KR970001063B1 - Ceramic dielectric composition - Google Patents
Ceramic dielectric composition Download PDFInfo
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- KR970001063B1 KR970001063B1 KR1019940008361A KR19940008361A KR970001063B1 KR 970001063 B1 KR970001063 B1 KR 970001063B1 KR 1019940008361 A KR1019940008361 A KR 1019940008361A KR 19940008361 A KR19940008361 A KR 19940008361A KR 970001063 B1 KR970001063 B1 KR 970001063B1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/472—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on lead titanates
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
내용없음.None.
Description
본 발명은 Pb(Mg1/3Nb2/3)O3계(이하, PMN으로 약칭함) 세라믹 유전체 조성물에 관한 것으로, 특히 PMN을 주성분으로 하고 여기에 소량의 CaO와 CuO를 첨가함으로써 유전율을 향상시킴과 아울러 소성온도를 저하시킬 수 있도록 한 고유전율 저온소성용 세라믹 조성물에 관한 것이다.The present invention relates to a Pb (Mg 1/3 Nb 2/3 ) O 3 based (hereinafter abbreviated as PMN) ceramic dielectric composition, and in particular, the dielectric constant is reduced by adding a small amount of CaO and CuO The present invention relates to a ceramic composition for low dielectric constant low-temperature firing that improves and lowers the firing temperature.
종래의 PMN계 유전체로서 우수한 특성을 나타내고 있는 조성의 경우 유전율은 20,000정도이고 소성온도는 1100℃정도로서, 특히 PMN계 세라믹 유전체 중에서도 유전율이 가장 높은 조성으로서는 (1-x)PMN+xPbTiO3(이하, PT로 약칭함,X=0.01∼0.15)로 알려지고 있다.The composition exhibiting excellent properties as a conventional PMN-based dielectric has a dielectric constant of about 20,000 and a firing temperature of about 1100 ° C. In particular, the composition having the highest dielectric constant among PMN-based ceramic dielectrics is (1-x) PMN + xPbTiO 3 (hereinafter, Abbreviated as PT, X = 0.01 to 0.15).
세라믹 유전체는 캐패시터를 비롯한 각종 전기, 전자소자의 재료로 사용되어 이들 소자의 소형화 및 제반 특성의 향상에 크게 기여하고 있으며, 최근에 이르러 많은 연구자들에 의해 보다 나은 특성을 갖는 새로운 조성의 개발을 위한 노력이 활발하게 진행되는 바, 그 연구개발의 주된 과제중의 하나로 소자의 소형화에 영향을 미치는 유전율을 보다 향상시키고 제조비용의 측면에서 소성온도를 낮출 수 있는 새로운 조성의 세라믹 유전체의 개발이 차지하고 있다.Ceramic dielectrics are used as materials for various electrical and electronic devices, including capacitors, which greatly contributes to the miniaturization and improvement of various properties of these devices. In recent years, many researchers have been working to develop new compositions having better properties. One of the main challenges of the research and development is the development of a ceramic dielectric with a new composition that can further improve the dielectric constant affecting the miniaturization of the device and lower the firing temperature in terms of manufacturing cost. .
따라서 본 발명은 세라믹 유전체의 유전율을 향상시키고 소성온도를 저하시킬 수 있는 새로운 조성으로서 기존의 PMN+PT 조성에 소량의 CaO와 CuO를 첨가하여 이루어진 고유전율 저온소성용 세라믹 유전체 조성물을 제공함에 발명의 목적이 있다.Accordingly, the present invention provides a ceramic dielectric composition for high dielectric constant low temperature firing made by adding a small amount of CaO and CuO to an existing PMN + PT composition as a new composition capable of improving the dielectric constant of the ceramic dielectric and lowering the firing temperature. There is a purpose.
본 발명 세라믹 유전체 조성물의 구체적인 조성은 다음과 같다.The specific composition of the ceramic dielectric composition of the present invention is as follows.
