KR970005881B1 - Dielectric composition for high frequencies - Google Patents
Dielectric composition for high frequencies Download PDFInfo
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Abstract
Description
첨부된 도면은 (Zr, Sn)TiO4계 고주파용 유전체의 기본조성도이다.The accompanying drawings are the basic composition of the (Zr, Sn) TiO 4 -based high frequency dielectric.
본 발명은 (Zr,Sn)TiO4계를 기본조성으로 하는 고주파용 저손실 유전체 제료에 관한 것으로, 특히 기본조성에 소결조제로서 산화붕소(B2O3)나 산화인(P2O5)을 소량 첨가하여 소결조제의 휘발이 없이 낮은 소결 온도에서 소결이 가능하면서도 우수한 유전특성과 품질계수를 갖도록 한 고주파용 유전체 조성물에 관한 것이다.The present invention relates to a low loss dielectric material for high frequency, which is based on a (Zr, Sn) TiO 4 system. Particularly, boron oxide (B 2 O 3 ) or phosphorus oxide (P 2 O 5 ) is used as a sintering aid in the basic composition. The present invention relates to a dielectric composition for high frequency, in which a small amount is added so that sintering is possible at low sintering temperature without volatilization of the sintering aid and has excellent dielectric properties and quality coefficient.
일반적으로 고주파용 유전체 재료는 자동차 전화기나 휴대용 무선전화기등의 이동통신을 비롯한 인공위성에 의한 직접 위성통신이나 위성방송등의 마이크로파를 이용한 정보통신 시스템의 공진기 소자로 널리 사용되고 있다.In general, high frequency dielectric materials are widely used as resonator elements of information communication systems using microwaves such as direct satellite communication or satellite broadcasting by satellites, including mobile communication such as automobile telephones and portable wireless telephones.
이와같이 마이크로파 통신기기등에 사용되는 고주파 유전체 재료에서는 유전상수와 품질계수가 크고, 또한 공진주파수의 온도의존도가 작아야 하는 특성이 요구되고 있다.As described above, high frequency dielectric materials used in microwave communication devices and the like require a high dielectric constant and quality coefficient and a low temperature dependence of the resonance frequency.
지금까지 보고된 유전체 자기중 대표적인 몇가지를 살펴보면, 유전율은 40이하이나 낮은 유전손실을 갖는 Ba(M+2 1/3M+5 2/3)O3(M+2= Mg, Zn, M+5= Ta, Nb 계 [참고문헌 :K.Matsumoto, T. Hiuga, K. Takada and H. Ichimura, Ba(Mg1/3Ta2/3)O3cerma.cs with ultra - Low Loss at microwave frequiencies Inproce, of the sixth IEEE International symposium on Applications of Ferroelectrics, pp. 118 ∼ 121(1986)], Ba2TiO20계 [참고문헌 : S. Nisikaki et al., 〃BaO - TiO2- WO3Microwave Ceramics and Crystaline BaWO4, J. Am. Ceram. Soc., 71(1) C - 11 - C - 17(1988)] 및 (Zr,Sn)TiO4계 [참고문헌 : K. Wakino etal., Microwave Characteristics of (Zr, Sn)TiO4and BaO - PbO - Nd2O3-TTO2Dielectric Resonators, J. Am. Ceram. Soc., 67(4), 278 ∼ 281(1983)] 이 알려져 있다.Some representative genome magnets reported so far have a dielectric constant of 40 or less, but low dielectric loss Ba (M +2 1/3 M +5 2/3 ) O 3 (M +2 = Mg, Zn, M + 5 = Ta, Nb system [Reference: K.Matsumoto, T. Hiuga, K. Takada and H. Ichimura, Ba (Mg 1/3 Ta 2/3 ) O 3 cerma.cs with ultra-Low Loss at microwave frequiencies Inproce, of the sixth IEEE International symposium on Applications of Ferroelectrics, pp. 118-121 (1986)], Ba 2 TiO 20 system [Reference: S. Nisikaki et al., 〃BaO-TiO 2 -WO 3 Microwave Ceramics and Crystaline BaWO 4 , J. Am. Ceram. Soc., 71 (1) C-11-C-17 (1988)] and (Zr, Sn) TiO 4 system [Ref. K. Wakino et al., Microwave Characteristics of (Zr, Sn) TiO 4 and BaO-PbO-Nd 2 O 3 -T T O 2 Dielectric Resonators, J. Am. Ceram. Soc., 67 (4), 278-281 (1983).
