KR100225880B1 - Composition of high frequency dielectrics - Google Patents

Composition of high frequency dielectrics Download PDF

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KR100225880B1
KR100225880B1 KR1019970004899A KR19970004899A KR100225880B1 KR 100225880 B1 KR100225880 B1 KR 100225880B1 KR 1019970004899 A KR1019970004899 A KR 1019970004899A KR 19970004899 A KR19970004899 A KR 19970004899A KR 100225880 B1 KR100225880 B1 KR 100225880B1
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dielectric
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high frequency
temperature coefficient
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김현재
정형진
윤석진
아이 쿠치코 세르게이
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박호군
한국과학기술연구원
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    • H—ELECTRICITY
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    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract

본 발명은 마이크로파 대역에서 높은 품질 계수와 유전율을 가지며 공진 주파수의 온도 계수가 안정한 고주파용 유전체 자기 조성물로서, (1-x)(La1/2Na1/2)TiO3-xCa(Fe1/2Nb1/2)O3(식중, 0.4 ≤ x ≤ 0.7)로 나타내지는 고주파용 유전체 자기 조성물에 관한 것이다. 이 조성물은 Ca(Fe1/2Nb1/2)O3의 함량을 조절함으로써 공진 주파수의 온도 계수의 조정이 용이해서, 유전체 공진기 소재로서의 응용이 적합하다.The present invention is a high-frequency dielectric ceramic composition having a high quality coefficient and dielectric constant in the microwave band and a stable temperature coefficient of resonant frequency, wherein (1-x) (La 1/2 Na 1/2 ) TiO 3 -xCa (Fe 1 / It relates to a dielectric ceramic composition for high frequency represented by 2 Nb 1/2 ) O 3 (wherein 0.4 ≦ x ≦ 0.7). By adjusting the content of Ca (Fe 1/2 Nb 1/2 ) O 3, the composition is easy to adjust the temperature coefficient of the resonant frequency, and is suitable for application as a dielectric resonator material.

Description

고주파용 유전체 조성물High Frequency Dielectric Composition

본 발명은 마이크로파 대역에서 높은 품질 계수와 유전율을 가지며 공진 주파수의 온도 계수가 안정한 (1-x)(La1/2Na1/2)TiO3-xCa(Fe1/2Nb1/2)O3계의 고주파용 유전체 자기 조성물에 관한 것이다.In the present invention, (1-x) (La 1/2 Na 1/2 ) TiO 3 -xCa (Fe 1/2 Nb 1/2 ) O, which has high quality factor and dielectric constant and stable temperature coefficient of resonant frequency in microwave band It relates to three types of high frequency dielectric ceramic composition.

최근 전자, 통신 및 정보 산업의 발전에 따라 이동 통신 또는 위성 방송 등 마이크로파를 이용한 통신 시스템이 급속히 발전하고 있으며, 이들 마이크로파 기기를 구성하는 핵심 부품인 마이크로파 필터의 위성 방송 송수신부의 국부 발진기, 마이크로파 집적 회로 기판 등에는 고주파용 유전체 세라믹스가 이용되고 있다. 이러한 통신 시스템에 응용되는 고주파용 유전체로서 요구되는 특성은, (1) 유전체 내에서 파장이

Figure kpo00001
에 반비례하므로 부품의 소형화를 위해서는 유전율이 커야하고, (2) 고주파 영역에서는 유전 손실이 작아야 하고 (3) 공진 주파수의 온도 계수가 작아야 한다(W. Wersing : Electronic Ceramics, (B. C. H. Steel 편저) Elsevier Sci. Publ. Co., New York, p.65(1991)참조).Recently, with the development of the electronics, telecommunications, and information industries, communication systems using microwaves such as mobile communication or satellite broadcasting are rapidly developing, and local oscillators and microwave integrated circuits of the satellite broadcasting transceiver of the microwave filter, which are the core components constituting these microwave devices, are being developed. High frequency dielectric ceramics are used for the substrate and the like. The characteristics required as a high frequency dielectric applied to such a communication system include (1) a wavelength in the dielectric.
Figure kpo00001
As it is inversely proportional, the dielectric constant must be large to reduce parts, (2) the dielectric loss must be small in the high frequency region, and (3) the temperature coefficient of the resonance frequency must be small (W. Wersing: Electronic Ceramics, (BCH Steel)) Elsevier Sci Publ.Co., New York, p. 65 (1991).

