KR100415981B1 - Ceramic Compositions of High Frequency Dielectrics Sintered at Low Temperature - Google Patents
Ceramic Compositions of High Frequency Dielectrics Sintered at Low Temperature Download PDFInfo
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- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 239000000919 ceramic Substances 0.000 title claims abstract description 10
- 239000003989 dielectric material Substances 0.000 title description 4
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 abstract description 4
- 239000010936 titanium Substances 0.000 description 7
- 239000000306 component Substances 0.000 description 6
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- 239000000654 additive Substances 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- 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
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
본 발명은 비화학양론적 조성을 갖는 일반식 Ca[(Li1/3Nb2/3)1-xTix]O3-δ으로 표시되고, 여기서 Ti의 몰분율 x는 0.5 이하인 것을 특징으로 하는 고주파용 유전체 세라믹 조성물을 제공한다.The present invention is represented by general formula Ca [(Li 1/3 Nb 2/3 ) 1-x Ti x ] O 3-δ with a non-stoichiometric composition, wherein the mole fraction x of Ti is 0.5 or less. It provides a dielectric ceramic composition for.
이 조성물은 유전율이 29.7 내지 35.2 이고, Qxfo(GHz)가 12,000 내지 26,000 이며, 공진 주파수의 온도 계수(τf)의 범위가 -16.8 내지 0 ppm/℃로서 조성의 변화에 따라 τf를 0 ppm/℃로 조절이 가능하다. 또한 소결온도가 1000℃ 이하로 고주파용 유전체 세라믹스 부품의 재료로서 사용될 수 있는 우수한 특성을 갖는 고주파 유전체 조성물이다.This composition is the dielectric constant 29.7 to 35.2, Qxf o (GHz) and the 12,000 to 26,000, temperature coefficients of resonant frequency (τ f) for f τ 0 according to the change of the composition range is as -16.8 to 0 ppm / ℃ of Adjustable at ppm / ° C. Moreover, it is a high frequency dielectric composition which has the outstanding characteristic which can be used as a material of high frequency dielectric ceramic components with sintering temperature below 1000 degreeC.
Description
본 발명은 높은 품질계수(Q값)와 유전율을 가지며 또한 공진 주파수의 온도계수가 우수하고 1000℃ 이하의 저온에서 소결가능한 고주파용 유전체 세라믹 조성물에 관한 것이다.The present invention relates to a dielectric ceramic composition for high frequency, which has a high quality factor (Q value) and dielectric constant, and is excellent in temperature coefficient of resonance frequency and sinterable at low temperature of 1000 ° C or lower.
최근, 무선 전화기, 자동차 전화기 등의 이동 통신, 위성 방송, 위성 통신 등에 주파수 대역이 300 MHz 내지 300 GHz인 마이크로파를 이용한 통신 시스템이 현저하게 발전하고 있으며, 개인 휴대 통신의 발달과 더불어 단말기의 소형화가 보편화됨에 따라 이에 사용되는 부품의 소형, 고 경량화, 표면 실장화가 가능한 적층형 부품의 요구가 증가되고 있다. 특히 통신용 기기의 핵심 부품인 필터, 듀플렉서, 공진기, 안테나 등의 수동소자는 소형화가 곤란했던 부품이었으나, 저온 소결 소재를 이용한 후막 적층 칩 소자들이 가능하게 되었다.In recent years, communication systems using microwaves having a frequency band of 300 MHz to 300 GHz for mobile communication, satellite broadcasting, and satellite communication of wireless telephones, automobile telephones, etc. have been remarkably developed. BACKGROUND OF THE INVENTION [0002] As the universalization of the components increases, there is an increasing demand for laminated components that can be miniaturized, lightweight, and surface mounted. In particular, passive components such as filters, duplexers, resonators, and antennas, which are core components of communication devices, were difficult to miniaturize, but thick-film laminated chip devices using low-temperature sintered materials became possible.
