JPS63291306A - Manufacture of dielectric resonator material - Google Patents

Manufacture of dielectric resonator material

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Publication number
JPS63291306A
JPS63291306A JP62125373A JP12537387A JPS63291306A JP S63291306 A JPS63291306 A JP S63291306A JP 62125373 A JP62125373 A JP 62125373A JP 12537387 A JP12537387 A JP 12537387A JP S63291306 A JPS63291306 A JP S63291306A
Authority
JP
Japan
Prior art keywords
powder
calcined
component
solution
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP62125373A
Other languages
Japanese (ja)
Inventor
Nobuyuki Oya
信之 大矢
Toshiki Sawake
佐分 淑樹
Shinichi Shirasaki
信一 白崎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute for Research in Inorganic Material
Denso Corp
Original Assignee
National Institute for Research in Inorganic Material
NipponDenso Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by National Institute for Research in Inorganic Material, NipponDenso Co Ltd filed Critical National Institute for Research in Inorganic Material
Priority to JP62125373A priority Critical patent/JPS63291306A/en
Publication of JPS63291306A publication Critical patent/JPS63291306A/en
Pending legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Insulating Materials (AREA)

Abstract

PURPOSE:To secure such a material that is high in Q-value by using Ba(Zn1/3 Me2/3)O3 system ceramics (Me is either of Nb and Ta) for dielectric resonator material, forming this into modified material powder of a submicron grade, and mixing another material powder in this powder, then sintering it. CONSTITUTION:When Ba(Zn1/3Me2/3)O3 system ceramics are manufactured, it is performed by dividing the process into three parts ranging from first to third ones. At the first process, a mixed solution consisting of at least one component other than Ba and Ba solution and another mixed solution consisting of at least one component other than Zn and a Zn solution both are produced, setting these solutions down to a coprecipitating material, and after being dried up, it is calcined at a temperature of 700-1300 deg.C. Here, another component is a small amount of sintering assistant for which Zr, Mg, Sc, Hf, Th or the like are used. At the second process, powder of the previously obtained calcined material and the remaining component of the target perovskite composition are mixed together and calcined at a temperature of 700-1300 deg.C. At the next third process, the obtained calcined material is molded and completely baked at a temperature of 1200-1700 deg.C.

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明はマイクロ波用の誘電体共振器材料を製造する方
法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method of manufacturing a dielectric resonator material for microwaves.

[従来技術] マイクロ波用の誘電体共振器材料にはQ値の高いものが
要求されるが、衛星通信等においては特に高いQ値が要
求される。
[Prior Art] A dielectric resonator material for microwaves is required to have a high Q value, and a particularly high Q value is required for satellite communications and the like.

Q値の高い材料としてBa (Zn1,3 Me2/3
 )03系セラミックス(但しMeはNbおよびTaの
いずれか)がある。
Ba (Zn1,3 Me2/3
)03 series ceramics (where Me is either Nb or Ta).

このセラミック材料は一般に、B a C03、ZnO
1Nb205 、Ta2−05を主成分とする混合粉末
を焼成することにより製造されているが、難焼結性で、
期待される高誘電率およびQ値が得られていない。
This ceramic material is generally B a C03, ZnO
It is manufactured by firing a mixed powder whose main components are 1Nb205 and Ta2-05, but it is difficult to sinter,
The expected high dielectric constant and Q value were not obtained.

[本発明が解決しようとする問題点] 本発明は上記の実情に濫み、組織が緻密で、誘電率およ
びQ値が向上されたBa (Zn1/3 Me2/3)
03系セラミックスを製造する方法を提供することを目
的とするものである。
[Problems to be Solved by the Present Invention] The present invention overcomes the above-mentioned circumstances and solves the problem of Ba (Zn1/3 Me2/3) having a dense structure and improved dielectric constant and Q value.
The object of the present invention is to provide a method for manufacturing 03 series ceramics.

[問題点を解決するための手段] 本発明はBa(Zn1/3Me2/3)03系セラミツ
クを製造するのに際し、先ず第1工程としてBa以外の
少なくとも1成分とBaの溶液との混合液、およびZn
以外の少なくとも1成分とZnの溶液との混合液のいず
れかを作り、該混合液と沈澱形成液とを混合して共沈体
を形成し、乾燥後700℃〜1300℃で仮焼する。
[Means for Solving the Problems] In the present invention, when producing a Ba(Zn1/3Me2/3)03 ceramic, the first step is to prepare a mixture of at least one component other than Ba and a solution of Ba; and Zn
A mixed solution of at least one component other than Zn and a solution of Zn is prepared, and the mixed solution and a precipitate forming solution are mixed to form a coprecipitate, which is dried and then calcined at 700°C to 1300°C.

