JP4100929B2 - Dielectric ceramic composition and manufacturing method thereof - Google Patents
Dielectric ceramic composition and manufacturing method thereof Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、誘電体磁器組成物に係り、特に、鉛（Ｐｂ）を含有せずに、高周波特性が優れ、且つ比較的低温で焼成が可能な誘電体磁器組成物及びその製造方法に関する。
【０００２】
【従来の技術】
近年、銀（Ａｇ）電極と同時焼成することができる誘電体磁器組成物が求められている。例えば、セラミック・グリーンシートと銀（Ａｇ）電極の積層体を８９０〜９２０℃の温度範囲にて同時焼成できる誘電体磁器組成物である。一般式ＣａＴｉＯ３で表されるペロブスカイト型結晶相を主結晶とする材料は、１３００〜１４００℃の高温で焼成され、緻密であり、比誘電率εｒ＝１７０，Ｑ＝１８００（周波数＝２ＧＨｚにおいて）と高周波帯域で優れた特性が得られる。しかしながら、１３００℃以下の焼成温度では緻密化せず、その特性が劣るという問題がある。
【０００３】
８９０〜９２０℃程度の比較的低温で焼成するためには、焼成助剤を多用することが必要である。しかし、これは、その特性を大きく変化させて高周波帯域において優れた高誘電率、高Ｑ値の特性が得られなくなってしまう。従来の材料でも、９００℃程度で焼成され高誘電率、高Ｑ値の特性を満足するものがある。しかし、それは、鉛（Ｐｂ）を含んだものしか確認されていない。
【０００４】
そこで、人体に有害な鉛（Ｐｂ）を含んでいない誘電体磁器組成物の開発が、多くのユーザから要求されている。また、環境保全の立場から各方面の関係者からもその開発が待たれている。
【０００５】
【発明が解決しようとする課題】
本発明は上述した事情に鑑みて為されたもので、鉛（Ｐｂ）を含有せずに、高周波数帯域で優れた誘電特性を有し、比較的低温で銀電極などと同時に加熱焼成が可能な緻密な誘電体磁器組成物およびその製造方法を提供することを目的とする。
【０００６】
【課題を解決するための手段】
上記の課題を解決するために、本発明の誘電体磁器組成物は、一般式 ＣａＴｉＯ３ で表されるペロブスカイト型結晶相を主結晶とする材料の１００重量部に対して、ガラスをｘ重量部（２.５≦ｘ≦１５.０）、Ｂ２Ｏ３ をｙ重量部（１.０≦ｙ≦１５.０）を混合して、８９０〜９２０℃で加熱焼成したことを特徴とする。
【０００７】
前記ガラスは、組成式＝ａＧｅＯ２-ｂＢａＯ-ｃＢｉ２Ｏ３で表され、
ここに、 ａ、ｂ、ｃは、モル比で、０.４≦ａ≦０.６、０.１≦ｂ≦０.５、０.１≦ｃ≦０.５、但し、ａ＋ｂ＋ｃ＝１の範囲内にあることを特徴としている。
【０００８】
本発明者は、少量の添加で加熱焼成を促進させることのできるガラスを開発し、それとＢ２Ｏ３を併用することで、比誘電率εｒ＝８０〜１３０，Ｑ＝１００〜３００（周波数＝４.５〜５.８ＧＨｚにおいて）の特性を有する緻密な誘電体磁器組成物を８９０〜９２０℃の範囲で加熱焼成することができることを見いだした。この緻密な構造により、セラミックの強度が向上し、比誘電率εｒ，Ｑ値の好ましい特性が得られ、バラツキが減少して安定化するという性能面の改良がある。誘電体磁器組成物と銀（Ａｇ）電極の同時に加熱焼成ができることにより、製造工程の短縮と製造コストの削減が達成できるという製造上のメリットがある。また、この誘電体磁器組成物は、人体に有害な鉛（Ｐｂ）を含んでいない点が環境保全から観たメリットである。
【０００９】
【発明の実施の形態】
以下、本発明に係る誘電体磁器組成物の実施形態について、表１、図１乃至図３を参照してさらに詳しく説明する。
【００１０】
表１は、２７件の試料についての組成と諸特性のデータをまとめたものである。試料の作製に当たり、ガラスとＢ２Ｏ３の添加率を変えること、ガラスの組成を変えること、焼結助剤としてガラスとＢ２Ｏ３の添加の有無、及び加熱焼成温度などを考慮した。ガラスの組成については、図１に示される。
