KR100297954B1 - High Frequency Dielectric Ceramic Composition - Google Patents
High Frequency Dielectric Ceramic Composition Download PDFInfo
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- KR100297954B1 KR100297954B1 KR1019980042392A KR19980042392A KR100297954B1 KR 100297954 B1 KR100297954 B1 KR 100297954B1 KR 1019980042392 A KR1019980042392 A KR 1019980042392A KR 19980042392 A KR19980042392 A KR 19980042392A KR 100297954 B1 KR100297954 B1 KR 100297954B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 17
- 239000000919 ceramic Substances 0.000 title claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000006104 solid solution Substances 0.000 claims description 6
- 238000010295 mobile communication Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000003989 dielectric material Substances 0.000 description 7
- 238000004891 communication Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002131 composite material Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- FHKPLLOSJHHKNU-INIZCTEOSA-N [(3S)-3-[8-(1-ethyl-5-methylpyrazol-4-yl)-9-methylpurin-6-yl]oxypyrrolidin-1-yl]-(oxan-4-yl)methanone Chemical compound C(C)N1N=CC(=C1C)C=1N(C2=NC=NC(=C2N=1)O[C@@H]1CN(CC1)C(=O)C1CCOCC1)C FHKPLLOSJHHKNU-INIZCTEOSA-N 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 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
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Abstract
본 발명은 이동체 통신에서 사용되는 유전체 공진기나 범지구 측위시스템(Global positioning system, GPS)등에 이용되는 고주파용 유전체 세라믹 조성물에 관한 것이다.The present invention relates to a dielectric ceramic composition for high frequency used in dielectric resonators, global positioning systems (GPS), and the like used in mobile communication.
본 발명의 조성물은 원료물질로서 CaCO3, TiO2, MgO, WO3을 다양한 몰비로 합성하여 일반식(1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3으로 나타낼 수 있으며 x가 0.3에서 0.7로 변함에 따라 5∼8㎓에서 유전률 33∼54, 품질계수(Qf)는 27,000∼12,000㎓의 값을 가지며 원료 조성의 변화에 따라 원하는 공진주파수의 온도계수를 제어할 수 있다.The composition of the present invention can be represented by the general formula (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -x CaTiO 3 by synthesizing CaCO 3 , TiO 2 , MgO, WO 3 as a raw material in various molar ratios. As x is changed from 0.3 to 0.7, the dielectric constant is 33 to 54 at 5 to 8 (and the quality factor (Qf) is 27,000 to 12,000㎓ and the temperature coefficient of the desired resonance frequency can be controlled according to the change of raw material composition. have.
Description
본 발명은 이동체 통신이나 위성통신 등에 사용되는 고주파용 유전체인 공진기나 범지구 측위시스템(Global positioning system, GPS)등에 이용되는 고주파용 유전체 세라믹 조성물에 관한 것이다.BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high frequency dielectric ceramic composition for use in resonators, global positioning systems (GPS), and the like, which are high frequency dielectrics used in mobile communications and satellite communications.
유전체 공진기는 각종 무선통신기기에 이용되는 부품으로 통신기기의 소형화, 경량화와 사용되는 주파수의 고주파화에 따라 고유전율, 고품질계수를 요구하고 있으며 정보통신 분야의 발전에 따라 이용범위는 더욱 확대될 것으로 기대 되고 있다. 따라서 최근의 제품이 소형화, 통신주파수의 광역화에 대응하기 위하여 높은 유전율과 높은 품질계수를 가진 유전체 개발의 필요성이 대두되고 있다.Dielectric resonator is a component used in various wireless communication devices, and it requires high dielectric constant and high quality coefficient according to the miniaturization, light weight of communication equipment and high frequency of used frequency. It is expected. Therefore, in order to cope with the miniaturization and wider range of communication frequency, recent development of dielectrics with high dielectric constant and high quality factor is emerging.
일반적으로 무선통신에 이용되는 유전체들은 사용 주파수가 매우 높기 때문에 고주파 유전특성이 우수한 재료가 이용되어야 하며 통상의 유전체 재료로는 사용할 수 없다.In general, since dielectrics used in wireless communication have a very high frequency of use, materials having excellent high frequency dielectric properties should be used and cannot be used as ordinary dielectric materials.
