JP3243873B2 - Dielectric porcelain composition - Google Patents
Dielectric porcelain compositionInfo
- Publication number
- JP3243873B2 JP3243873B2 JP06399493A JP6399493A JP3243873B2 JP 3243873 B2 JP3243873 B2 JP 3243873B2 JP 06399493 A JP06399493 A JP 06399493A JP 6399493 A JP6399493 A JP 6399493A JP 3243873 B2 JP3243873 B2 JP 3243873B2
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- Prior art keywords
- dielectric
- composition
- oxide powder
- porcelain composition
- dielectric porcelain
- Prior art date
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- Inorganic Insulating Materials (AREA)
- Control Of Motors That Do Not Use Commutators (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、誘電体共振器等の材料
として好適な誘電体磁器組成物に関する。本発明の誘電
体磁器組成物は、誘電体共振器材料の他に、例えばマイ
クロ波ＩＣ用誘電体基板、誘電体調整棒などにも適用さ
れる。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a dielectric ceramic composition suitable as a material for a dielectric resonator or the like. The dielectric ceramic composition of the present invention can be applied to, for example, a dielectric substrate for microwave IC, a dielectric adjustment rod, and the like, in addition to the dielectric resonator material.
【０００２】[0002]
【従来技術およびその問題点】近年、マイクロ波回路の
集積化に伴い、小型で高性能の誘電体共振器が求められ
ている。このような誘電体共振器に使用される誘電体磁
器組成物には、比誘電率εr が大きいこと、また共振周
波数の温度係数τf の安定度および共振周波数の温度特
性の直線性が優れ、無負荷Ｑが大きいことなどが要求さ
れている。このような誘電体磁器組成物として従来Ｔｉ
Ｏ2 、ＭｇＯ−ＣａＯ−ＴｉＯ2などを主成分とするも
のが知られているが、前者は温度係数が大きく、後者は
比誘電率が小さいという問題点がある。2. Description of the Related Art In recent years, with the integration of microwave circuits, a small and high-performance dielectric resonator has been demanded. Such dielectric dielectric ceramic composition used in the resonator, the ratio is large dielectric constant epsilon r, also the linearity of the temperature characteristics of stability and resonance frequency temperature coefficient tau f of resonance frequency is excellent It is required that the no-load Q is large. As such a dielectric porcelain composition, Ti
Although those containing O 2 , MgO—CaO—TiO 2 as main components are known, the former has a problem that the temperature coefficient is large, and the latter has a small relative dielectric constant.
【０００３】この改良系としてＢａＯ−ＴｉＯ2 −Ｎｄ
2 Ｏ3 系の誘電体磁器組成物についての提案〔Ber.Dt.K
eram.Ges.55(1978)Nr.7 ；特開昭６０−３５４０６号公
報等〕、あるいは、ＢａＯ−ＴｉＯ2 −Ｎｄ2 Ｏ3 −Ｂ
ｉ2 Ｏ3 系（特開昭６２−７２５５８号公報）について
の提案がなされているが、さらに小型の誘電体共振器が
求められ、そのためさらに誘電率の大きい材料の開発が
望まれている。As an improved system, BaO-TiO 2 -Nd
Proposal for 2 O 3 based dielectric porcelain composition [Ber. Dt.
eram.Ges.55 (1978) Nr.7; JP 60-35406 Publication], or, BaO-TiO 2 -Nd 2 O 3 -B
Although proposals have been made for the i 2 O 3 system (Japanese Patent Application Laid-Open No. 62-72558), a smaller dielectric resonator is required, and therefore, development of a material having a higher dielectric constant is desired.
【０００４】[0004]
【発明の目的】本発明の目的は、マイクロ波誘電体共振
器材料としてさらに優れた特性を有する誘電体磁器組成
物、特に高誘電率で、無負荷Ｑが大きく、共振周波数の
温度変化の小さい誘電体磁器組成物を提供することにあ
る。An object of the present invention is to provide a dielectric ceramic composition having more excellent characteristics as a microwave dielectric resonator material, particularly a high dielectric constant, a large unloaded Q, and a small temperature change of the resonance frequency. An object of the present invention is to provide a dielectric ceramic composition.
