KR100234011B1 - Dielectric ceramic composition - Google Patents

Dielectric ceramic composition Download PDF

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KR100234011B1
KR100234011B1 KR1019970039640A KR19970039640A KR100234011B1 KR 100234011 B1 KR100234011 B1 KR 100234011B1 KR 1019970039640 A KR1019970039640 A KR 1019970039640A KR 19970039640 A KR19970039640 A KR 19970039640A KR 100234011 B1 KR100234011 B1 KR 100234011B1
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dielectric
dielectric ceramic
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temperature coefficient
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KR19990016911A (en
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김경용
최환
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박호군
한국과학기술연구원
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00Fixed capacitors; Processes of their manufacture
    • H01G4/002Details
    • H01G4/018Dielectrics
    • H01G4/06Solid dielectrics
    • H01G4/08Inorganic dielectrics
    • H01G4/12Ceramic dielectrics
    • H01G4/1209Ceramic dielectrics characterised by the ceramic dielectric material
    • H01G4/1218Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
    • H01G4/1227Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates

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Abstract

마이크로파용 유전체 세라믹 조성물에 있어서, CaTiO3와 La(Zn1/2Ti1/2)O3및 NdAIO3를 주성분으로 하는 페로브스카이트형 고용체로 유전체 세라믹을 구성하므로서, 유전율이 커서 유전손실이 작고, Q ×f0(GHz)특성이 우수하며, 공진주파수의 온도계수가 ±10 ppm/℃이하인 우수한 마이크로파용 유전체 세라믹을 제공할 수 있다. 한편, CaTiO3의 함량을 미세하게 조절하므로서, 동일한 제조조건에서 공진주파수의 온도계수를 0 ppm/℃을 중심으로 자유로이 +와 -로 제어할 수 있다.In the dielectric ceramic composition for microwave, the dielectric ceramic is composed of a perovskite solid solution mainly composed of CaTiO 3 , La (Zn 1/2 Ti 1/2 ) O 3, and NdAIO 3 , and the dielectric constant is large, resulting in small dielectric loss. It is possible to provide an excellent microwave dielectric ceramic having excellent Q × f 0 (GHz) characteristics and a temperature coefficient of resonant frequency of ± 10 ppm / ° C or less. On the other hand, by finely adjusting the content of CaTiO 3 , under the same manufacturing conditions it is possible to freely control the temperature coefficient of the resonant frequency centered around 0 ppm / ℃ to + and-.

Description

고주파용 유전체 세라믹 조성물High Frequency Dielectric Ceramic Composition

본 발명은 저손실이며, 공진주파수의 온도계수가 양호한 마이크로파용 유전체 세라믹 조성물에 관련된 것이다.The present invention relates to a dielectric ceramic composition for microwaves with low loss and good temperature coefficient of resonance frequency.

최근 정보화 사회의 전진과 더불어 무선전화기, 자동차전화기 등의 이동 통신 및 위성방송, 위성통신 분야에서의 마이크로파(주파수대역 : 300MHz - 300GHz)를 이용한 통신시스템이 현저하게 발전하고 있으며, 이러한 뉴미디어의 실용화에 있어서, 공진기, 대역통과(또는 저지) 필터 및 마이크로파 집적회로(MIC : Microwave Integrated Circuit)등에 고주파용 유전체 세라믹의 응용이 크게 증대 되고 있다. 지금까지 이러한 조건을 만족하는 세라믹의 개발을 위해 많은 연구가 진행되었는데, 대표적인 마이크로파용 유전체 세라믹 재료로는 유전율이 20 - 30대 이며, 높은 Q(quality factor)값 (Q × f0= 100000)을 나타내는 복합 페로브스카이트형 고용체(BMT, BZT등), 유전율이 30 - 40이며, 중간정도의 Q값(Q × f0= 30000)을 갖는 단순 고용체(BT4, BT9등), 그리고 유전율이 90 - 100정도로 높이나 비교적 낮은 Q값 (Q × f0= 4500)을 보이는 혼합상 재료(BPNT, PCZ등)등이 있다.Recently, with the advancement of the information society, communication systems using microwaves (frequency band: 300MHz-300GHz) in mobile communication, satellite broadcasting, and satellite communication fields such as wireless telephones and automobile telephones have been remarkably developed. BACKGROUND OF THE INVENTION The application of high frequency dielectric ceramics to resonators, bandpass (or stop) filters, microwave integrated circuits (MIC), and the like has been greatly increased. Until now, many studies have been conducted to develop ceramics that satisfy these conditions. Representative microwave dielectric ceramic materials have a dielectric constant of 20 to 30 years and have high Q (Q × f 0 = 100000). The composite perovskite solid solution (BMT, BZT, etc.), the dielectric constant is 30-40, the simple solid solution (BT 4 , BT 9, etc.) having a moderate Q value (Q × f 0 = 30000), and the dielectric constant Mixed phase materials (BPNT, PCZ, etc.) that have a height of 90-100 but a relatively low Q (Q x f 0 = 4500).