본 발명과 관련된 종래기술로는 미국특허 4,330,631호, 4,968,649호, 5219809호, 5,538,928호 등과 와키노(K. Wakino et al, J. Am. Ceram. Sec. Vol. 67, p278, 1984), 가토(J. Kato et al. Jpn. J. Appl. Phys. Vol. 30, p2343, 1991), 노무라(S. Nomura et al.Vol. 21, p624, 1982), 울프람(G. Wolfram Vol. 6, P1455, 1981) 등이 있으나 이들은 고주파 유전체들이 낮은 유전율을 가지면 높은 품질계수를 갖게되고, 높은 유전율을 가지면 낮은 품질계수를 갖는 반면에 본 발명에 의한 유전체 조성물은 중간값의 유전율과 품질계수 갖는다.Prior arts related to the present invention include US Pat. Nos. 4,330,631, 4,968,649, 5219809, 5,538,928 and K. Wakino et al, J. Am. Ceram. J. Kato et al. Jpn. J. Appl. Phys. Vol. 30, p2343, 1991), Nomura (S. Nomura et al. Vol. 21, p624, 1982), Wolfram (G. Wolfram Vol. 6, P1455, 1981), but these high frequency dielectrics have a low dielectric constant, have a high quality factor, and have a high dielectric constant have a low quality factor, whereas the dielectric composition of the present invention has a medium dielectric constant and quality factor.
본 발명은 원료물질로서 CaCO3, TiO2, MgO, WO3을 다양한 몰비로 합성하여 일반식 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3으로 나타낼 수 있는 고주파용 세라믹 유전체 조성물에 있어서 x가 0.3에서 0.7로 변함에 따라 5∼8㎓에서 유전율 33∼54, 품질계수(Qf)는 27,000∼12,000㎓의 고주파 유전특성을 가지는 단일상 유전체 자기 조성물을 제조하고자 한다.The present invention synthesizes CaCO 3 , TiO 2 , MgO, WO 3 as a raw material in various molar ratios and can be represented by general formula (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 In the ceramic dielectric composition for the present invention, a single-phase dielectric ceramic composition having a high frequency dielectric property of 33 to 54 and a quality factor (Qf) of 27,000 to 12,000 Hz at 5 to 8 Hz as x is changed from 0.3 to 0.7 is intended. .
제1도는 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3고용계에서 x가 0.3∼0.7일 때 5∼8㎓ 대역에서 측정한 유전율과 품질계수의 값을 나타낸 그래프이다.FIG. 1 shows the values of permittivity and quality factor measured in the band 5-8 ㎓ when x is 0.3-0.7 in (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 solid solution It is a graph.
제2도는 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3고용계에서 x가 0.3∼0.7일 때 1MHz에서 측정된 각 실시예에서 조성에 따른 유전율의 온도계수 변화를 나타낸 그래프이다.2 shows the change in the temperature coefficient of the dielectric constant according to the composition in each example measured at 1 MHz when x is 0.3 to 0.7 in a (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 solid solution Is a graph.
제3도는 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3고용계에서 x가 0∼0.9일 때 X - 선 회절 패턴을 나타낸 그래프이다.3 is a graph showing an X-ray diffraction pattern when x is 0 to 0.9 in a (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 solid solution.
현재 응용되고 있는 고주파용 유전체 자기 조성물들은 크게 두 가지로 분류할 수 있다. 한가지는 높은 유전율(εr=80∼90)과 낮은 품질계수(Qf ≒ 5,000㎓)로 대변되는 BaO - Re2O3- TiO2(Re=희토류금속(rate earth metal))와 (Pb, Ca)ZrO3계이며, 다른 하나는 낮은 유전율과 높은 품질계수를 가지는 복합 페롭스카이트인 Ba(Mg,Ta)O3(εr=25, Qf = 16,800 at 10.5 ㎓)와 (Zr, Sn)TiO4(εr= 36, Qf = 6,500 at 7 ㎓)이다. 이러한 두 가지 유전체들은 높은 유전율을 가지면 낮은 품질계수를 가지거나 혹은 낮은 유전율을 가지면 높은 품질계수를 가진다.Currently, high frequency dielectric ceramic compositions can be classified into two types. One is BaO-Re 2 O 3 -TiO 2 (Re = rate earth metal) and (Pb, Ca), which are represented by high dielectric constant (ε r = 80-90) and low quality factor (Qf ㎓ 5,000㎓). ZrO 3 series, the other is Ba (Mg, Ta) O 3 (ε r = 25, Qf = 16,800 at 10.5 0.5) and (Zr, Sn) TiO 4 , a composite perovskite with low dielectric constant and high quality factor (ε r = 36, Qf = 6,500 at 7 kHz). These two dielectrics have a low quality factor if they have high permittivity or high quality factors if they have low permittivity.
