KR100268462B1 - Temperature compensation dielectric composition - Google Patents

Temperature compensation dielectric composition Download PDF

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KR100268462B1
KR100268462B1 KR1019980005070A KR19980005070A KR100268462B1 KR 100268462 B1 KR100268462 B1 KR 100268462B1 KR 1019980005070 A KR1019980005070 A KR 1019980005070A KR 19980005070 A KR19980005070 A KR 19980005070A KR 100268462 B1 KR100268462 B1 KR 100268462B1
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oxide
composition
rare earth
temperature compensation
temperature
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KR19990070308A (en
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김호기
박융
놀즈 캐빈
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윤덕용
한국과학기술원
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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
    • H01B3/10—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances metallic oxides
    • 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
    • H01B3/008—Other insulating material
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Insulating Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

PURPOSE: A dielectric ceramic composition is provided to attain relatively stabilized temperature characteristics or a high temperature coefficient, high insulation resistance, and high frequency. CONSTITUTION: The dielectric ceramic composition for temperature compensation is characterized by having high insulation resistance and high frequency. The composition is comprised of 29.49-30.6 wt.% of magnesium oxide, 2.95-3.4 wt.% of calcium oxide, 65.55-67.06 wt.% of tin oxide, 0.4-0.6 wt.% of silicon oxide, 0.5-2.0 wt.% of rare earth oxide, and 0.01-0.1 wt.% of aluminum oxide. Moreover, the rare earth oxide can be one or two kinds selected from a group consisting of niobium oxide, praseodymium oxide, lanthanum oxide, and cerium oxide.

Description

[발명의 명칭][Name of invention]

온도보상용 유전체 자기조성물Temperature Compensation Dielectric Self Composition

[발명의 상세한 설명]Detailed description of the invention

[발명의 목적][Purpose of invention]

[발명이 속하는 기술분야 및 그 분야의 종래기술][Technical field to which the invention belongs and the prior art in that field]

본 발명은 온도보상용 유전체 자기 조성물에 관한 것으로, 특히 산화마그네슘(MgO), 산화칼슘(CaO), 산화티탄(TiO2), 산화규소(SiO2)등과 희토류 산화물인 Nd2O3, Pr6O11, La2O3, CeO2및 Al2O3중 하나 또는 둘이상의 희토류 산화물이 포함된 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dielectric ceramic composition for temperature compensation, in particular magnesium oxide (MgO), calcium oxide (CaO), titanium oxide (TiO 2 ), silicon oxide (SiO 2 ), and the like, and rare earth oxides Nd 2 O 3 , Pr 6 A composition comprising one or two or more rare earth oxides of O 11 , La 2 O 3 , CeO 2, and Al 2 O 3 .

본 발명과 관련이 있는 종래기술은 가토(Kato)등("Dielectric properties of lead alkaline-earth zirconate at microwave frequencies", Jpn. J. Appl. Phys. 30 (9B) 2343(1991))이 발표한 것으로 그 내용은 PbZrO3를 기본으로 한 조성물에 Pb의위치의 일부를 Ba, Sr, Ca로 치환한 마이크로파 유전체 조성에 대한 공진주파수의 온도의존계수(τf), 유전율(k), 품질계수(Q)에 대한 측정 데이터를 제공하고 있다. 또한 가토(Kato)등("Crystal structure refinement of Pb1-xCaxZrO3by the Rietvelt Method." Jpn. J. Appl. Phys. 32(9B) 4356(1993).)이 발표한 Pb1-xCaxZrO3사방정계 내의 초격자 구조를 X-ray Rietvelt 방법에 의해서 분석하였고 유전율(k), 공진주파수의 온도 의존계수(τf), 품질계수(Q)와의 구조와의 관계를 분석하였다. 이들 종래기술은 마이크로파 유전특성 및 결정구조의 분석이 대부분으로 본 발명과는 다르다는 것을 알 수 있다.The prior art related to the present invention is published by Kato et al. ("Dielectric properties of lead alkaline-earth zirconate at microwave frequencies", Jpn. J. Appl. Phys. 30 (9B) 2343 (1991)). The contents are described as follows: temperature dependence coefficient (τ f ), dielectric constant (k), and quality factor (Q) of the resonant frequency for microwave dielectric composition in which a part of the position of Pb is replaced with Ba, Sr, and Ca in a composition based on PbZrO 3 . We provide measurement data for). Pb 1-, also published by Kato et al. (“Crystal structure refinement of Pb 1-x Ca x ZrO 3 by the Rietvelt Method.” Jpn. J. Appl. Phys. 32 (9B) 4356 (1993).). The superlattice structure in x Ca x ZrO 3 tetragonal system was analyzed by X-ray Rietvelt method and its relationship with dielectric constant (k), temperature dependence coefficient of resonant frequency (τ f ) and quality factor (Q) . It can be seen that these prior arts mostly differ from the present invention in the analysis of microwave dielectric properties and crystal structure.

온도보상용 세라믹 콘덴서는 일반적으로 고주파(1MHz 이상)에서 사용되며, 주파수의 증가에 따라 손실계수(tanδ, 1/Q)가 증가하게 된다. 이러한 현상은 고주파 전자부품의 경우에 더욱 심화되는데, 튜너 또는 방향 탐지장치의 고주파 부품에서는 이로 인한 노이즈등이 발생되어 제품의 질이 떨어지게 된다. 따라서, 본 발명은 전술한 문제점을 극복할 수 있는 세라믹 조성물을 제공하는데 그 목적이 있다.Ceramic capacitors for temperature compensation are generally used at high frequencies (over 1MHz), and the loss coefficient (tanδ, 1 / Q) increases with increasing frequency. This phenomenon is intensified in the case of high-frequency electronic components, the noise caused by the high-frequency components of the tuner or direction detection device resulting in poor product quality. Accordingly, an object of the present invention is to provide a ceramic composition that can overcome the above-mentioned problems.

[발명이 이루고자 하는 기술적 과제][Technical problem to be achieved]

본 발명은 고주파(마이크로파)에서도 낮은 손실값을 갖는 MgTiO3와 CaTiO3를 주성분으로 하고, 소결온도를 낮출수 있는 SiO2, 소결촉진효과를 갖는 Nd2O3, Pr6O11, La2O3, CeO2중 하나 또는 둘이상의 희토류 산화물을 부성분으로 하는 조성에 적절한 입도의 Al2O3를 소량 첨가함으로써, NPO(Negative-Positive-Zero) 온도특성을 만족시키며, 고주파 특성이 우수한 재료를 만들 수 있다.The present invention is composed mainly of MgTiO 3 and CaTiO 3 having a low loss value even at high frequency (microwave), SiO 2 to reduce the sintering temperature, Nd 2 O 3 , Pr 6 O 11 , La 2 O having a sintering promoting effect 3 by small amount of an appropriate particle size of the Al 2 O 3 in the composition of the rare earth oxides on one of CeO 2, or the two of the sub-component, satisfies the NPO (Negative-Positive-Zero) temperature characteristic and the high frequency characteristics to make an excellent material Can be.

[발명의 구성 및 작용][Configuration and Function of Invention]