이러한 고주파용 유전체 세라믹 재료에 요구되는 중요한 특성으로는Important characteristics required for such high frequency dielectric ceramic materials include

ⅰ) 사용주파수에 대응하여 높은 비유전율을 가질 것.V) have a high relative dielectric constant corresponding to the frequency used;

ⅱ) Q값이 클것.Ii) The Q value is large.

ⅲ) 공진주파수의 온도계수가 0 ppm/℃에 가까울 것.온도계) The temperature coefficient of resonant frequency is close to 0 ppm / ℃.

ⅳ) 물리화학적으로 안정하며 경시 변화가 작을 것.Viii) It is physicochemically stable and the change over time is small.

ⅴ) 기계적강도 및 열전도율이 크고 열확산성이 양호하며, 열팽창계수가 작을 것, 등이 있다.I) The mechanical strength and thermal conductivity are large, the thermal diffusivity is good, and the coefficient of thermal expansion is small.

일반적으로는 유전율이 큰 재료는 유전체 내부의 쌍극자와의 결함등으로 인하여 유전손실이 작고, 공진주파수의 온도계수가 ±30 ppm/℃정도로 안정하여야 사용이 가능하다. CaTiO3의 경우 3GHz에서 유전율이 170 - 180정도로 매우 높으나, 공진주파수의 온도계수가 약 +800 ppm/℃로 매우 크다는 단점이 있으며, La(Zn1/2Ti1/2)O3의 경우에는 유전율은 34정도로 낮으나 Q × f0(GHz)가 60000정도로 매우 높고 공진주파수의 온도계수가 -60 ppm/℃정도이다. 따라서 본 발명에서는 이러한 두 재료의 문제점을 개선하여 유전율이 40이상이며, 유전손실이 작고 공진주파수의 온도계수가 0 ppm/℃을 중심으로 +와 -쪽으로 필요에 따라 쉽게 이동시킬수 있는 새로운 마이크로파용 유전체 세라믹 조성물을 제공하고자 한다.In general, materials with high dielectric constants have low dielectric losses due to defects with dipoles in the dielectric and can be used only when the temperature coefficient of the resonance frequency is stable at about ± 30 ppm / ℃. In the case of CaTiO 3 , the dielectric constant is very high at 170 GHz at 3 GHz, but the temperature coefficient of the resonance frequency is about +800 ppm / ℃, which is very large. In the case of La (Zn 1/2 Ti 1/2 ) O 3 , the dielectric constant is high. Is low as 34, but Q × f 0 (GHz) is very high as 60000 and the temperature coefficient of resonant frequency is about -60 ppm / ℃. Therefore, the present invention improves the problems of these two materials, the dielectric constant is more than 40, the dielectric loss is small and the temperature coefficient of the resonant frequency can be easily moved to + and-as needed around 0 ppm / ℃ as needed It is intended to provide a composition.

제1도는 본 발명에 의한 유전체 세라믹 조성물의 조성범위를 보여주는 조성상태도이다.1 is a composition state diagram showing the composition range of the dielectric ceramic composition according to the present invention.