여기서, x=0.01∼0.15Where x = 0.01 to 0.15
y=0.001∼0.02y = 0.001 to 0.02
z=0.01∼0.15z = 0.01 to 0.15
상기 조성의 본 발명 세라믹 유전체는, 먼저 PMN와 PT를 각각 합성한 후에 이들 PMN과 PT에 CaO와 CuO를 첨가하여 일반적인 세라믹 제조공정에 따라 혼합→하소→분쇄→성형→소성을 행하는 제조공정을 통하여 제조한다.The ceramic dielectric of the above composition is first synthesized with PMN and PT, and then CaO and CuO are added to the PMN and PT, and then mixed, calcined, pulverized, molded, and fired according to a general ceramic manufacturing process. Manufacture.
이때, PMN은 PbO+MgO+Nb2O5직접 혼합에 의해서는 상합성이 거의 불가능하므로 1982년에 S.L. Swartz와 T.R. Shrout가 제안한 콜럼바이트 프리커서(Columbite precursor)방법, 즉 MgNb2O6를 먼저 합성한 후에 이를 PbO와 반응시키는 방법을 사용하여 PMN을 제조하는 것이 바람직하다.At this time, since PMN is almost impossible by PbO + MgO + Nb 2 O 5 direct mixing, the Columbite precursor method proposed by SL Swartz and TR Shrout in 1982, that is, MgNb 2 O 6 is used first. It is preferable to produce PMN using a method of synthesis and then reacting it with PbO.
본 발명의 세라믹 유전체 조성물은 유전율이 20,000 이상(최대 24,000)이고 소결온도가 950℃ 이하의 특성을 나타내는데, 이는 종래의 PMN+PT계 조성에 비해 다음과 같은 작용효과상의 장점을 지니고 있다.The ceramic dielectric composition of the present invention exhibits a dielectric constant of 20,000 or more (maximum 24,000) and a sintering temperature of 950 ° C. or less, which has the following advantages over the conventional PMN + PT-based composition.
첫째, 유전율이 최대 20% 정도 높으므로 같인 크기인 경우 정전용량이 20% 증가하며, 같은 정전용량인 경우 소자의 크기를 보다 줄일 수 있으므로 소형화에 유리하다.First, since the dielectric constant is up to 20% higher, the capacitance of the same size increases by 20%, and the same capacitance can reduce the size of the device more advantageous to miniaturization.
둘째, 소결온도가 200℃ 정도 낮으므로 에너지 절감이 가능할 뿐만아니라 적층 캐패시터의 경우 내부 전극으로 고가인 Ag+Pd 대신 순수 Ag를 사용할 수 있어 제조비용의 절감을 가져올 수 있다.Secondly, since the sintering temperature is about 200 ° C., energy saving is possible, and in the case of the multilayer capacitor, pure Ag can be used instead of expensive Ag + Pd as an internal electrode, thereby reducing the manufacturing cost.
셋째, CaO 첨가량이 0.3% 이상인 조성은 내환원성을 가지므로 가격이 싼 Cu 내부전극의 사용도 가능하다.Third, since the composition having a CaO added amount of 0.3% or more has reduction resistance, it is possible to use a cheap Cu internal electrode.
본 발명 세라믹 유전체 조성물의 자세한 제조과정과 실시예 및 시편의 특성측정결과는 다음의 실시예를 통하여 보다 구체적으로 이해될 것이다.Detailed manufacturing process of the ceramic dielectric composition of the present invention and the results of measuring the characteristics of the examples and specimens will be understood in more detail through the following examples.
실시예Example
본 실시예에서는 CaO의 첨가량은 0.5mol/%로 고정한 상태에서 CuO의 첨가량을 변화시킨 유전체 시편을 제조하였는 바, 물론 본 발명의 조성범위가 이에 국한되는 것은 아니다.In the present embodiment, a dielectric specimen in which the addition amount of CuO was changed while the addition amount of CaO was fixed at 0.5 mol /% was manufactured, but the composition range of the present invention is not limited thereto.