유전체 내에서 마이크로파의 파장은 유전율의 1/2 승과 주파수에 반비례하므로 부품의 소형화를 위해서는 유전율과 사용 주파수가 커야 한다. 일반적으로 유전율(εr)과 품질계수(Q) 값은 반비례 관계에 있으며 부품의 소형화를 위해서는 큰 유전율을 갖는 유전체 소재가 요구되나 앞에서 언급되었듯이 사용주파수가 1∼2 GHz 이상으로 커짐에 따라 부품의 크기가 충분히 작아져, 현재 유전율 20∼40 영역의 소재가 이용되고 있으며 각종 칩 안테나, 칩 필터 등에 활발히 이용되어지고 있다.Since the wavelength of microwaves in the dielectric is inversely proportional to the half power of the permittivity and the frequency, the permittivity and frequency of use must be large for the miniaturization of components. In general, the dielectric constant (ε r ) and the quality factor (Q) are inversely related, and miniaturization of the component requires a dielectric material having a large dielectric constant, but as mentioned above, as the frequency of use increases from 1 to 2 GHz or higher, The size of P is sufficiently small, and materials in the dielectric constant region of 20 to 40 are currently used, and are actively used in various chip antennas and chip filters.
지금까지 개발된 대표적인 저온소결용 고주파 유전체로는, CuO와 V2O5가 포함된 BiNbO4계를 들 수 있는데, 이러한 유형의 유전체는 Q·f0값이 18300 GHz 이며 유전율이 43 그리고 공진주파수의 온도계수(TCF, τf)가 +38 ppm/℃로써 이 조성의 소결온도는 875℃로 낮으나 공진주파수의 온도계수가 매우 높아 실제 부품으로의 적용이 불가능하여 BiNbO4계에 여러 첨가제를 넣어 공진주파수의 온도계수를 안정화시키는 연구가 현재 활발히 진행 중이다. [H. Kagata, Jpn. J. Appl. Phys., 31, p.3152 (1992)].Representative low-temperature sintering high frequency dielectrics developed so far include the BiNbO 4 system containing CuO and V 2 O 5 , which have a Q · f 0 of 18300 GHz with a dielectric constant of 43 and a resonant frequency. the temperature coefficient (TCF, τ f) is the sintering temperature of the composition is put in a multiple resonance-based additives to BiNbO 4 to low, but the number of the temperature coefficient of resonant frequency is very high can not be applied to the real part by 875 ℃ as +38 ppm / ℃ Research into stabilizing the temperature coefficient of the frequency is currently active. [H. Kagata, Jpn. J. Appl. Phys., 31, p. 3152 (1992).
또한, BiNbO4계를 적층소결시 전극과 비스무스(Bi)의 반응으로 인한 특성저하에 관한 보고가 있어 Bi를 포함하지 않은 저온소결 유전체 소재에 대한 요구가 대두되고 있다.In addition, there has been a report on the deterioration of the characteristics due to the reaction between the electrode and bismuth (Bi) when laminating the BiNbO 4 system, there is a need for a low-temperature sintered dielectric material containing no Bi.
따라서, 본 발명은 상기한 종래 기술의 문제점을 제거하기 위하여 안출된 것으로, 본 발명의 목적은 유전율과 품질계수값이 크고 공진 주파수의 온도 계수를 조절할 수 있으며 1000℃ 이하의 저온소결이 가능한 고주파용 유전체 조성물을 제공하고자 것이다.Accordingly, the present invention has been made to eliminate the above problems of the prior art, the object of the present invention is to control the temperature coefficient of the dielectric constant and quality coefficient and the resonant frequency is high frequency for high temperature sintering less than 1000 ℃ It is intended to provide a dielectric composition.
이와 같은 목적을 달성하기 위하여, 본 발명에 따르면, 비화학양론적 조성을 갖는 일반식 Ca[(Li1/3Nb2/3)1-xTix]O3-δ으로 표시되고, 여기서 Ti의 몰분율 x는 0.5 이하인 것을 특징으로 하는 고주파용 유전체 세라믹 조성물이 제공된다.In order to achieve this object, according to the present invention, it is represented by general formula Ca [(Li 1/3 Nb 2/3 ) 1-x Ti x ] O 3-δ having a nonstoichiometric composition, wherein A high frequency dielectric ceramic composition is provided, wherein the mole fraction x is 0.5 or less.
