KR100362881B1 - Dielectric composition and the manufacturing method - Google Patents
Dielectric composition and the manufacturing method Download PDFInfo
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- KR100362881B1 KR100362881B1 KR1019990046040A KR19990046040A KR100362881B1 KR 100362881 B1 KR100362881 B1 KR 100362881B1 KR 1019990046040 A KR1019990046040 A KR 1019990046040A KR 19990046040 A KR19990046040 A KR 19990046040A KR 100362881 B1 KR100362881 B1 KR 100362881B1
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Abstract
본 발명은 고주파수 대역에서 사용되는 유전체 조성물 및 그 제조방법에 관한 것으로서,The present invention relates to a dielectric composition used in the high frequency band and a method of manufacturing the same,
탄산바륨(BaCO3) 19.85∼22.02 중량％, 산화네오븀(Nb2O3) 36.60∼39.32 중량％, 산화티탄(TiO2) 36.73∼37.56 중량％, 산화납(PbO) 2.27∼5.34 중량％을 기본조성물으로 하고; 산화망간(MnO2) 0.05∼0.10 중량％, 이산화규소(SiO2) 0.10∼0.20 중량％을 첨가함으로써 유전율이 90 이상이 되며 1300℃ 정도의 온도에서 소결 가능하고, 품질 계수가 6000이상, 공진주파수의 온도 계수가 0±10 PPM/℃ 이하 특성을 갖는 것으로 고주파용에 적합함은 물론이고 부품의 소형화를 실현시킬 수 있는 효과를 제공하게 된다.19.85 to 22.02% by weight of barium carbonate (BaCO 3 ), 36.60 to 39.32% by weight of nebium oxide (Nb 2 O 3 ), 36.73 to 37.56% by weight of titanium oxide (TiO 2 ), and 2.27 to 5.34% by weight of lead oxide (PbO) As a basic composition; By adding 0.05 to 0.10% by weight of manganese oxide (MnO 2 ) and 0.10 to 0.20% by weight of silicon dioxide (SiO 2 ), the dielectric constant becomes 90 or more and can be sintered at a temperature of about 1300 ° C., the quality factor is 6000 or more, and the resonance frequency Since the temperature coefficient of is 0 ± 10 PPM / ℃ or less, it is suitable for high frequency and provides the effect of realizing miniaturization of components.
Description
본 발명은 고주파수 대역에서 사용되는 유전체 조성물 및 그 제조방법에 관한 것으로서, 특히 유전 상수가 90 이상, 공진주파수의 온도 계수가 0±10 PPM/℃ 이하인 유전체 조성물 및 그 제조방법에 관한 것이다.TECHNICAL FIELD The present invention relates to a dielectric composition used in a high frequency band and a method of manufacturing the same, and more particularly, to a dielectric composition having a dielectric constant of 90 or more and a temperature coefficient of resonant frequency of 0 ± 10 PPM / ° C. or less and a method of manufacturing the same.
여기서, 유전체 조성물은 WLL(Wireless Local Loop), GPS(Global Positioning System), FLMTS(Future Land Mobile Telecommunication System), PCS(Personal Communication Service)의 마이크로파 대역 서비스 단말기 및 기지국 등의 시스템에 사용되는 부품인 듀플렉서 필터(Duplexer Filter), 대역통과 필터(Band pass Filter), 적층 LC 필터(Multi-layer LC Filter) 등의 소재로 사용되거나, 전압 제어 발진소자(VCO) 등의 능동소자 및 초고주파용 커패시터, 마이크로파 집적회로(MIC)의 소재로 사용되게 된다.Here, the dielectric composition is a duplexer that is a component used in systems such as a wireless local loop (WLL), a global positioning system (GPS), a furniture land mobile telecommunication system (FLMTS), a microwave band service terminal and a base station of a personal communication service (PCS). Used as materials such as Duplexer Filter, Band pass Filter, Multi-layer LC Filter, Active element such as Voltage Controlled Oscillator (VCO), Microwave Capacitor, Microwave Integrated It is used as the material of the circuit MIC.