【００１１】
(実施例)
本発明の出発原料にＣａＣＯ３粉末とＴｉＯ２粉末を用い、ＣａとＴｉのモル比が０.９５（Ｃａ／Ｔｉ＝０.９５）になるように所定量秤量する。この秤量原料をボールミルで１８時間湿式混合した後、乾燥させて混合粉末を得る。この混合粉末を大気中において１２００℃で仮焼した後、ボールミルで２４時間湿式粉砕して平均粒径０.５μｍのＣａＴｉＯ３粉末を得る。Ｘ線回折パターンにより、その粉末がＣａＴｉＯ３であることを同定した。（図２を参照。）
【００１２】
次に、ガラスを作製した。出発原料にＧｅＯ２粉末とＢａＣＯ３粉末とＢｉ２Ｏ３ 粉末を用い、表１に示した試料組成になるように秤量する。この秤量原料を乳鉢・乳棒で１０分間乾式混合する。混合した粉末をアルミナ質るつぼに入れ、１０００℃の炉内で３０分溶融させる。３０分後、炉からるつぼを取り出し、室内で放冷してガラスを固化させる。るつぼからガラスだけを取り出し、自動乳鉢機で１時間粗粉砕する。粗粉砕したガラス粉末をボールミルで８時間湿式粉砕して平均粒径１μｍのガラス 粉末を得る。Ｘ線回折パターンにより、その粉末が非晶質ガラスであることを同定した。（図３を参照。）
【００１３】
ＣａＴｉＯ３粉末に表１の試料の組成になるようにガラス粉末とＢ２Ｏ３を秤量する。（Ｂ２Ｏ３は、Ｈ３ＢＯ３で秤量する）。それをボールミルで３時間湿式混合した後、乾燥させて混合粉を得る。この混合粉にバインダー水溶液を添加して造粒する。この造粒粉をφ（直径）１６.５mmの金型に詰めて、７５０kgf／cm２以下の一軸加圧する。さらにその成形体に対して冷間等方プレス（Cold isostatic press）を使って１０００kgf／cm２の力で２分間等方加圧し成形する。それを空気中において、８９０〜９２０℃の温度で２時間加熱焼成し、焼結体を得る。
【００１４】
両端短絡形誘電体共振器法を使って得られた焼結体の比誘電率εｒとＱの測定データを表１に示す。
【００１５】
表１の２７件にうち試料１５件、即ち、試料１〜７、試料９、試料１１、試料１３、試料１５，試料１８〜２１は、ａ，ｂ，ｃ，ｘ，ｙの値が本発明の範囲にある。即ち、一般式ＣａＴｉＯ３で表されるペロブスカイト型結晶相を主結晶とする材料１００重量部に対して、ガラスをｘ重量部（２.５≦ｘ≦１５.０）、Ｂ２Ｏ３をｙ重量部（１.０≦ｙ≦１５.０）を混合して加熱焼成したもので、前記ガラスは、組成式＝ａＧｅＯ２-ｂＢａＯ-ｃＢｉ２Ｏ３で表され、ここに、 ａ、ｂ、ｃは、モル比で、０.４≦ａ≦０.６、０.１≦ｂ≦０.５、０.１≦ｃ≦０.５、但し、ａ＋ｂ＋ｃ＝１の範囲内にある。
【００１６】
試料１〜３、は、加熱焼成温度が９０７℃であり、試料４〜７，９、１１、１３は、加熱焼成温度が９１７℃であり、試料１５は，８９１℃であり、試料１８〜２１は、加熱焼成温度が９１７℃である。これら試料１５件については、加熱焼成温度８９１〜９１７℃の範囲で緻密な構造を有する誘電体磁器組成物が得られている。比誘電率εｒについて、試料１９が最高値（εｒ＝１３０．１）を有し、試料３が最低値（εｒ＝８０.６）を有している。Ｑ値については、試料１が最高値（Ｑ＝２８７[周波数＝５.３９ＧＨｚにおいて]）を有し、試料１９が最低値(Ｑ＝１０２[周波数＝４.５３ＧＨｚにおいて]）を有している。試料１５件については、表１に示されているように焼結性、比誘電率、Ｑともに良好なデータが得られている。
【００１７】
(比較例)
試料８は、Ｂ２Ｏ３の添加率が下限値１.０重量部より少ないので９１７℃における加熱焼成では焼結が不十分で構造が緻密化しない誘電体磁器組成物となる。試料１０は、ガラスを１７.５重量部添加しているがＢ２Ｏ３の添加率が下限値１.０重量部より少ないので９１７℃における加熱焼成では焼結が不十分で構造が緻密化しない。試料１２と試料１４は、Ｂ２Ｏ３の添加率が上限値１５.０重量部を超えているので過焼結を起こし緻密な構造にならない。試料１７は、焼結温度が高すぎると過焼結を起こして試料全体に発泡した跡が残り緻密な構造にならない。試料２２は、ｂ＝０（＜０.１）であり、試料２４は、ｃ＝０（＜０.１）であり、試料２５は、ａ＝０.３（＜０.４）である。即ち、試料２２と試料２４と試料２５は、ガラスの組成が最適範囲外であるので、９１７℃における焼成では焼結が不十分となり緻密な構造とならない。試料２６と試料２７は、前記ガラスとＢ２Ｏ３の添加がない試料である。緻密な構造を得て、比誘電率εｒ≧１７０，Ｑ≧１８００の特性を得るには１３００℃の焼成温度が必要である。