페롭스카이트 CaTiO3은 유전율이 170, 품질계수(Qf)가 3,600 ㎓, 그리고 공진주파수의 온도계수(τf) 800 ppm/℃로 고주파 유전체로서는 유용한 특성을 가지고 있지 않다. τf= - l/2τε- α(τf: 공진주파수의 온도계수, τε: 유전률의 온도계수, α : 선팽창계수)의 관계식에서 τf와 τε의 부호가 반대이므로 CaTiO3의 τε는 음의 값을 가진다. 여기에 복합페롭스카이트 Ca(Mg1/2W1/2)O3이 첨가됨에 따라 유전율은 낮아지고 품질계수는 높아진다. 그리고, τε는 음의 값에서 양의 값으로 변하게 된다.Perovskite CaTiO 3 has a dielectric constant of 170, quality factor (Qf) of 3,600 ㎓, and temperature coefficient of resonant frequency (τ f ) of 800 ppm / ° C. τ f =-l / 2τ ε -α (τ f : temperature coefficient of resonant frequency, τ ε : temperature coefficient of dielectric constant, α: linear expansion coefficient), so that the sign of τ f and τ ε is opposite, so τ of CaTiO 3 ε has a negative value. As the composite perovskite Ca (Mg 1/2 W 1/2 ) O 3 is added, the dielectric constant is lowered and the quality factor is increased. Τ ε is changed from a negative value to a positive value.
본 발명은 중간정도의 품질계수와 유전율(Qf = 15000∼30000 ㎓, εr= 25∼50)을 가지는 고주파용 유전체 자기조성물을 제조하기 위해 Ca(Mg1/2W1/2)O3과 CaTiO3을 기존의 방법인 고상 반응법을 이용하여 일반식 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3에서 x가 0∼0.9범위를 가지도록 제조하였다.The present invention relates to Ca (Mg 1/2 W 1/2 ) O 3 and to prepare a dielectric high-frequency magnetic composition having a moderate quality factor and dielectric constant (Qf = 15000-30000 ㎓, ε r = 25-50). CaTiO 3 was prepared in the general formula (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -x CaTiO 3 by using a conventional solid-phase reaction method so that x has a range from 0 to 0.9.
이하 본 발명을 다음의 실시예와 시험예에 의하여 자세히 설명하고자 한다. 이들은 본 발명을 보다 상세히 설명하기 위한 것으로 이들 실시예와 시험예에 의하여 본 발명의 기술적 범위가 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail by the following examples and test examples. These are for explaining the present invention in more detail, and the technical scope of the present invention is not limited by these examples and test examples.
[실시예 1 - 10][Examples 1-10]
본 발명은 A(B′B″)O3구조의 A위치에 Ca이 1㏖ 결합되고 B′와 B″위치에 Mg2+와 W6+가 각각 1/2 ㏖씩 결합된 복합페롭스카이트Ca(Mg1/2W1/2)O3(이하 CMW이라 명명)와 ABO3구조에서 A위치에 Ca이 1㏖ 결합되고 B위치에 Ti4+가 1 ㏖ 결합되는 페롭스카이트 CaTiO3(이하 CT이라 명명)의 고용계를 구성하여 아래의 표 1에서 나타낸 조건으로 고상 반응법을 이용하여 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3에서 x가 0∼0.9범위를 가지도록 하는 단일상 고용계인 유전체 자기 조성물을 제조하였다.The present invention provides a composite perovskite in which 1 mol of Ca is bonded to the A position of the A (B′B ″) O 3 structure and 1/2 mol of Mg 2+ and W 6+ are bonded to the B ′ and B ″ positions, respectively. Perovskite CaTiO 3 (1 g of Ca is bonded to A position and 1 mol of Ti 4+ is bonded to B position in Ca (Mg 1/2 W 1/2 ) O 3 (hereinafter referred to as CMW) and ABO 3 structure) The solid solution system of CT is hereinafter referred to and (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 in the solid phase reaction method under the conditions shown in Table 1 below. A single-phase solid solution dielectric ceramic composition was prepared to have a range of ˜0.9.
