KR100234017B1 - Dielectric ceramic composition - Google Patents
Dielectric ceramic composition Download PDFInfo
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- KR100234017B1 KR100234017B1 KR1019970073470A KR19970073470A KR100234017B1 KR 100234017 B1 KR100234017 B1 KR 100234017B1 KR 1019970073470 A KR1019970073470 A KR 1019970073470A KR 19970073470 A KR19970073470 A KR 19970073470A KR 100234017 B1 KR100234017 B1 KR 100234017B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 25
- 239000000919 ceramic Substances 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 description 5
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 CaZrO 3 Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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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
- H01G4/1263—Ceramic dielectrics characterised by the ceramic dielectric material based on niobium or tungsteen, tantalum oxides or niobates, tantalates containing also zirconium oxides or zirconates
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Abstract
40 이상의 유전율을 갖고 유전 손실이 적으며 공진 주파수의 온도 계수가 양호한 마이크로파용 유전체 세라믹 조성물로서, (1-x){(1-y)CaTiO3+ yCaZrO3} + xCa(Mg1/3Nb2/3)O3(식 중, 0.5 ≤ x ≤ 0.6, 0 ≤ y ≤ 0.3)로 나타내지는 고주파용 유전체 세라믹 조성물을 제공한다. 이 조성물은 필요에 따라 CaZrO3와 Ca(Mg1/3Nb2/3)O3의 조성비를 달리하여, 유전율과 공진 주파수의 온도 계수의 조정이 용이하다.A dielectric ceramic composition for microwaves having a dielectric constant of 40 or more, low dielectric loss and good temperature coefficient of resonance frequency, wherein (1-x) {(1-y) CaTiO 3 + yCaZrO 3 } + xCa (Mg 1/3 Nb 2 / 3 ) Provides a dielectric ceramic composition for high frequency represented by O 3 (wherein 0.5 ≤ x ≤ 0.6, 0 ≤ y ≤ 0.3). This composition changes the composition ratio of CaZrO 3 and Ca (Mg 1/3 Nb 2/3 ) O 3 as needed, and it is easy to adjust the temperature coefficient of dielectric constant and resonance frequency.
Description
본 발명은 40∼55의 유전율을 가지며 유전 손실이 적고 공진 주파수의 온도 계수가 양호한 마이크로파용 유전체 세라믹의 조성물에 관한 것이다.The present invention relates to a composition of a microwave dielectric ceramic having a dielectric constant of 40 to 55, low dielectric loss, and good temperature coefficient of resonance frequency.
최근 무선 전화기, 자동차 전화기 등의 이동 통신 및 위선 방송, 위성 통신 등에 마이크로파(주파수 대역: 300 MHz부터 30 GHz)를 이용한 통신 시스템이 현저하게 발전하고 있으며, 이러한 뉴미디어의 실용화에 사용되는 공진기, 대역 통과, 저지 필터 및 마이크로파 집적 회로(MIC: Microwave Intergrate Circuit) 등에 고주파용 세라믹 유전체 응용이 크게 증가하였다.Recently, communication systems using microwaves (frequency band: 300 MHz to 30 GHz) for mobile communication, hypocrisy broadcasting, satellite communication of wireless telephones, automobile telephones, etc. have been remarkably developed. Applications of ceramic dielectrics for high frequency applications have increased significantly, for example, stop filters and microwave integrated circuits (MICs).
이러한 고주파용 세라믹 유전체가 통신 시스템에 사용되기 위해서는, 유전체 내에서 전파의 파장은 유전율의 1/2승에 반비례하므로 부품의 소형화를 위해서는 유전율이 커야하고, 유전손실은 유전율에 비례하여 증가하게 되므로 고주파의 고성능화를 위해서는 Q값(유전손실의 역수)이 높아야 한다. 즉, 유전 손실이 작아야 한다. 또한 유전체의 공진주파수의 온도 계수가 작아야 하며 열전도율이 좋고 높은 기계적 강도가 요구된다.In order for the high frequency ceramic dielectric to be used in a communication system, the wavelength of the radio wave in the dielectric is inversely proportional to the power of 1/2 of the dielectric constant. Therefore, the dielectric constant must be large for the miniaturization of components, and the dielectric loss is increased in proportion to the dielectric constant. For high performance, the Q value (inverse of the dielectric loss) must be high. That is, the dielectric loss should be small. In addition, the temperature coefficient of the resonance frequency of the dielectric should be small, and the thermal conductivity is good and high mechanical strength is required.
