KR100444359B1 - Ceramic Material with Low-Dielectric Constant for LTCC - Google Patents

Ceramic Material with Low-Dielectric Constant for LTCC Download PDF

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KR100444359B1
KR100444359B1 KR10-2001-0082431A KR20010082431A KR100444359B1 KR 100444359 B1 KR100444359 B1 KR 100444359B1 KR 20010082431 A KR20010082431 A KR 20010082431A KR 100444359 B1 KR100444359 B1 KR 100444359B1
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dielectric constant
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김경용
박일환
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한국과학기술연구원
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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
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Abstract

본 발명은 하기 화학식 1의 조성을 갖는 LTCC용 저유전율 세라믹 조성물에 관한 것이다.The present invention relates to a low dielectric constant ceramic composition for LTCC having a composition of the following formula (1).

y[xA - (1-x)B] - (1-y)Cy [xA-(1-x) B]-(1-y) C

상기 식에서,Where

A는 BaWO4이고,A is BaWO 4 ,

B는 Mg2SiO4이며,B is Mg 2 SiO 4 ,

C는 SiO260∼90 중량%, B2O315∼30 중량%, K2O 1∼10 중량%로 이루어진 보로실리케이트 유리이고,C is SiO260 to 90% by weight, B2O315-30 wt%, K2O Borosilicate glass consisting of 1 to 10% by weight,

x는 0.5 ≤x ≤0.9를 충족시키는 값이며,x is a value that satisfies 0.5 ≤ x ≤ 0.9,

y는 0.4 ≤y ≤0.8을 충족시키는 값이다.y is a value satisfying 0.4 ≦ y ≦ 0.8.

본 발명에 따른 조성물을 LTCC용 기판 재료로 사용하여, 종래의 LTCC용 기판 재료와 비교하여 유전율이 낮고 품질계수가 우수한 기판 재료를 얻을 수 있다.By using the composition according to the present invention as a substrate material for LTCC, it is possible to obtain a substrate material having a low dielectric constant and excellent quality factor compared with the conventional LTCC substrate material.

Description

ＬＴＣＣ용 저유전율 세라믹 조성물 {Ceramic Material with Low-Dielectric Constant for LTCC}Low dielectric constant ceramic composition for LTCC {Ceramic Material with Low-Dielectric Constant for LTCC}

본 발명은 기판 재료로서 많이 사용되는 저온 소성 LTCC 조성물, 보다 상세하게는 유전율이 낮고 품질계수가 우수한 저온 소성 LTCC 조성물에 관한 것이다.The present invention relates to low temperature calcined LTCC compositions commonly used as substrate materials, and more particularly to low temperature calcined LTCC compositions having a low dielectric constant and an excellent quality factor.

종래로부터 저온 소성 LTCC 조성물은 기판 재료로서 많이 사용되고 있기 때문에, 저온에서 은전극과의 동시 소성을 위해서는 800∼900℃에서 소성 가능하고, 유전율은 10이하로 낮으며 품질 계수(전기적 손실의 역수)가 높은 특성이 요구되고 있다.Since the low temperature calcined LTCC composition is conventionally used as a substrate material, it can be calcined at 800 to 900 ° C for simultaneous firing with silver electrodes at low temperatures, the dielectric constant is lower than 10, and the quality factor (inverse of the electrical loss) is low. High characteristics are required.

상기 요구에 따라 낮은 유전율 및 우수한 전기적 특성을 얻기 위하여 알루미나를 주조성으로 하고, 저온 소성이 가능해지도록 유리를 첨가하여 900℃이하에서 소성가능한 재료들이 연구되고 있다. 이같이 알루미나에 유리를 첨가하여 기판 재료로서 사용할 경우, 알루미나 자체 조성에 비하여 전기적 특성은 낮으나 소결온도를 절반 이하로 낮출 수 있다는 장점이 있었다. 그러나 알루미나의 높은 소결온도(1600℃이상)로 인해 과량의 유리(40∼80 중량%)가 첨가되기 때문에 이같이 제조된 기판은 품질계수가 낮은 문제를 가지고 있다.In order to obtain a low dielectric constant and excellent electrical properties in accordance with the above requirements, alumina is castable, and glass materials are calcinable below 900 ° C by adding glass to enable low-temperature firing. As such, when glass is added to alumina and used as a substrate material, the electrical properties are lower than that of the alumina itself, but the sintering temperature can be lowered to less than half. However, because the high sintering temperature (above 1600 ° C) of the alumina is added to the excess glass (40 ~ 80% by weight) has a problem of low quality factor.