그리고 유전손실은 비교적 크나 (Qxfo(㎓)〈1000) 유전율이 80이상인 재료로서 BaO - Sm2O3- TiO2계 [J.M. Wu and M. C. Chang Reaction Sequence and Effects of Calcination and Sintering on Mictowave Properties of (Ba, Sr)O - Sm2O3- TiO2Ceramics, J, Am. Ceram. Ceram. Soc., 73(6), 1599 ∼ 1605(1990)] , (Ba,Pb)O - Nd2O3- TiO3계 [참고문헌 : K. Wakino et al., Microwave Characteristics of (Zr,Sn)TiO4계 and Bao - PbO - Nd2O3- TiO2Dielectric Resonators, J. Am. Ceram. Soc., 67(4), 278 ∼ 281(9183)] 및 (Pb,Ca)ZrO3계 [참고문헌 : J. Kato, Material Produces Small Resonators with High Dielectric Constan, JEE, Sep., 114 ∼ 118(1991)] 등이 알려져 있다.The dielectric loss is relatively large (Qxfo (㎓) <1000) and the material has a dielectric constant of 80 or more, which is BaO-Sm 2 O 3 -TiO 2 system [JM Wu and MC Chang Reaction Sequence and Effects of Calcination and Sintering on Mictowave Properties of (Ba , Sr) O-Sm 2 O 3 -TiO 2 Ceramics, J, Am. Ceram. Ceram. Soc., 73 (6), 1599-1605 (1990)], (Ba, Pb) O-Nd 2 O 3 -TiO 3 system [Reference: K. Wakino et al., Microwave Characteristics of (Zr, Sn) TiO 4 based and Bao-PbO-Nd 2 O 3 -TiO 2 Dielectric Resonators, J. Am. Ceram. Soc., 67 (4), 278-281 (9183)] and (Pb, Ca) ZrO 3 system [Reference: J. Kato, Material Produces Small Resonators with High Dielectric Constan, JEE, Sep., 114-118 ( 1991).
일반적인 경향으로서 유전율이 큰 재료는 유전체 내부의 쌍극자와 결합등으로 인해서 유전손실과 공진주파수의 온도계수가 증가되는 특징을 지니게 되는데, 고주파용 유전체는 우선적으로 공진주파수의 온도계수가 ±10ppm/℃ 정도로 안정하여야 응용이 가능하다.As a general tendency, materials with high dielectric constants have characteristics of increasing dielectric loss and resonant frequency due to dipoles and couplings in the dielectric. High-frequency dielectrics should be stable at ± 10 ppm / ℃. Application is possible.
그리고, 또 다른 종래의 고주파용 유전체 재료로서 유전상수가 35 ∼ 38정도이만 품질계수가 7㎓에서 50000이상인 (Zr,Sn)TiO4계의 재료가 알려져 있다.As another conventional high frequency dielectric material, a material of (Zr, Sn) TiO 4 type having a dielectric constant of about 35 to 38 but having a quality factor of 7 to 50000 or more is known.