지금까지 개발된 유전체 세라믹스로는, 고유전율 계로서 유전율이 80 내지 90인 BaO-PbO-Nd2O3-TiO2계, (Pb,Ca)ZrO3계 등이 있으며 유전율이 비교적 낮은 40 이하인 MgTiO3-CaTiO3, Ba(Sn,Mg,Ta)O3, Ba(Sn,Mg,Ta)O3, Ba(Zr,Zn,Ta)O3, (Zr,Sn)TiO4계 등이 알려져 있다(Kikuo Wakino, Toshio Nishikawa and Youhei Ishikawa : Br. Cream. Trans. J., 89(1990)No.2,p.39참조).The dielectric ceramics developed so far include BaO-PbO-Nd 2 O 3 -TiO 2 type having a dielectric constant of 80 to 90, (Pb, Ca) ZrO 3 type , and MgTiO having a relatively low dielectric constant of 40 or less. 3 -CaTiO 3 , Ba (Sn, Mg, Ta) O 3 , Ba (Sn, Mg, Ta) O 3 , Ba (Zr, Zn, Ta) O 3 , (Zr, Sn) TiO 4 , etc. are known. (Kikuo Wakino, Toshio Nishikawa and Youhei Ishikawa: Br. Cream. Trans. J., 89 (1990) No. 2, p. 39).

일반적으로, 유전율이 큰 재료는 유전체 내부의 쌍극자 및 결함 등으로 인하여 유전 손실과 온도 계수가 증가하게 되어 고주파 유전체로서 3가지 요구 조건 즉 높은 유전율, 낮은 유전 손실 및 공진 주파수의 안정한 온도 계수를 가지는 이러한 조성이 현실적으로 어려우며, 특히 고주파용 유전체는 공진 주파수의 온도 계수가 안정해야 그 응용이 가능하다.In general, materials with high dielectric constants have increased dielectric losses and temperature coefficients due to dipoles and defects in the dielectrics, and thus are high frequency dielectric materials having stable temperature coefficients of three requirements: high dielectric constant, low dielectric loss and resonant frequency. The composition is practically difficult, and especially for high frequency dielectrics, the temperature coefficient of the resonant frequency is stable to enable the application thereof.

(La1/2Na1/2)TiO3의 경우, 유전율이 122 정도로 매우 높고 Q·f0가 9800으로 우수한 특성을 가지나, 온도 계수가 +480 ppm/℃로 매우 불안정하며 [Jpn. J. Appl. phys., 30, 2339~42(1991) 참조], Ca(Fe1/2Nb1/2)O3는 유전율은 40 정도로 작지만 , Q·f0가 20000 정도이며 온도 계수가 -76 ppm/℃가 된다 [Jpn. J. Appl. phys., 33, 5463~65(1994) 참조].In the case of (La 1/2 Na 1/2 ) TiO 3 , the dielectric constant is very high as 122 and Q · f 0 is excellent as 9800, but the temperature coefficient is very unstable at +480 ppm / ° C. [Jpn. J. Appl. phys., 30, 2339 ~ 42 (1991)], Ca (Fe 1/2 Nb 1/2 ) O 3 has a low dielectric constant of about 40, but Q · f 0 is about 20000 and temperature coefficient is -76 ppm / ℃. Becomes [Jpn. J. Appl. phys., 33, 5463-65 (1994).

따라서, 본 발명의 목적은 공진 주파수의 온도 계수가 불안정하여 실용화할 수 없는 두 재료의 합성을 통해, 유전율이 50 내지 70정도이며 유전 손실은 작고 공진 주파수의 온도 계수가 조절 가능한 유전체 조성물을 제공하는 것이다.Accordingly, an object of the present invention is to provide a dielectric composition having a dielectric constant of about 50 to 70 and a low dielectric loss and having a adjustable temperature coefficient of resonant frequency through the synthesis of two materials that are unusable due to unstable temperature coefficient of resonant frequency. will be.