본 발명에 의한 마이크로파용 유전체 세라믹 조성물은 CaTiO3와 La(Zn1/2Ti1/2)O3및 NdAIO3를 주성분으로 하는 페로브스카이트형 고용체로서 각 성분사이의 범위는 도 1의 조성상태도에 표시된 바와 같다. 이와 같이 범위를 한정시킨 이유는 이들 조성에 의한 유전체의 공진주파수의 온도계수가 대략 +80 - -50 ppm/℃이므로 이 자체로써 또는 첨가제를 소량 첨가시키므로서, 유전손실이 작고 온도 특성이 양호한 마이크로파용 유전체 세라믹을 제조할 수 있기 때문이다.The dielectric ceramic composition for microwaves according to the present invention is a perovskite solid solution mainly composed of CaTiO 3 , La (Zn 1/2 Ti 1/2 ) O 3, and NdAIO 3 . As shown in The reason for limiting the range is that the temperature coefficient of the resonant frequency of the dielectric material by these compositions is approximately +80--50 ppm / ° C, so by itself or by adding a small amount of additives, the dielectric loss is small and the temperature characteristics are good for the microwave. It is because a dielectric ceramic can be manufactured.

이러한 본 발명의 내용을 실시예를 통하여 상세히 설명하고자 한다.It will be described in detail through the embodiments of the present invention.

[실시예]EXAMPLE

원료분말은 99.9%의 순도를 갖는 CaTiO3, La2O3, Al2O3, TiO2, Nd2O3및 ZnO를 사용하여, 표 1에 나타낸 조성이 되도록 각 원료들을 정확히 평량한 후 서로 혼합하였다. 혼합분말은 대기중 1250℃의 온도에서 4시간 정도 하소하여 페로브스카이트구조를 갖는 고용체를 합성하였다.The raw material powder was calibrated with each raw material exactly to the composition shown in Table 1 using CaTiO 3 , La 2 O 3 , Al 2 O 3 , TiO 2 , Nd 2 O 3 and ZnO having a purity of 99.9%. Mixed. The mixed powder was calcined at a temperature of 1250 ° C. for about 4 hours to synthesize a solid solution having a perovskite structure.

합성분말은 잘 분쇄한 후 직경 15mm, 두께 6 - 7mm인 원판형 시편으로 가압 성형하여, 대기중 1450 - 1550℃의 온도에서 2 - 6시간 동안 소결하였다. 소결후 시편의 수축율은 15 - 20%정도이다.The synthetic powder was pulverized well, press-molded into a disc-shaped specimen having a diameter of 15 mm and a thickness of 6-7 mm, and sintered at a temperature of 1450-1550 ° C. for 2-6 hours. After sintering, the shrinkage of the specimen was about 15-20%.

소결시편의 양면을 연마지(#3000까지)를 이용하여 잘 연마한 후 유전체 공전기법으로 유전율, Q값 및 공진 주파수의 온도계수를 측정하였다. 이때 측정주파수는 4 - 6GHz이며 측정온도 범위는 -30℃ 내지 80℃였다. 각 조성별 시편의 마이크로파 유전특성은 표 1에 나타낸 바와 같다.Both surfaces of the sintered specimens were polished well using abrasive paper (up to # 3000), and then the dielectric constant, Q value, and temperature coefficient of the resonance frequency were measured by dielectric dielectric method. At this time, the measurement frequency was 4-6GHz and the measurement temperature range was -30 ° C to 80 ° C. Microwave dielectric properties of the specimens for each composition are shown in Table 1.