상기 조성의 본 발명 시편에 대한 단계별 제조공정은 다음과 같다.Step-by-step manufacturing process for the present invention specimen of the composition is as follows.
i) PMN 합성i) PMN synthesis
아래의 콜럼바이트 프리커서(Columbite precursor)법을 사용하여,Using the Columbite precursor method below,
합성된 Mg2Nb2O6(Columbite)를 분쇄한 후 다시 1200℃에서 2시간 동안 열처리하였다. 이렇게 합성된 콜럼바이트를 유발에서 분쇄한 후 Pbo : MgNb2O6=3 : 1의 비율로 혼합, 건조하여 얻어진 혼합체를 900℃에서 2시간 동안 하소하여 PMN상을 얻었다.The synthesized Mg 2 Nb 2 O 6 (Columbite) was ground and then heat-treated again at 1200 ℃ for 2 hours. The synthesized Columbite was ground in a mortar and then mixed and dried in a ratio of Pbo: MgNb2O6 = 3: 1 to obtain a PMN phase by calcining the mixture at 900 ° C for 2 hours.
ii) PT의 합성ii) synthesis of PT
PbO : TiO2=1 : 1의 비율로 혼합, 건조하여 얻어진 혼합체를 800℃에서 2시간 동안 하소하여 PT상을 합성하였다.The mixture obtained by mixing and drying in the ratio of PbO: TiO 2 = 1: 1 was calcined at 800 ° C. for 2 hours to synthesize a PT phase.
iii) 원료분말의 혼합→소결iii) Mixing of raw material powder → sintering
상기 i), ii) 공정에 의해 합성된 PMN과 PT에 CaO와 CuO를 첨가하여 혼합, 건조하여 혼합체를 얻고, 이 혼합체를 800℃에서 2시간 동안 하소하였다. 하소된 분말은 볼밀을 이용하여 24시간 동안 분쇄한 후 건조, 성형하였다.CaO and CuO were added to PMN and PT synthesized by the steps i) and ii), mixed and dried to obtain a mixture, and the mixture was calcined at 800 ° C. for 2 hours. The calcined powder was ground for 24 hours using a ball mill and then dried and molded.
성형체의 크기는 직경 1cm, 두께 1.5mm였으며, 성형압력은 1000kg/cm2였다. 성형체의 소결은 900,925,950,975,1000℃에서 2시간 동안 행하였으며, 이때 사용한 승온속도 및 냉각속도는 모두 분당 5℃로 하였다.The size of the molded body was 1 cm in diameter and 1.5 mm in thickness, and the molding pressure was 1000 kg / cm 2 . Sintering of the molded body was carried out at 900,925,950,975,1000 ℃ for 2 hours, the temperature increase rate and cooling rate used at this time were all 5 ℃ per minute.
iv) 소결체의 유전특성iv) dielectric properties of sintered body
본 발명의 조성중 가장 우수한 특성을 나타내는 조성인 (0.945-z)PMN+5.0PT+0.5CaO+zCuO의 소결 온도에 따라 유전율(K) 및 유전손실(%DF) 측정결과는 아래의 표 1과 같다.Dielectric constant (K) and dielectric loss (% DF) measurement results according to the sintering temperature of (0.945-z) PMN + 5.0PT + 0.5CaO + zCuO, the composition showing the best characteristics among the compositions of the present invention, are shown in Table 1 below. .
유전특성 측정용 시편은 소결시편의 양면에 은전극을 도포하고 600℃에서 10분간 소부하여 전극을 형성하였으며, 소결된 유전체 시편의 유전특성(유전율 및 유전손실)은 상온(20℃), 1KHz, 1.0Vrms의 조건에서 LCR미터를 이용하여 측정한 값이다.The dielectric measuring specimens were coated with silver electrodes on both sides of the sintered specimen and baked for 10 minutes at 600 ° C. The dielectric properties (dielectric constant and dielectric loss) of the sintered dielectric specimens were measured at room temperature (20 ℃), 1KHz, Measured using an LCR meter under 1.0Vrms.