본 발명의 조성물은 MgO, CaO, TiO, SiO2로 구성된 기본 조성물에 희토류 산화물과 Al2O3가 미량 첨가되어 구성된다. 상기의 기본 조성물에 있어서, 좀 더 상세한 조성 wt％는 MgO 29.49∼30.6, CaO 2.95∼3.4, TiO265.55∼67.06, SiO20.4∼0.6이고, 상기의 희토류 산화물은 Nd2O3, Pr6O11, La2O3, CeO2중 하나 또는 둘이상이 기본 조성물에 대해 0.5∼2.0wt％ 함유되고, 상기 Al2O3는 기본 조성물에 대해 0.01∼0.1wt％가 함유된다. 상기 본 발명의 조성범주를 벗어난 경우 절연저항이 상대적으로 작고, 온도계수가 NPO 특성인 ±30ppm/℃를 벗어나게 된다.The composition of the present invention is composed of a rare earth oxide and a small amount of Al 2 O 3 added to a basic composition composed of MgO, CaO, TiO, and SiO 2 . In the above basic composition, more detailed composition wt% is MgO 29.49 to 30.6, CaO 2.95 to 3.4, TiO 2 65.55 to 67.06, SiO 2 0.4 to 0.6, and the rare earth oxide is Nd 2 O 3 , Pr 6 O One or two or more of 11 , La 2 O 3 , CeO 2 is contained in an amount of 0.5 to 2.0 wt% based on the base composition, and the Al 2 O 3 is contained in an amount of 0.01 to 0.1 wt% based on the base composition. When the composition range of the present invention is out of the range, the insulation resistance is relatively small, and the temperature coefficient is outside the NPO characteristic of ± 30 ppm / ° C.

이상과 같이 제조된 본 발명의 조성물은 첫째, 안정된 소결온도(1280∼1320℃)로 인하여, MLCC(Multilayer Ceramic Capacitor)제조시 산화로 인한 전극불량을 제거할 수 있으며, 둘째, 캐패시터 제조시 고주파에도 안정된 유전손실 값을 갖는다. 본 발명은 다음의 실시예와 비교예를 통하여 보다 구체적으로 설명하고자 한다. 그러나 이들 실시예는 본 발명의 기술적 범위를 한정하는 것은 아니다.The composition of the present invention prepared as described above, first, due to the stable sintering temperature (1280 ~ 1320 ° C), can remove the electrode defects due to oxidation during the manufacturing of MLCC (Multilayer Ceramic Capacitor), and second, even at high frequency during capacitor manufacturing It has a stable dielectric loss value. The present invention will be described in more detail through the following examples and comparative examples. However, these examples do not limit the technical scope of the present invention.

[실시예]EXAMPLE

본 발명에서는 99.9％ 이상의 순도를 갖는 산화마그네슘(MgO), 산화칼슘(CaO), 산화티타늄(TiO2)에 희토류 산화물인 Nd2O3, Pr6O11, La2O3, CeO2등을 선택하여, 하기의 표1과 같이 혼합하고, Al2O3의 양을 하기의 표1과 같이 변화시켜 조합한 뒤, 비닐 자(Jar)와 ZrO2볼(Ball)을 이용하여 플레너터리 밀(Planetary Mill)을 혼합하였다.In the present invention, magnesium oxide (MgO), calcium oxide (CaO) and titanium oxide (TiO 2 ) having a purity of 99.9% or more include Nd 2 O 3 , Pr 6 O 11 , La 2 O 3 , CeO 2 , and the like, which are rare earth oxides. After mixing, mixing as shown in Table 1 below, varying the amount of Al 2 O 3 as shown in Table 1 below, and then combined with a planetary mill (Var) and ZrO 2 ball (Ball) Planetary Mill) was mixed.

이때에 분산매로는 아세톤(Aceton)을 사용하였으며, 잘 혼합된 슬러리(slurry)는 건조후 조성에 따라, 1050∼1100℃에서 하소하고, 이를 다시 적절한 입도를 가지도록 분쇄하였다.At this time, acetone was used as a dispersion medium, and a well mixed slurry was calcined at 1050 to 1100 ° C., depending on the composition after drying, and then pulverized to have an appropriate particle size.

이렇게 얻어진 분말을 건식 프레스(press)로, 소결후의 크기가 직경이 10.00±0.5mm, 두께가 1.00±0.05mm가 되는 원판형으로 성형하며, 이때의 성형압은 1ton/㎠으로 하였다.The powder thus obtained was formed into a disc shape in which a size after sintering was 10.00 ± 0.5 mm in diameter and 1.00 ± 0.05 mm in thickness after dry pressing, and the molding pressure at this time was 1 ton / cm 2.

