KR20180115373A - Method of dielectric ceramic composition for mlcc - Google Patents
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Abstract
Description
본 발명은 고용량이면서 높은 신뢰성을 가지는 MLCC용 유전체 조성물의 제조 방법에 관한 것이다.The present invention relates to a method for producing a dielectric composition for MLCC having high capacity and high reliability.
적층 세라믹 커패시터(Multilayer Ceramic Capacitor, MLCC)는 부피가 작으면서 신뢰성과 내전압 특성이 좋고 실장이 용이한 특성이 있어, 컴퓨터, 휴대폰, 각종 통신 기기 등의 부품으로 널리 사용되고 있다.Multilayer ceramic capacitors (MLCCs) are widely used for components such as computers, mobile phones, and various communication devices because they have small volume, good reliability, good withstand voltage characteristics, and easy mounting.
이러한 MLCC는 복수의 세라믹 유전체 시트, 상기 복수의 세라믹 유전체 시트 사이에 삽입된 내부전극 및 상기 내부전극에 전기적으로 접속된 외부전극을 포함한다.The MLCC includes a plurality of ceramic dielectric sheets, internal electrodes interposed between the plurality of ceramic dielectric sheets, and external electrodes electrically connected to the internal electrodes.
최근, 기후 환경이 갈수록 가혹해짐에 따라 MLCC는 가혹한 환경(고온, 다습, 고압, 고ESD 등)에서의 신뢰성(즉, 절연 저항(Insulation Resistance; IR) 특성)이 요구되고 있으며, 각종 IT기기의 복합화에 따라 전자 부품의 소형화 요구가 지속되고 있다. 이에 따라, MLCC는 일정한 부피에서 더 높은 용량과 더 향상된 신뢰성이 요구되고 있다.Recently, as the climate environment becomes increasingly severe, MLCCs are required to have reliability (i.e. Insulation Resistance (IR) characteristics) in harsh environments (high temperature, high humidity, high pressure and high ESD) There is a continuing demand for miniaturization of electronic components according to the complexity. Accordingly, MLCCs are required to have higher capacity and higher reliability at a certain volume.
이러한 초고용량 고신뢰성 MLCC 제조에 있어서 가장 중요한 것은 얇은 유전체 층의 실현이라고 할 수 있다. 유전체의 유전용량은 유전체 층의 두께가 얇을수록 그리고 유전체 층의 적층 수가 늘어날수록 증가하게 되는데 유전체 층의 박층화가 실현될수록 일정한 부피에 더 많은 유전체 층을 쌓을 수 있게 되어 전체 유전용량은 증가하게 되기 때문이다.The most important thing in manufacturing such a high-capacity, high-reliability MLCC is realization of a thin dielectric layer. The dielectric capacity of the dielectric increases as the thickness of the dielectric layer becomes thinner and as the number of stacks of dielectric layers increases. As the thickness of the dielectric layer becomes thinner, more dielectric layers can be stacked at a constant volume, to be.
최근 유전체 층은 두께 2㎛ 이하 심지어 두께 0.5㎛ 이하이면서 적층되는 수는 300층 이상, 더 나아가 1000층 이상인 고신뢰성의 고용량 MLCC에 대한 요구가 증대되고 있다.Recently, the demand for high-reliability high-capacity MLCC having a thickness of 2 탆 or less, thickness of 0.5 탆 or less, stacking number of 300 layers or more, and 1000 layers or more has been recently increased.
유전체 층의 박층화를 위해서는, 주로 사용되는 유전체 분말인 BaTiO3 분말의 입도 미세화 및 균일화가 매우 중요한데, 이러한 미세한 BaTiO3 분말을 얻기 위해는 주로 수열합성법이 많이 사용되고 있다.In order to make the dielectric layer thin, it is very important to miniaturize and uniformize the particle size of the BaTiO 3 powder, which is a dielectric powder mainly used. In order to obtain such a fine BaTiO 3 powder, a hydrothermal synthesis method is mainly used.
