JP2617939B2 - Manufacturing method of dielectric resonator material - Google Patents
Manufacturing method of dielectric resonator materialInfo
- Publication number
- JP2617939B2 JP2617939B2 JP62132202A JP13220287A JP2617939B2 JP 2617939 B2 JP2617939 B2 JP 2617939B2 JP 62132202 A JP62132202 A JP 62132202A JP 13220287 A JP13220287 A JP 13220287A JP 2617939 B2 JP2617939 B2 JP 2617939B2
- Authority
- JP
- Japan
- Prior art keywords
- dielectric resonator
- solution
- resonator material
- manufacturing
- powder
- 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.)
- Expired - Lifetime
Links
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- Compositions Of Oxide Ceramics (AREA)
- Inorganic Insulating Materials (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は例えば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。The present invention relates to a method for producing a dielectric resonator material for microwaves, for example.
［従来の技術］ マイクロ波用の誘電体共振器材料にはＱ値の高いもの
が望まれている。このような材料としてBaTi4O9,Ba2Ti9
O2oなどのセラミックスがある。[Related Art] A dielectric resonator material for microwaves having a high Q value is desired. BaTi 4 O 9 , Ba 2 Ti 9
There are ceramics such as O 2o .
ところで、従来は、このセラミックスを乾式法で製造
していた。しかし、この方法では得られるセラミックス
の誘電率εｒは40程度、Ｑは8000程度（4GHz）が限界で
あり、これ以上のＱ値の向上は望めなかった。By the way, conventionally, this ceramic was manufactured by a dry method. However, in this method, the dielectric constant εr of the obtained ceramic is limited to about 40 and the Q is limited to about 8000 (4 GHz), and further improvement of the Q value cannot be expected.
［発明が解決しようとする問題点］ 本発明は上記の実情に鑑みてなされたもので、比較的
低い温度で焼成が可能で、かつ組織が緻密で、Ｑ値の優
れたセラミックスを製造することが可能な誘導体共振器
材料の製造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 Invention] The present invention has been made in view of the above circumstances, and is intended to produce ceramics that can be fired at a relatively low temperature, have a fine structure, and have an excellent Q value. It is an object of the present invention to provide a method for manufacturing a dielectric resonator material that can perform the above method.
［問題点を解決するための手段］ 本発明は（１−ｘ）BaO−xTiO2系のセラミックス（但
し、0.75≦ｘ≦0.9）を製造するに際し、先ず第１工程
として、Ba溶液（水溶液又はアルコール溶液）とTi溶液
（水溶液又はアルコール溶液）をそれぞれ適量作り、こ
れと沈殿形成液とを混合して共沈体を形成し、乾燥後60
0℃〜1100℃で仮焼する。[Means for Solving the Problems] In the present invention, when producing (1-x) BaO—xTiO 2 ceramics (0.75 ≦ x ≦ 0.9), first, as a first step, a Ba solution (aqueous solution or An alcohol solution) and a Ti solution (aqueous solution or alcohol solution) are respectively prepared in appropriate amounts, and this is mixed with a precipitate forming solution to form a coprecipitate.
Calcinate at 0 ° C to 1100 ° C.
次に、第２工程として、この仮焼物と目的とする組成
物の残りの構成成分の化合物とを混合して800℃〜1200
℃で仮焼する。Next, as a second step, the calcined product and a compound of the remaining constituent components of the target composition are mixed and mixed at 800 ° C to 1200 ° C.
Calcinate at ℃.
そして、第３工程として、得られた仮焼粉末を成形
し、1100℃〜1500℃で焼成する。Then, as a third step, the obtained calcined powder is molded and fired at 1100 ° C to 1500 ° C.
MnO,MnO2,Cr2O3,CoO,ZiO2,NiO,SnO2,MgO,Ta2O5,Nb
2O5,WO3,La2O3,Sn2O3,Nd2O3,Al2O3,SiO2等の添加物は第
1,第２の工程で添加すればよい。MnO, MnO 2 , Cr 2 O 3 , CoO, ZiO 2 , NiO, SnO 2 , MgO, Ta 2 O 5 , Nb
Additives such as 2 O 5 , WO 3 , La 2 O 3 , Sn 2 O 3 , Nd 2 O 3 , Al 2 O 3 , SiO 2
1, It may be added in the second step.