한편, 한국 세라믹 학회지에는 (1-x) BaWO4- x Mg2SiO4(x=0.1∼0.9)의 조성을 갖는 세라믹스는 유전율 εr이 10 이하, 구체적으로 6.37∼8.21로 낮으며, 품질계수 Q×f0가 15000 ∼ 99422이며, 공진 주파수의 온도계수 τf가 -73.9∼-48.9 ppm/℃의 고주파 유전특성을 갖는 것으로 기재되어 있다 (표제 「BaWO4-Mg2SiO4세라믹스의 CaTiO3첨가에 따른 고주파 유전 특성」, 한국 세라믹 학회 Vol 38. No.3, 2001년 3월, pp. 280∼286, 저자 박일환).On the other hand, in the Journal of the Korean Ceramic Society, ceramics having a composition of (1-x) BaWO 4 -x Mg 2 SiO 4 (x = 0.1 to 0.9) have a low dielectric constant ε r of 10 or less, specifically 6.37 to 8.21, and a quality factor Q It is described that xf 0 is 15000 to 99422, and the temperature coefficient τ f of the resonance frequency has a high frequency dielectric characteristic of -73.9 to 48.9 ppm / ° C (title "CaOO 3 addition of BaWO 4 -Mg 2 SiO 4 ceramics). High Frequency Dielectric Properties, "Journal of the Korean Ceramic Society, Vol 38. No.3, March 2001, pp. 280-286, Park Il-hwan).

본 발명자들은 기존의 알루미나-유리 시스템에서 알루미나를 BaWO4-Mg2SiO4로 대체함으로써 기존의 알루미나-유리 시스템에서 나타나는 문제점, 즉 과량의 유리 첨가로 인해 기판의 품질계수가 낮아지는 문제점을 해결할 수 있음을 발견하고 본 발명을 완성하였다.The present inventors have solved the problem of conventional alumina-glass systems by replacing alumina with BaWO 4 -Mg 2 SiO 4 in the existing alumina-glass system, that is, the problem of lowering the quality factor of the substrate due to the addition of excess glass. The present invention was completed.

본 발명의 목적은 과량의 유리를 첨가하지 않아도 저온(900℃ 이하)에서 소결 가능하며, 품질계수가 우수하고, 유전율이 낮은 LTCC용 저유전율 세라믹 조성물을 제공하는 것이다.It is an object of the present invention to provide a low dielectric constant ceramic composition for LTCC that can be sintered at low temperatures (900 ° C. or less), has an excellent quality factor, and has a low dielectric constant without adding excess glass.

도 1은 본 발명에서 세라믹 조성물의 조성 변화와 소결온도에 따른 유전율의 변화를 나타내는 그래프.1 is a graph showing the change in dielectric constant according to the composition change and sintering temperature of the ceramic composition in the present invention.

도 2는 본 발명에서 세라믹 조성물의 조성 변화의 소결온도에 따른 Q×f0의 변화를 나타내는 그래프.2 is a graph showing the change of Q × f 0 with the sintering temperature of the composition change of the ceramic composition in the present invention.

상기와 같은 본 발명의 목적은 하기 화학식 1의 조성을 갖는 저유전율 세라믹 조성물을 제공함으로써 달성된다.The object of the present invention as described above is achieved by providing a low dielectric constant ceramic composition having a composition of the following formula (1).

<화학식 1><Formula 1>

y[xA - (1-x)B] - (1-y)Cy [xA-(1-x) B]-(1-y) C

상기 식에서,Where

A는 BaWO4이고,A is BaWO 4 ,

B는 Mg2SiO4이며,B is Mg 2 SiO 4 ,

C는 SiO260∼84 중량%, B2O315∼30 중량%, K2O 1∼10 중량%로 이루어진 보로실리케이트 유리이고,C is SiO260 to 84% by weight, B2O315-30 wt%, K2O Borosilicate glass consisting of 1 to 10% by weight,

x는 0.5 ≤x ≤0.9를 충족시키는 값이며,x is a value that satisfies 0.5 ≤ x ≤ 0.9,

y는 0.4 ≤y ≤0.8을 충족시키는 값이다.y is a value satisfying 0.4 ≦ y ≦ 0.8.