【０００５】[0005]
【問題点を解決するための手段】本発明は、組成式、
（Ｂａ1-xＰｂx）（Ｎｄ1-y-zＳｍyＢｉz）2+AＴｉ4+B
Ｏ12+3A/2+2B（式中、０．２≦ｘ≦０．４、０≦ｙ≦
０．７、０．３２≦ｚ≦０．５、−０．２≦Ａ≦＋０．
５、−０．５≦Ｂ≦＋０．５、ただし０．３２≦ｙ＋ｚ
≦１）で表されるバリウム、鉛、ネオジム、サマリウ
ム、ビスマス、チタンおよび酸素からなる誘電体磁器組
成物に関する。前記組成式において、−０．２≦Ａ≦＋
０．３、−０．３≦Ｂ≦＋０．３が好ましく、特にＡ＝
０、Ｂ＝０であることが好ましい。 Means for Solving the Problems The present invention provides a composition represented by the following formula:
(Ba 1-x Pb x) (Nd 1-yz Sm y Bi z) 2 + A Ti 4 + B
O 12 + 3A / 2 + 2B (where 0.2 ≦ x ≦ 0.4, 0 ≦ y ≦
0.7, 0.32 ≦ z ≦ 0.5, −0.2 ≦ A ≦ + 0.
5, -0.5 ≦ B ≦ + 0.5, but 0.32 ≦ y + z
<1) a dielectric porcelain composition comprising barium, lead, neodymium, samarium, bismuth, titanium and oxygen. In the above composition formula, -0.2 ≦ A ≦ +
0.3, −0.3 ≦ B ≦ + 0.3 is preferable, and especially A =
It is preferable that 0 and B = 0.
【０００６】本発明によれば、ＢａＮｄ2 Ｔｉ4 Ｏ12構
造においてＢａの一部をＰｂで置換することによって、
誘電率を大きく、共振周波数の温度係数を小さくするこ
とができる。置換量が多くなりすぎると、Ｑ値が低下す
るので置換量ｘは上記の範囲に設定される。According to the present invention, by substituting a part of Ba with Pb in the BaNd 2 Ti 4 O 12 structure,
The dielectric constant can be increased and the temperature coefficient of the resonance frequency can be reduced. If the replacement amount is too large, the Q value decreases, so the replacement amount x is set in the above range.
【０００７】また、Ｎｄの一部または全部をＳｍで置換
することによって大きな誘電率を保持しながら、共振周
波数の温度変化を小さくできる。さらにＮｄの一部をＢ
ｉで置換することによってさらに誘電率を大きくでき、
共振周波数の温度変化を小さくできるが、Ｎｄの置換量
が多くなるとＱ値が低下するので置換量ｚは上記の範囲
に設定される。Further, by replacing part or all of Nd with Sm, it is possible to reduce the temperature change of the resonance frequency while maintaining a large dielectric constant. Part of Nd is B
Substitution with i can further increase the dielectric constant,
Although the temperature change of the resonance frequency can be reduced, the Q value decreases as the replacement amount of Nd increases, so the replacement amount z is set in the above range.
【０００８】さらに、組成式、（Ｂａ1-xＰｂx）（Ｎｄ
1-y-zＳｍyＢｉz）2+AＴｉ4+BＯ12+3A/2+2Bにおいて、
−０．２≦Ａ≦＋０．５、−０．５≦Ｂ≦＋０．５の範
囲からはずれると、ＢａＮｄ2Ｔｉ4Ｏ12基本構造以外の
異相を形成しやすくなり、誘電率、共振周波数の温度係
数、Ｑ値のいずれか一つ、あるいは二つ以上の特性が低
下する。またこの範囲からはずれるとＰｂやＢｉなどが
焼成時に離脱しやすくなり、また、その離脱量も安定せ
ず電気的特性のばらつきを生じやすくなり、好ましくな
い。なお、Ａ＝０、Ｂ＝０のとき、すなわちＢａＮｄ2
Ｔｉ4Ｏ12構造において良好な特性が得られる。Further, the composition formula (Ba 1-x Pb x ) (Nd
In 1-yz Sm y Bi z) 2 + A Ti 4 + B O 12 + 3A / 2 + 2B,
If it is out of the range of −0.2 ≦ A ≦ + 0.5 and −0.5 ≦ B ≦ + 0.5, it becomes easy to form a different phase other than the basic structure of BaNd 2 Ti 4 O 12 , and the dielectric constant and resonance frequency Either one of the temperature coefficient and the Q value, or two or more characteristics deteriorate. Further, if it is out of this range, Pb, Bi, and the like are easily released during firing, and the amount of the release is not stable, and the electrical characteristics are likely to vary, which is not preferable. When A = 0 and B = 0, that is, BaNd 2
Good characteristics are obtained in the Ti 4 O 12 structure.