표 1에 나타나 있는 바와 같이 La(Zn1/2Ti1/2)O3및 NdAlO3의 양에 따라서는 고주파 유전특성이 크게 변화가 없으나 CaTiO3의 양에 따라서는 그 특성이 크게 변화하고 있다. 그 CaTiO3의 함량이 증가함에 따라 유전율은 40 - 70의 범위에서 서서히 증가하나 Q ×f0(GHz)는 감소하고 있으며 공진주파수의 온도계수는 -에서 +로 점진적으로 변화된다. 따라서 CaTiO3의 함량이 0.5 - 0.6mol부근에서 유전율 및 Q ×f0(GHz)특성이 우수하고 공진주파수의 온도계수가 ±10 ppm/℃이하인 우수한 마이크로파용 유전체 세라믹을 제조할 수 있다. 한편, CaTiO3의 함량을 미세하게 조절하므로서, 동일한 제조조건에서 공진주파수의 온도계수를 0 ppm/℃을 중심으로 자유로이 +와 -로 제어할 수 있다.As shown in Table 1, the high frequency dielectric properties did not change significantly depending on the amount of La (Zn 1/2 Ti 1/2 ) O 3 and NdAlO 3 , but the properties changed significantly depending on the amount of CaTiO 3 . . As the CaTiO 3 content increases, the dielectric constant gradually increases in the range of 40-70 but Q x f 0 (GHz) decreases and the temperature coefficient of the resonant frequency changes gradually from-to +. Accordingly, excellent dielectric ceramics for microwaves having excellent dielectric constant and Q x f 0 (GHz) characteristics and a resonant frequency temperature of less than ± 10 ppm / ° C can be produced at around 0.5-0.6 mol of CaTiO 3 . On the other hand, by finely adjusting the content of CaTiO 3 , under the same manufacturing conditions it is possible to freely control the temperature coefficient of the resonant frequency centered around 0 ppm / ℃ to + and-.

Figure kpo00002
Figure kpo00002

Figure kpo00003
Figure kpo00003

본 발명에 의한 마이크로파용 유전체 세라믹 조성물은 CaTiO3와 La (Zn1/2Ti1/2)O3및 NdAlO3를 주성분으로 하는 페로브스카이트형 고용체로서 유전손실이 작고 공진주파수의 온도계수가 0 ppm/℃을 중심으로 +와 -쪽으로 필요에 따라 쉽게 이동시킬수 있는 새로운 마이크로파용 유전체 세라믹 조성물을 제공할 수 있다.Microwave dielectric ceramic composition according to the present invention is a perovskite solid solution mainly composed of CaTiO 3 and La (Zn 1/2 Ti 1/2 ) O 3 and NdAlO 3, which has a low dielectric loss and a temperature coefficient of resonant frequency of 0 ppm. It is possible to provide a novel dielectric ceramic composition for microwaves that can be easily moved as needed towards + and-centered at / ° C.

Claims (2)

일반식 (1-x)CaTiO3- x[(1-y)La(Zn1/2Ti1/2)O3- NdAlO3]으로 표시되는 조성계에서 x 및 y의 범위가, 각각 0.2≤x≤0.5 및 0〈y〈1인 것을 특징으로 하는 고주파용 유전체 세라믹 조성물.In the composition system represented by general formula (1-x) CaTiO 3 -x [(1-y) La (Zn 1/2 Ti 1/2 ) O 3 -NdAlO 3 ], the ranges of x and y are each 0.2≤x <0.5 and 0 <y <1, the dielectric ceramic composition for high frequency. 제1항에서 있어서, 상기 x의 범위가 0.4≤x≤0.5인 것을 특징으로 하는 고주파용 유전체 세라믹 조성물.The dielectric ceramic composition for high frequency as claimed in claim 1, wherein the range of x is 0.4 ≦ x ≦ 0.5.
KR1019970039640A 1997-08-20 1997-08-20 Dielectric ceramic composition KR100234011B1 (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960000819A (en) * 1994-06-30 1996-01-25 김은영 High Frequency Dielectric Composition
KR970015536A (en) * 1995-09-07 1997-04-28 김은영 High Frequency Dielectric Magnetic Composition

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960000819A (en) * 1994-06-30 1996-01-25 김은영 High Frequency Dielectric Composition
KR970015536A (en) * 1995-09-07 1997-04-28 김은영 High Frequency Dielectric Magnetic Composition

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