상기한 바와 같은 본 발명의 목적은 다음과 같은 화학식 1을 갖는 유전체 자기 조성물을 제공함으로써 달성된다.The object of the present invention as described above is achieved by providing a dielectric ceramic composition having the following formula (1).

(1-x)(La1/2Na1/2)TiO3-xCa(Fe1/2Nb1/2)O3 (1-x) (La 1/2 Na 1/2 ) TiO 3 -xCa (Fe 1/2 Nb 1/2 ) O 3

(단, 0.4 ≤ x ≤ 0.7)(0.4 ≤ x ≤ 0.7)

본 발명의 유전체 자기 조성물의 특성은(La1/2Na1/2)TiO3와 Ca(Fe1/2Nb1/2)O3의 조성 변화에 따라 달라진다. Ca(Fe1/2Nb1/2)O3의 함량이 증가함에 따라 표 1에서 보이는 바와 같이 유전율이 74에서 46으로 감소하는 경향을 보이며, Q·f0(GHz)는 5310에서 15920으로 증가하고, 공진 주파수의 온도 계수(TCF)가 81에서 -54 ppm/℃로 크게 감소한다.The properties of the dielectric ceramic composition of the present invention depend on the composition change of (La 1/2 Na 1/2 ) TiO 3 and Ca (Fe 1/2 Nb 1/2 ) O 3 . As the content of Ca (Fe 1/2 Nb 1/2 ) O 3 increases, the dielectric constant decreases from 74 to 46 as shown in Table 1, and Q · f 0 (GHz) increases from 5310 to 15920. Then, the temperature coefficient TCF of the resonance frequency is greatly reduced from 81 to -54 ppm / 占 폚.

특히 Ca(Fe1/2Nb1/2)O3의 함량이 0.58 mol 일때 유전율은 58.9 내지 60.6 정도이고 Q·f0는 14070 내지 13040 정도이며 온도 계수는 0 ppm/℃로 통신 시스템에서의 응용에 적합한 유전체 세라믹스를 얻을 수 있다. 이와 같은 본 발명의 유전체 자기 조성물은 일반적으로 널리 사용되는 산화물 혼합 방법으로 용이하게 제작할 수 있다.Especially when the content of Ca (Fe 1/2 Nb 1/2 ) O 3 is 0.58 mol, the dielectric constant is about 58.9 to 60.6, Q · f 0 is about 14070 to 13040, and the temperature coefficient is 0 ppm / ℃. Dielectric ceramics suitable for the present invention can be obtained. Such a dielectric ceramic composition of the present invention can be easily produced by an oxide mixing method which is generally widely used.

예를 들어 출발 물질로서 La2O3, NaCO3, CaCO3, TiO2, Fe2O3, Nb2O5를 사용하여 일정 조성비로 정확히 평량하여 혼합, 분쇄한다. 혼합이 완료된 분말을 대기중에서 1100℃에서 4시간정도 하소한 후 다시 재분쇄하여 페로브스카이트 구조를 갖는 고용체를 합성하고, 이 분말을 10㎜ 원통형 금형을 사용하여 1ton/㎠의 압력으로 가압 성형하여 대기 중에서 1300~1400 ℃의 온도에서 5 ~10 시간 동안 소결하였다. 이와 같이 제조된 소결체의 유전율, Q 값 및 공진 주파수의 온도 계수등의 특성은 이미 잘 알려진 유전체 공진 기법으로 측정할 수 있다.For example, La 2 O 3 , NaCO 3 , CaCO 3 , TiO 2 , Fe 2 O 3 , Nb 2 O 5 as a starting material, exactly basis weight at a constant composition ratio is mixed and ground. The mixed powder was calcined at 1100 ° C. for 4 hours in the air, and then pulverized again to synthesize a solid solution having a perovskite structure. The powder was press-molded at a pressure of 1 ton / cm 2 using a 10 mm cylindrical mold. And sintered for 5 to 10 hours at a temperature of 1300 ~ 1400 ℃ in the air. The characteristics such as the dielectric constant, Q value, and temperature coefficient of the resonance frequency of the manufactured sintered body can be measured by a well-known dielectric resonance technique.

이하, 실시예와 함께 본 발명을 상세히 설명하고자 한다. 그러나, 본 발명을 이 실시예로 한정시키고자 하는 것은 아니다.Hereinafter, the present invention will be described in detail with examples. However, it is not intended to limit the present invention to this embodiment.