【００１８】
表１は、２７件の試料について組成と諸特性のデータをまとめて示したものである。
【表１】
なお、本発明の誘電体磁器組成物は、上述の図示例にのみ限定されるものではなく、本発明の要旨を逸脱しない範囲内において種々変更を加え得ることは勿論である。
【００２０】
【発明の効果】
本発明の誘電体磁器組成物によれば、比誘電率εｒ＝８０〜１３０，Ｑ＝１００〜３００（周波数＝４.５〜５.８ＧＨｚにおいて）の特性を有する緻密な誘電体磁器組成物を８９０〜９２０℃の範囲で加熱焼成することができる。この緻密な構造により、セラミックの強度が向上し、比誘電率εｒ，Ｑ値のバラツキが減少して安定化する。また、誘電体磁器組成物と銀（Ａｇ）電極の同時焼成ができることにより、製造工程の短縮と製造コストの削減が達成できる。また、この誘電体磁器組成物は、人体に有害な鉛（Ｐｂ）を含んでいないので、環境保全上、有用である。
【図面の簡単な説明】
【図１】図１は、本発明のガラスの３元組成図である。
【図２】図２は、粉末がＣａＴｉＯ３であることを示すＸ線回折パターン図である。
【図３】図３は、粉末が非晶質ガラスであることを示すＸ線回折パターン図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a dielectric ceramic composition, and more particularly to a dielectric ceramic composition that does not contain lead (Pb), has excellent high-frequency characteristics, and can be fired at a relatively low temperature, and a method for manufacturing the same.
[0002]
[Prior art]
In recent years, there has been a demand for a dielectric ceramic composition that can be fired simultaneously with a silver (Ag) electrode. For example, it is a dielectric ceramic composition capable of simultaneously firing a laminate of a ceramic green sheet and a silver (Ag) electrode in a temperature range of 890 to 920 ° C. A material whose main crystal is a perovskite type crystal phase represented by the general formula CaTiO 3 is fired at a high temperature of 1300 to 1400 ° C. and dense, and has a relative dielectric constant εr = 170, Q = 1800 (at frequency = 2 GHz). Excellent characteristics can be obtained in the high frequency band. However, there is a problem that densification is not achieved at a firing temperature of 1300 ° C. or lower, and the characteristics are poor.