기존에 개발된 유전체 조성물로는, 유전율은 40 이하이지만 낮은 유전 손실을 갖는 Ba(M2+ 1/3M5+ 2/3)O3(M2+= Mg, Zn, M5+= Ta, Nb)계, BaTi4O9와 Ba2Ti9O20계, (Zr,Sn)TiO4계 등이 있다. 또한 유전 손실은 비교적 크지만(Q×f0≤ 10000), 유전율이 80 이상인 BaO-Sm2O3-TiO2계, (Ba,Pb)O-Nd2O3-TiO2계 및 (Pb,Ca)ZrO3계 등이 보고되어 있다.Existing dielectric compositions have Ba (M 2+ 1/3 M 5+ 2/3 ) O 3 (M 2+ = Mg, Zn, M 5+ = Ta) with a dielectric constant of 40 or less but low dielectric loss. , Nb) system, BaTi 4 O 9 and Ba 2 Ti 9 O 20 system, and (Zr, Sn) TiO 4 system. In addition, although the dielectric loss is relatively large (Q × f 0 ≦ 10000), the BaO—Sm 2 O 3 —TiO 2 system, (Ba, Pb) O—Nd 2 O 3 —TiO 2 system, and (Pb, Ca) ZrO 3 system and the like have been reported.
일반적으로, 유전율이 큰 재료는 유전체 내부의 쌍극자와 결함 등으로 인하여 유전 손실과 공진 주파수의 온도 계수가 증가하게 된다.In general, a material having a high dielectric constant increases the temperature coefficient of dielectric loss and resonance frequency due to dipoles and defects in the dielectric.
CaTiO3의 경우, 2 GHz에서 유전율이 170 정도로 매우 높으나 공진 주파수의 온도 계수가 +800 ppm/℃로 매우 커서 실제 응용에는 문제점이 있다. 따라서 본 발명에서는 CaTiO3에 온도 계수가 음인 Ca(Mg1/3Nb2/3)O3와 CaZrO3를 고용시켜 유전 손실이 작고, 유전율과 공진 주파수의 온도 계수를 필요에 따라 쉽게 조절할 수 있는 새로운 마이크로파용 유전체 세라믹 조성물을 제공하고자 한다.In the case of CaTiO 3 , the dielectric constant is very high at 170 GHz at 2 GHz, but the temperature coefficient of the resonance frequency is very high at +800 ppm / ° C., which causes problems in practical applications. Therefore, in the present invention, by the temperature coefficient of the CaTiO 3 employs the O 3 and CaZrO 3 negative, Ca (Mg 1/3 Nb 2/3) dielectric loss is small, which easily can be adjusted as needed, the temperature coefficient of the dielectric constant and the resonant frequency The present invention seeks to provide a dielectric ceramic composition for microwaves.
도 1은 본 발명에 의한 유전체 재료의 조성 범위를 보여주는 조성 상태도이고,1 is a composition state diagram showing a composition range of a dielectric material according to the present invention,
도 2는 본 발명에 의한 유전체 공진기의 조성 변화에 따른 유전 특성을 나타낸 것이고,Figure 2 shows the dielectric properties according to the composition change of the dielectric resonator according to the present invention,
도 3은 본 발명에 의한 유전체 공진기의 조성 변화에 따른 공진 주파수의 온도 계수 특성을 나타낸 것이다.Figure 3 shows the temperature coefficient characteristics of the resonance frequency according to the composition change of the dielectric resonator according to the present invention.
