and printed layer overlaps when manufacturing low-capacity MLCCs, resulting in increased capacitance and reduced ESR.
이렇게 설계된 MLCC는 k=1500±200의 유전상수를 갖으며 낮은 손실값 및 ESR = 500mΩ이하(200±50MHz)의 값을 보인다. 그리고 온도 특성은 X8R을 만족한다.The designed MLCC has a dielectric constant of k = 1500 ± 200, low loss value and less than ESR = 500mΩ (200 ± 50MHz). And the temperature characteristic satisfies X8R.
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2001-0081018AKR100444226B1 (en) | 2001-12-19 | 2001-12-19 | A Dielectric Composition Having Low Dielectric Constant And A Multi Layered Ceramic Capacitor Prepared By Using The Same |
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2001-0081018AKR100444226B1 (en) | 2001-12-19 | 2001-12-19 | A Dielectric Composition Having Low Dielectric Constant And A Multi Layered Ceramic Capacitor Prepared By Using The Same |
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| KR20030050559A KR20030050559A (en) | 2003-06-25 |
| KR100444226B1true KR100444226B1 (en) | 2004-08-11 |
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| KR10-2001-0081018AExpired - Fee RelatedKR100444226B1 (en) | 2001-12-19 | 2001-12-19 | A Dielectric Composition Having Low Dielectric Constant And A Multi Layered Ceramic Capacitor Prepared By Using The Same |
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| KR100790682B1 (en)* | 2006-09-14 | 2008-01-02 | 삼성전기주식회사 | Glass composition for low temperature sintering, glass frit, dielectric composition, multilayer ceramic capacitor using the same |
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| US5361187A (en)* | 1993-03-11 | 1994-11-01 | Ferro Corporation | Ceramic dielectric compositions and capacitors produced therefrom |
| US5646080A (en)* | 1995-11-20 | 1997-07-08 | Tam Ceramics, Inc. | Dielectric stable at high temperature |
| JPH1025157A (en)* | 1996-07-08 | 1998-01-27 | Murata Mfg Co Ltd | Dielectric ceramic composition and multilayer capacitor |
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