次に第2工程として上記により得られた仮焼物粉末と目
的とするペロブスカイト組成の残りの成分の粉末とを混
合して700℃〜1300℃で仮焼する。
Next, as a second step, the calcined powder obtained above and the powder of the remaining components of the desired perovskite composition are mixed and calcined at 700°C to 1300°C.

そして第3工程として、得られた仮焼物粉末を成形し、
1200℃〜1700℃で焼成する。
Then, as a third step, the obtained calcined powder is molded,
Calculate at 1200°C to 1700°C.

第1工程において、Ba溶液、Zn溶液、Nb溶液、タ
ンタル溶液としては、塩化バリウム、塩素酸バリウム、
過塩素酸バリウム、硝酸バリウム、酢酸バリウム、バリ
ウムエチレート、バリウムイソプロピレート、塩化亜鉛
、硫酸亜鉛、硝酸亜鉛、酢酸亜鉛、塩化ニオビウム、ニ
オブメトキシド、ニオビウムエチレート、塩化タンタル
、タンクルアルコキシド等の水溶液またはアルコール溶
液が用いられ得る。
In the first step, the Ba solution, Zn solution, Nb solution, and tantalum solution include barium chloride, barium chlorate,
Barium perchlorate, barium nitrate, barium acetate, barium ethylate, barium isopropylate, zinc chloride, zinc sulfate, zinc nitrate, zinc acetate, niobium chloride, niobium methoxide, niobium ethylate, tantalum chloride, tantalum alkoxide, etc. Aqueous or alcoholic solutions may be used.

沈澱形成液作製のための試薬としては、アンモニア、炭
酸アンモニウム、苛性アリカリ、しゆう酸、しゆう酸ア
ンモニウム、アミン、オキシン等の有機試薬が用いられ
得る。
As the reagent for preparing the precipitate-forming solution, organic reagents such as ammonia, ammonium carbonate, caustic alkali, oxalic acid, ammonium oxalate, amines, and oxins can be used.

Baと(Z n173 Ne2/3 )のモル比は1.
0ないし、それに近似した値とする。
The molar ratio of Ba and (Z n173 Ne2/3) is 1.
It should be 0 or a value close to it.

しかして第1工程において、共沈体を仮焼することによ
り分散性のよいサブミクロン級の微細粉末が得られる。
Thus, in the first step, by calcining the coprecipitate, a submicron-level fine powder with good dispersibility can be obtained.

第2工程では、上記仮焼物粉末と目的とするセラミック
組成を構成するに必要な残りの成分の粉末を混合し、仮
焼する。この残りの成分の粉末は、上記仮焼物粉末とほ
ぼ同じ粒度のものを用いることが望ましい。
In the second step, the above-mentioned calcined powder and the powders of the remaining components necessary to form the desired ceramic composition are mixed and calcined. It is desirable that the remaining component powder has approximately the same particle size as the calcined powder.

なお、製造の工程において微量の焼結助剤を添加するこ
とができる。焼結助剤としては、Zr、Mg、、Sc、
Hf、Th、W、Nb、Ta、Cr、Mo、Ti、Mn
、Fe、Co、Ni、、Cd、Afl 、Sn、As、
Bi、Zn、La、Ce、Sr等が用いられ得る。Ba
ZrO3、BaSnO3、S r T i 03 B 
a T i 02等も用いられ得る。
Note that a small amount of sintering aid can be added during the manufacturing process. Sintering aids include Zr, Mg, Sc,
Hf, Th, W, Nb, Ta, Cr, Mo, Ti, Mn
, Fe, Co, Ni, , Cd, Afl, Sn, As,
Bi, Zn, La, Ce, Sr, etc. may be used. Ba
ZrO3, BaSnO3, S r T i 03 B
a T i 02 etc. may also be used.