【０００９】本発明による誘電体磁器組成物は、バリウ
ム、鉛、ネオジム、サマリウム、ビスマスおよびチタン
の炭酸塩、酸化物などの仮焼・焼成により酸化物となる
ような出発原料を混合して仮焼した後、成形、焼成して
焼結させる方法で製造することができる。The dielectric porcelain composition according to the present invention is prepared by mixing starting materials such as barium, lead, neodymium, samarium, bismuth and titanium carbonates and oxides, which become oxides by calcining and firing. After baking, it can be manufactured by a method of molding, baking and sintering.
【００１０】まず、炭酸バリウム、酸化鉛、酸化ネオジ
ム、酸化サマリウム、酸化ビスマスおよび酸化チタンを
各所定量ずつ水、アルコール等の溶媒と共に湿式混合す
る。続いて、水、アルコール等を除去した後、粉砕し、
酸素含有ガス雰囲気（例えば空気雰囲気）下に９００〜
１１００℃で約１〜５時間程度仮焼する。これによって
形成された仮焼物を湿式あるいは乾式で粉砕した後、ポ
リビニルアルコールの如き有機バインダを加え、乾燥
後、加圧成形（圧力１００〜１０００ｋｇ／ｃｍ 2 程
度）する。成形方法としては、一軸加圧成形の他、ＨＩ
Ｐ、ドクター成形、鋳込み成形などでもよい。得られた
成形体を空気の如き酸素含有ガス雰囲気下に１２００〜
１４００℃で焼成すれば、上記誘電体磁器組成物が得ら
れる。First, barium carbonate, lead oxide, neodymium oxide
Samarium oxide, bismuth oxide and titanium oxide
Wet-mix each predetermined amount with a solvent such as water or alcohol.
You. Then, after removing water, alcohol, etc., pulverize,
900 ~ under an oxygen-containing gas atmosphere (for example, air atmosphere)
Calcinate at 1100 ° C for about 1 to 5 hours. by this
After crushing the formed calcined product by wet or dry method,
Add an organic binder such as vinyl alcohol and dry
After that, pressure molding (pressure 100 to 1000 kg / cm TwoAbout
Degree). Molding methods include uniaxial pressure molding, HI
P, doctor molding, cast molding and the like may be used. Got
The molded body was placed in an atmosphere containing oxygen such as air at 1200 to 1200
By firing at 1400 ° C., the above dielectric ceramic composition is obtained.
It is.
【００１１】こうして得られた誘電体磁器組成物は、そ
のまま又は必要に応じて適当な形状およびサイズに加工
することにより、誘電体共振器、マイクロ波ＩＣ用誘電
体基板、誘電体調整棒などの材料として利用することが
でき、特にＭＨｚ〜ＧＨｚ帯で使用される場合に優れた
効果が奏される。The thus obtained dielectric porcelain composition can be used as it is or, if necessary, processed into an appropriate shape and size to obtain a dielectric resonator, a microwave IC dielectric substrate, a dielectric adjustment rod, and the like. It can be used as a material, and exhibits an excellent effect particularly when used in the MHz to GHz band.
【００１２】[0012]
【実施例】以下に実施例および比較例を示し、本発明を
更に具体的に説明する。 実施例１ 炭酸バリウム粉末（ＢａＣＯ3 ）０．０８０モル、酸化
鉛粉末（ＰｂＯ）０．０２０モル、酸化ネオジム粉末
（Ｎｄ2 Ｏ3 ）０．０６８モル、酸化ビスマス粉末（Ｂ
ｉ2 Ｏ3 ）０．０３２モル、および酸化チタン粉末（Ｔ
ｉＯ2 ）０．４００モルをエタノールと共にボールミル
に入れ、１２時間湿式混合した。溶媒のエタノールを蒸
発させ、らい潰機で１時間粉砕した。粉砕物は空気雰囲
気下に１０００℃で仮焼した後、再びらい潰機で１時間
粉砕した。この粉砕物に適量のポリビニルアルコール溶
液を加えて乾燥後、直径約９mm、厚さ４mmのペレットに
成形し、空気雰囲気下に１２９０℃で２時間焼成、焼結
して本実施例の誘電体磁器組成物（Ｂａ0.8 Ｐｂ0.2 ）
（Ｎｄ0.68Ｂｉ0.32）2 Ｔｉ4 Ｏ12を得た。こうして得
られた磁器組成物を直径約７mm、厚さ約２mmのペレット
に加工した後、誘電共振法によって測定し、共振周波数
（４〜５ＧＨｚ）における無負荷Ｑおよび比誘電率εr
を求めた。また、共振周波数の温度依存性については、
０℃から５０℃の範囲で測定し、温度係数τf を求め
た。その結果を表１および表２に示す。The present invention will be described more specifically with reference to the following Examples and Comparative Examples. Example 1 Barium carbonate powder (BaCO 3 ) 0.080 mol, lead oxide powder (PbO) 0.020 mol, neodymium oxide powder (Nd 2 O 3 ) 0.068 mol, bismuth oxide powder (B