한편, 수열합성법으로 제조할 수 있는 유전특성이 있는 정방정(tetragonal)계 결정구조의 BaTiO3 분말 입도는 일반적으로 100nm 이상이며, 그 이하의 입도에서는 유전특성이 없는 입방정(cubic)계 결정구조의 BaTiO3가 합성된다.On the other hand, BaTiO 3 powder having a dielectric structure with a dielectric property capable of being produced by hydrothermal synthesis has a grain size of 100 nm or more and a cubic crystal structure BaTiO 3 is synthesized.
이러한 100nm 이하인 입방정 BaTiO3 는 열처리를 통해 유전특성을 갖는 결정구조로 변환시킬 수 있으나, 열처리 과정에 미세한 입도가 유지되지 않고 커지게 되는 문제가 있다.The cubic BaTiO 3 having a thickness of 100 nm or less can be converted into a crystal structure having a dielectric property through heat treatment, but the fine grain size is not maintained in the heat treatment process, and thus the crystal grain size is increased.
또한, 유전체 층의 박층화를 위해 중요한 부분은 BaTiO3와 함께 혼합되어 유전체 층을 이루는 다양한 첨가제의 균일한 분산이라 할 것이다. 일반적으로 유전체 층은 유전체 분말인 BaTiO3와 함께 신뢰성 향상, 내환원성 향상, 입성장 억제, 소결온도 저하 등의 목적으로 다양한 첨가제가 포함되는데, 최종 유전체 층은 이러한 다양한 첨가제 들을 유전체 분말과 함께 균일하게 분산 처리하여 그린 시트를 제조한 후 소결하여 만들어지게 된다. 이러한 유전체 층을 제조할 때 첨가제와 유전체 분말의 균일 분산이 이루어지지 않게 되면 박층화 또한 어려워지게 된다.In addition, an important part for thinning the dielectric layer will be a uniform dispersion of various additives in the dielectric layer mixed with BaTiO 3 . In general, the dielectric layer includes various additives for the purpose of improving reliability, improving reduction resistance, suppressing grain growth, and lowering sintering temperature, together with dielectric powder BaTiO 3. The final dielectric layer is formed by uniformly mixing these various additives with the dielectric powder Dispersed to prepare a green sheet, and then sintered. If uniform dispersion of the additive and the dielectric powder is not achieved in the production of such a dielectric layer, thinning becomes difficult.
본 발명의 목적은 얇으면서 높은 신뢰성을 가지는 유전체 층을 형성할 수 있는 MLCC용 유전체 조성물의 제조 방법을 제공하는데 있다.An object of the present invention is to provide a method for producing a dielectric composition for MLCC capable of forming a thin and highly reliable dielectric layer.
상기 과제를 달성하기 위해 본 발명은, (a) Ho, Yb, Gd, Dy, Sm 및 Y 중에서 선택되는 1종 또는 2종 이상의 금속 산화물로 이루어진 A 성분과, W, Mo 및 V 중에서 선택되는 1종 또는 2종 이상의 금속 산화물로 이루어진 B 성분과, Mn, Cr 및 Co 중에서 선택되는 1종 또는 2종 이상의 금속 산화물로 이루어진 C 성분과, Mg, Ca, 및 Ba 중에서 선택되는 1종 또는 2종 이상의 탄산염으로 이루어진 D 성분을 혼합 및 분산하여 첨가제 슬러리를 제조하는 단계; (b) 상기 첨가제 슬러리에 BaTiO3 분말을 혼합하고 하소하는 단계; 및 (c) 상기 하소된 분말에 Si, Li, Al 및 B 중에서 선택되는 1종 또는 2종 이상의 산화물로 이루어진 E 성분을 혼합하여 분산하는 단계;를 포함하며, 상기 (a) 및 (c) 단계에서, 상기 BaTiO3 100몰을 기준으로, 상기 A 성분은 0.5~2.0몰, 상기 B 성분은 0.2~0.8몰, 상기 C 성분은 0.1~0.5몰, 상기 D 성분은 0.2~0.8몰, 상기 E 성분은 0.2~1.0몰의 비율로 혼합되며, 상기 BaTiO3 분말은 수열합성법으로 제조된 입방정 결정구조를 가지며 그 입도(D50)가 20~80nm인, 적층 세라믹 커패시터용 유전체 조성물의 제조 방법을 제공한다.(A) an A component composed of one or two or more metal oxides selected from Ho, Yb, Gd, Dy, Sm and Y; and an A component selected from W, Mo and V A component C composed of one or more metal oxides selected from the group consisting of Mn, Cr and Co, and one or more elements selected from Mg, Ca and Ba Mixing and dispersing a component D of a carbonate to prepare an additive slurry; (b) mixing and calcining BaTiO 3 powder into the additive slurry; And (c) mixing and dispersing an E component composed of one or more oxides selected from Si, Li, Al and B into the calcined powder, wherein (a) and (c) in the BaTiO 3 based on 100 moles of the component a is 0.5 to 2.0 mol, and the B component is 0.2% to 0.8 mole, the component C is 0.1 to 0.5 mole, the component D is 0.2 and 0.8 molar, the component E Wherein the BaTiO 3 powder has a cubic crystal structure prepared by hydrothermal synthesis and has a particle size (D50) of 20 to 80 nm. The present invention also provides a method for producing a dielectric composition for a multilayer ceramic capacitor.