본 발명의 저유전율 세라믹 조성물은 기존 알루미나 - 유리 시스템에서 알루미나를 BaWO4-Mg2SiO4로 대체한 것으로서, BaWO4는 알루미나와 비교하여 품질계수는 유사하지만 소결온도가 상대적으로 낮아(1100-1200℃) 저온소결에 유리하며, Mg2SiO4는 상기 BaWO4에 첨가됨으로써 유전율을 더 낮아지게 하는 효과를 나타낸다.The low dielectric constant ceramic composition of the present invention is to replace alumina with BaWO 4 -Mg 2 SiO 4 in the existing alumina-glass system, BaWO 4 has a similar quality coefficient compared to alumina but relatively low sintering temperature (1100-1200 ℃) is advantageous for low temperature sintering, Mg 2 SiO 4 is added to the BaWO 4 has an effect of lowering the dielectric constant.

즉, 상기 특성에 의해 주성분인 BaWO4-Mg2SiO4이 낮은 소결온도를 가지므로, 유리 첨가량을 20 중량% 정도까지 낮추어도 저온에서 은전극과 동시 소성이 가능한 기판 재료를 얻을 수 있다. 따라서 기존의 알루미나-유리 시스템에 비해 과량의 유리를 첨가하지 않아도 저온(900℃ 이하)에서 소결 가능하며, 품질계수가 우수하고, 유전율이 낮은 기판 재료를 제조할 수 있었다.That is, since the main component BaWO 4 -Mg 2 SiO 4 has a low sintering temperature, it is possible to obtain a substrate material capable of co-firing with the silver electrode at low temperature even if the amount of glass added is reduced to about 20% by weight. Therefore, it is possible to manufacture a substrate material which can be sintered at low temperature (below 900 ° C.), has excellent quality factor, and has a low dielectric constant, without adding excessive glass, compared to the conventional alumina-glass system.

상기와 같은 본 발명의 세라믹 조성물은 유전율 εr이 3.63 내지 6.27이고, 품질계수 Q×f0(GHz)가 4666 ∼ 12191이며, 공진 주파수의 온도계수 τf가 -46∼-17 ppm/℃로서, LTCC 용 저유전율 세라믹스가 요구되는 기판 재료에 적합하게 사용될 수 있다.As described above, the ceramic composition of the present invention has a dielectric constant ε r of 3.63 to 6.27, a quality factor Q × f 0 (GHz) of 4666 to 12191, and a temperature coefficient τ f of a resonance frequency of −46 to −17 ppm / ° C. Low dielectric constant ceramics for LTCC can be suitably used for the substrate materials required.

본 발명에 의한 고주파용 LTCC 조성물은 출발물질로서 예를 들어 BaCO3, WO3, MgO, SiO2및 보로실리케이트 유리를 사용하여 제조할 수 있다. 구체적으로 설명하면, BaCO3와 WO3를 몰비 1:1로 혼합하고 MgO와 SiO2를 몰비 2:1로 혼합하여 제조한 BaWO4와 Mg2SiO4분말을 각각 대기중에서 예를 들어 700℃와 1100℃에서 3시간씩 하소하여 합성한다. 보로실리케이트 유리는 SiO260∼84 중량%, B2O315∼30 중량%, K2O 1∼10 중량%의 조성을 갖는다. 합성 분말은 잘 분쇄한 후, 예를 들어 직경 14 mm의 원판형 시편으로 가압 성형하여 대기 중에서 예를 들어 800∼900℃의 온도에서 2시간 동안 소결시켜 제조할 수 있다. 이때, 소결후 시편의 수축율은 12∼20% 정도이다. 소결 시편의 유전율, Q×f0값 및 공진주파수의 온도계수 등의 유전특성은 유전체 공진기법으로 측정할 수 있다.High frequency LTCC composition according to the present invention is a starting material for example BaCO3, WO3, MgO, SiO2And borosilicate glass. Specifically, BaCO3And WO3Mixed in a molar ratio of 1: 1 and MgO and SiO2BaWO prepared by mixing at a molar ratio 2: 14And Mg2SiO4The powders are respectively synthesized by calcination at atmospheric temperature, for example, at 700 ° C. and 1100 ° C. for 3 hours. Borosilicate glass is SiO260 to 84% by weight, B2O315-30 wt%, K2O It has a composition of 1 to 10% by weight. Synthetic powder can be prepared by pulverizing well, for example, by press molding into a disk-shaped specimen having a diameter of 14 mm, and sintering in the air at a temperature of, for example, 800 to 900 ° C. for 2 hours. At this time, the shrinkage of the specimen after sintering is about 12 to 20%. Permittivity of Sintered Specimen, Q × f0Dielectric properties such as the value and the temperature coefficient of the resonance frequency can be measured by the dielectric resonant technique.