상기 본 발명에서 티타늄(Ti)의 몰분율 x가 지나치게 크면 공진주파수 온도계수가 지나치게 큰 양의 값을 가지므로 바람지하지 않고, 후술하는 B2O3의 첨가를 고려하여공진주파수 온도계수가 90이하의 값을 가지도록 x를 0.5이하, 바람직하게는 0.3이하로 제한한다.In the present invention, if the mole fraction x of titanium (Ti) is too large, the resonant frequency temperature coefficient has an excessively large amount of value, so it is not recommended, and considering the addition of B 2 O 3 described later, the resonance frequency temperature coefficient is 90 or less. X is limited to 0.5 or less, preferably 0.3 or less.
또한, 본 발명에서는 유전체 조성물의 저온소결을 위하여 B2O3를 전체 조성물에 대하여 2중량%이하, 바람직하게는 1.5중량%이하로 첨가하는데, B2O3의 양이 지나치게 많게 되면 품질계수 및 공진 주파수 온도 계수 등의 유전특성이 저하하므로 바람직하지 않다.In addition, when the present invention, in addition to B 2 O 3 to a low firing temperature of the dielectric composition in a 2% by weight, preferably not more than 1.5% by weight based on the total composition, the amount of B 2 O 3 is too lot quality factor and It is not preferable because the dielectric properties such as the resonance frequency temperature coefficient are lowered.
이하, 본 발명을 실시예로써 더욱 자세히 설명한다. 그러나, 본 발명이 실시 예에 의해서만 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with examples. However, the present invention is not limited only by the embodiment.
(실시예)(Example)
순도 99 %의 CaCO3, Li2CO3, Nb2O5및 TiO2를 사용 전에 잘 건조시킨 후 이들 시료를 표 1의 조성비로 혼합하고, 혼합 분말을 대기 중에서 800∼900 ℃의 온도에서 2 시간 정도 하소하여 분쇄한 후 B2O3를 첨가한다. 성형 첨가제로 5 % PVA 수용액을 5 wt% 첨가하여 직경 10 mm, 두께 5 내지 6 mm의 원기둥형 시편으로 가압 성형하였으며 성형된 시편은 유기 바인더를 제거하기 위해 600 ℃의 온도에서 1 시간 동안 열처리한 후 대기 중에서 950∼1050 ℃의 온도에서 3 시간 동안 소결하였다.CaCO 3 , Li 2 CO 3 , Nb 2 O 5, and TiO 2 with 99% purity were dried well before use, and these samples were mixed at the composition ratios in Table 1, and the mixed powder was mixed at ambient temperature of 800-900 ° C. in air. After calcining for about an hour, the B 2 O 3 is added. 5 wt% of a 5% PVA aqueous solution was added as a molding additive and pressure-molded into a cylindrical specimen having a diameter of 10 mm and a thickness of 5 to 6 mm. The molded specimen was heat-treated at a temperature of 600 ° C. for 1 hour to remove the organic binder. After sintering in the air at a temperature of 950 ~ 1050 ℃ for 3 hours.
소결시편의 양면을 잘 연마한 후, 도파관 속에 넣고 유전체 공진기법으로 유전율, Q 값 및 공진 주파수의 온도 계수를 측정하였다. 이때, 측정 주파수는 7 내지 8 GHz이고, 측정 온도 범위는 -15 내지 85 ℃이었다. 각 시편의 마이크로파 유전 특성은 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 resonance frequency were measured by dielectric resonant technique. At this time, the measurement frequency was 7 to 8 GHz, and the measurement temperature range was -15 to 85 ° C. The microwave dielectric properties of each specimen are shown in Table 1.