[실시예 1]Example 1

순도 99.9％의 La2O3, NaCO3, CaCO3, TiO2, Fe2O3, Nb2O5를 다음의 표 1과 같은 조성비로 평량하고, 지르코니아볼을 이용하여 볼밀로 16 시간 동안 혼합 분쇄한 후 건조시켰다. 이 분말을 대기 중에서 1100℃에서 4시간 동안 하소하여 페로브스카이트 구조의 고용체를 합성하였다.La 2 O 3 , NaCO 3 , CaCO 3 , TiO 2 , Fe 2 O 3 , Nb 2 O 5 with a purity of 99.9% were weighed in the composition ratio as shown in Table 1 below, and mixed for 16 hours using a ball mill using zirconia balls. After grinding it was dried. The powder was calcined at 1100 ° C. for 4 hours in air to synthesize a solid solution of perovskite structure.

하소된 이 분말에 5％ PVA 바인더를 5 wt％ 첨가한 후, 재볼밀하여 분쇄하고 건조시킨 후 원통형 금형(ψ = 10 ㎜)을 이용하여 1 ton/㎠의 압력으로 가압 성형하였다. 600℃의 온도에서 1시간 동안 열처리하여 유기 바인더를 제거한 후, 대기 중에서 1300 ~ 1400 ℃의 온도에서 5 ~10시간 동안 고온 소결하여 시편의 높이/직경의 비가 0.4 ~ 0.5가 되는 시편을 얻었다.5 wt% of a 5% PVA binder was added to the calcined powder, followed by reball milling, pulverization and drying, followed by pressure molding at a pressure of 1 ton / cm 2 using a cylindrical mold (ψ = 10 mm). After removing the organic binder by heat treatment at a temperature of 600 ℃ for 1 hour, and high temperature sintering for 5 to 10 hours at a temperature of 1300 ~ 1400 ℃ in the air to obtain a specimen with a height / diameter ratio of 0.4 ~ 0.5.

소결된 시편의 양면을 연마지(＃1200까지)와 알루미나 연마제로 연마한 후, 두 평행 도체판 사이에 넣고 6~7 GHz에서 유전율, Q 값, 공진 주파수의 온도 계수를 측정하였다. 온도 계수의 측정 온도 범위는 25℃에서 80℃로 하였다. 각 시편의 조성에 따른 결과를 다음의 표 1에 나타내었다.Both sides of the sintered specimen were ground with abrasive paper (up to 1200) and alumina abrasive, and then sandwiched between two parallel conductor plates, and the temperature coefficients of the dielectric constant, Q value, and resonance frequency were measured at 6 to 7 GHz. The measurement temperature range of the temperature coefficient was 25 degreeC to 80 degreeC. The results according to the composition of each specimen are shown in Table 1 below.

[표 1]TABLE 1

Figure kpo00002
Figure kpo00002

상기 표 1에서 알 수 있는 바와 같이, 조성물인 Ca(Fe1/2Nb1/2)O3의 함량을 조절함으로써 온도 계수가 안정하며 비교적 높은 Q 값을 갖는 마이크로파 기기의 소자로서 응용이 가능한 소결체를 얻을 수 있다.As can be seen in Table 1, by controlling the content of the composition Ca (Fe 1/2 Nb 1/2 ) O 3 The temperature coefficient is stable and can be applied as a device of a microwave device having a relatively high Q value Can be obtained.

Claims (2)

다음의 화학식, (1-x)(La1/2Na1/2)TiO3-xCa(Fe1/2Nb1/2)O3(단, 0.4 ≤ x ≤ 0.7)으로 나타내어지는 고주파용 유전체 조성물.High frequency dielectric represented by the following chemical formula, (1-x) (La 1/2 Na 1/2 ) TiO 3 -xCa (Fe 1/2 Nb 1/2 ) O 3 (wherein 0.4 ≦ x ≦ 0.7) Composition. 제1항에 있어서, 상기 x의 범위가 0.55 ≤ x ≤ 0.60인 고주파용 유전체 조성물.The dielectric composition for high frequency of claim 1, wherein x is in a range of 0.55 ≦ x ≦ 0.60.
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