이하, 본 발명을 보다 구체적으로 실시예를 들어서 상세히 설명한다. 그러나, 본 발명이 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail with reference to Examples. However, the present invention is not limited by the following examples.

<실시예><Example>

BaWO4는 순도 99.9%의 BaCO3와 WO3를 몰비 1:1로 혼합하고, 혼합 분말은 대기 중에서 700℃의 온도에서 3시간 정도 하소한 후, 분쇄함으로써 제조할 수 있다.BaWO 4 may be prepared by mixing BaCO 3 and WO 3 having a purity of 99.9% in a molar ratio of 1: 1, and calcining the mixed powder after calcining at a temperature of 700 ° C. for about 3 hours.

Mg2SiO4는 순도 99.9%의 MgO와 SiO2를 몰비 2:1로 혼합하고, 혼합 분말은 대기중에서 1100℃의 온도에서 3시간 정도 하소한 후, 분쇄함으로써 제조할 수 있다.Mg 2 SiO 4 can be produced by mixing MgO and SiO 2 with a purity of 99.9% in a molar ratio of 2: 1, and mixed powder is calcined at about 1100 ° C. in the air for about 3 hours and then pulverized.

유리는 SiO2-B2O3-K2O계의 보로실리케이트 유리로서, 조성 범위는 SiO260∼84 중량%, B2O315∼30 중량%, K2O 1∼10 중량%이다. 본 실시예에서는 아사히 글라스 (Asahi Glass)에서 시판되는 ASF-103H를 사용하여 실험하였다.Glass is SiO2-B2O3-K2O-based borosilicate glass, the composition range of SiO260 to 84% by weight, B2O315-30 wt%, K2O 1 to 10% by weight. In this example, the experiment was carried out using ASF-103H which is commercially available from Asahi Glass.

BaWO4, MgSiO4및 유리를 표 1에 나타낸 조성비로 혼합하였다.BaWO 4 , MgSiO 4 and glass were mixed at the composition ratios shown in Table 1.

혼합한 분말을 잘 분쇄한 후 직경 14 mm의 원판형 시편으로 가압 성형하여 대기 중에서 800∼900℃의 온도에서 2시간 동안 소결시켰다. 소결후 시편은 12∼20% 정도 수축되었다.The mixed powder was pulverized well and pressure molded into a disk-shaped specimen having a diameter of 14 mm, followed by sintering for 2 hours at an air temperature of 800 to 900 ° C. After sintering, the specimens shrink about 12 to 20%.