仮焼温度については600℃附近より目的とする組成物
の結晶が生成され、1200℃以上においては、仮焼粉末粒
径が大きくなり、焼成特性を著しく悪化させる。As for the calcination temperature, crystals of the target composition are formed at around 600 ° C., and at 1200 ° C. or more, the calcined powder particle size becomes large and the calcination characteristics are remarkably deteriorated.
Ba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などが挙げら
れる。また、Ti溶液としては、四臭化チタン，四塩化チ
タン，テトラメトキシチタン，テトラエトキシチタン，
テトラプロポキシチタン，テトラブトキシチタンなどが
挙げられる。Examples of the Ba solution include barium chloride, barium chlorate, barium perchlorate, barium nitrate, barium acetate, barium ethylate, and barium isopropylate. As the Ti solution, titanium tetrabromide, titanium tetrachloride, tetramethoxytitanium, tetraethoxytitanium,
Tetrapropoxytitanium, tetrabutoxytitanium and the like can be mentioned.
第２の工程で添加する化合物はサブミクロン級の粒子
の粉末とする。The compound added in the second step is a powder of submicron class particles.
沈殿形成液作成のための試薬としては、例えばアンモ
ニア，炭酸アンモニウム，苛性アルカリ，しゅう酸，し
ゅう酸アンモニウムやアミン，オキシン等の有機試薬が
挙げられる。Examples of the reagent for preparing the precipitate forming liquid include organic reagents such as ammonia, ammonium carbonate, caustic alkali, oxalic acid, ammonium oxalate, amine and oxine.
［作用効果］ しかして、本発明では、分散性の良いサブミクロン級
のBaTi4O9（BaO・4TiO2）,Ba2Ti9O2o（2BaO・9TiO2）系
原料粉末を作成し、この粉末を用いて単なる乾式法によ
って混合して本来希望する組成物原料とすることで、比
較的低い温度で焼成が可能で、組織が緻密で、Ｑ値の優
れた（１−ｘ）BaO−xTiO2系のセラミツクスを得ること
ができる。[Effects] According to the present invention, a submicron-class BaTi 4 O 9 (BaO.4TiO 2 ), Ba 2 Ti 9 O 2o (2BaO.9TiO 2 ) -based raw material powder having good dispersibility is prepared. By using a powder and mixing it by a simple dry method to obtain the originally desired composition raw material, it is possible to bake at a relatively low temperature, a dense structure, and an excellent Q value of (1-x) BaO-xTiO. Two types of ceramics can be obtained.
［実施例］ 以下、この発明に係る誘電体共振器材料の製造方法の
一実施例について説明する。なお、以下の説明では、Ba
Ti4O9を形成する場合を代表として説明する。EXAMPLES Hereinafter, an example of a method for manufacturing a dielectric resonator material according to the present invention will be described. In the following description, Ba
The case of forming Ti 4 O 9 will be described as a representative.
硝酸バリウム水溶液（1.4/mol溶液）140ccと四塩化
チタン水溶液（1.3/mol溶液）390ccとを混合した。こ
の混合水溶液を、撹拌している6N−アンモニア水１中
に徐々に添加してBa2+とTi4+の水酸化共沈体を得た。こ
れを洗浄，乾燥した後、800℃で仮焼してBaTi3O7系粉末
を作製した。この粉末10gに市販のTiO2を2.029g加えボ
ールミルで一昼夜混合した後、1000℃で１時間仮焼し
て、BaTi4O9粉末を得た。粒径は0.2μｍである。該粉末
を0.7ton/cm2で成形し、脱脂後1250℃,1275℃,1300℃,1
350℃にて仮焼を１時間行った。140 cc of barium nitrate aqueous solution (1.4 / mol solution) and 390 cc of titanium tetrachloride aqueous solution (1.3 / mol solution) were mixed. This mixed aqueous solution was gradually added to 6N-aqueous ammonia water 1 under stirring to obtain a co-precipitated hydroxide of Ba 2+ and Ti 4+ . After washing and drying, it was calcined at 800 ° C. to produce a BaTi 3 O 7- based powder. 2.029 g of commercially available TiO 2 was added to 10 g of this powder, mixed for 24 hours in a ball mill, and calcined at 1000 ° C. for 1 hour to obtain a BaTi 4 O 9 powder. The particle size is 0.2 μm. The powder was molded at 0.7 ton / cm 2 and after degreasing 1250 ° C, 1275 ° C, 1300 ° C, 1
Calcination was performed at 350 ° C. for 1 hour.
