KR20050105392A - Microwave dielectric ceramic composition for low temperature firing and preparation method thereof - Google Patents

Microwave dielectric ceramic composition for low temperature firing and preparation method thereof Download PDF

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KR20050105392A
KR20050105392A KR1020040030517A KR20040030517A KR20050105392A KR 20050105392 A KR20050105392 A KR 20050105392A KR 1020040030517 A KR1020040030517 A KR 1020040030517A KR 20040030517 A KR20040030517 A KR 20040030517A KR 20050105392 A KR20050105392 A KR 20050105392A
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ceramic composition
sintering
temperature
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nbo
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오영제
임혁
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한국과학기술연구원
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Priority to JP2004370941A priority patent/JP4468155B2/en
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    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
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    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
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    • E—FIXED CONSTRUCTIONS
    • E04—BUILDING
    • E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
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Abstract

본 발명은 하기 화학식 1 또는 2의 조성을 갖는 비스무스계 세라믹 조성물 및 그의 제조 방법에 관한 것이다.The present invention relates to a bismuth-based ceramic composition having a composition of the following formula (1) or (2) and a method for producing the same.

<화학식 1><Formula 1>

Bi1-xAxNbO4 Bi 1-x A x NbO 4

<화학식 2><Formula 2>

BiNb1-xBxO4 BiNb 1-x B x O 4

상기 식에서,Where

A는 Sm 또는 Dy이고, B는 Sb 또는 P이며, x는 0 < x ≤0.1이다.A is Sm or Dy, B is Sb or P, and x is 0 <x ≦ 0.1.

또한, 본 발명에 따른 세라믹 조성물은 소결 조제로서 CuO 및(또는) V2O5를 더 포함할 수 있다.In addition, the ceramic composition according to the present invention may further include CuO and / or V 2 O 5 as a sintering aid.

본 발명에 따른 조성물은 높은 유전율 및 품질계수 및 안정된 공진주파수의 온도계수를 가지며, 880 내지 960℃의 낮은 온도 범위에서 소성이 가능하여 소결 온도가 낮은 Ag, Cu 전극을 내부전극으로 사용할 수 있어 비교적 가격이 저렴한 다층형 마이크로파 유전체 소자 제조에 사용될 수 있다.The composition according to the present invention has a high dielectric constant and quality coefficient and a temperature coefficient of stable resonant frequency, and can be fired at a low temperature range of 880 to 960 ° C, so that Ag and Cu electrodes having a low sintering temperature can be used as internal electrodes. It can be used to manufacture low cost multilayer microwave dielectric devices.

Description

저온 소성용 마이크로파 유전체 세라믹 조성물 및 그의 제조 방법{Microwave Dielectric Ceramic Composition for Low Temperature Firing and Preparation Method Thereof}Microwave Dielectric Ceramic Composition for Low Temperature Firing and Manufacturing Method Thereof {Microwave Dielectric Ceramic Composition for Low Temperature Firing and Preparation Method Thereof}

본 발명은 각종 통신용 전자기기의 부품에 사용되는 마이크로파 유전체 세라믹 조성물에 관한 것으로, 보다 상세하게는 높은 유전율 및 품질계수 및 안정된 공진주파수의 온도계수 (Temperature Coefficient of Resonant Frequency : TCF)를 가지며 880 내지 960℃의 낮은 온도 범위에서 소성이 가능한 저온 소성용 마이크로파 유전체 세라믹 조성물 및 그의 제조 방법에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to microwave dielectric ceramic compositions for use in components of various communication electronic devices. The present invention relates to a microwave dielectric ceramic composition for low temperature firing capable of firing at a low temperature range of &lt; RTI ID = 0.0 &gt;

최근 들어 이동통신 및 위성방송 등 정보·통신 기술의 발달에 의하여 통신부품에 사용되는 주파수가 점점 마이크로파 영역화 되어가고 있다. 특히 IMT-2000과 같은 새로운 이동통신 서비스뿐만 아니라 기존의 휴대폰, GPS(Global Positioning System), 위성통신 분야에서도 더욱 많은 용량의 정보를 주고 받기 위한 주파수 대역의 고주파화 및 디지털화가 진행되고 있다. 따라서 마이크로파 영역에서 작동하는 통신기기에 대한 중요성이 부각되고 있다.Recently, due to the development of information and communication technologies such as mobile communication and satellite broadcasting, the frequency used for communication parts is gradually becoming a microwave region. In particular, in addition to new mobile communication services such as IMT-2000, existing mobile phones, GPS (Global Positioning System), and satellite communication fields are increasing in frequency and digitization of frequency bands to transmit and receive more information. Therefore, the importance of communication devices operating in the microwave range is emerging.

이동통신에 사용되는 전자부품은 크게 능동부품과 수동부품으로 나눌 수 있으며, 특히, 듀플렉서, 필터, 안테나 등과 같은 수동부품은 마이크로파 유전체 세라믹을 핵심 소재로 사용하고 있다. 유전체 세라믹을 마이크로파 소자로 사용하기 위해서는 큰 유전율을 가져야 하며, 이를 위해 유전 손실을 작게 하기 위해서는 높은 품질계수를 가져야 하고, 마이크로파 기기의 공진주파수가 안정화되고 공진회로의 온도보상이 용이하려면 공진소자로 쓰이는 유전체 재료의 공진주파수의 온도계수가 작아야 한다.Electronic components used in mobile communication can be largely divided into active components and passive components. In particular, passive components such as duplexers, filters, and antennas use microwave dielectric ceramic as a core material. In order to use the dielectric ceramic as a microwave device, it has to have a large dielectric constant, and in order to reduce the dielectric loss, it has to have a high quality factor, and in order to stabilize the resonance frequency of microwave equipment and to easily compensate the temperature of the resonance circuit, it is used as a resonance device. The temperature coefficient of the resonant frequency of the dielectric material should be small.

최근 들어 이동통신기기의 소형화, 집적화, 고기능화를 위해 MMIC (Microwave Monolithic IC) 등 개별 부품의 모듈화가 시도되고 있고 이는 MCMC (Multi-Chip Module on Ceramics) 기술에 의해 현실이 가능하게 된다. MCMC 기술은 세라믹이 개별 부품으로 사용되는 안테나, 듀플렉서, 대역통과 필터의 소자 등을 적층형태로 만들어 금속전극 패턴과 동시소결하여 일체형으로 만듦으로써 부품의 소형화 및 대량 생산화를 이룰 수 있는 기술로서 이는 LTCC (Low temperature cofiring ceramic) 기술에 의해 실현 가능하다.In recent years, modularization of individual components such as MMIC (Microwave Monolithic IC) has been attempted for miniaturization, integration, and high functionality of mobile communication devices. MCMC technology enables the miniaturization and mass production of parts by stacking antennas, duplexers, bandpass filters, etc., in which ceramics are used as individual parts, and simultaneously sintering them with metal electrode patterns. It can be realized by LTCC (Low temperature cofiring ceramic) technology.

현재 개발된 마이크로파 유전체 세라믹 조성들의 경우에는 소결 온도 (1200℃ 이상)가 매우 높기 때문에 융점이 높은 금속전극인 Pt, Pd 또는 W를 사용하여야 한다. 그러나 Pt 또는 Pd를 전극으로 사용하는 경우에는 이들 금속이 고가이기 때문에 생산원가가 상당히 상승하는 문제가 있고 W의 경우에는 환원분위기 하에서 소결하여야 한다는 문제가 있다. 따라서, 비교적 가격이 싸고 전기전도도가 우수한 Ag (융점 960℃) 또는 Cu (융점 1083℃)를 내부전극으로 사용하기 위한 시도가 진행되고 있다. 마이크로파 유전체 세라믹은 Ag 또는 Cu와의 동시소성을 위해서는 이 전극들의 융점보다 낮은 온도에서 소결이 가능하여야 하기 때문에 그 온도에 상응하는 소결 온도를 갖는 저온소결 세라믹 유전체가 필요하다.Currently developed microwave dielectric ceramic compositions have a very high sintering temperature (above 1200 ° C.), so Pt, Pd, or W, which are metal melting points, should be used. However, in the case of using Pt or Pd as an electrode, since these metals are expensive, there is a problem in that the production cost increases considerably, and in the case of W, there is a problem of sintering under a reducing atmosphere. Therefore, attempts have been made to use Ag (melting point 960 DEG C) or Cu (melting point 1083 DEG C), which is relatively inexpensive and has excellent electrical conductivity, as an internal electrode. Microwave dielectric ceramics require low-temperature sintered ceramic dielectrics having a sintering temperature corresponding to that temperature because they must be sintered at temperatures lower than the melting point of these electrodes for simultaneous firing with Ag or Cu.

현재까지 보고된 저온소결 세라믹 유전체는 주로 기존에 유전체 조성에 융점이 낮은 유리 프릿 (glass frit)을 첨가하여 소결 온도를 낮추거나 공침법이나 졸-겔법을 사용하여 유전체 세라믹 원료의 입자크기를 작게 하는 방법들이 이루어지고 있으나 유리 프릿을 첨가하는 경우에는 유전체 특성이 크게 저하된다는 단점이 있으며 공침법이나 졸-겔법으로 유전체 세라믹 원료 입자크기를 작게 하는 경우에는 제조공정이 복잡하고 출발 물질이 비싸, 제조단가가 높아진다는 문제점이 있다.The low temperature sintered ceramic dielectrics reported to date are mainly used to reduce the sintering temperature by adding glass frit having low melting point to the dielectric composition or to reduce the particle size of the dielectric ceramic raw materials by using coprecipitation method or sol-gel method. Although methods are being used, there is a disadvantage in that the dielectric properties are greatly reduced when glass frit is added. When the particle size of the dielectric ceramic raw material is reduced by the coprecipitation method or the sol-gel method, the manufacturing process is complicated and the starting material is expensive. There is a problem that becomes high.

한편, 비스무스는 그 자체의 낮은 융점 (825℃) 때문에 세라믹의 액상 소결을 위한 조제로 많이 거론되어온 물질로서, 이를 기본으로 한 세라믹 물질은 상대적으로 낮은 소결 온도를 가지고 있어, 비스무스계 세라믹을 마이크로파 유전체로 사용하기 위한 연구가 진행되어 BiNbO4계, Bi2O3-CaO계, Bi2O 3-CaO-ZnO-Nb2O5계 등에 각종 소결 조제를 첨가하여 저온 소결이 가능한 유전체 세라믹이 개발되었다.On the other hand, bismuth has been widely used as a preparation for liquid phase sintering of ceramics due to its low melting point (825 ° C), and the ceramic material based thereon has a relatively low sintering temperature. Research into the use of the present invention has progressed to develop a dielectric ceramic capable of low-temperature sintering by adding various sintering aids to BiNbO 4 , Bi 2 O 3 -CaO, Bi 2 O 3 -CaO-ZnO-Nb 2 O 5 .

이들 중 BiNbO4에 소결 조제로 CuO, V2O5를 첨가한 조성의 경우가 가장 좋은 유전 특성을 보였으나 실제 부품으로 적용하기에는 그 유전 특성이 열악하여, 우수한 유전 특성을 가지며 낮은 온도에서 소결이 가능한 유전체 조성물이 여전히 요구되고 있다.Among them, CuO and V 2 O 5 added to BiNbO 4 as the sintering aid showed the best dielectric properties, but the dielectric properties were poor to be applied to actual parts, and they had excellent dielectric properties and sintering at low temperature. Possible dielectric compositions are still needed.

본 발명은 높은 유전율 및 품질계수 및 안정된 공진주파수의 온도계수를 가지며, 880 내지 960℃의 낮은 온도 범위에서 소성이 가능하여 내부 전극으로 Ag 또는 Cu를 사용할 수 있는 마이크로파 유전체 세라믹 조성물 및 그의 제조 방법을 제공하는데 목적이 있다.The present invention provides a microwave dielectric ceramic composition having a high dielectric constant and quality coefficient and a temperature coefficient of stable resonant frequency, capable of firing at a low temperature range of 880 to 960 ° C, and using Ag or Cu as an internal electrode, and a method of manufacturing the same. The purpose is to provide.

이하, 본 발명에 따른 마이크로파 유전체 세라믹 조성물 및 그의 제조 방법에 관해 상세히 설명한다.Hereinafter, a microwave dielectric ceramic composition and a method of manufacturing the same according to the present invention will be described in detail.

본 발명에 따른 마이크로파 유전체 세라믹 조성물은 하기 화학식 1 또는 2로 나타낸 조성을 가진다. The microwave dielectric ceramic composition according to the present invention has a composition represented by the following formula (1) or (2).

Bi1-xAxNbO4 Bi 1-x A x NbO 4

BiNb1-xBxO4 BiNb 1-x B x O 4

상기 식에서,Where

A는 Sm 또는 Dy이고, B는 Sb 또는 P이며, x는 0 < x ≤0.1이다.A is Sm or Dy, B is Sb or P, and x is 0 <x ≦ 0.1.

본 발명에 따른 유전체 조성물은 유전율이 40 이상이고, 품질 계수가 20,000 내지 42,000이고, 공진주파수의 온도계수는 -2 내지 -26이다. 또한, 880 내지 960 ℃의 온도범위에서 소결 가능하여, 융점이 낮은 Ag 또는 Cu와 함께 소성이 가능하다.The dielectric composition according to the present invention has a dielectric constant of 40 or more, a quality factor of 20,000 to 42,000, and a temperature coefficient of resonant frequency of -2 to -26. In addition, sintering is possible in the temperature range of 880 to 960 ℃, it is possible to sinter with Ag or Cu having a low melting point.

또한, 본 발명에 따른 유전체 세라믹 조성물은 CuO 또는 V2O5를 소결 조제로 포함할 수 있다. 이때, CuO 또는 V2O5 중 하나를 포함할 때보다 CuO 및 V2O 5를 모두 포함할 경우 보다 좋은 소결성을 나타낸다. 이러한 소결 조제의 함유량은 전제 조성물의 대하여 0.03 내지 0.5 중량％로서, 0.03 내지 0.25 중량％ CuO 및 0.03 내지 0.25 중량％ V2O5를 포함할 때 가장 바람직하다. 상기 소결 조제의 첨가량이 0.03 중량％ 미만일 경우에는 충분한 소결성을 나타내지 못한다는 문제가 있으며, 소결 조제들의 중량％가 0.5％를 초과한 경우에는 소결성은 크게 항상되지만 유전 특성이 저하된다는 문제점을 가지고 있다.In addition, the dielectric ceramic composition according to the present invention may include CuO or V 2 O 5 as a sintering aid. At this time, than when it includes one of CuO, or V 2 O 5 indicates a good degree of sintering than that contain both CuO and V 2 O 5. The content of such a sintering aid is most preferably 0.03 to 0.5% by weight based on the total composition, and includes 0.03 to 0.25% by weight CuO and 0.03 to 0.25% by weight V 2 O 5 . If the added amount of the sintering aid is less than 0.03% by weight, there is a problem in that it does not exhibit sufficient sinterability. If the weight percentage of the sintering aids is more than 0.5%, the sintering property is always large, but there is a problem that the dielectric properties are lowered.

본 발명에 따른 유전체 세라믹 조성물은 일반적인 산화물 합성법으로 제조될 수 있다. 예를 들면, 다음과 같이 제조될 수 있다.The dielectric ceramic composition according to the present invention can be prepared by a general oxide synthesis method. For example, it can be manufactured as follows.

Bi2O3, Nb2O5, 및 Sb+5, P+5, Sm+3 또는 Dy+3 원소를 갖은 화합물을 일정 화학양론적 조성비로 용매에 습식 혼합하고 건조한 후, 열처리하여 제조할 수 있다.Compounds containing Bi 2 O 3 , Nb 2 O 5 , and Sb +5 , P +5 , Sm +3 or Dy +3 elements can be prepared by wet mixing with a solvent in a constant stoichiometric composition, drying and heat treatment. have.

또한, 이렇게 제조된 Bi1-xAxNbO4 (A = Sm 또는 Dy) 또는 BiNb1-x BxO4 (B = Sb 또는 P) 조성의 분말에 소결 조제로 일정 량의 CuO 및(또는) V2O5를 첨가하고 습식 혼합·건조한 후 소결하여 제조할 수 있다.In addition, a predetermined amount of CuO and / or V as a sintering aid to the powder of Bi 1-x A x NbO 4 (A = Sm or Dy) or BiNb 1-x BxO 4 (B = Sb or P) composition thus prepared It was added 2 O 5 and can be produced by sintering and then wet-mixed and dried.

상기에서 Sb+5, P+5, Sm+3 또는 Dy+3 원소를 갖은 화합물로는 Sb2O5, H3PO4, Sm2O3, Dy2O3 등이 있으나, 이에 제한되는 것은 아니다.Examples of the compound having an Sb +5 , P +5 , Sm +3 or Dy +3 element include Sb 2 O 5 , H 3 PO 4 , Sm 2 O 3 , and Dy 2 O 3 , but are not limited thereto. no.

이하, 실시예를 통해 본 발명을 더욱 상세히 설명하기로 한다. 다만, 본 발명은 아래의 실시예로 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the present invention is not limited to the following examples.

<실시예><Example>

본 실시예에서는 기본원료로서 순도 99.9％ 이상의 Bi2O3, Nb2O5, Sb2O5, H3PO4, Sm2O3 및 Dy2O3를 사용하였으며 저온에서 소결을 촉진하기 위한 소결 조제로서 순도 99％ 이상의 CuO 및 V2O5를 사용하였다. 분말 합성은 BiNb1-XBX O4 (B = Sb+5, P+5)와 Bi1-XAxNbO4 (A = Sm+3, Dy+3)의 조성에 대하여 일반적인 산화물 합성법을 사용하였다.In this embodiment, Bi 2 O 3 , Nb 2 O 5 , Sb 2 O 5 , H 3 PO 4 , Sm 2 O 3 and Dy 2 O 3 with a purity of 99.9% or more were used as basic raw materials. CuO and V 2 O 5 with a purity of 99% or more were used as the sintering aid. Powder synthesis is based on general oxide synthesis for the composition of BiNb 1-X B X O 4 (B = Sb +5 , P +5 ) and Bi 1-X A x NbO 4 (A = Sm +3 , Dy +3 ). Used.

각 출발 물질을 화학양론적 조성비에 따라 전자저울을 사용하여 각각 칭량한 후 에탄올을 용매로 하여 지름이 10 mm인 안정화 지르코니아 볼을 사용하여 24 시간 동안 습식 혼합하였다. 혼합 후 건조기를 이용하여 24 시간동안 건조한 후 건조 분말을 알루미나 도가니에 넣어 800℃에서 2시간 동안 하소하였다.Each starting material was weighed using an electronic balance according to the stoichiometric composition ratio, and then wet mixed for 24 hours using a stabilized zirconia ball having a diameter of 10 mm using ethanol as a solvent. After mixing and drying for 24 hours using a dryer, the dried powder was placed in an alumina crucible and calcined at 800 ° C. for 2 hours.

이렇게 얻은 BiNb1-XBXO4 (B = Sb 또는 P) 또는 Bi1-XAx NbO4 (A = Sm 또는 Dy)의 조성의 하소된 분말에 소결 조제로 일정 량의 CuO와 V2O5를 첨가하고 다시 에탄올과 함께 안정화 지르코니아 볼을 이용하여 24 시간 동안 습식 혼합한 후 다시 건조기를 이용하여 24시간 건조하여 건조된 분말 조성물을 50 메쉬 체로 분말 조성물을 조립하였다. 조립한 분말 조성물은 지름 12 mm 몰드를 사용하여 150 psi의 압력으로 일축 성형한 후 20,000 psi의 압력으로 냉간등압성형하였다. 성형된 시편은 5℃/min의 승온 속도로 공기 중에서 880 내지 960℃에서 2시간 소결 후 노냉하였다.The calcined powders of BiNb 1-X B X O 4 (B = Sb or P) or Bi 1-X A x NbO 4 (A = Sm or Dy) thus obtained were subjected to sintering aids with a certain amount of CuO and V 2. O 5 was added and again wet mixed with ethanol for 24 hours using a stabilized zirconia ball, and then dried for 24 hours using a dryer to assemble the powder composition into a 50 mesh sieve. The granulated powder composition was uniaxially molded at a pressure of 150 psi using a 12 mm diameter mold and then cold isostatically molded at a pressure of 20,000 psi. The molded specimen was sintered after sintering at 880 to 960 ° C. for 2 hours in air at a temperature rising rate of 5 ° C./min.

이렇게 하여 얻은 소결 시편은 휴렛 패커드사(HP 8720C)의 네트워크 분석기를 이용하여 하끼 (Hakki)와 콜먼 (Coleman)에 의해 제시되고 고바야시 (Kobayashi)와 다나까 (Tanaka)가 보정한 post resonant method를 사용하여 마이크로파 유전 특성을 측정하였고, 아래 수학식 1에 따라 각 온도에서의 공진주파수의 변화를 측정하여 공진주파수의 온도 계수를 구하여, 그 결과를 하기 표 2 내지 6에 나타내었다.The sintered specimens thus obtained were presented by Haki and Coleman using a network analyzer from Hewlett-Packard (HP 8720C) and using the post resonant method corrected by Kobayashi and Tanaka. The microwave dielectric properties were measured, and the temperature coefficient of the resonance frequency was obtained by measuring the change of the resonance frequency at each temperature according to Equation 1 below, and the results are shown in Tables 2 to 6 below.

상기 식에서, fT₁ = 온도 T1에서의 공진주파수, fT₂ = 온도 T2에서의 공진주파수, T2 = 80 ℃, T1 = 20 ℃이다.Wherein the expression, f = resonant frequency T₁, T₂ f = resonance frequency at temperature T 2 at a temperature T 1, T 2 = 80 ℃ , T 1 = 20 ℃.

또한, 본 발명의 비교예로서 출발 물질로서 Bi2O3와 Nb2O4를 사용하여 BiNbO4 조성의 세라믹 조성물을 상기 방법과 동일하게 제조하고 각 유전 특성을 측정하여 그 결과를 표 1에 나타내었다.In addition, as a comparative example of the present invention, using Bi 2 O 3 and Nb 2 O 4 as starting materials, a ceramic composition having a BiNbO 4 composition was prepared in the same manner as described above, and the dielectric properties thereof were measured. It was.

BiNbO4 조성의 세라믹 조성물의 유전 특성 (비교예)Dielectric Properties of Ceramic Composition of BiNbO 4 Composition (Comparative Example) 조성Furtherance 소결 조제Sintering aid 소결온도 (℃)Sintering Temperature (℃) 밀도 (g/cm3)Density (g / cm 3 ) 유전상수 (εr)Dielectric constant (ε r ) 품질계수(Q·f(GHz))Quality factor (Q · f (GHz)) CuO(중량％)CuO (% by weight) V2O5 (중량％)V 2 O 5 (wt%) BiNbO4 BiNbO 4 0.03 0.03 0.07 0.07 880880 7.037.03 41.7241.72 19,80019,800 900900 7.127.12 42.3242.32 21,90021,900 920920 7.147.14 42.6242.62 19,80019,800 940940 7.157.15 42.7042.70 16,60016,600 960960 7.157.15 42.9042.90 14,90014,900 0.1 0.1 0.1 0.1 900900 7.267.26 42.9842.98 19,50019,500 920920 7.267.26 42.8342.83 18,30018,300 940940 7.257.25 42.7942.79 16,00016,000 960960 7.257.25 42.6542.65 13,60013,600

BiNb1-xSbxO4 조성의 세라믹 조성물의 유전 특성 (실시예)Dielectric Properties of Ceramic Compositions of BiNb 1-x Sb x O 4 Compositions (Examples) 조성Furtherance 소결 조제Sintering aid 소결온도 (℃)Sintering Temperature (℃) 밀도 (g/cm3)Density (g / cm 3 ) 유전상수 (εr)Dielectric constant (ε r ) 품질계수(Q·f(GHz))Quality factor (Q · f (GHz)) CuO(중량％)CuO (% by weight) V2O5 (중량％)V 2 O 5 (wt%) BiNb0.99Sb0.01O4 BiNb 0.99 Sb 0.01 O 4 0.03 0.03 0.07 0.07 880880 7.047.04 41.8341.83 30,80030,800 900900 7.137.13 42.6542.65 31,40031,400 920920 7.147.14 42.8242.82 32,80032,800 940940 7.167.16 42.8342.83 27,80027,800 960960 7.157.15 43.0243.02 23,80023,800 BiNb0.975Sb0.025O4 BiNb 0.975 Sb 0.025 O 4 0.03 0.03 0.07 0.07 880880 7.067.06 43.0243.02 35,90035,900 900900 7.167.16 43.4143.41 36,20036,200 920920 7.207.20 43.6343.63 41,80041,800 940940 7.217.21 43.7243.72 40,70040,700 960960 7.217.21 43.9943.99 35,30035,300 BiNb0.95Sb0.05O4 BiNb 0.95 Sb 0.05 O 4 0.03 0.03 0.07 0.07 880880 7.197.19 43.3143.31 32,10032,100 900900 7.217.21 43.6543.65 32,50032,500 920920 7.247.24 43.7843.78 34,30034,300 940940 7.237.23 44.0644.06 32,20032,200 960960 7.227.22 44.2044.20 32,00032,000 BiNb0.9Sb0.1O4 BiNb 0.9 Sb 0.1 O 4 0.03 0.03 0.07 0.07 880880 7.227.22 43.9543.95 24,30024,300 900900 7.257.25 44.3844.38 23,80023,800 920920 7.267.26 44.6744.67 22,30022,300 940940 7.257.25 44.6444.64 19,90019,900 960960 7.257.25 44.7044.70 14,40014,400

BiNb1-xPxO4 조성의 세라믹 조성물의 유전 특성 (실시예)Dielectric Properties of Ceramic Compositions of BiNb 1-x P x O 4 Compositions (Examples) 조성Furtherance 소결 조제Sintering aid 소결온도 (℃)Sintering Temperature (℃) 밀도 (g/cm3)Density (g / cm 3 ) 유전상수 (εr)Dielectric constant (ε r ) 품질계수(Q·f(GHz))Quality factor (Q · f (GHz)) CuO(중량％)CuO (% by weight) V2O5 (중량％)V 2 O 5 (wt%) BiNb0.99P0.01O4 BiNb 0.99 P 0.01 O 4 0.03 0.03 0.07 0.07 880880 6.966.96 40.0040.00 23,00023,000 900900 7.017.01 40.9540.95 25,20025,200 920920 7.067.06 41.6641.66 28,20028,200 940940 7.117.11 42.2642.26 29,60029,600 960960 7.107.10 42.2442.24 30,30030,300 BiNb0.975P0.025O4 BiNb 0.975 P 0.025 O 4 0.03 0.03 0.07 0.07 880880 6.916.91 39.5339.53 24,00024,000 900900 6.976.97 40.4240.42 27,20027,200 920920 7.027.02 41.5041.50 29,30029,300 940940 7.017.01 42.0842.08 33,30033,300 960960 7.017.01 42.1642.16 34,00034,000 BiNb0.95P0.05O4 BiNb 0.95 P 0.05 O 4 0.03 0.03 0.07 0.07 880880 6.896.89 38.9638.96 21,60021,600 900900 6.946.94 40.1840.18 22,90022,900 920920 6.976.97 40.7140.71 26,00026,000 940940 7.037.03 41.5741.57 27,20027,200 960960 7.037.03 41.8741.87 28,00028,000 BiNb0.9P0.1O4 BiNb 0.9 P 0.1 O 4 0.03 0.03 0.07 0.07 880880 6.826.82 38.6138.61 20,40020,400 900900 6.906.90 39.2139.21 20,70020,700 920920 6.946.94 40.4240.42 23,80023,800 940940 7.017.01 41.1541.15 26,20026,200 960960 7.037.03 41.4941.49 27,20027,200

Bi1-xSmxNbO4 조성의 세라믹 조성물의 유전 특성 (실시예)Dielectric Properties of Ceramic Compositions of Bi 1-x Sm x NbO 4 Compositions (Examples) 조성Furtherance 소결 조제Sintering aid 소결온도 (℃)Sintering Temperature (℃) 밀도 (g/cm3)Density (g / cm 3 ) 유전상수 (εr)Dielectric constant (ε r ) 품질계수(Q·f(GHz))Quality factor (Q · f (GHz)) CuO(중량％)CuO (% by weight) V2O5 (중량％)V 2 O 5 (wt%) Bi0.99Sm0.01NbO4 Bi 0.99 Sm 0.01 NbO 4 0.1 0.1 0.1 0.1 900900 7.137.13 41.9841.98 29,70029,700 920920 7.207.20 42.2942.29 32,10032,100 940940 7.237.23 42.4142.41 30,00030,000 960960 7.237.23 42.2842.28 26,10026,100 Bi0.975Sm0.025NbO4 Bi 0.975 Sm 0.025 NbO 4 0.1 0.1 0.1 0.1 900900 7.107.10 41.5341.53 22,70022,700 920920 7.207.20 42.0642.06 28,50028,500 940940 7.227.22 42.3042.30 25,90025,900 960960 7.217.21 42.1742.17 25,70025,700 Bi0.95Sm0.05NbO4 Bi 0.95 Sm 0.05 NbO 4 0.1 0.1 0.1 0.1 900900 7.027.02 40.9540.95 20,00020,000 920920 7.137.13 41.8641.86 25,40025,400 940940 7.187.18 42.1242.12 22,30022,300 960960 7.197.19 42.1342.13 19,50019,500 Bi0.9Sm0.1NbO4 Bi 0.9 Sm 0.1 NbO 4 0.1 0.1 0.1 0.1 900900 6.926.92 40.5940.59 17,90017,900 920920 7.067.06 41.7341.73 21,50021,500 940940 7.127.12 41.7141.71 21,50021,500 960960 7.147.14 41.7841.78 19,50019,500

Bi1-xDyxNbO4 조성의 세라믹 조성물의 유전 특성 (실시예)Dielectric Properties of Ceramic Compositions of Bi 1-x Dy x NbO 4 Compositions (Examples) 조성Furtherance 소결 조제Sintering aid 소결온도 (℃)Sintering Temperature (℃) 밀도 (g/cm3)Density (g / cm 3 ) 유전상수 (εr)Dielectric constant (ε r ) 품질계수(Q·f(GHz))Quality factor (Q · f (GHz)) CuO(중량％)CuO (% by weight) V2O5 (중량％)V 2 O 5 (wt%) Bi0.99Dy0.01NbO4 Bi 0.99 Dy 0.01 NbO 4 0.1 0.1 0.1 0.1 900900 7.207.20 41.9141.91 29,50029,500 920920 7.247.24 42.2042.20 28,60028,600 940940 7.247.24 42.3942.39 25,40025,400 960960 7.327.32 42.2042.20 23,90023,900 Bi0.975Dy0.025NbO4 Bi 0.975 Dy 0.025 NbO 4 0.1 0.1 0.1 0.1 900900 7.187.18 41.2141.21 32,40032,400 920920 7.237.23 42.0242.02 33,80033,800 940940 7.247.24 42.2542.25 28,90028,900 960960 7.237.23 41.9741.97 28,10028,100 Bi0.95Dy0.05NbO4 Bi 0.95 Dy 0.05 NbO 4 0.1 0.1 0.1 0.1 900900 7.197.19 40.9340.93 24,20024,200 920920 7.217.21 41.2441.24 25,40025,400 940940 7.227.22 41.7641.76 24,10024,100 960960 7.207.20 41.4641.46 21,10021,100 Bi0.9Dy0.1NbO4 Bi 0.9 Dy 0.1 NbO 4 0.1 0.1 0.1 0.1 900900 7.177.17 40.5340.53 23,60023,600 920920 7.207.20 40.8140.81 24,80024,800 940940 7.207.20 40.9440.94 22,30022,300 960960 7.187.18 40.0840.08 20,80020,800

BiNb1-xBxO4 (B = Sb+5, P+5) 세라믹 조성물 및 Bi1-xAxNbO4 (A = Sm+3, Dy+3) 세라믹 조성물의 공진주파수의 온도계수 (τf (ppm/℃)) (소결온도: 920℃)Temperature coefficients of the resonant frequencies of BiNb 1-x B x O 4 (B = Sb +5 , P +5 ) ceramic compositions and Bi 1-x A x NbO 4 (A = Sm +3 , Dy +3 ) ceramic compositions τ f (ppm / ℃)) (sintering temperature: 920 ℃) 조성Furtherance 소결 조제Sintering aid τf (ppm/℃)τ f (ppm / ℃) CuO (중량％)CuO (wt%) V2O5(중량％)V 2 O 5 (wt%) BiNbO4 BiNbO 4 0.030.03 0.070.07 -3.91-3.91 BiNb0.99Sb0.01O4 BiNb 0.99 Sb 0.01 O 4 0.030.03 0.070.07 -7.10-7.10 BiNb0.975Sb0.025O4 BiNb 0.975 Sb 0.025 O 4 0.030.03 0.070.07 -14.40-14.40 BiNb0.95Sb0.05O4 BiNb 0.95 Sb 0.05 O 4 0.030.03 0.070.07 -18.30-18.30 BiNb0.9Sb0.1O4 BiNb 0.9 Sb 0.1 O 4 0.030.03 0.070.07 -26.09-26.09 BiNb0.99P0.01O4 BiNb 0.99 P 0.01 O 4 0.030.03 0.070.07 -3.91-3.91 BiNb0.975P0.025O4 BiNb 0.975 P 0.025 O 4 0.030.03 0.070.07 -3.03-3.03 BiNb0.95P0.05O4 BiNb 0.95 P 0.05 O 4 0.030.03 0.070.07 -2.81-2.81 BiNb0.9P0.1O4 BiNb 0.9 P 0.1 O 4 0.030.03 0.070.07 -2.14-2.14 BiNbO4 BiNbO 4 0.10.1 0.10.1 -2.30-2.30 Bi0.99Sm0.01NbO4 Bi 0.99 Sm 0.01 NbO 4 0.10.1 0.10.1 -5.23-5.23 Bi0.975Sm0.025NbO4 Bi 0.975 Sm 0.025 NbO 4 0.10.1 0.10.1 -6.76-6.76 Bi0.95Sm0.05NbO4 Bi 0.95 Sm 0.05 NbO 4 0.10.1 0.10.1 -9.46-9.46 Bi0.9Sm0.1NbO4 Bi 0.9 Sm 0.1 NbO 4 0.10.1 0.10.1 -11.39-11.39 Bi0.99Dy0.01NbO4 Bi 0.99 Dy 0.01 NbO 4 0.10.1 0.10.1 -6.14-6.14 Bi0.975Dy0.025NbO4 Bi 0.975 Dy 0.025 NbO 4 0.10.1 0.10.1 -9.13-9.13 Bi0.95Dy0.05NbO4 Bi 0.95 Dy 0.05 NbO 4 0.10.1 0.10.1 -12.93-12.93 Bi0.9Dy0.1NbO4 Bi 0.9 Dy 0.1 NbO 4 0.10.1 0.10.1 -14.84-14.84

상기 표에서 볼 수 있는 바와 같이, 본 발명에 따른 마이크로파 유전체 세라믹 조성물은 960℃이하의 온도에서 소결이 가능하며, 기존의 BiNbO4 조성의 유전체 세라믹 조성물에 비해 유전상수 및 품질계수 특성이 우수하고 공진주파수의 온도계수가 양호하였다. 구체적으로, BiNb1-xBxO4 조성의 세라믹 조성물의 경우 유전율이 40 내지 44, 품질계수는 14,000 내지 42,000을 나타내었으며, Bi1-xAxNbO4 조성의 세라믹 조성물의 경우 유전율이 40 내지 42, 품질계수는 20,000 내지 32,000를 나타내었다.As can be seen in the above table, the microwave dielectric ceramic composition according to the present invention is capable of sintering at a temperature of 960 ° C. or less, and has better dielectric constant and quality coefficient characteristics and resonance than the conventional dielectric ceramic composition of BiNbO 4 composition. The temperature coefficient of the frequency was good. Specifically, the dielectric constant is 40 to 44, the quality factor is 14,000 to 42,000 for the ceramic composition of BiNb 1-x B x O 4 composition, the dielectric constant is 40 for the ceramic composition of Bi 1-x A x NbO 4 composition To 42, the quality factor is 20,000 to 32,000.

본 발명에 따른 마이크로파 유전체 세라믹 조성물은 880 내지 960℃의 온도에서 소결이 가능하며 유전상수 및 품질계수 특성이 우수하고 공진주파수의 온도계수가 양호하여 적층형 통신기기 소자의 내부 전극으로 사용되는 Ag 또는 Cu 전극과 동시 소결이 가능하여 적층형 통신 소자의 유전체 재료로서 이용될 수 있다.The microwave dielectric ceramic composition according to the present invention can be sintered at a temperature of 880 to 960 ℃, excellent dielectric constant and quality coefficient characteristics, good temperature coefficient of resonance frequency Ag or Cu electrode used as the internal electrode of the laminated communication device element Simultaneous sintering is possible and can be used as a dielectric material for stacked communication devices.

Claims (6)

하기 화학식 1의 조성을 갖는 저온 소성용 마이크로파 유전체 세라믹 조성물.Microwave dielectric ceramic composition for low-temperature baking having a composition of the formula (1). <화학식 1><Formula 1> Bi1-xAxNbO4 Bi 1-x A x NbO 4 상기 식에서,Where A는 Sm 또는 Dy이고, 0 < x ≤0.1이다.A is Sm or Dy and 0 <x ≦ 0.1. 제1항에 있어서, 소결 조제로서 0.03 내지 0.25 중량％ CuO 및 0.03 내지 0.25 중량％ V2O5를 더 포함하는 저온 소성용 마이크로파 유전체 세라믹 조성물.The microwave dielectric ceramic composition according to claim 1, further comprising 0.03 to 0.25 wt% CuO and 0.03 to 0.25 wt% V 2 O 5 as a sintering aid. 하기 화학식 2의 조성을 갖는 저온 소성용 마이크로파 유전체 세라믹 조성물.Microwave dielectric ceramic composition for low-temperature baking having a composition of the formula (2). <화학식 2><Formula 2> BiNb1-xBxO4 BiNb 1-x B x O 4 상기 식에서,Where B는 Sb 또는 P이며, x는 0 < x ≤0.1이다.B is Sb or P, and x is 0 <x ≦ 0.1. 제3항에 있어서, 소결 조제로서 0.03 내지 0.25 중량％ CuO 및 0.03 내지 0.25 중량％ V2O5를 더 포함하는 저온 소성용 마이크로파 유전체 세라믹 조성물.4. The microwave dielectric ceramic composition for low temperature firing according to claim 3, further comprising 0.03 to 0.25 wt% CuO and 0.03 to 0.25 wt% V 2 O 5 as a sintering aid. Sb2O5, H3PO4, Sm2O3 및 Dy2O 3로 이루어진 군으로부터 선택된 화합물과 Bi2O3 및 Nb2O5을 습식 혼합한 후, 건조하고 열처리하는 단계를 포함하는, 제1항 또는 제3항에 기재된 세라믹 조성물의 제조 방법.And wet mixing a compound selected from the group consisting of Sb 2 O 5 , H 3 PO 4 , Sm 2 O 3, and Dy 2 O 3 with Bi 2 O 3 and Nb 2 O 5 , followed by drying and heat treatment. The manufacturing method of the ceramic composition of Claim 1 or 3. 제1항 또는 제3항에 기재된 세라믹 조성물에 소결 조제로서 CuO 및 V2O5를 첨가하여 습식 혼합 및 건조한 후 소결하는 단계를 포함하는, 제2항 또는 제4항에 기재된 세라믹 조성물의 제조 방법.The method for producing the ceramic composition according to claim 2 or 4, comprising the step of adding CuO and V 2 O 5 as a sintering aid to the ceramic composition according to claim 1 or 3, followed by wet mixing, drying and sintering. .
KR1020040030517A 2004-04-30 2004-04-30 Microwave dielectric ceramic composition for low temperature firing and preparation method thereof KR20050105392A (en)

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