소결 시편의 양면을 연마지 (#2000 까지)로 잘 연마한 후, 유전체 공진기법으로 유전율, Q×f0값 및 공진주파수의 온도계수를 측정하였다. 이때, 측정 주파수는 11∼14 GHz이고, 측정온도 범위는 -25∼85℃였다. 각 시편의 조성과 소결 온도에 따른 마이크로파 유전특성을 표 1에 나타내었다.After polishing both surfaces of the sintered specimen with abrasive paper (up to # 2000), the dielectric constant, Q × f 0 value, and temperature coefficient of the resonance frequency were measured by a dielectric resonant technique. At this time, the measurement frequency was 11-14 GHz and the measurement temperature range was -25-85 degreeC. Table 1 shows the microwave dielectric properties according to the composition and sintering temperature of each specimen.

y[xA - (1-x)B] - (1-y)C 복합체 (식 중, A는 BaWO4이고, B는 Mg2SiO4이며, C는 SiO2-B2O3-K2O계의 보로실리케이트 유리인 ASF-103H 유리임)의 고주파 유전특성y [xA-(1-x) B]-(1-y) C complex, wherein A is BaWO 4 , B is Mg 2 SiO 4 , and C is SiO 2 -B 2 O 3 -K 2 O High Frequency Dielectric Properties of Borosilicate Glass, ASF-103H Glass) 조성Furtherance εr ε r Q ×fo Q × f o τf τ f 소결온도Sintering Temperature x(몰)x (mole) y(중량)y (weight) 0.90.9 0.80.8 5.325.32 1207312073 -46-46 800℃800 ℃ 0.90.9 0.80.8 6.276.27 1219112191 -46-46 850℃850 ℃ 0.90.9 0.80.8 6.266.26 1166111661 -45-45 900℃900 ℃ 0.90.9 0.70.7 5.625.62 1100411004 -43-43 800℃800 ℃ 0.90.9 0.70.7 5.605.60 1036110361 -44-44 850℃850 ℃ 0.90.9 0.70.7 5.575.57 1101711017 -45-45 900℃900 ℃ 0.90.9 0.60.6 5.215.21 92369236 -34-34 800℃800 ℃ 0.90.9 0.60.6 4.844.84 89848984 -36-36 850℃850 ℃ 0.90.9 0.60.6 4.534.53 87798779 -36-36 900℃900 ℃ 0.90.9 0.50.5 4.784.78 88808880 -28-28 800℃800 ℃ 0.90.9 0.50.5 4.414.41 83918391 -30-30 850℃850 ℃ 0.90.9 0.50.5 4.324.32 82788278 -30-30 900℃900 ℃ 0.90.9 0.40.4 4.404.40 86298629 -23-23 800℃800 ℃ 0.90.9 0.40.4 4.174.17 85678567 -23-23 850℃850 ℃ 0.90.9 0.40.4 4.094.09 59825982 -25-25 900℃900 ℃ 0.70.7 0.80.8 4.844.84 82378237 -43-43 800℃800 ℃ 0.70.7 0.80.8 4.854.85 84928492 -41-41 850℃850 ℃ 0.70.7 0.80.8 4.944.94 89368936 -42-42 900℃900 ℃ 0.70.7 0.70.7 4.144.14 80718071 -37-37 800℃800 ℃ 0.70.7 0.70.7 4.624.62 81188118 -35-35 850℃850 ℃ 0.70.7 0.70.7 5.515.51 84848484 -35-35 900℃900 ℃ 0.70.7 0.60.6 4.594.59 88208820 -31-31 800℃800 ℃ 0.70.7 0.60.6 5.015.01 90189018 -30-30 850℃850 ℃ 0.70.7 0.60.6 4.904.90 92309230 -30-30 900℃900 ℃ 0.70.7 0.50.5 4.834.83 93429342 -25-25 800℃800 ℃ 0.70.7 0.50.5 4.764.76 90469046 -26-26 850℃850 ℃ 0.70.7 0.50.5 4.444.44 63896389 -29-29 900℃900 ℃ 0.70.7 0.40.4 4.694.69 91589158 -22-22 800℃800 ℃ 0.70.7 0.40.4 4.564.56 88278827 -20-20 850℃850 ℃ 0.70.7 0.40.4 4.224.22 71037103 -22-22 900℃900 ℃ 0.50.5 0.80.8 3.633.63 47334733 -35-35 800℃800 ℃ 0.50.5 0.80.8 3.883.88 46664666 -36-36 850℃850 ℃ 0.50.5 0.80.8 4.054.05 53815381 -35-35 900℃900 ℃ 0.50.5 0.70.7 4.084.08 56835683 -25-25 800℃800 ℃ 0.50.5 0.70.7 4.274.27 57175717 -21-21 850℃850 ℃ 0.50.5 0.70.7 4.434.43 61886188 -22-22 900℃900 ℃ 0.50.5 0.60.6 4.624.62 58095809 -20-20 800℃800 ℃ 0.50.5 0.60.6 4.654.65 58375837 -18-18 850℃850 ℃ 0.50.5 0.60.6 4.814.81 62186218 -18-18 900℃900 ℃ 0.50.5 0.50.5 4.574.57 50625062 -17-17 800℃800 ℃ 0.50.5 0.50.5 4.964.96 69266926 -20-20 850℃850 ℃ 0.50.5 0.50.5 4.954.95 69506950 -18-18 900℃900 ℃ 0.50.5 0.40.4 4.834.83 68336833 -18-18 800℃800 ℃ 0.50.5 0.40.4 4.884.88 73317331 -17-17 850℃850 ℃ 0.50.5 0.40.4 4.924.92 75127512 -17-17 900℃900 ℃