종래 기술에 의한 유전체 조성물은 유전 상수가 80∼90 정도로 유전 손실의 역수인 품질계수(Quality factor, Q) 값이 5000 정도인 BaO-PbO-Nd2O3-TiO2계, BaO-PbO-Sm2O3-TiO2계가 주로 사용되고 있다.The dielectric composition according to the prior art has a BaO-PbO-Nd 2 O 3 -TiO 2 type , BaO-PbO-Sm having a quality factor (Q) value of 5000, which is an inverse of the dielectric loss, with a dielectric constant of 80 to 90. 2 O 3 -TiO 2 type is mainly used.
상기와 같은 조성물은 사용 온도 범위에서 안정된 공진주파수의 온도계수를 갖는 반면에 1350℃ 이상의 높은 소결 온도를 갖고, 공진주파수의 온도계수 및 소결 온도를 저하시키기 위해 사용되는 산화납(PbO)이 다량 함유되어 있다.Such a composition has a high temperature coefficient of sintering temperature of 1350 ° C. or higher while having a stable temperature coefficient of resonant frequency in the use temperature range, and contains a large amount of lead oxide (PbO) used to lower the temperature coefficient and sintering temperature of the resonance frequency. It is.
따라서, 종래의 유전체 조성물은 높은 소결 온도를 갖으며, 산화납의 다량 함유로 인해 소결 과정 중 휘발, 내화물 침식, 재현성 확보 곤란과 같은 문제점이 발생하게 된다.Therefore, the conventional dielectric composition has a high sintering temperature, and a large amount of lead oxide causes problems such as volatilization, refractory erosion, and difficulty in securing reproducibility during the sintering process.
본 발명은 상기한 종래 기술의 문제점을 해결하기 위하여 안출된 것으로서, 그 목적은 유전율이 90이상이되며 1300℃ 정도의 온도에서 소결 가능하고, 품질 계수가 6000이상, 공진주파수의 온도 계수가 0±10 PPM/℃ 이하 특성을 갖는 고주파용에 적합함은 물론이고 부품의 소형화를 실현시킬 수 있는 유전체 조성물 및 그 제조방법을 제공하는데 있다.The present invention has been made to solve the above problems of the prior art, the object of which is the dielectric constant of 90 or more and sinterable at a temperature of about 1300 ℃, the quality coefficient of 6000 or more, the temperature coefficient of the resonance frequency is 0 ± 10 The present invention provides a dielectric composition and a method for manufacturing the same, which are suitable for high frequency having a characteristic of PPM / ° C. or lower and can realize miniaturization of components.
상기한 과제를 해결하기 위한 본 발명에 의한 유전체 조성물의 제1 특징에 따르면, 탄산바륨(BaCO3) 19.85∼22.02 중량％, 산화네오븀(Nb2O3) 36.60∼39.32 중량％, 산화티탄(TiO2) 36.73∼37.56 중량％, 산화납(PbO) 2.27∼5.34 중량％을 기본조성물로 전체 중량의 합이 100이 되도록 탄산바륨(BaCO3)의 중량 조정이 가능하다.According to the first aspect of the dielectric composition according to the present invention for solving the above problems, 19.85 to 22.02 wt% of barium carbonate (BaCO 3 ), 36.60 to 39.32 wt% of neobium oxide (Nb 2 O 3 ), titanium oxide ( It is possible to adjust the weight of barium carbonate (BaCO 3 ) so that the total of the total weight of the base composition is 36.73 to 37.56% by weight of TiO 2 ) and 2.27 to 5.34% by weight of lead oxide (PbO).
또한, 본 발명의 제2 특징에 따르면, 탄산바륨(BaCO3) 19.85∼22.02 중량％, 산화네오븀(Nb2O3) 36.60∼39.32 중량％, 산화티탄(TiO2) 36.73∼37.56 중량％, 산화납(PbO) 2.27∼5.34 중량％을 기본 조성물로 하고; 산화망간(MnO2) 0.05∼0.10 중량％, 이산화규소(SiO2) 0.10∼0.20 중량％을 첨가한다.Further, according to the second aspect of the present invention, 19.85 to 22.02 wt% of barium carbonate (BaCO 3 ), 36.60 to 39.32 wt% of neobium oxide (Nb 2 O 3 ), 36.73 to 37.56 wt% of titanium oxide (TiO 2 ), 2.27 to 5.34 wt% of lead oxide (PbO) is used as the base composition; Manganese oxide (MnO 2 ) 0.05 to 0.10 wt% and silicon dioxide (SiO 2 ) 0.10 to 0.20 wt% are added.