본 발명에 따르면, 고신뢰성 및 박형화에 필수적인 코어-쉘 구조(코어는 BaTiO3이고 쉘은 여러 첨가제로 이루어지는)의 유전체 조성물을 얻을 수 있다.According to the present invention, it is possible to obtain a dielectric composition of a core-shell structure (core is BaTiO 3 and shell is made of various additives) essential for high reliability and thinning.
또한, 입도가 균일하고 작은 입방정의 BaTiO3 를 사용함으로써 최종 유전체 조성물의 입도 균일화와 미세화를 가능하게 하며, 이를 통해 높은 신뢰성과 고용량의 MLCC 제조를 가능하게 한다.In addition, a small cubic BaTiO 3 Enables the uniformization and fineness of the particle size of the final dielectric composition, thereby enabling high reliability and high-capacity MLCC production.
이하 본 발명의 바람직한 실시 예에 따른 방법에 대해 상세하게 설명하겠지만 본 발명이 하기의 실시예들에 제한되는 것은 아니다. 따라서 해당 분야에서 통상의 지식을 가진 자라면 본 발명의 기술적 사상을 벗어나지 않는 범위 내에서 본 발명을 다양하게 변경할 수 있음은 자명하다.Hereinafter, a method according to a preferred embodiment of the present invention will be described in detail, but the present invention is not limited to the following embodiments. Accordingly, it is obvious that those skilled in the art can variously change the present invention without departing from the technical idea of the present invention.
본 발명에 따른 유전체 조성물의 제조 방법은 우선 유전체 조성물에 포함되며 소결 보조제가 아닌 첨가제를 먼저 혼합 및 분산 처리하는 1 단계, 이러한 분산 처리된 혼합물에 BaTiO3를 투입하고 다시 혼합, 분산 후 하소 처리를 하는 2 단계 및 하소 처리된 혼합물에 추가 첨가제(소결 보조제)를 혼합 및 분산 처리하는 3 단계를 포함한다.The method for preparing the dielectric composition according to the present invention comprises a first step of first mixing and dispersing the additive which is contained in the dielectric composition and is not a sintering aid, and the BaTiO 3 is added to the thus dispersed mixture, And a third step of mixing and dispersing an additional additive (sintering aid) to the calcined mixture.
상기 유전체 조성물은 BaTiO3, A, B, C, D 및 E 물질을 포함한다.Wherein the dielectric composition comprises a BaTiO 3, A, B, C , D and E materials.
이중, 상기 A는 Ho, Yb, Gd, Dy, Sm 및 Y로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물이 바람직하고, 그 함량은 BaTiO3 100몰 대비 0.5~2.0몰이 바람직하다.Of these, A is preferably one or more metal oxides selected from the group consisting of Ho, Yb, Gd, Dy, Sm and Y, and the content thereof is preferably 0.5 to 2.0 moles per 100 moles of BaTiO 3 .
