KR20010028177A - Compositions of High Frequency Dielectrics - Google Patents
Compositions of High Frequency Dielectrics Download PDFInfo
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- KR20010028177A KR20010028177A KR1019990040271A KR19990040271A KR20010028177A KR 20010028177 A KR20010028177 A KR 20010028177A KR 1019990040271 A KR1019990040271 A KR 1019990040271A KR 19990040271 A KR19990040271 A KR 19990040271A KR 20010028177 A KR20010028177 A KR 20010028177A
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- 239000000203 mixture Substances 0.000 title claims abstract description 24
- 239000003989 dielectric material Substances 0.000 title description 4
- 239000000919 ceramic Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000011230 binding agent Substances 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 abstract 2
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract 1
- 229910052808 lithium carbonate Inorganic materials 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 238000004891 communication Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000001354 calcination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1254—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
Description
본 발명은 높은 품질계수(Q값)와 유전율을 가지며, 또한 공진 주파수의 온도계수가 안정하고, 소결 온도가 낮은 고주파용 유전체 세라믹스 조성물에 관한 것이다.The present invention relates to a high frequency dielectric ceramic composition having a high quality factor (Q value) and a dielectric constant, a stable temperature coefficient of resonance frequency, and a low sintering temperature.
최근, 무선 전화기, 자동차 전화기 등의 이동 통신, 위성 방송, 위성 통신 등 주파수 대역이 300 ㎒ 내지 300 ㎓인 마이크로파를 이용한 통신 시스템이 현저하게 발전하고 있으며, 이러한 뉴미디어의 실용화를 위해 공진기, 대역 통과 (또는 저지) 필터, 듀플렉서 및 마이크로파 집적회로(MIC) 등에 고주파용 유전체 세라믹스의 응용이 크게 증대되고 있다.Recently, communication systems using microwaves with a frequency band of 300 MHz to 300 GHz, such as mobile communication, satellite broadcasting, and satellite communication of wireless telephones and automobile telephones, have been remarkably developed, and resonators and band pass ( Or the application of high frequency dielectric ceramics to a filter, a duplexer, a microwave integrated circuit (MIC), and the like, has been greatly increased.
이러한 고주파용 유전체가 통신 시스템에 사용되기 위해서는, (1) 유전체 내에서 마이크로파의 파장이 유전율의 1/2 제곱에 반비례하므로, 부품의 소형화를 위해서는 유전율이 높아야 하고, (2) 유전 손실은 주파수에 비례하여 증가하므로, Q값 (즉, 유전 손실의 역수)이 높아야 하며, (3) 유전체 공진기의 공진 주파수의 온도 계수가 작아야 한다 [워싱(W. Wersing)의 Electronic Ceramics (B.C.H. Steele 편저), 제67 페이지, 미합중국 뉴욕주 소재 Elsevier Sci. Pub. Co. 발행 (1991) 참조].In order to use such a high frequency dielectric in a communication system, (1) the wavelength of the microwave in the dielectric is inversely proportional to the square of the dielectric constant, so the dielectric constant must be high for the miniaturization of components, and (2) the dielectric loss is As it increases proportionally, the Q value (i.e. reciprocal of the dielectric loss) must be high, and (3) the temperature coefficient of the resonance frequency of the dielectric resonator must be small [W. Wersing's Electronic Ceramics (BCH Steele), Page 67, Elsevier Sci. Pub. Co. Publication (1991).
또한, 통신 시스템에 사용되는 고주파용 유전체는 경시 변화가 작고, 열전도율이 커야 하며, 기계적 강도가 양호하고 소결 온도가 낮아야 한다.In addition, high frequency dielectrics used in communication systems should have small changes over time, large thermal conductivity, good mechanical strength and low sintering temperature.
지금까지 개발된 유전율 30 내지 40 정도의 대표적인 유전체로는 Ba2Ti9O20계 [오브라이언(H.M.O'Bryan) 등의 J. Am. Ceram. Soc., 57[10], 제450-453 페이지 (1974) 참조]와 (Zr, Sn)TiO4계 [와키노(K.Wakino) 등의 J. Am. Ceram. Soc., 67[4] 제278-281 페이지 (1984) 참조]를 들 수 있다. 그러나, 이러한 유형의 유전체는 Q·f0값이 각각 32000과 49000 ㎓로 다소 높은 편이나, 소결 온도가 1400℃ 내외로 높아 부품 생산시 생산 단가가 높아지므로, 이를 절감하기 위해서는 소결 온도가 낮은 유전체 재료가 요구되고 있다.Representative dielectric materials having a dielectric constant of about 30 to 40 developed so far are Ba 2 Ti 9 O 20- based [HMO'Bryan et al. J. Am. Ceram. Soc., 57 [10], pages 450-453 (1974)] and (Zr, Sn) TiO 4 system [K.Wakino et al. J. Am. Ceram. Soc., 67 [4], page 278-281 (1984). However, this type of dielectric has a slightly higher Q · f 0 value of 32000 and 49000 각각, respectively, but the sintering temperature is around 1400 ° C., which leads to higher production cost during component production. Material is required.