본 발명은 다음 화학식 1을 갖는 조성물을 제조하여, 40∼55의 유전율을 가지며 유전 손실이 작고 공진 주파수의 온도 계수가 양호한 마이크로파용 유전체 세라믹의 조성물을 제공한다.The present invention provides a composition of the dielectric ceramic for microwave having a dielectric constant of 40 to 55, a low dielectric loss, and a good temperature coefficient of resonance frequency.
(식 중, 0.5≤ x ≤ 0.6, 0 ≤ y ≤ 0.3)(Wherein 0.5 ≦ x ≦ 0.6, 0 ≦ y ≦ 0.3)
본 발명의 유전체 세라믹 조성물의 특성은 CaZrO3와 Ca(Mg1/3Nb2/3)O3의 조성비에 따라 달라진다. 다음 표 1에 나타낸 바와 같이 상기 화학식 1에서의 x 값과 y 값이 증가하여 CaZrO3와 Ca(Mg1/3Nb2/3)O3의 함량이 증가함에 따라 유전율은 55에서 40으로 감소하는 경향을 보이며 공진 주파수의 온도 계수는 +에서 -로 변화됨을 볼 수 있다. 따라서, (1-x){(1-y)CaTiO3+ yCaZrO3} + xCa(Mg1/3Nb2/3)O3계에서 x값과 y값을 조절함으로써 유전 손실이 작고 유전율이 40∼52, 온도 계수가 ±10 ppm/℃ 이내로 뛰어난 특성을 갖는 마이크로파용 유전체 세라믹 조성물을 제조할 수 있다.The properties of the dielectric ceramic composition of the present invention depend on the composition ratio of CaZrO 3 and Ca (Mg 1/3 Nb 2/3 ) O 3 . As shown in Table 1, the dielectric constant decreases from 55 to 40 as the content of CaZrO 3 and Ca (Mg 1/3 Nb 2/3 ) O 3 is increased by increasing x and y values in Chemical Formula 1. It can be seen that the temperature coefficient of the resonant frequency changes from + to-. Therefore, in the (1-x) {(1-y) CaTiO 3 + yCaZrO 3 } + xCa (Mg 1/3 Nb 2/3 ) O 3 system, the dielectric constant is small and the dielectric constant is 40 by adjusting the x and y values. The dielectric ceramic composition for microwaves which has the outstanding characteristic to -52 and a temperature coefficient within +/- 10 ppm / degreeC can be manufactured.
상기 화학식 1을 갖는 본 발명의 조성물의 제조 방법 및 그 특성의 검측 방법은 다음 실시예를 통해 상세히 설명하고자 한다. 하지만, 본 발명을 이에 한정시키고자 하는 것은 아니다.Method for producing a composition of the present invention having the formula (1) and the detection method of its properties will be described in detail through the following examples. However, the present invention is not intended to be limited thereto.
실시예Example
고순도 화학 연구소의 CaCO3(99.9%), TiO2(99.9%), MgO(99.9%), Nb2O5(99.9%), ZrO2(CSZ)를 CaTiO3와 CaZrO3, Ca(Mg1/3Nb2/3)O3각각의 조성비에 따라 칭량한 후에, 알코올과 지르코니아볼을 매체로 하여 12 시간 동안 습식 혼합하여 건조시킨 후, 1100 ℃에서 3 시간 동안 하소하여 CaTiO3분말과 CaZrO3, Ca(Mg1/3Nb2/3)O3분말을 제조하였다.Of high purity chemical laboratory CaCO 3 (99.9%), TiO 2 (99.9%), an MgO (99.9%), Nb 2 O 5 (99.9%), ZrO 2 (CSZ) CaTiO 3 and CaZrO 3, Ca (Mg 1 / After weighing according to the composition ratio of 3 Nb 2/3 ) O 3 , the mixture was wet mixed for 12 hours with alcohol and zirconia ball as a medium, and then calcined at 1100 ° C. for 3 hours, thereby CaTiO 3 powder, CaZrO 3 , Ca (Mg 1/3 Nb 2/3 ) O 3 powder was prepared.