[0003]
In order to bake at a relatively low temperature of about 890 to 920 ° C., it is necessary to use a lot of baking aids. However, this greatly changes the characteristics, and an excellent high dielectric constant and high Q value characteristic cannot be obtained in the high frequency band. Some conventional materials are fired at about 900 ° C. and satisfy the characteristics of high dielectric constant and high Q value. However, only those containing lead (Pb) have been confirmed.
[0004]
Therefore, development of dielectric ceramic compositions that do not contain lead (Pb) that is harmful to the human body is required by many users. In addition, from the standpoint of environmental conservation, the development is also awaited from the various parties concerned.
[0005]
[Problems to be solved by the invention]
The present invention has been made in view of the above-described circumstances. It does not contain lead (Pb), has excellent dielectric properties in a high frequency band, and can be fired at the same time as a silver electrode at a relatively low temperature. It is an object to provide a dense dielectric ceramic composition and a method for producing the same.
[0006]
[Means for Solving the Problems]
In order to solve the above-mentioned problems, the dielectric ceramic composition of the present invention comprises x parts by weight of glass with respect to 100 parts by weight of a material having a perovskite crystal phase represented by the general formula CaTiO 3 as a main crystal. (2.5 ≦ x ≦ 15.0), B 2 O 3 and y parts by weight (1. 0 ≦ y ≦ 15.0 ) were mixed, characterized in that the firing at eight hundred ninety to nine hundred twenty ° C..
[0007]
The glass is represented by a composition formula = aGeO 2 -bBaO-cBi 2 O 3 ,
Here, a, b and c are molar ratios of 0.4 ≦ a ≦ 0.6, 0.1 ≦ b ≦ 0.5, 0.1 ≦ c ≦ 0.5, provided that a + b + c = 1. It is characterized by being within range.
[0008]
The present inventor has developed a glass capable of promoting heating and baking with a small amount of addition, and using it together with B 2 O 3 , the relative dielectric constant εr = 80 to 130, Q = 100 to 300 (frequency = It has been found that a dense dielectric ceramic composition having the characteristics of 4.5 to 5.8 GHz can be heated and fired in the range of 890 to 920 ° C. Due to this dense structure, the strength of the ceramic is improved, and preferable characteristics such as relative dielectric constant εr, Q value are obtained, and there is an improvement in performance such that variation is reduced and stabilization is achieved. Since the dielectric ceramic composition and the silver (Ag) electrode can be heated and fired at the same time, there is a manufacturing merit that the manufacturing process can be shortened and the manufacturing cost can be reduced. Moreover, this dielectric ceramic composition is advantageous from the viewpoint of environmental conservation in that it does not contain lead (Pb) harmful to the human body.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the dielectric ceramic composition according to the present invention will be described in more detail with reference to Table 1 and FIGS. 1 to 3.
[0010]
Table 1 summarizes the composition and characteristics data for 27 samples. In preparing the sample, the addition ratio of glass and B 2 O 3 was changed, the composition of the glass was changed, the presence or absence of addition of glass and B 2 O 3 as a sintering aid, and the firing temperature were considered. The composition of the glass is shown in FIG.