또한, 상기 B는 W, Mo 및 V로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물이 바람직하고, 그 함량은 BaTiO3 100몰 대비 0.2~0.8몰이 바람직하다.The B is preferably at least one metal oxide selected from the group consisting of W, Mo and V, and its content is preferably 0.2 to 0.8 mol based on 100 mol of BaTiO 3 .
또한, 상기 C는 Mn, Cr 및 Co로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물이 바람직하고, 그 함량은 BaTiO3 100몰 대비 0.1~0.5몰이 바람직하다.The C is preferably at least one metal oxide selected from the group consisting of Mn, Cr and Co, and the content thereof is preferably 0.1 to 0.5 mol based on 100 mol of BaTiO 3 .
또한, 상기 D는 Mg, Ca, 및 Ba으로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 탄산염이 바람직하고, 그 함량은 BaTiO3 100몰 대비 0.2~0.8몰이 바람직하다.The above D is preferably at least one carbonate selected from the group consisting of Mg, Ca and Ba, and its content is preferably 0.2 to 0.8 mol, based on 100 mol of BaTiO 3 .
또한, 상기 E는 Si, Li, Al 및 B으로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 산화물이 바람직하고, 그 함량은 BaTiO3 100몰 대비 0.2~1.0몰이 바람직하다.The E is preferably at least one oxide selected from the group consisting of Si, Li, Al and B, and its content is preferably 0.2 to 1.0 mole based on 100 moles of BaTiO 3 .
또한, 상기 A, B, C, D 및 E를 구성하는 산화물 및 탄산염의 평균 입도는, 제조 과정을 통해 BaTiO3 입자의 표면에 코팅되어 쉘을 형성하여 최종적으로 코어-쉘 구조의 분말을 형성할 수 있도록, 10nm 이하가 바람직하다.In addition, the average particle size of the oxides and carbonate constituting A, B, C, D and E is coated on the surface of the BaTiO 3 particles through the manufacturing process to form a shell to finally form a core-shell structure powder 10 nm or less is preferable.
본 발명에서 상기 2 단계에 사용된 BaTiO3는 수열합성법으로 제조되어 결정구조상 입방정 구조를 가지는 것으로, 그 입도(D50)는 20nm 미만일 경우 화학양론비에 맞는 BaTiO3를 제조하기 어렵고, 80nm 초과일 경우 미세한 유전체 층을 형성하기 어려우므로 20~80nm가 바람직하고, 보다 바람직한 입도(D50)은 30~60nm일 수 있다.BaTiO 3 used in the second step of the present invention is prepared by hydrothermal synthesis and has a cubic crystal structure on the crystal structure. When the particle size (D50) is less than 20 nm, it is difficult to produce BaTiO 3 meeting the stoichiometric ratio. Since it is difficult to form a fine dielectric layer, it is preferably 20 to 80 nm, and more preferably, the particle size (D50) may be 30 to 60 nm.
상기 입방정 결정구조를 갖는 BaTiO3는 하소 공정을 통해 유전특성이 있는 정방정 구조의 BaTiO3로 변환된다. 이때, 하소 온도는 600℃ 미만일 경우 첨가제와 BaTiO3와의 안정적인 코어-쉘 구조를 형성하기 어렵고, 900℃ 초과일 경우에는 하소 후 과도한 입성장이 발생하므로, 600~900℃가 바람직하다.BaTiO 3 having a cubic crystal structure is converted to BaTiO 3 in a tetragonal structure with a dielectric property through a calcination process. If the calcination temperature is less than 600 ° C, it is difficult to form a stable core-shell structure between the additive and BaTiO 3. If the calcination temperature is higher than 900 ° C, 600 ° C to 900 ° C is preferable because excessive grain growth occurs after calcination.
또한, 하소 후 혼합 분말의 입도는 100nm 미만일 경우 정방정의 결정구조가완전히 나타나지 않아 충분한 유전특성을 나타내기 어렵고, 200nm 초과일 경우 미세한 유전체 층을 형성하기 어려우므로, 100~200nm인 것이 바람직하다.When the particle size of the mixed powder after calcination is less than 100 nm, the tetragonal crystal structure does not completely appear and it is difficult to exhibit sufficient dielectric characteristics. When the particle size exceeds 200 nm, it is difficult to form a fine dielectric layer.