본 발명의 유전체의 조성물의 제조방법의 특징에 따르면, 탄산바륨(BaCO3), 산화네오븀(Nb2O3), 산화티탄(TiO2), 산화납(PbO)을 기본 조성물로 하고, 산화망간(MnO2), 이산화규소(SiO2) 중에서 적어도 하나 이상을 첨가하여 각각을 일정 중량비로 칭량하는 제1 과정과;According to a feature of the method for producing a composition of the dielectric of the present invention, barium carbonate (BaCO 3 ), neodymium oxide (Nb 2 O 3 ), titanium oxide (TiO 2 ), and lead oxide (PbO) are used as base compositions and are oxidized. A first step of adding at least one of manganese (MnO 2 ) and silicon dioxide (SiO 2 ) to weigh each of them at a predetermined weight ratio;
상기 제1 과정의 결과물을 지르코니아(ZrO2) 볼과 물을 매개체로 하여 15∼24시간 동안 교반 건조한 후에 1100∼1150℃에서 2∼3시간 동안 하소시키는 제2 과정과;A second step of drying the resultant of the first step for 15 to 24 hours using a zirconia (ZrO 2 ) ball and water as a medium, and then calcining at 1100 to 1150 ° C. for 2 to 3 hours;
상기 제2 과정을 통해 형성된 분말을 100∼200 메시(mesh)로 체거름한 다음 지름 10㎜ 정도가 되도록 가압 성형한 후에 1300∼1330℃에서 3시간 정도 소결함으로써 유전체 조성물을 완료하는 제3 과정을 포함한다.The third step of completing the dielectric composition by sieving the powder formed through the second process to 100 ~ 200 mesh (mesh) and press-molded to a diameter of about 10mm and then sintering at 1300 ~ 1330 ℃ for about 3 hours Include.
이하, 본 발명의 유전체 조성물 및 그 제조방법에 대한 바람직한 실시예를 상세히 설명한다.Hereinafter, preferred embodiments of the dielectric composition of the present invention and a method of manufacturing the same will be described in detail.
본 발명에서는 탄산바륨(BaCO3) 19.85∼22.02 중량％, 산화네오븀(Nb2O3) 36.60∼39.32 중량％, 산화티탄(TiO2) 36.73∼37.56 중량％, 산화납(PbO) 2.27∼5.34 중량％을 기본 조성물로 하고; 산화망간(MnO2) 0.05∼0.10 중량％, 이산화규소(SiO2) 0.10∼0.20 중량％을 첨가하게 된다.In the present invention, 19.85 to 22.02 wt% of barium carbonate (BaCO 3 ), 36.60 to 39.32 wt% of nebium oxide (Nb 2 O 3 ), 36.73 to 37.56 wt% of titanium oxide (TiO 2 ), and 2.27 to 5.34 lead oxide (PbO) Weight percent as the base composition; Manganese oxide (MnO 2 ) 0.05 to 0.10 wt%, silicon dioxide (SiO 2 ) 0.10 to 0.20 wt% is added.
이때, 상기 이산화규소(SiO2)를 제외한 탄산바륨(BaCO3), 산화네오븀(Nb2O3), 산화티탄(TiO2), 산화납(PbO), 산화망간(MnO2)만으로 유전체 조성물을 구성할 수 있는데, 이렇게 형성된 유전체 조성물은 유전율이 80∼90, 온도 계수가 0±10 PPM/℃ 로 소형화가 크게 중요하지 않는 부품에 적용될 수 있다.At this time, the dielectric composition with only barium carbonate (BaCO 3 ), neodymium oxide (Nb 2 O 3 ), titanium oxide (TiO 2 ), lead oxide (PbO), manganese oxide (MnO 2 ) excluding the silicon dioxide (SiO 2 ). The dielectric composition thus formed may be applied to a component having a dielectric constant of 80 to 90 and a temperature coefficient of 0 ± 10 PPM / ° C. in which miniaturization is not important.
상기한 구성 물질은 원료 평량, 조합, 밀링(Mixing, Milling), 건조, 분쇄, 하소, 분쇄의 제조 공정에 따라 제조되게 됨으로써 그 유전체 조성이 마이크로파 유전 특성이 우수하며, 각종 부품에 적용되어 신뢰성이 향상될 수 있다.The above constituent materials are manufactured according to the raw material basis weight, combination, milling, milling, drying, milling, calcination, milling process, so that the dielectric composition is excellent in the microwave dielectric properties, and applied to various components, and reliable Can be improved.