[0011]
(Example)
CaCO 3 powder and TiO 2 powder are used as starting materials of the present invention, and a predetermined amount is weighed so that the molar ratio of Ca to Ti is 0.95 (Ca / Ti = 0.95). This weighed raw material is wet mixed in a ball mill for 18 hours and then dried to obtain a mixed powder. This mixed powder is calcined at 1200 ° C. in the air and then wet-ground by a ball mill for 24 hours to obtain CaTiO 3 powder having an average particle size of 0.5 μm. The powder was identified as CaTiO 3 by the X-ray diffraction pattern. (See Figure 2)
[0012]
Next, glass was produced. Using GeO 2 powder, BaCO 3 powder, and Bi 2 O 3 powder as starting materials, the sample composition shown in Table 1 is weighed. This weighing material is dry mixed for 10 minutes with a mortar and pestle. The mixed powder is put into an alumina crucible and melted in a 1000 ° C. furnace for 30 minutes. After 30 minutes, the crucible is removed from the furnace and allowed to cool indoors to solidify the glass. Remove only the glass from the crucible and coarsely grind in an automatic mortar machine for 1 hour. The coarsely pulverized glass powder is wet pulverized for 8 hours by a ball mill to obtain glass powder having an average particle diameter of 1 μm. An X-ray diffraction pattern identified the powder as amorphous glass. (See Figure 3)
[0013]
The glass powder and B 2 O 3 are weighed so that the CaTiO 3 powder has the composition of the sample shown in Table 1. (B 2 O 3 is weighed with H 3 BO 3 ). It is wet mixed with a ball mill for 3 hours and then dried to obtain a mixed powder. An aqueous binder solution is added to the mixed powder and granulated. This granulated powder is packed in a mold having a φ (diameter) of 16.5 mm and uniaxially pressed at 750 kgf / cm 2 or less. Further, the molded body is subjected to isostatic pressing for 2 minutes with a force of 1000 kgf / cm 2 using a cold isostatic press. It is heated and fired in air at a temperature of 890 to 920 ° C. for 2 hours to obtain a sintered body.
[0014]
Table 1 shows measurement data of the relative permittivity εr and Q of the sintered body obtained by using the both-end short-circuited dielectric resonator method.
[0015]
Of the 27 samples in Table 1, 15 samples, ie, samples 1 to 7, sample 9, sample 11, sample 13, sample 15, and samples 18 to 21, have values of a, b, c, x, and y according to the present invention. It is in the range. That is, with respect to 100 parts by weight of a material having a perovskite type crystal phase represented by the general formula CaTiO 3 as a main crystal, x parts by weight of glass (2.5 ≦ x ≦ 15.0) and B 2 O 3 by y in which the firing was mixed parts by weight of (1. 0 ≦ y ≦ 15.0 ), the glass is expressed by a composition formula = aGeO 2 -bBaO-cBi 2 O 3, here, a, b, c is a molar ratio of 0.4.ltoreq.a.ltoreq.0.6, 0.1.ltoreq.b.ltoreq.0.5, 0.1.ltoreq.c.ltoreq.0.5, provided that a + b + c = 1.
[0016]
Samples 1 to 3 have a heating and firing temperature of 907 ° C., Samples 4 to 7, 9, 11, and 13 have a heating and firing temperature of 917 ° C., Sample 15 has 891 ° C., and Samples 18 to 21 Has a heating and baking temperature of 917 ° C. For these 15 samples, a dielectric ceramic composition having a dense structure at a heating and firing temperature of 891 to 917 ° C. has been obtained. Regarding the relative dielectric constant εr, the
[0017]
(Comparative example)
Sample 8 is a dielectric ceramic composition in which the sintering is insufficient and the structure is not densified by heating and baking at 917 ° C. because the addition ratio of B 2 O 3 is less than the lower limit of 1.0 part by weight. In sample 10, 17.5 parts by weight of glass was added, but the addition rate of B 2 O 3 was less than the lower limit of 1.0 part by weight. do not do. In Samples 12 and 14, the addition rate of B 2 O 3 exceeds the upper limit of 15.0 parts by weight, so oversintering occurs and a dense structure is not obtained. When the sintering temperature of the sample 17 is too high, oversintering is caused and a trace of foaming remains in the entire sample, so that a dense structure is not formed. Sample 22 has b = 0 (<0.1),
[0018]
Table 1 summarizes the composition and characteristics data for 27 samples.
[Table 1]
It should be noted that the dielectric ceramic composition of the present invention is not limited to the illustrated examples described above, and it is needless to say that various modifications can be made without departing from the gist of the present invention.
[0020]
【The invention's effect】
According to the dielectric ceramic composition of the present invention, a dense dielectric ceramic composition having characteristics of relative dielectric constant εr = 80 to 130, Q = 100 to 300 (at frequency = 4.5 to 5.8 GHz) is obtained. Heat baking can be performed in the range of 890 to 920 ° C. With this dense structure, the strength of the ceramic is improved, and variations in the relative permittivity εr and Q value are reduced and stabilized. In addition, since the dielectric ceramic composition and the silver (Ag) electrode can be fired simultaneously, the manufacturing process can be shortened and the manufacturing cost can be reduced. Moreover, since this dielectric ceramic composition does not contain lead (Pb) harmful to the human body, it is useful for environmental protection.