또한, 본 발명에서는 소결 온도 저하 목적으로 첨가하게 되는 소결 보조제를 다른 첨가제와 BaTiO3와의 혼합 및 하소가 완료된 후에 혼합 및 분산 처리함으로써 하소 시에 BaTiO3의 과도한 입성장이 일어나는 것을 방지한다.Further, in the present invention, the sintering aid added for the purpose of lowering the sintering temperature is mixed and dispersed after completion of mixing and calcination of BaTiO 3 with other additives, thereby preventing the excessive growth of BaTiO 3 in the calcination.
[실시예][Example]
본 발명의 바람직한 실시예에 따른 유전체 조성물의 제조 단계는, 첨가제 분산 슬러리를 제조하는 1 단계와, 제조된 첨가제 분산 슬러리와 BaTiO3 분말을 혼합하고, BaTiO3의 결정구조를 변환하는 하소하는 2단계와, 하소된 분말을 소결 보조제와 혼합하는 3단계를 포함하여 이루어지며, 구체적인 공정은 다음과 같다.The step of preparing the dielectric composition according to a preferred embodiment of the present invention comprises a first step of preparing an additive dispersion slurry, two calcination steps of mixing the prepared additive dispersion slurry and BaTiO3 powder and transforming the crystal structure of BaTiO3, And a third step of mixing the calcined powder with the sintering aid. The specific process is as follows.
1 단계Stage 1 (첨가제 분산 슬러리 제조 단계) (Preparation step of additive dispersed slurry)
평균 입도가 10nm 이하인, Ho, Yb, Gd, Dy, Sm 및 Y로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물과, W, Mo 및 V로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물과, Mn, Cr 및 Co로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 금속 산화물과, Mg, Ca, 및 Ba으로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 탄산염으로 이루어진 분말을, 아래 공정에서 투입할 BaTiO3 분말 대비 몰비로 각각 100:0.5~2.0, 100:0.2~0.8, 100:0.1~0.5, 100:0.2~0.8로 칭량하여 습식으로 혼합 및 분산시킨다.One or more metal oxides selected from the group consisting of Ho, Yb, Gd, Dy, Sm and Y having an average particle size of 10 nm or less and one or two or more species selected from the group consisting of W, Mo and V A metal oxide and at least one metal oxide selected from the group consisting of Mn, Cr and Co and at least one carbonate selected from the group consisting of Mg, Ca and Ba, 100: 0.2 to 0.8, 100: 0.1 to 0.5, and 100: 0.2 to 0.8, respectively, at a molar ratio relative to the BaTiO 3 powder to be added in the process.
이때, 분산 공정에서 용매는 탈이온수 또는 알코올을 사용하고, 0.1mm 직경의 지르코니아 볼을 이용한 비즈밀로 균일하게 혼합 및 분산시켜 첨가제가 분산 슬러리를 제조한다.At this time, in the dispersing step, deionized water or alcohol is used as a solvent, and the mixture is uniformly mixed and dispersed with a bead mill using a zirconia ball having a diameter of 0.1 mm to prepare an additive dispersed slurry.
2 단계Step 2 ( ( BaTiOBaTiO 33 분말 혼합, 분산, 건조 및 Powder mixing, dispersion, drying and 하소calcination 단계) step)
상기 첨가제 분산 슬러리에 전술한 혼합비로 BaTiO3 분말을 투입하고, 0.1mm 지르코니아 볼을 이용한 비즈밀을 이용하여 분산시킨다.In the above additive dispersion slurry, BaTiO 3 Powder was added and dispersed using a bead mill using 0.1 mm zirconia balls.
이때, BaTiO3 분말은 수열합성법으로 제조한 입도 20~80nm의 입방정 결정구조를 갖는 것을 사용한다.At this time, BaTiO 3 The powder has a cubic crystal structure of 20 to 80 nm in particle size prepared by hydrothermal synthesis.
분산된 BaTiO3 분말을 포함하는 슬러리는 분무 건조기를 사용하여 액적 형태로 분무하면서 건조하여, 10nm 이하의 입도를 갖는 첨가제 분말들이 BaTiO3 입자와 고르게 분산된 상태가 되도록 한다.The dispersed BaTiO 3 The slurry containing the powder was sprayed and dried in a droplet form using a spray drier, and the additive powders having a particle size of 10 nm or less were dispersed in BaTiO 3 So as to be evenly dispersed with the particles.