아래 표 1을 참조하여 본 발명에 의한 유전체 조성물의 제조방법을 더욱 상세히 살펴보면 다음과 같다.Referring to Table 1 below in more detail look at the method for producing a dielectric composition according to the present invention.
먼저, 제1 단계에서는 유전체 조성물을 제조하기 위한 탄산바륨(BaCO3), 산화네오븀(Nb2O3), 산화티탄(TiO2), 산화납(PbO), 산화망간(MnO2), 이산화규소(SiO2)를 표 1에 나타낸 실시예에서와 같은 중량비에 따라 칭량하게 된다.First, in the first step, barium carbonate (BaCO 3 ), neodymium oxide (Nb 2 O 3 ), titanium oxide (TiO 2 ), lead oxide (PbO), manganese oxide (MnO 2 ), and manganese dioxide to prepare a dielectric composition Silicon (SiO 2 ) is weighed according to the weight ratio as in the example shown in Table 1.
그 후, 제2 단계에선,S 상기 제1 단계의 결과물을 지르코니아(ZrO2) 볼과 물을 매개체로 하여 15∼24 시간 동안 교반 건조시키게 된다.After that, in the second step, the resultant of the first step S is dried by stirring for 15 to 24 hours using a zirconia (ZrO 2 ) ball and water as a medium.
제3 단계에서는 상기 제2 단계에서 건조된 조성물을 1100∼1150℃에서 2∼3 시간 동안 하소시킨다. 이렇게 형성된 분말을 제4 단계에서는 100∼200 메시로 체거름한 다음 지름 10㎜가 되도록 가압 성형하게 된다.In the third step, the composition dried in the second step is calcined for 2 to 3 hours at 1100 ~ 1150 ℃. The powder thus formed is sieved to 100 to 200 mesh and then press-molded to have a diameter of 10 mm.
마지막으로, 제5 단계에서는 상기 제4 단계에서 성형된 조성물을 1300∼1330℃에서 3시간 소결한 후 유전체의 TE 모드 특성인 유전율(K), 품질 계수(Q), 온도 계수(TCF) 값 측정과 미세 구조등의 재료 특성 분석을 수행하게 된다.Lastly, in the fifth step, the composition molded in the fourth step is sintered at 1300 to 1330 ° C. for 3 hours, and the dielectric constant (K), quality factor (Q) and temperature coefficient (TCF) values, which are the TE mode characteristics of the dielectric, are measured. Material characterization such as and microstructure is performed.
이때, TE 모드는 도파관에서 특정한 전기적 횡파가 전파하는 모드를 의미한다.In this case, the TE mode refers to a mode in which a specific electric shear wave propagates in the waveguide.
상기와 같은 유전체 조성물의 제조방법은 1100∼1150℃의 조건에서 하소 공정을 수행하고, 하소 공정을 구행한 후 별도의 밀링 공정이 필요 없이 1300∼1330℃의 소성조건으로 유전체 조성물의 제조가 가능해지게 된다.In the method of preparing the dielectric composition as described above, the calcination process is performed under the conditions of 1100 to 1150 ° C, and after the calcination process is performed, the dielectric composition can be manufactured under the firing conditions of 1300 to 1330 ° C without the need for a separate milling process. do.
상기와 같이 구성되는 본 발명의 유전체 조성물 및 그 제조방법은 유전율이 90이상이되며 1300℃ 정도의 온도에서 소결 가능하고, 품질 계수가 6000이상, 공진주파수의 온도 계수가 0±10 PPM/℃ 이하 특성을 갖는 고주파용에 적합함은 물론이고 부품의 소형화를 실현시킬 수 있는 효과가 있다.Dielectric composition of the present invention and the manufacturing method of the present invention is configured as described above has a dielectric constant of 90 or more and can be sintered at a temperature of about 1300 ℃, quality coefficient of 6000 or more, the temperature coefficient of the resonance frequency is 0 ± 10 PPM / ℃ or less It is suitable for high frequency having a high efficiency and has the effect of realizing miniaturization of components.
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