상기 (Zr,Sn)TiO4계 저손실 유전체 재료는 첨부된 도면의 ZrO2- SnO2- TiO2삼원계도에 나타난 바와같이 몰비로 0.7ZrO2+0.3SnO2+1.0TiO2으로 이루어진 기본조정에 일반적으로 소결성과 유전특성의 증진을 위하여 산화아연(ZnO) 또는 산화비스머스(Bi2O3)가 소량 첨가되어서 이루진다. [참조 : K. Wakino et. al., Microwave Characteristics of (Zr,Sn)TiO4and BaO - PbO - Nd2O3- TiO2Dielectric Resonators, J. Am Ceram. Soc., 67(4) 278 ∼ 281(1983)]The (Zr, Sn) TiO 4 -based low loss dielectric material is generally used for basic adjustment of 0.7ZrO 2 + 0.3SnO 2 + 1.0TiO 2 in molar ratio as shown in the ZrO 2 -SnO 2 -TiO 2 ternary diagram of the accompanying drawings. As a result, a small amount of zinc oxide (ZnO) or bismuth oxide (Bi 2 O 3 ) is added to enhance the sinterability and dielectric properties. [See K. Wakino et. al., Microwave Characteristics of (Zr, Sn) TiO 4 and BaO-PbO-Nd 2 O 3 -TiO 2 Dielectric Resonators, J. Am Ceram. Soc., 67 (4) 278-281 (1983)].
그런데, (Zr,Sn)TiO4계 저손실 유전체 재료에서 소결성과 유전특성의 향상을 위해서 첨가된 산화아연(ZnO)과 산화비스머스(Bi2O3)는 유전체의 소결온도를 150 ∼ 200℃ 가량 낮추어 줌으로써 소결성의 향상에는 크게 기여하는 반면에 소결중에 높은 휘발특성으로 인해 소결상황에 따라 얻어진 유전체의 색과 특성이 변화를 일으킴으로써 동일한 색채와 균일한 유전특성을 갖는 유전체의 제조가 곤란하여 생산수율을 저하시키는 문제점을 지니고 있다.However, zinc oxide (ZnO) and bismuth oxide (Bi 2 O 3 ) added to improve the sinterability and dielectric properties of (Zr, Sn) TiO 4 based low loss dielectric materials have a sintering temperature of about 150 to 200 ° C. By lowering, it greatly contributes to the improvement of sinterability, while the high volatility during sintering changes the color and characteristics of the dielectric obtained according to the sintering situation, making it difficult to manufacture dielectrics with the same color and uniform dielectric properties. It has a problem of degrading.
따라서, 본 발명은 상기 종래의 (Zr,Sn)Tio4계 유전체 재료의 소결조제가 지니고 있는 문제점을 해결하기 위하여(Zr,Sn)Tio4계를 주조성으로 하여 여기에 용융온도가 낮고 소결중에 휘발이나 분해 및 주조성과의 반응성이 낮은 산화붕소(B2O3)나 산화인(P2O5)을 소결조제로 사용하는 한편 유전체의 특성향을 위해 La2o3를 2.0wt%까지 첨가하여 저온소성이 가능하면서도 우수한 유전특성과 품질계수를 갖는 고주파용 유전체 조성물을 제공하는데 발명의 목적이 있다.Accordingly, the present invention is low in the prior art (Zr, Sn) Tio 4 system to solve the problems which have a sintering aid of a dielectric material and the Tio 4 series (Zr, Sn) in the main composition of the melting temperature here during sintering Boron oxide (B 2 O 3 ) or phosphorus oxide (P 2 O 5 ) with low reactivity with volatilization, decomposition and castability are used as sintering aids, and La 2 O 3 is added up to 2.0wt% to improve the characteristics of the dielectric. It is an object of the present invention to provide a dielectric composition for high frequency having a low-temperature firing and excellent dielectric properties and quality coefficients.
본 발명 고주파용 유전체 조성물의 구체적인 조성은 다음과 같다.The specific composition of the high frequency dielectric composition of the present invention is as follows.
Zro2,SnO2및 TiO2의 총량을 100으로 할 때,When the total amount of Zro 2 , SnO 2 and TiO 2 is 100,
37.6〈ZrO2〈47.237.6 <ZrO 2 <47.2
19.3〈SnO2〈24.819.3 <SnO 2 <24.8
37.6〈 TiO2〈38.3인 (ZR,Sn)Tio4계(ZR, Sn) Tio 4 series with 37.6 <TiO 2 <38.3
를 기본조성으로 하여, 여기에 소결조체로서 0.3 ∼ 2.0wt%B2O3또는 0.3 ∼ 2.0wt%P2O5가 첨가되고, 유전특성의 향상을 위해 0.5 ∼ 2.0wt%NiO 및 0.3 ∼ 1.0wt%La2O3가 첨가된 조성이다.As a basic composition, 0.3 to 2.0 wt% B 2 O 3 or 0.3 to 2.0 wt% P 2 O 5 is added thereto as a sintered body, and 0.5 to 2.0 wt% NiO and 0.3 to 1.0 for improving the dielectric properties. wt% La 2 O 3 is added.