일반적으로, 유전율이 큰 재료는 유전체 내부의 쌍극자와의 결함 등으로 인하여 유전 손실과 공진 주파수의 온도 계수가 증가하게 되는데, 고주파용 유전체는 우선적으로 공진 주파수의 온도 계수가 안정하여야 마이크로파를 이용한 통신 시스템 등에 응용이 가능하다.In general, materials with high dielectric constants increase dielectric loss and temperature coefficients of resonance frequencies due to defects with dipoles in the dielectrics. Application is possible.
따라서, 본 발명의 목적은 유전율이 30 이상이며, 유전 손실이 적고, 소결 온도가 낮으며, 공진 주파수의 온도 계수를 유효 범위 내에서 조절할 수 있는 고주파용 유전체 세라믹스 조성물을 제공하는 것이다.Accordingly, an object of the present invention is to provide a dielectric ceramic composition for high frequency, which has a dielectric constant of 30 or more, low dielectric loss, low sintering temperature, and can adjust the temperature coefficient of the resonance frequency within an effective range.
도 1은 본 발명에 따른 고주파용 유전체 세라믹스 조성물의 조성 변화에 따른 공진 주파수의 온도 계수 변화를 나타내는 그래프도.1 is a graph showing the temperature coefficient change of the resonance frequency according to the composition change of the high-frequency dielectric ceramic composition according to the present invention.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
상기 본 발명의 목적은 다음 화학식 (1)로 표시되는 조성을 갖는 고주파용 유전체 세라믹스 조성물을 제공함으로써 달성된다.The object of the present invention is achieved by providing a dielectric ceramic composition for high frequency having a composition represented by the following formula (1).
식 중, x는 0≤x≤0.5 이다.In the formula, x is 0 ≦ x ≦ 0.5.
상기 본 발명의 고주파용 유전체 세라믹스 조성물은 페로브스카이트형 고용체로서, 유전율이 약 30 내지 56이고, Qxf0(㎓)가 18600 내지 40000이다. 공진 주파수의 온도 계수(TCF)의 범위는 -21 내지 +83 ppm/℃로 조성의 변화에 따라 TCF를 0 ppm/℃로 조절할 수 있으며 따라서, 고주파용 유전체 세라믹스 부품의 재료로서 이용될 수 있다.The high frequency dielectric ceramic composition of the present invention is a perovskite solid solution, having a dielectric constant of about 30 to 56 and a Qxf 0 (kV) of 18600 to 40000. The range of the temperature coefficient TCF of the resonance frequency is -21 to +83 ppm / ° C, and the TCF can be adjusted to 0 ppm / ° C according to the composition change, and thus can be used as a material of the high frequency dielectric ceramic component.
본 발명에 따른 고주파용 유전체 세라믹스 조성물은 Ti의 양에 따라 그 특성이 변화한다. 즉, 유전율은 Ti의 함량이 증가함에 따라 30 내지 56의 범위에서 서서히 증가하는 반면, Qxf0(㎓)는 40000 내지 18600의 범위내에서 서서히 감소한다. 공진 주파수의 온도 계수는 제1도에서 보는 바와 같이 -에서 +로 점진적으로 변화된다. 특히, Ti의 함량이 0.05 mol인 부근에서는 1150℃ 에서 3시간 소결시킬 경우, 유전율이 32.3이고, Qxf0가 29800 이상이며, 공진주파수의 온도 계수가 0 ppm/℃인 우수한 마이크로파용 유전체 세라믹스를 제조할 수 있다.The characteristics of the dielectric ceramic composition for high frequency according to the present invention vary depending on the amount of Ti. That is, the dielectric constant gradually increases in the range of 30 to 56 as the Ti content increases, while Qxf 0 (㎓) gradually decreases in the range of 40000 to 18600. The temperature coefficient of the resonant frequency changes gradually from-to + as shown in FIG. Particularly, when sintered at 1150 ° C. for 3 hours in the vicinity of 0.05 mol of Ti, excellent microwave dielectric ceramics having a dielectric constant of 32.3, Qxf 0 of 29800 or more, and a temperature coefficient of resonance frequency of 0 ppm / ° C. were prepared. can do.
본 발명의 고주파용 유전체 세라믹스 조성물은, 출발 물질로서 CaCO3, Li2CO3, Nb2O5및 TiO2를 사용전에 약 600℃의 온도에서 약 10시간 정도 건조시킨 후, 이들 시료를 본 발명의 고주파용 유전체 세라믹스 조성물을 제공하는 일정 조성비로 혼합한 분말을 약 700∼900℃의 온도에서 약 2시간 동안 하소하여 분쇄한 후, 성형 첨가제(유기 바인더)로서, 예를들면 5% PVA 수용액을 첨가하여 가압 성형하고, 약 600℃의 온도에서 약 1시간 동안 열처리하여 유기 바인더를 제거한 후, 대기중에서 약 1000∼1300℃의 온도에서 약 1 내지 5시간 동안 소결시킴으로써 제조할 수 있다.In the dielectric ceramic composition for high frequency of the present invention, CaCO 3 , Li 2 CO 3 , Nb 2 O 5 and TiO 2 are dried at a temperature of about 600 ° C. for about 10 hours before use, and then these samples are subjected to the present invention. The powder mixed at a constant composition ratio to provide a high frequency dielectric ceramic composition of was calcined and pulverized at a temperature of about 700 to 900 ° C. for about 2 hours, and then, for example, a 5% PVA aqueous solution was used as a molding additive (organic binder). It can be prepared by addition and pressure molding, heat treatment at a temperature of about 600 ° C. for about 1 hour to remove the organic binder, and then sintering at about 1000 to 1300 ° C. in air for about 1 to 5 hours.