이어서, 박스 로 또는 터널식 로를 사용하여, 600℃에서 2시간 동안 하소하며, 이 하소 과정에서 입방정 결정구조를 갖는 BaTiO3는 정방정 결정구조로 변환된다.Subsequently, calcination is performed at 600 ° C for 2 hours using a box furnace or a tunnel furnace, and BaTiO 3 having a cubic crystal structure is converted into a tetragonal crystal structure.
3 단계Step 3 ( ( 소결보조제Sintering aid 혼합 단계) Mixing step)
하소된 분말에, Si, Li, Al 및 B로 이루어진 그룹으로부터 선택되는 1종 또는 2종 이상의 산화물을 투입된 BaTiO3 분말 대비 몰비로 100:0.2~1.0가 되도록 칭량하여 투입하고 혼합 및 분산 처리하여 최종 유전체 조성물을 얻게 된다.One or more oxides selected from the group consisting of Si, Li, Al, and B were weighed so as to have a molar ratio of 100: 0.2 to 1.0 based on the amount of the BaTiO 3 powder added to the calcined powder, A dielectric composition is obtained.
여기서 혼합 및 분산은 직경 0.1mm 지르코니아 볼을 이용한 비즈밀을 이용하고 최종 분무 건조기를 이용하여 건조함으로써, 소결보조제가 고르게 분산된 유전체 조성물을 얻는다.Here, the mixing and dispersion are performed by using a bead mill using a zirconia ball having a diameter of 0.1 mm and drying using a final spray drier to obtain a dielectric composition in which the sintering aid is evenly dispersed.
아래 표 1~3은 상기 방법으로 제조된 유전체 조성물의 조성, 공정 조건 및 유전체 층 두께에 따른 MLCC 특성에 대한 구체적인 예를 나타낸 것이다. 아래 표에서 HALT(h)는 가속수명시험(Highly Accelerated Life Test)을 의미하고, 각 성분의 첨가량 수치는 mol을 기준으로 한다. 가속수명시험은 150℃에서 20 KV/mm 직류전압을 인가하여 수행되었다.Tables 1 to 3 below show specific examples of MLCC characteristics according to the composition, process conditions, and dielectric layer thickness of the dielectric composition prepared by the above method. In the table below, HALT (h) stands for Highly Accelerated Life Test, and the value of each component is based on mol. The accelerated life test was carried out by applying a DC voltage of 20 KV / mm at 150 ° C.
가속수명시험에 사용된 샘플은 아래와 같이 제작되었다.The samples used in the accelerated life test were made as follows.
상술한 방법에 따라 제조된 유전체 조성물을 비율에 따라, 바인더, 용매 등과 혼합 및 분산하여 페이스트를 제작하여 박막을 만든다. 이 표면에 스크린 인쇄를 통해 니켈 또는 니켈 합금 전극을 인쇄하여 적층한다. 이후 CIP(Cool Isostatic Press)를 행한 후 절단하였으며, 절단된 시편들은 300℃에서 열처리하여 결합제를 제거한 후 터널 로 또는 튜브 로를 이용하여 환원분위기에서 소결을 행하여 유전특성 측정을 위한 표준시편을 제조하였다.The dielectric composition prepared according to the method described above is mixed with a binder, a solvent or the like in accordance with the ratio and dispersed to prepare a paste to form a thin film. A nickel or nickel alloy electrode is printed on the surface by screen printing and laminated. After the CIP (Cool Isostatic Press) was performed, the cut specimens were annealed at 300 ° C to remove the binder, and then sintered in a reducing atmosphere using a tunnel or a tube furnace to prepare standard specimens for measurement of dielectric properties .