[Brief description of the drawings]
FIG. 1 is a ternary composition diagram of the glass of the present invention.
FIG. 2 is an X-ray diffraction pattern diagram showing that the powder is CaTiO 3 .
FIG. 3 is an X-ray diffraction pattern showing that the powder is amorphous glass.
Claims (4)
前記ガラスは、組成式＝ａＧｅＯ ２ - ｂＢａＯ - ｃＢｉ ２ Ｏ ３ で表され、ここに、 ａ、ｂ、ｃは、モル比で、
０ . ４≦ａ≦０ . ６、０ . １≦ｂ≦０ . ５、０ . １≦ｃ≦０ . ５、
但し、ａ＋ｂ＋ｃ＝１
の範囲内にあり、
加熱焼成する温度が、８９０〜９２０℃の範囲にあることを特徴とする誘電体磁器組成物。For 100 parts by weight of a material having a perovskite crystal phase represented by the general formula CaTiO 3 as the main crystal, x parts by weight of glass (2.5 ≦ x ≦ 15.0) and y parts by weight of B 2 O 3 Parts (1.0 ≦ y ≦ 15.0) mixed and heated and fired ,
The glass composition formula = aGeO 2 - bBaO - represented by CBI 2 O 3, here, a, b, c are, in a molar ratio,
0. 4 ≦ a ≦ 0. 6,0. 1 ≦ b ≦ 0. 5,0. 1 ≦ c ≦ 0. 5,
However, a + b + c = 1
In the range of
A dielectric ceramic composition characterized in that the temperature for heating and firing is in the range of 890 to 920 ° C.
ＣａＴｉＯ３粉末の１００重量部に対してガラス粉末をｘ重量部（２ . ５≦ｘ≦１５ . ０）とＢ２Ｏ３粉末をｙ重量部（１．０≦ｙ≦１５ . ０）とを秤量して、
前記ガラス粉末は、組成式＝ａＧｅＯ ２ - ｂＢａＯ - ｃＢｉ ２ Ｏ ３ で表され、ここに、ａ、ｂ、ｃは、モル比で、
０ . ４≦ａ≦０ . ６、０ . １≦ｂ≦０ . ５、０ . １≦ｃ≦０ . ５、
但し、ａ＋ｂ＋ｃ＝１
の範囲内にあり、
それらを湿式混合して、乾燥させて混合粉末を得て、該混合粉末にバインダー水溶液を添加し造粒して、該造粒粉末を金型に充填して一軸加圧で適当な大きさに仮成形して、さらに該仮成形体に対して等方加圧し成形して、該成形体を空気中において８９０〜９２０℃の範囲の温度で加熱焼成することを特徴とする誘電体磁器組成物の製造方法。A method for producing a dielectric ceramic composition having a perovskite crystal phase represented by a general formula CaTiO 3 as a main crystal,
CaTiO 3 x parts by weight of glass powder with respect to 100 parts by weight of the powder (2. 5 ≦ x ≦ 15 . 0) and B 2 O 3 powder y parts by weight (1.0 ≦ y ≦ 15. 0 ) and the Weigh and
The glass powder composition formula = aGeO 2 - bBaO - represented by CBI 2 O 3, here, a, b, c are, in a molar ratio,
0. 4 ≦ a ≦ 0. 6,0. 1 ≦ b ≦ 0. 5,0. 1 ≦ c ≦ 0. 5,
However, a + b + c = 1
In the range of
They are wet-mixed and dried to obtain a mixed powder, and an aqueous binder solution is added to the mixed powder and granulated. The granulated powder is filled in a mold and uniaxially pressed to an appropriate size. The dielectric ceramic composition is characterized in that it is temporarily molded, isotropically pressed against the temporary molded body and molded, and the molded body is heated and fired at a temperature in the range of 890 to 920 ° C. in air. Manufacturing method.
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