본 발명의 LTCC용 저유전율 세라믹 조성물은 900℃ 이하의 저온에서 소성이 가능하며, 유전율이 낮고 품질계수가 우수한 조성물임을 표 1로부터 확인할 수 있었다.Low dielectric constant ceramic composition for LTCC of the present invention can be baked at a low temperature of 900 ℃ or less, it was confirmed from Table 1 that the composition is low dielectric constant and excellent quality coefficient.

본 발명에 따르면, 기존의 알루미나-유리 시스템에서 알루미나를 BaWO4-Mg2SiO4로 대체함으로써 과량의 유리를 첨가하지 않아도 저온에서 소결 가능하며, 품질계수가 우수하고, 유전율이 낮은 LTCC용 저유전율 세라믹 조성물을 얻을 수 있다. 이에 따라, 종래 전량 수입에 의존하던 LTCC용 재료를 일부 수입 대체할 수 있을 것으로 기대된다.According to the present invention, by replacing alumina with BaWO 4 -Mg 2 SiO 4 in the existing alumina-glass system, it is possible to sinter at low temperature without adding excess glass, and has a low dielectric constant for LTCC with excellent quality coefficient and low dielectric constant. A ceramic composition can be obtained. Accordingly, it is expected that some parts of the LTCC material, which previously depended on the total amount of imports, can be replaced.

Claims (1)

하기 화학식 1의 조성을 갖는 LTCC용 저유전율 세라믹 조성물.A low dielectric constant ceramic composition for LTCC having the composition of Formula 1. <화학식 1><Formula 1> y[xA - (1-x)B] - (1-y)Cy [xA-(1-x) B]-(1-y) C 상기 식에서,Where A는 BaWO4이고,A is BaWO 4 , B는 Mg2SiO4이며,B is Mg 2 SiO 4 , C는 SiO260∼84 중량%, B2O315∼30 중량%, K2O 1∼10 중량%로 이루어진 보로실리케이트 유리이고,C is SiO260 to 84% by weight, B2O315-30 wt%, K2O Borosilicate glass consisting of 1 to 10% by weight, x는 0.5 ≤x ≤0.9를 충족시키는 값이며,x is a value that satisfies 0.5 ≤ x ≤ 0.9, y는 0.4 ≤y ≤0.8을 충족시키는 값이다.y is a value satisfying 0.4 ≦ y ≦ 0.8.
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KR102005291B1 (en) * 2015-02-27 2019-07-30 페로 코포레이션 Low-K and Mid-K LTCC dielectric compositions and devices
CN111410524B (en) * 2020-03-17 2022-03-04 广东风华高新科技股份有限公司 LTCC microwave dielectric material and preparation method thereof

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US5070046A (en) * 1989-10-19 1991-12-03 E. I. Du Pont De Nemours And Company Dielectric compositions
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US5070046A (en) * 1989-10-19 1991-12-03 E. I. Du Pont De Nemours And Company Dielectric compositions
JPH04124074A (en) * 1990-09-17 1992-04-24 Fujitsu Ltd Production of ceramic base plate having low dielectric constant and production of green sheet
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11203552B2 (en) * 2019-07-05 2021-12-21 University Of Electronic Science And Technology Of China Ceramic material and method of preparing the same

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