[시험예 1][Test Example 1]
상기 실시예에서 물질특성이 좋은 실시예 2 - 8(0.3≤x≤0.7)만을 택하여 지름 10㎜의 소결된 시편을 두께 1㎜로 잘라서 시편 양면에 은(Ag) 전극을 도포한 후 600℃에서 5분 동안 열처리하고 휴렛 펙커드사의 HP4194 분석기(Impedance gain/phase analyzer)를 이용하여 전기적 특성인 1㎒에서의 실유전율을 측정하여 표 2에 나타내었다.In the above embodiment, the material having good material properties was selected as Example 2-8 (0.3 ≦ x ≦ 0.7), and the sintered specimen having a diameter of 10 mm was cut to 1 mm in thickness to apply silver (Ag) electrodes to both sides of the specimen, followed by 600 ° C. After heat treatment for 5 minutes at Hewlett-Packard's HP4194 analyzer (Impedance gain / phase analyzer) was measured in the actual dielectric constant at 1MHz the electrical properties are shown in Table 2.
또한 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3에서 x가 0.3∼0.7의 범위에서 측정한 조성에 따른 유전률의 온도의존계수 변화는 측정된 유전율 곡선으로부터의 관계식을 이용하여 제1도에 나타내었다.In addition, the temperature dependence coefficient of dielectric constant according to the composition of x measured in the range of 0.3 to 0.7 in (1-x) Ca (Mg 1/2 W 1/2 ) O 3 -xCaTiO 3 can be obtained from the measured dielectric constant curve. It is shown in Figure 1 using the relationship of.
[시험예 2][Test Example 2]
상기 실시예에서 (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3의 조성물의 0.3≤x≤0.7인 영역에서 마이크로파 유전특성을 측정하기 위하여 소결된 시편들의 높이/직경의 비가 0.4∼0.5가 되도록 표면을 연마하였다. 준비된 시편을 두 평행 도체판 사이에 넣고 Network Analyzer(HP 8720C)를 사용하여 Hakki - Coleman 방법으로 TE011 공진주파수와 삽입손실 그리고 3 ㏈에서의 대역폭을 측정하여 유전체의 품질계수와 유전율을 계산하였다. 측정결과는 다음 표 3과 같다.Height / diameter of sintered specimens for measuring microwave dielectric properties in the region of 0.3 ≦ x ≦ 0.7 of the composition of (1−x) Ca (Mg 1/2 W 1/2 ) O 3 −xCaTiO 3 in the above example The surface was polished so that the ratio was 0.4 to 0.5. The prepared specimens were sandwiched between two parallel conductor plates and the quality factor and dielectric constant of dielectrics were calculated by measuring TE011 resonance frequency, insertion loss and bandwidth at 3 으로 using Hakki-Coleman method using Network Analyzer (HP 8720C). The measurement results are shown in Table 3 below.
상기의 시험예에서 알 수 있듯이 본 발명에 따른 유전체 자기 조성물은 고주파 영역에서 CaTiO3의 양이 증가함에 따라 유전률은 증가하고 품질계수는 낮아지는 경향을 보이며 특히, (1 - x)Ca(Mg1/2W1/2)O3- xCaTiO3에서 x = 0.5일 때 5∼8㎓에서의 실유전률이 약 40, 품질계수가 약 16,000 ㎓인 우수한 고주파 유전체 재료로서의 특성을 보인다.As can be seen from the above test examples, the dielectric ceramic composition according to the present invention has a tendency of increasing the dielectric constant and decreasing the quality coefficient as the amount of CaTiO 3 increases in the high frequency region, and in particular, (1-x) Ca (Mg 1 / 2 W 1/2 ) O 3 -xCaTiO 3 , x = 0.5, has excellent dielectric constant of about 40 and quality coefficient of about 16,000 때 at 5 to 8 ㎓.
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| KR1019980042392A KR100297954B1 (en) | 1998-10-10 | 1998-10-10 | High Frequency Dielectric Ceramic Composition |
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| KR1019980042392A KR100297954B1 (en) | 1998-10-10 | 1998-10-10 | High Frequency Dielectric Ceramic Composition |
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| KR100297954B1 true KR100297954B1 (en) | 2001-11-14 |
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| KR19980020389A (en) * | 1996-09-09 | 1998-06-25 | 손영목 | Dielectric composition for high frequency large capacity ceramic capacitor |
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| KR19980020389A (en) * | 1996-09-09 | 1998-06-25 | 손영목 | Dielectric composition for high frequency large capacity ceramic capacitor |
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