i 2 O 3) 0.032 mol, and titanium oxide powder (T
0.400 mol of iO 2 ) was placed in a ball mill together with ethanol and wet-mixed for 12 hours. Ethanol as a solvent was evaporated, and the mixture was pulverized for 1 hour with a crusher. The pulverized material was calcined at 1000 ° C. in an air atmosphere, and then pulverized again with a crusher for 1 hour. An appropriate amount of a polyvinyl alcohol solution is added to the pulverized product, dried, formed into pellets having a diameter of about 9 mm and a thickness of 4 mm, and fired and sintered at 1290 ° C. for 2 hours in an air atmosphere to obtain a dielectric ceramic of this embodiment. Composition (Ba 0.8 Pb 0.2 )
(Nd 0.68 Bi 0.32 ) 2 Ti 4 O 12 was obtained. The thus obtained porcelain composition was processed into a pellet having a diameter of about 7 mm and a thickness of about 2 mm, and then measured by a dielectric resonance method. The unloaded Q and the relative permittivity ε r at a resonance frequency (4 to 5 GHz) were obtained.
I asked. Regarding the temperature dependence of the resonance frequency,
The temperature was measured in the range of 0 ° C. to 50 ° C., and the temperature coefficient τ f was determined. The results are shown in Tables 1 and 2.
【００１３】実施例２〜１５および比較例１ 炭酸バリウム粉末（ＢａＣＯ3）、酸化鉛粉末（Ｐｂ
Ｏ）、酸化ネオジム粉末（Ｎｄ2Ｏ3）、酸化サマリウム
粉末（Ｓｍ2Ｏ3）、酸化ビスマス粉末（Ｂｉ2Ｏ3）、お
よび酸化チタン粉末（ＴｉＯ2）原料の仕込比、および
焼成温度を１２５０〜１３５０℃にかえた他は、実施例
１と同様にして誘電体磁器組成物を製造し、特性を測定
した。その結果を表１および表２に示す。Examples 2 to 15 and Comparative Example 1 Barium carbonate powder (BaCO 3 ), lead oxide powder (Pb
O), neodymium oxide powder (Nd 2 O 3 ), samarium oxide powder (Sm 2 O 3 ), bismuth oxide powder (Bi 2 O 3 ), and titanium oxide powder (TiO 2 ). Except having changed to 1250-1350 degreeC, it carried out similarly to Example 1, manufactured the dielectric ceramic composition, and measured the characteristic. The results are shown in Tables 1 and 2.
【００１４】比較例２ 炭酸バリウム粉末（ＢａＣＯ3）、酸化ネオジム粉末
（Ｎｄ2Ｏ3）、および酸化チタン粉末（ＴｉＯ2）を表
３に示すようなモル比になるようにし、焼成温度を１３
５０℃にかえた他は実施例１と同様にして誘電体磁器組
成物を製造し、物性を測定した。その結果を表３および
表４に示す。Comparative Example 2 Barium carbonate powder (BaCO 3 ), neodymium oxide powder (Nd 2 O 3 ), and titanium oxide powder (TiO 2 ) were adjusted to have a molar ratio as shown in Table 3, and the firing temperature was 13
A dielectric ceramic composition was manufactured in the same manner as in Example 1 except that the temperature was changed to 50 ° C., and the physical properties were measured. The results are shown in Tables 3 and 4.
【００１５】比較例３〜１３ 炭酸バリウム粉末（ＢａＣＯ3）、酸化鉛粉末（Ｐｂ
Ｏ）、酸化ネオジム粉末（Ｎｄ2Ｏ3）、酸化サマリウム
粉末（Ｓｍ2Ｏ3）、酸化ビスマス粉末（Ｂｉ2Ｏ3）、お
よび酸化チタン粉末（ＴｉＯ2）の原料仕込比、および
焼成温度を１２５０〜１３５０℃にかえた他は実施例１
と同様にして誘電体磁器組成物を製造し、物性を測定し
た。その結果を表３および表４に示す。Comparative Examples 3 to 13 Barium carbonate powder (BaCO 3 ), lead oxide powder (Pb
O), neodymium oxide powder (Nd 2 O 3 ), samarium oxide powder (Sm 2 O 3 ), bismuth oxide powder (Bi 2 O 3 ), and titanium oxide powder (TiO 2 ). Example 1 except that the temperature was changed to 1250 to 1350 ° C.