표 1. 본 발명에 따른 유전체 조성물의 고주파 유전특성Table 1. High Frequency Dielectric Properties of Dielectric Compositions According to the Present Invention
표 1에서 보는 바와 같이, 본 발명에 따른 유전체 조성물은 유전율이 29.7 내지 35.2 이고, Qxfo(GHz)가 12,000 내지 26,000 이며, 공진 주파수의 온도 계수의 범위가 -16.8 내지 0 ppm/℃로 변화되었다. 특히, 본 발명의 조성물은 유전율 32, Qxfo(GHz)가 약 25,000 이며 공진주파수의 온도계수가 0 ppm/℃인Ca[(Li1/3Nb2/3)0.95Ti0.05]O3-δ와, 유전율 35, Qxfo(GHz)가 약 23,000이며 공진주파수의 온도계수가 +2.9 ppm/℃인 Ca[(Li1/3Nb2/3)0.9Ti0.1]O3-δ에 저온소결을 유도하기 위해 B2O3를 첨가하였으며, 1,000℃에서 소결시 B2O3의 첨가량에 따라 유전율과 Qxfo(GHz)가 증가하였으며, 공진주파수 온도계수는 음의 방향으로 증가되었다.As shown in Table 1, the dielectric composition according to the present invention had a dielectric constant of 29.7 to 35.2, a Qxf o (GHz) of 12,000 to 26,000, and a range of temperature coefficients of the resonance frequency was changed to -16.8 to 0 ppm / ° C. . In particular, the composition of the present invention has a dielectric constant of 32, Qxf o (GHz) of about 25,000 and Ca [(Li 1/3 Nb 2/3 ) 0.95 Ti 0.05 ] O 3-δ having a temperature coefficient of resonant frequency of 0 ppm / ° C. To induce low temperature sintering in Ca [(Li 1/3 Nb 2/3 ) 0.9 Ti 0.1 ] O 3-δ with a dielectric constant of 35 and a Qxf o (GHz) of about 23,000 and a temperature coefficient of resonance of +2.9 ppm / ℃ B 2 O 3 was added, and the dielectric constant and Qxf o (GHz) were increased according to the amount of B 2 O 3 added at sintering at 1,000 ℃, and the resonance frequency temperature coefficient was increased in the negative direction.
또한, 표 1에는 나타나 있지 않으나, 본 발명자들의 연구결과에 의하면, Ti의 함량이 증가할수록 유전율 및 공진주파수의 온도계수가 증가하는 것으로 확인되어 0.1 몰분율 이상의 Ti를 함유하는 조성에 있어서도 B2O3를 첨가함으로써 큰 유전율을 가지면서 공진주파수의 온도계수가 안정한 마이크로파용 유전체를 제조할 수 있었다.In addition, although not shown in Table 1, according to the results of the present inventors, it is confirmed that the temperature coefficient of the dielectric constant and the resonant frequency increases as the content of Ti increases, so that B 2 O 3 is obtained even in a composition containing Ti of 0.1 mole fraction or more. By adding it, it was possible to produce a microwave dielectric with a large dielectric constant and stable temperature coefficient of resonant frequency.
본 발명에 따른 유전체 조성물은 유전율이 29.7 내지 35.2 이고, Qxfo(GHz)가 12,000 내지 26,000 이며, 공진 주파수의 온도 계수의 범위가 -16.8 내지 0 ppm/℃로 조성의 변화에 따라 공진 주파수의 온도 계수를 0 ppm/℃ 근처로 조절이 가능하여 고주파용 유전체 세라믹스의 부품으로 사용되는 재료로서 이용될 수 있다.The dielectric composition according to the present invention has a dielectric constant of 29.7 to 35.2, a Qxf o (GHz) of 12,000 to 26,000, and a temperature coefficient of resonant frequency of -16.8 to 0 ppm / ° C. according to the change of composition, the temperature of the resonant frequency The modulus can be adjusted to around 0 ppm / ° C and can be used as a material used as a component of high frequency dielectric ceramics.
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| CN103922725B (en) * | 2014-03-20 | 2015-09-09 | 南京航空航天大学 | A kind of low-temperature sintering temperature-stabilized microwave medium ceramic material and preparation method thereof |
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