本発明の第1工程において、沈澱体の仮焼温度は700
℃より低いと凝集が生じ、1300℃を越えると粉末粒
子が粗大化する。
In the first step of the present invention, the calcination temperature of the precipitate is 700
If the temperature is lower than 1300°C, agglomeration occurs, and if the temperature exceeds 1300°C, the powder particles become coarse.

また第2工程において、仮焼温度は、固相反応がほぼま
たは完全に完了する最低温度以上で、顕著な粒子成長が
生じない最高温度範囲内であることが必要で、700℃
〜1300℃が望ましい。
In addition, in the second step, the calcination temperature must be at least the minimum temperature at which the solid phase reaction is almost or completely completed, and within the maximum temperature range at which significant particle growth does not occur, and is 700°C.
~1300°C is desirable.

第3工程における焼成温度は、1200℃より低いと全
体の焼結が不充分であり、1700℃を越えると粒子が
粗大化したり、構成成分の揮発が起きる。
If the firing temperature in the third step is lower than 1200°C, the entire sintering will be insufficient, and if it exceeds 1700°C, the particles will become coarse or the constituent components will volatilize.

[作用効果] しかして本発明では、第1工程で極めて分散性のよいサ
ブミクロン級の変成原料粉末を得、これと他の原料粉末
を混合して目的とする組成物原料となし、これを焼成す
ることで、緻密で、誘電率およびQ値の高いB a (
Z n 173 M e 2/3 > 03系セラミッ
クスを得ることができ、誘電体共振器材料として好適に
使用することができる。
[Operation and Effect] According to the present invention, a submicron grade modified raw material powder with extremely good dispersibility is obtained in the first step, and this is mixed with other raw material powders to obtain the desired composition raw material. By firing, B a (
Z n 173 M e 2/3 > 03 series ceramics can be obtained and suitably used as a dielectric resonator material.

[実施例] 塩化バリウム水溶液(1、641/1Tloρ 濃度)
800CCと、塩化亜鉛水溶液(1、8,11/mo、
ll濃度)900ccLを混合した。この混合水溶液を
、6N−アンモニア水1g中にこれを攪拌し2+ つつ徐々に添加して、Ba、  とZn2+ の水酸化
物共沈体を得た。これを洗浄、乾燥した後、1100℃
で仮焼してBaZnO2粉末を得た。
[Example] Barium chloride aqueous solution (1,641/1Tloρ concentration)
800CC and zinc chloride aqueous solution (1, 8, 11/mo,
11 concentration) was mixed with 900 ccL. This mixed aqueous solution was gradually added to 1 g of 6N ammonia water while stirring to obtain a hydroxide coprecipitate of Ba and Zn. After washing and drying this, 1100℃
The powder was calcined to obtain BaZnO2 powder.

上記により得られた粉末10gと、市販のBaCO3粉
末16.816g (0,0852moIJ)、Nb2
O5粉末11.324g (0,0426m0」)とを
、ボールミルで一昼夜混合した後、1000℃で1時間
仮焼してBa (Zn1/3 Nb2/3 ) 03粉
末を作成した。平均粒径は0.4μmであった。
10 g of the powder obtained above, 16.816 g (0,0852 moIJ) of commercially available BaCO3 powder, and Nb2
11.324 g (0,0426 m0'') of O5 powder were mixed in a ball mill overnight and then calcined at 1000° C. for 1 hour to create Ba (Zn1/3 Nb2/3) 03 powder. The average particle size was 0.4 μm.

得られた粉末を1t/a11で成形したダブレットを大
気中で、1400℃で2時間焼成しな。
A doublet formed by molding the obtained powder at 1 t/a11 was fired at 1400° C. for 2 hours in the air.

得られたセラミックス焼結体の密度、9GHzにおける
誘電率、Q値を下表に示す。
The density, dielectric constant at 9 GHz, and Q value of the obtained ceramic sintered body are shown in the table below.

[比較例] 市販のBaCO3、ZnO5Nb205粉末をBa(Z
n1/3Nb2/3)03の組成となるように、B a
 CO3を25.224g (0,1278moρ>、
ZnOを3.467g <0.0426m ow! )
 、N b205を11.324g <0.0426m
oj! )配合し、ボールミルで一昼夜混合した後12
00℃で1時間仮焼した。仮焼粉末の平均粒径は約1.
2μmであった。
[Comparative example] Commercially available BaCO3, ZnO5Nb205 powder was converted into Ba(Z
B a so that the composition becomes n1/3Nb2/3)03
25.224g of CO3 (0,1278moρ>,
3.467g of ZnO <0.0426m ow! )
, N b205 11.324g <0.0426m
oj! ) and mixed in a ball mill for a day and night 12
It was calcined at 00°C for 1 hour. The average particle size of the calcined powder is approximately 1.
It was 2 μm.