A dielectric porcelain composition was manufactured in the same manner as described above, and the physical properties were measured. The results are shown in Tables 3 and 4.
【００１６】[0016]
【表１】 [Table 1]
【００１７】[0017]
【表２】 [Table 2]
【００１８】[0018]
【表３】 [Table 3]
【００１９】[0019]
【表４】 [Table 4]
【００２０】[0020]
【発明の効果】本発明の誘電体磁器組成物は、特に高誘
電率で、無負荷Ｑが大きく、共振周波数の温度変化が小
さく、誘電体共振器材料、特にＭＨｚからＧＨｚ帯で使
用される共振器材料として好適である。また、本発明の
誘電体磁器組成物は、誘電体共振器材料の他に、例えば
マイクロ波ＩＣ用誘電体基板、誘電体調整棒等にも適用
できる。Industrial Applicability The dielectric ceramic composition of the present invention has a particularly high dielectric constant, a large unloaded Q, a small change in resonance frequency with temperature, and is used in a dielectric resonator material, especially in the MHz to GHz band. It is suitable as a resonator material. Further, the dielectric ceramic composition of the present invention can be applied to, for example, a dielectric substrate for microwave IC, a dielectric adjustment rod, and the like, in addition to the dielectric resonator material.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭61−8806（ＪＰ，Ａ) 特開 昭62−78154（ＪＰ，Ａ) 特開 昭56−82501（ＪＰ，Ａ) 特開 平６−139820（ＪＰ，Ａ) 特開 平６−333425（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) H01B 3/12 303 C04B 35/46 H01P 7/10 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-61-8806 (JP, A) JP-A-62-78154 (JP, A) JP-A-56-8501 (JP, A) JP-A-6-78501 139820 (JP, A) JP-A-6-333425 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) H01B 3/12 303 C04B 35/46 H01P 7/10
Claims (3)
ｍyＢｉz）2+AＴｉ4+BＯ12+3A/2+2B（式中、０．２≦ｘ
≦０．４、０≦ｙ≦０．７、０．３２≦ｚ≦０．５、−
０．２≦Ａ≦＋０．５、−０．５≦Ｂ≦＋０．５、ただ
し０．３２≦ｙ＋ｚ≦１）で表されるバリウム、鉛、ネ
オジム、サマリウム、ビスマス、チタンおよび酸素から
なる誘電体磁器組成物。1. The composition formula: (Ba 1-x Pb x ) (Nd 1-yz S
m y Bi z) 2 + A Ti 4 + B O 12 + 3A / 2 + 2B ( wherein, 0.2 ≦ x
≦ 0.4, 0 ≦ y ≦ 0.7, 0.32 ≦ z ≦ 0.5, −
Barium, lead, neodymium, samarium, bismuth, titanium represented by 0.2 ≦ A ≦ + 0.5, −0.5 ≦ B ≦ + 0.5, but 0.32 ≦ y + z ≦ 1) And a dielectric porcelain composition comprising oxygen.
０．３、−０．３≦Ｂ≦＋０．３である請求項１記載の2. The method according to claim 1, wherein 0.3 and -0.3≤B≤ + 0.3.
誘電体磁器組成物。Dielectric porcelain composition.
る請求項１記載の誘電体磁器組成物。The dielectric ceramic composition according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06399493A JP3243873B2 (en) | 1993-03-23 | 1993-03-23 | Dielectric porcelain composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP06399493A JP3243873B2 (en) | 1993-03-23 | 1993-03-23 | Dielectric porcelain composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06275125A JPH06275125A (en) | 1994-09-30 |
| JP3243873B2 true JP3243873B2 (en) | 2002-01-07 |
Family
ID=13245341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP06399493A Expired - Fee Related JP3243873B2 (en) | 1993-03-23 | 1993-03-23 | Dielectric porcelain composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3243873B2 (en) |
-
1993
- 1993-03-23 JP JP06399493A patent/JP3243873B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06275125A (en) | 1994-09-30 |
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