(℃)Calcination temperature
(° C)
(㎛)Medium thickness
(탆)
온도
(℃)calcination
Temperature
(° C)
(㎛)Medium thickness
(탆)
(㎛)Medium thickness
(탆)
상기 표 1~3에서 확인되는 바와 같이, 본 발명에 따른 유전체 조성물을 사용하여 MLCC를 제작할 경우, 매우 얇은 두께로 유전체 층을 형성하더라도 높은 신뢰성을 확보할 수 있게 된다.As can be seen from Tables 1 to 3, when MLCCs are manufactured using the dielectric composition according to the present invention, high reliability can be ensured even when a dielectric layer is formed with a very small thickness.
Claims (4)
(b) 상기 첨가제 슬러리에 BaTiO3 분말을 혼합하고 하소하는 단계; 및
(c) 상기 하소된 분말에 Si, Li, Al 및 B 중에서 선택되는 1종 또는 2종 이상의 산화물로 이루어진 E 성분을 혼합하여 분산하는 단계;를 포함하며,
상기 (a) 및 (c) 단계에서, 상기 BaTiO3 100몰을 기준으로, 상기 A 성분은 0.5~2.0몰, 상기 B 성분은 0.2~0.8몰, 상기 C 성분은 0.1~0.5몰, 상기 D 성분은 0.2~0.8몰, 상기 E 성분은 0.2~1.0몰의 비율로 혼합되며,
상기 BaTiO3 분말은 수열합성법으로 제조된 입방정 결정구조를 가지며 그 입도(D50)가 20~80nm인, 적층 세라믹 커패시터용 유전체 조성물의 제조 방법.(a) a B component composed of one or more metal oxides selected from Ho, Yb, Gd, Dy, Sm and Y and one or more metal oxides selected from W, Mo and V, Component and a component C composed of one or more kinds of metal oxides selected from Mn, Cr and Co and a component D composed of one or more kinds of carbonates selected from Mg, Ca and Ba are mixed and dispersed Preparing an additive slurry;
(b) mixing and calcining BaTiO 3 powder into the additive slurry; And
(c) mixing and dispersing the calcined powder with an E component composed of one or more oxides selected from Si, Li, Al and B,
Wherein (a) and (c) in step, the BaTiO 3 based on 100 moles of the component A is 0.5 to 2.0 mol, and the B component is 0.2% to 0.8 mole, the component C is 0.1 to 0.5 mole, the component D Is 0.2 to 0.8 mol and the E component is mixed in a ratio of 0.2 to 1.0 mol,
Wherein the BaTiO 3 powder has a cubic crystal structure prepared by hydrothermal synthesis and has a particle size (D50) of 20 to 80 nm.
상기 (a) 단계의 분산은, 용매를 탈이온수 또는 알코올을 사용하는, 적층 세라믹 커패시터용 유전체 조성물의 제조 방법.The method according to claim 1,
The dispersion of step (a) uses deionized water or alcohol as the solvent. The method of producing a dielectric composition for a multilayer ceramic capacitor,
상기 (b) 단계에서의 하소는, 600~900℃에서 이루어지는, 적층 세라믹 커패시터용 유전체 조성물의 제조 방법.3. The method according to claim 1 or 2,
Wherein the calcination in the step (b) is performed at 600 to 900 占 폚.
상기 (b) 단계 완료 후, 혼합 분말의 평균 입도는 100~200nm인, 적층 세라믹 커패시터용 유전체 조성물의 제조 방법.3. The method according to claim 1 or 2,
Wherein the average particle size of the mixed powder after the completion of the step (b) is 100 to 200 nm.
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CN114999817A (en) * | 2022-06-20 | 2022-09-02 | 山东国瓷功能材料股份有限公司 | Dielectric material for thin dielectric X7R characteristic MLCC and preparation method thereof |
US11776744B2 (en) | 2020-05-19 | 2023-10-03 | Samhwa Capacitor Co., Ltd. | Multilayer ceramic capacitor and manufacturing method thereof |
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US11776744B2 (en) | 2020-05-19 | 2023-10-03 | Samhwa Capacitor Co., Ltd. | Multilayer ceramic capacitor and manufacturing method thereof |
CN114999817A (en) * | 2022-06-20 | 2022-09-02 | 山东国瓷功能材料股份有限公司 | Dielectric material for thin dielectric X7R characteristic MLCC and preparation method thereof |
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