하소된 이 CaTiO3분말과 CaZrO3, Ca(Mg1/3Nb2/3)O3분말을 다음 표 1에서와 같은 x, y 값을 갖는 조성비로 칭량하여, 20 시간 동안 습식 혼합 및 분쇄하였으며, 분쇄 완료 30 분 전에 바인더로서 5% PVA 수용액을 8 중량%로 첨가하였다. 분쇄된 분말을 건조시켜 체거름한 후에 직경이 15 mm인 금속제 주형에서 1 ton/cm의 압력으로 가압하여 두께가 6 mm 정도인 시편을 성형하였다. 성형된 시편은 박스형 전기로를 이용하여 1550∼1650 ℃의 온도에서 소결하였다. 이때, 유기 성분을 제거하기 위해 650 ℃에서 1 시간 동안 유지하였으며 승온 속도 및 냉각 속도는 300 ℃/hr이였다.The calcined CaTiO 3 powder and CaZrO 3 , Ca (Mg 1/3 Nb 2/3 ) O 3 powder were weighed at a composition ratio having x and y values as shown in Table 1, followed by wet mixing and grinding for 20 hours. 5% PVA aqueous solution was added as a
유전율은 두 장의 은판 사이에서 TE11공진 모드를 이용한 Hakki-Coleman 방법으로 측정하였으며, 같은 지름을 갖고 높이가 3 배인 유전체 2 개를 만들어 TE11과 TE013그리고 은판의 표면 저항을 측정하여 Q 값을 계산하였다. 또한, 25 ℃와 65 ℃에서의 공진 주파수 변화를 측정하여 공진 주파수의 온도 계수를 구하였다. 각 조성별 시편의 마이크로파 유전 특성은 다음 표 1에 나타낸 바와 같다.The dielectric constant was measured by the Hakki-Coleman method using the TE 11 resonance mode between two sheets of silver. Two Q dielectrics of the same diameter and three times the height were made to measure the surface resistances of TE 11 , TE 013 and the silver plate. Calculated. In addition, the temperature coefficient of the resonant frequency was determined by measuring the change in the resonant frequency at 25 ° C and 65 ° C. Microwave dielectric properties of the specimens for each composition are shown in Table 1 below.
상기 표 1의 결과를 통해 알 수 있는 바와 같이, CaZrO3와 Ca(Mg1/3Nb2/3)O3을 CaTiO3에 고용시킴으로써, 40 이상의 유전율을 갖고 유전 손실이 작으며 공진 주파수의 온도 계수가 안정한 마이크로파용 유전체 세라믹 조성물을 제조할 수 있으며, 경우에 따라 이 조성비를 달리하여 이 조성물의 유전율과 공진 주파수의 온도 계수를 조절할 수도 있다.As can be seen from the results of Table 1, CaZrO 3 and Ca (Mg 1/3 Nb 2/3 ) O 3 are dissolved in CaTiO 3 to have a dielectric constant of 40 or more, the dielectric loss is small, and the temperature of the resonance frequency. It is possible to produce a dielectric ceramic composition for microwaves with stable coefficients, and in some cases, by changing the composition ratio, it is also possible to adjust the temperature coefficient of the dielectric constant and resonance frequency of the composition.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100349006B1 (en) * | 2000-06-22 | 2002-08-17 | 주식회사 어드밴택 | A dielectric material for microwave |
| CN106747415A (en) * | 2017-03-03 | 2017-05-31 | 华东理工大学 | A kind of preparation of low-dielectric loss calcium titanate ceramics |
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| CN114075070A (en) * | 2020-08-13 | 2022-02-22 | 华为技术有限公司 | Complex-phase microwave ceramic material, manufacturing method thereof and electronic device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100349006B1 (en) * | 2000-06-22 | 2002-08-17 | 주식회사 어드밴택 | A dielectric material for microwave |
| CN106747415A (en) * | 2017-03-03 | 2017-05-31 | 华东理工大学 | A kind of preparation of low-dielectric loss calcium titanate ceramics |
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