본 발명은 소결조제로서의 B2O3나 P2O5와 아울러 La+3이온이 함께 첨가되어 ZST결정구조내에서 전자농도를 증가시켜 소결을 촉진시킴으로써 유전특성의 향상을 도모할 수 있다.In the present invention, B 2 O 3 or P 2 O 5 as a sintering aid and La + 3 ions are added together to increase the electron concentration in the ZST crystal structure to promote sintering, thereby improving dielectric properties.
또한 유전율과 관련하여서는 La+3이 증가할수록 유전율이 증가함을 볼 수 있으며 이와같은 결과는 시편의 수축율 및 밀도와 연관이 있음을 볼 수 있다.In terms of dielectric constant, it can be seen that the dielectric constant increases as La +3 increases, and this result is related to the shrinkage and density of the specimen.
본 발명의 조성물에서 소결조제로서 사용되는 B2O3와 P2O5의 겨우 ZnO를 첨가한 조성에 비해 소결온도를 50℃가량 저하시키며 소결과정에서 소결조제 성분의 휘발이 일어나지 않음에 따라 우수하고 균일한 유전특성을 갖는 고주파용 유전체 소자의 대량생산의 용이하다는 장점이 있다.Compared with the composition of B 2 O 3 and P 2 O 5 used as the sintering aid in the composition of the present invention, the sintering temperature is lowered by about 50 ° C. and the volatilization of the sintering aid component does not occur during the sintering process. And it has the advantage of easy mass production of high frequency dielectric elements having uniform dielectric properties.
본 발명의 고주파용 유전체는 일반적으로 널리 사용되고 있는 산화물 혼합방법을 통하여 용이하게 제작된다.The high frequency dielectric of the present invention is easily manufactured through an oxide mixing method which is generally used.
즉, 본 발명 고주파용 유전체 재료의 조성이 유지되도록 기본조성의 원료분말과 첨가제 원료분말을 칭량하여 볼밀중에서 습식혼합과 분쇄과정을 거친 다음 후속공정으로서의 건조→하소→압축성형→소결공정을 수행하여 유전체 소자의 제작이 완료된다.That is, the raw powder and the additive raw powder of the basic composition are weighed so that the composition of the high frequency dielectric material of the present invention is maintained, followed by wet mixing and grinding in a ball mill, followed by drying, calcining, compression molding, and sintering. Fabrication of the dielectric element is completed.
본 발명 고주파용 유전체 재료는 소결조제로서의 B2O3, P2O5와 함께 유전특성의 향상을 위한 La2O3가 첨가됨에 따라 낮은 소결온도에서의 소결이 가능하며, 소결과정에서 우수하고 균일한 유전특성을 갖는 고주파용 유전체 소자의 대량 생산이 가능하다는 장점이 있기 때문에 5 ∼ 10㎓ 대역의 위성통신용 수신기, 고주파용 센서 및 스피드 건(speed gun)의 레이저 디텍트등에 사용 가능하다.The high frequency dielectric material of the present invention is capable of sintering at low sintering temperature as La 2 O 3 is added to improve dielectric properties together with B 2 O 3 and P 2 O 5 as sintering aids. Since it is possible to mass-produce high frequency dielectric elements with uniform dielectric properties, it can be used for satellite communication receivers in 5 to 10 GHz bands, high frequency sensors and laser detectors of speed guns.
본 발명 고주파용 유전체 재료의 제반 특성과 자세한 제조공정은 다음의 실시예를 통하여 보다 명확하게 이해될 것이다.Various characteristics and detailed manufacturing process of the high frequency dielectric material of the present invention will be more clearly understood through the following examples.