この粉末をIt/aaで成形し、上記実施例と同じ条件
下で焼成した。
This powder was molded to It/aa and fired under the same conditions as in the above example.

得られたセラミックス焼結体の密度、誘電率、Q値を下
表に併記する。
The density, dielectric constant, and Q value of the obtained ceramic sintered body are also listed in the table below.

なお、MeとしてTaを用いた場合も、上記とほぼ同様
の結果が得られた。
Note that almost the same results as above were obtained when Ta was used as Me.

このように本発明によるときは、従来法によるよりも緻
密で、高誘電率であり、特にQ値が格段に高いBa (
Zn173 Nb2/3 )03系セラミックスを得る
ことができる。そして本発明で得られたセラミックスは
高いQ値が要求される誘電体共振器材料として好適に用
いられる。
As described above, when using the present invention, Ba (
Zn173 Nb2/3 )03 series ceramics can be obtained. The ceramic obtained according to the present invention can be suitably used as a dielectric resonator material that requires a high Q value.

Claims (1)

【特許請求の範囲】 誘電体共振器材料用のBa(Zn_1_/_3Me_2
_/_3)O_3系セラミックス(但しMeはNbおよ
びTaのいずれか)を製造する方法であって、 (1)Ba以外の少なくとも1成分とBaの溶液との混
合液、およびZn以外の少なくとも1成分とZnの溶液
との混合液のいずれかを作り、該混合液と沈澱形成液と
を混合して共沈体を形成し、乾燥後700℃〜1300
℃で仮焼する第1工程、(2)得られた仮焼物粉末と、
目的とする組成の残りの成分の粉末を混合して700℃
〜1300℃で焼成する工程、 (3)得られた仮焼物粉末を成形して1200℃〜17
00℃で焼成する工程、 とよりなることを特徴とする誘電体共振器材料の製造方
法。
[Claims] Ba(Zn_1_/_3Me_2) for dielectric resonator material
_/_3) A method for producing O_3-based ceramics (where Me is either Nb or Ta), comprising: (1) a mixture of at least one component other than Ba and a solution of Ba; and at least one component other than Zn; A mixture of the components and a solution of Zn is prepared, the mixture and a precipitate forming liquid are mixed to form a coprecipitate, and after drying, the mixture is heated at 700°C to 1300°C.
A first step of calcining at °C, (2) the obtained calcined powder,
Mix the powders of the remaining ingredients of the desired composition and heat to 700°C.
a step of firing at ~1300°C, (3) molding the obtained calcined powder to 1200°C ~17
1. A method for manufacturing a dielectric resonator material, comprising: a step of firing at 00°C.
JP62125373A 1987-05-22 1987-05-22 Manufacture of dielectric resonator material Pending JPS63291306A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62125373A JPS63291306A (en) 1987-05-22 1987-05-22 Manufacture of dielectric resonator material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62125373A JPS63291306A (en) 1987-05-22 1987-05-22 Manufacture of dielectric resonator material

Publications (1)

Publication Number Publication Date
JPS63291306A true JPS63291306A (en) 1988-11-29

Family

ID=14908525

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62125373A Pending JPS63291306A (en) 1987-05-22 1987-05-22 Manufacture of dielectric resonator material

Country Status (1)

Country Link
JP (1) JPS63291306A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004189589A (en) * 2002-11-25 2004-07-08 Ngk Spark Plug Co Ltd Dielectric ceramic composition and dielectric resonator using the same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61269805A (en) * 1985-05-23 1986-11-29 松下電器産業株式会社 Manufacture of dielectric ceramic for microwave

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61269805A (en) * 1985-05-23 1986-11-29 松下電器産業株式会社 Manufacture of dielectric ceramic for microwave

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004189589A (en) * 2002-11-25 2004-07-08 Ngk Spark Plug Co Ltd Dielectric ceramic composition and dielectric resonator using the same
JP4494756B2 (en) * 2002-11-25 2010-06-30 日本特殊陶業株式会社 Dielectric ceramic composition and dielectric resonator using the same

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