상기 표 1에서 알 수 있듯이 본 발명의 유전체 조성물은 가장 우수한 경우 유전율(K) 24,000, 유전손실(%DF) 1.3%를 나타냄에 따라 종래의 PMN+PT 조성에 비하여 유전율이 25% 가량 향상된 결과를 보여주고 있다.As can be seen in Table 1, the dielectric composition of the present invention exhibits a dielectric constant (K) of 24,000 and dielectric loss (% DF) of 1.3%, which is 25% higher than that of the conventional PMN + PT composition. Is showing.
본 발명의 유전체 조성물은 정전용량의 온도변화율이 +3∼5%, -50∼35%로 미국 EIA 규격중 Z5U 조성 범위에 해당된다.The dielectric composition of the present invention has a temperature change rate of capacitance of +3 to 5% and -50 to 35%, which corresponds to the Z5U composition range in the US EIA standard.
다음, 아래의 표 2는 본 발명 실시예 시편에 대한 절연저항 측정결과를 나타낸 것으로, 시편의 비저항(Specific Resistivity)은 고저항 미터(High Resistance Meter)를 사용하여 50V 적류전계를 인가하여 1분간 충전한 후 측정하였다.Next, Table 2 below shows the measurement results of the insulation resistance of the specimen of the present invention, the specific resistance of the specimen (Specific Resistivity) using a high resistance meter (High Resistance Meter) charged by applying a 50V current meter for 1 minute It was measured after.
위의 표 2에서, 본 발명 조성의 실시예 시편은 매우 우수한 절연저항(1011Ω·cm)을 가지고 있어 유전체 조성으로 사용하는데 문제가 없음을 알 수 있다.In the above Table 2, it can be seen that the example specimens of the composition of the present invention have a very good insulation resistance (1011 Ω · cm), so there is no problem in using it as the dielectric composition.
표 3은 본 발명 실시예 조성의 소결밀도 측정결과를 나타낸 것으로, 소결밀도는 증류수를 사용하여 알키메데스법으로 측정하였다.Table 3 shows the measurement results of the sintered density of the composition of the present invention, and the sintered density was measured by the Alkimedes method using distilled water.
위의 표 3을 통해 본 발명 조성의 유전체는 900℃의 저온 소결시에도 매우 높은 밀도를 나타냄을 알 수 있다.It can be seen from the above Table 3 that the dielectric of the present composition exhibits a very high density even at low temperature sintering at 900 ° C.
다음 아래의 표 4, 표 5는 본 발명의 (1-x-y-z)PMN+yCaO+zCuO 조성의 실시예 시편에 대한 유전 특성의 결과치를 보인 것으로 표 4는 유전율에 대한 것이고, 표 5는 유전손실에 대한 것이다.Table 4 and Table 5 below show the results of the dielectric properties for the sample of the (1-xyz) PMN + yCaO + zCuO composition of the present invention, Table 4 is for dielectric constant, and Table 5 is for dielectric loss. It is about.
이상의 사실을 종합하여 볼때, 본 발명의 세라믹 유전체 조성물은 종래의 조성에 비해 유전율을 비롯한 제반 유전특성이 우수할 뿐 아니라 소결온도도 상당히 낮아 새로운 유전체 조성으로이 응용이 기대된다.Taken together, the ceramic dielectric composition of the present invention is not only excellent in all dielectric properties, including dielectric constant, but also considerably lower in sintering temperature than the conventional composition.
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| KR970001063B1 true KR970001063B1 (en) | 1997-01-25 |
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| US7944341B2 (en) | 2005-04-18 | 2011-05-17 | Lg Electronics Inc. | Network system using DC power bus and auto power control method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US7944341B2 (en) | 2005-04-18 | 2011-05-17 | Lg Electronics Inc. | Network system using DC power bus and auto power control method |
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