이하, 본 발명을 실시예로써 더욱 구체적으로 설명한다. 그러나, 본 발명이 이들 실시예로 한정되는 것은 아니다. 하기 실시예에서 소결 시편의 유전율, Q값 및 공진 주파수의 온도 계수 등의 유전 특성은 공지된 유전체 공진기법으로 측정하였다.Hereinafter, the present invention will be described in more detail with reference to Examples. However, the present invention is not limited to these examples. In the following examples, dielectric properties such as dielectric constant, Q value, and temperature coefficient of resonance frequency of the sintered specimen were measured by a known dielectric resonator technique.
＜실시예＞<Example>
순도 99%의 CaCO3, 99.99%의 Li2CO3와, 99.9%의 Nb2O5및 TiO2를 사용전에 약 600℃의 온도에서 약 10시간 정도 건조시킨 후, 이들 시료를 표 1에 나타낸 조성비로 혼합하고, 혼합 분말을 대기 중에서 약 850 ℃의 온도에서 약 2시간 정도 하소하여 분쇄한 후 성형 첨가제로 5% PVA 수용액을 첨가하여 직경 10 ㎜, 두께 약 5 내지 6 ㎜의 원기둥형 시편으로 가압 성형하고, 성형된 시편을 약 600℃의 온도에서 약 1시간 동안 열처리하여 유기 바인더를 제거한 후, 대기중에서 약 1150℃의 온도에서 약 1 내지 5 시간 동안 소결하였다.After purity 99% CaCO 3 , 99.99% Li 2 CO 3 and 99.9% Nb 2 O 5 and TiO 2 were dried at a temperature of about 600 ° C. for about 10 hours, these samples were shown in Table 1. The mixture is mixed at a composition ratio, and the mixed powder is calcined by calcination at about 850 ° C. in the air for about 2 hours, and then a 5% PVA aqueous solution is added as a molding additive to form a cylindrical specimen having a diameter of 10 mm and a thickness of about 5 to 6 mm. Press-molding, the molded specimen was heat treated at a temperature of about 600 ℃ for about 1 hour to remove the organic binder, and then sintered for about 1 to 5 hours at a temperature of about 1150 ℃ in the air.
소결 시편의 양면을 잘 연마한 후, 도파관 속에 넣고 유전체 공진기법으로 유전율, Q값 및 공진 주파수의 온도 계수를 측정하였다. 이때, 측정 주파수는 7.0 내지 9.8 ㎓이고, 측정 온도 범위는 -15 내지 85℃였다. 각 시편의 마이크로파 유전 특성은 하기 표 1과 같다.After both surfaces of the sintered specimen were polished well, they were placed in a waveguide and the dielectric constant, Q value, and temperature coefficient of the resonance frequency were measured by dielectric resonant technique. At this time, the measurement frequency was 7.0-9.8 Hz, and the measurement temperature range was -15-85 degreeC. Microwave dielectric properties of each specimen are shown in Table 1 below.
본 발명의 고주파용 유전체 세라믹스 조성물은 높은 품질 계수(Q값)와 유전율을 가지며, 공진주파수의 온도 계수가 안정하여 마이크로파용 통신 시스템 등에 사용될 수 있다. 또한, 본 발명의 고주파용 유전체 세라믹스 조성물은 제조시 소결 온도가 낮아 생산 단가를 낮출 수 있다.The high frequency dielectric ceramic composition of the present invention has a high quality factor (Q value) and dielectric constant, and the temperature coefficient of the resonant frequency is stable and can be used for a microwave communication system and the like. In addition, the high-frequency dielectric ceramic composition of the present invention can lower the production cost of low sintering temperature during manufacture.
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| KR100763284B1 (en) * | 2006-07-31 | 2007-10-04 | 요업기술원 | Microwave dielectric ceramics and the manufacturing method thereof |
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| KR100471932B1 (en) | 2002-05-13 | 2005-03-08 | 한국과학기술연구원 | Low Temperature Co-Firing Ceramic (LTCC) Composition for Microwave Frequency |
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|---|---|---|---|---|
| KR20040075131A (en) * | 2003-02-20 | 2004-08-27 | 필코전자주식회사 | Magnetic composition for low temperature co fired ceramics lc filter |
| KR100763284B1 (en) * | 2006-07-31 | 2007-10-04 | 요업기술원 | Microwave dielectric ceramics and the manufacturing method thereof |
| CN108863345A (en) * | 2018-07-20 | 2018-11-23 | 广东奥胜新材料有限公司 | A kind of luminescence medium ceramic material and preparation method thereof |
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