성형된 시편은 조성에 따라, 1280∼1340℃로 소결한 후, 은(Ag) 페이스트(paste)로 전극을 부착하여 전기적 특성을 측정하였다.The molded specimen was sintered at 1280 to 1340 ° C according to the composition, and then the electrical properties were measured by attaching an electrode with a silver (Ag) paste.

하기의 표1에서의 유전상수 및 유전손실계수는 LCR메터를 사용하여, 25℃에서 1MHz로 측정하였고, 비저항(절연저항)은 고저항 메터를 사용하여, 직류전압 100V로 측정하였다.The dielectric constant and dielectric loss coefficient of Table 1 were measured at 1 MHz at 25 ° C. using an LCR meter, and the specific resistance (insulation resistance) was measured at a DC voltage of 100 V using a high resistance meter.

[비교예][Comparative Example]

표 1에 나타난 바와 같이 조성비를 정하여 Nd2O3첨가와 무첨가 그룹에 대한 유전율, 품질계수, 온도계수, 절연 저항을 측정하여 표 1과 같이 나타냈다.As shown in Table 1, the dielectric constant, quality factor, temperature coefficient, and insulation resistance for the Nd 2 O 3 addition and no addition groups were determined and the results are shown in Table 1.

[발명의 효과][Effects of the Invention]

본 발명은 기존 재료의 문제점을 극복할 수 있는 세라믹 조성물을 제공하는데 그 목적이 있는 것으로서, 본 발명은 고주파(마이크로파)에서도 낮은 손실값을 갖는 MgTiO3와 CaTiO3를 주성분으로 하고, 소결온도를 낮출 수 있는 SiO2, 소결촉진효과를 갖는 Nd2O3, Pr6O11, La2O3, CeO2중 하나 또는 둘이상의 희토류 산화물을 부성분으로 하는 조성에 적절한 입도의 Al2O3를 소량 첨가함으로써, NPO(Negative-Positive-Zero) 온도특성을 만족시키며, 고주파 특성이 우수한 재료를 만들 수 있다.The present invention is to provide a ceramic composition that can overcome the problems of the existing material, the present invention is based on MgTiO 3 and CaTiO 3 having a low loss value even at high frequency (microwave), and the sintering temperature is lowered A small amount of Al 2 O 3 with a particle size suitable for a composition containing SiO 2 , Nd 2 O 3 , Pr 6 O 11 , La 2 O 3 , CeO 2 , or two or more rare earth oxides having a sintering promoting effect as a secondary component As a result, a material that satisfies NPO (Negative-Positive-Zero) temperature characteristics and has excellent high frequency characteristics can be made.

Claims (2)

MgO 29.49~30.6 wt%, CaO 2.95~3.4 wt%, TiO265.55~67.06 wt%, SiO20.4~0.6 wt%로 구성된 기본 조성물에 대해 희토류사화물 0.5~2.0wt%과 Al2O30.01~0.1wt%이 첨가됨을 특징으로 하는 온도 보상용 세라믹 유전체 자기조성물.0.5 to 2.0 wt% of rare earth tetrachloride and 0.01 to Al 2 O 3 for the base composition consisting of MgO 29.49 to 30.6 wt%, CaO 2.95 to 3.4 wt%, TiO 2 65.55 to 67.06 wt%, SiO 2 0.4 to 0.6 wt% Ceramic dielectric composition for temperature compensation, characterized in that 0.1wt% is added. 제1항에 있어서, 희토류 산화물은 Nd2O3, Pr6O11, La2O3, CeO2중에서 하나 또는 둘 이상인 것을 특징으로 하는 온도 보상용 유전체 자기 조성물.The dielectric ceramic composition of claim 1, wherein the rare earth oxide is one or two or more of Nd 2 O 3 , Pr 6 O 11 , La 2 O 3 , and CeO 2 .
KR1019980005070A 1998-02-19 1998-02-19 Temperature compensation dielectric composition KR100268462B1 (en)

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