실시예Example
먼저, (Zr,Sn)Tio4계 기본조성을 이루는 원료분말로 TiO2, ZrO2및 SnO2와 소결조제로서의 B2O3또는 P2O5를 첨가한 후 유전특성 향상을 위한 NiO와 La2O3를 아래의 표 1 및 표 2 범위로 칭량하여 첨가하고 이들 원료분말을 알코과 지르코니아볼을 사용하여 24시간 동안 습식혼합과 분쇄를 행한 후 감압건조기에서 완전히 건조하였다.First, TiO 2 , ZrO 2 and SnO 2 and B 2 O 3 or P 2 O 5 as sintering aids were added as raw material powders for the basic composition of (Zr, Sn) Tio 4 system, followed by NiO and La 2 to improve dielectric properties. O 3 was added in the following Table 1 and Table 2, and the raw powders were wet mixed and ground for 24 hours using alcohol and zirconia balls, and then completely dried in a reduced pressure dryer.
다음, 혼합과 건조가 완료된 혼합분말 원료는 1000 ∼ 1200℃에서 2 ∼ 6시간 동안 하소한 후 결합체로 PVA수용액을 미량 첨가하여 200메쉬(mesh)체로 체가름하였다.Next, the mixed and dried powder raw material was calcined at 1000 ~ 1200 ℃ for 2 to 6 hours and then sifted into 200 mesh (mesh) by adding a small amount of PVA solution as a binder.
체가름이 행해진 하소분말을 직경이 10㎜인 금속제 몰드(mold)에서 1.5 ∼ 2ton/㎠의 압력으로 가압하여 두께가 4 ∼5㎚인 성형시편으로 제작하였다.The calcined powder subjected to the sieving was pressurized at a pressure of 1.5 to 2 ton / cm 2 in a metal mold having a diameter of 10 mm to form a molded specimen having a thickness of 4 to 5 nm.
성형시편은 전기로를 이용하여 1300 ∼ 1500℃의 온도에서 2 ∼ 4시간 동안 소결하였다. 이때 유기물의 휘발을 위하여 600℃에서 2시간 유지하였으며 승온속도와 냉각속도는 300℃/hr로 하였다.The molded specimen was sintered for 2 to 4 hours at a temperature of 1300 ~ 1500 ℃ using an electric furnace. At this time, it was maintained for 2 hours at 600 ℃ for volatilization of the organic matter, the temperature increase rate and cooling rate was 300 ℃ / hr.
한편, 소결체의 유전율은 두장의 은판 사이에서 TEo11공진모드를 이용하는 Hakki와 Coleman의 방법으로 측정하였으며, Q값은 Kobayashi 와 Tanaka의 방법으로 측정 및 계산하였고, 공진주파수의 온도계수는 아래의 (1)식으로 계산하였으며 측정온도는 25℃에서 75℃ 범위에서 측정하였다.On the other hand, the dielectric constant of the sintered body was measured by the method of Hakki and Coleman using TE o11 resonance mode between two sheets of silver, and the Q value was measured and calculated by the method of Kobayashi and Tanaka, and the temperature coefficient of the resonance frequency was The temperature was measured in the range of 25 ℃ to 75 ℃.
상기 본 발명의 실시예 시편의 구체적인 조성과 유전특성의 측정결과는 다음의 표 1 및 표 2에 나타나있다.The measurement results of specific compositions and dielectric properties of the sample specimens of the present invention are shown in Tables 1 and 2 below.
표 1. (Zr,Sn)TiO4계 고주파 유전체의 B2O3, NiO, La2O3첨가량에 따른 고주파 유전체의 유전특성 및 공진주파수 온도계수 변화Table 1. Dielectric Characteristics and Resonant Frequency Temperature Changes of High Frequency Dielectrics with Addition of B 2 O 3 , NiO, and La 2 O 3 in (Zr, Sn) TiO 4 -based High Frequency Dielectrics
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| KR1019940018290A KR970005881B1 (en) | 1994-07-27 | 1994-07-27 | Dielectric composition for high frequencies |
| JP7108748A JP3010420B2 (en) | 1994-07-27 | 1995-05-02 | High frequency dielectric composition |
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