［比較例］ 比較例として、市販のBaCO3,TiO2をBaTi4O9の組成に
なるよう秤量し、秤量した粉末25gをボールミル中で一
昼夜混合した後、1000℃で１時間仮焼し、1.5μｍの粉
末を得た。後は、上記実施例と同様の方法にて試料を作
成した。[Comparative Example] As a comparative example, commercially available BaCO 3 and TiO 2 were weighed so as to have a composition of BaTi 4 O 9 , 25 g of the weighed powder was mixed in a ball mill for 24 hours, and then calcined at 1000 ° C. for 1 hour. A 1.5 μm powder was obtained. Thereafter, a sample was prepared in the same manner as in the above example.
図にその結果を示すが、焼成温度は全体的に25℃程度
乾式法に比べ低下し、密度およびＱ値の向上がみられ
た。The results are shown in the figure. As a result, the firing temperature was reduced by about 25 ° C. as compared with the dry method, and the density and the Q value were improved.
［発明の効果］ 以上述べたようにこの発明に係る誘電体共振器材料の
製造方法によれば、比較的低い温度で焼成が可能で、か
つ組織が緻密で、Ｑ値の優れたセラミックスを製造する
ことができる。[Effects of the Invention] As described above, according to the method for manufacturing a dielectric resonator material according to the present invention, ceramics that can be fired at a relatively low temperature, have a fine structure, and have an excellent Q value can be manufactured. can do.
図はこの発明に係る誘電体共振器材料の製造方法の一実
施例の効果を説明するための特性図である。The figure is a characteristic diagram for explaining the effect of one embodiment of the method for manufacturing a dielectric resonator material according to the present invention.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭61−269805（ＪＰ，Ａ) 特公 平７−29848（ＪＰ，Ｂ２) ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-61-269805 (JP, A) JP 7-29848 (JP, B2)
Claims (1)
（但し、0.75≦ｘ≦0.9）からなる誘電体共振器材料の
製造方法において、 （ａ） Ba溶液とTi溶液をそれぞれ適量作り、これらと
沈殿形成液とを混合して共沈体を形成し、乾燥後600℃
〜1100℃で仮焼する第１の工程、 （ｂ） この第１の工程で得られた仮焼物と目的とする
組成物の残りの構成成分の化合物とを混合して800℃〜1
200℃で仮焼する第２の工程、 （ｃ） あこの第２の工程で得られた仮焼粉末を成形
し、1100℃〜1500℃で焼成する第３の工程、 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。1. A method of manufacturing a dielectric resonator material comprising (1-x) BaO—xTiO 2 ceramics (0.75 ≦ x ≦ 0.9), comprising: (a) preparing appropriate amounts of a Ba solution and a Ti solution; , These are mixed with a precipitate forming solution to form a coprecipitate, which is dried at 600 ° C.
A first step of calcining at 〜1100 ° C., (b) mixing the calcined product obtained in the first step with a compound of the remaining constituents of the target composition, and
A second step of calcining at 200 ° C., and (c) a third step of molding the calcined powder obtained in the second step and firing at 1100 ° C. to 1500 ° C. A method for producing a dielectric resonator material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62132202A JP2617939B2 (en) | 1987-05-28 | 1987-05-28 | Manufacturing method of dielectric resonator material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62132202A JP2617939B2 (en) | 1987-05-28 | 1987-05-28 | Manufacturing method of dielectric resonator material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63298910A JPS63298910A (en) | 1988-12-06 |
| JP2617939B2 true JP2617939B2 (en) | 1997-06-11 |
Family
ID=15075782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62132202A Expired - Lifetime JP2617939B2 (en) | 1987-05-28 | 1987-05-28 | Manufacturing method of dielectric resonator material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2617939B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8420560B2 (en) * | 2010-03-31 | 2013-04-16 | Tdk Corporation | Dielectric ceramic, method for producing dielectric ceramic, and method for producing powder for producing dielectric ceramic |
Family Cites Families (1)
| 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 |
-
1987
- 1987-05-28 JP JP62132202A patent/JP2617939B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63298910A (en) | 1988-12-06 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |