JPH0729848B2 - Method for manufacturing dielectric resonator material - Google Patents
Method for manufacturing dielectric resonator materialInfo
- Publication number
- JPH0729848B2 JPH0729848B2 JP30089786A JP30089786A JPH0729848B2 JP H0729848 B2 JPH0729848 B2 JP H0729848B2 JP 30089786 A JP30089786 A JP 30089786A JP 30089786 A JP30089786 A JP 30089786A JP H0729848 B2 JPH0729848 B2 JP H0729848B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- dielectric resonator
- tio
- solution
- resonator material
- 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
- 239000000463 material Substances 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 title description 2
- 239000000843 powder Substances 0.000 claims description 26
- 239000000919 ceramic Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000010304 firing Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 description 7
- 239000010936 titanium Substances 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 229910006404 SnO 2 Inorganic materials 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- LTSUHJWLSNQKIP-UHFFFAOYSA-J tin(iv) bromide Chemical compound Br[Sn](Br)(Br)Br LTSUHJWLSNQKIP-UHFFFAOYSA-J 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- 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。TECHNICAL FIELD The present invention relates to a method for 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, but a particularly high Q value is required in satellite communication and the like.
Ｑ値の高い材料として（ZrｘSn１−ｘ）TiO4系セラミッ
クス（但し0.6＜ｘ＜1.0）がある。As a material having a high Q value, there is (Zr x Sn 1-x ) TiO 4 -based ceramics (provided that 0.6 <x <1.0).
このセラミックス材料は一般に、ZrO2、SnO2、TiO2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 manufactured by firing a mixed powder containing ZrO 2 , SnO 2 , and TiO 2 as main components, but it is difficult to sinter, and the expected high dielectric constant and Q value are obtained. Not not.
［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鑑み、組織が緻密で、誘電率およ
びＱ値が向上された（Zr、Sn）TiO4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] In view of the above circumstances, the present invention provides a method for producing (Zr, Sn) TiO 4 -based ceramics having a dense structure and improved dielectric constant and Q value. That is the purpose.
［問題点を解決するための手段］ 本発明は（ZrｘSn１−ｘ）TiO4系セラミックを製造する
のに際し、先ず第１工程としてZr以外の少なくとも１成
分とZr溶液との混合液、およびSn以外の少なくとも１成
分とSn溶液との混合液のいずれかを作り、加水分解反応
を行なってゾルを生成せしめ、乾燥後700℃〜1300℃で
仮焼する。[Means for Solving the Problems] In the production of the (Zr x Sn 1-x ) TiO 4 -based ceramics, the present invention first comprises, as a first step, a mixed solution of at least one component other than Zr and a Zr solution, Then, any one of a mixed solution of at least one component other than Sn and Sn solution is prepared, and a hydrolysis reaction is performed to generate a sol. After drying, calcination is performed 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
的とする組成の残りの成分の粉末とを混合して700℃〜1
300℃で仮焼する。Next, in the second step, the calcined powder obtained above is mixed with the powders of the remaining components having the desired composition to obtain a temperature of 700 ° C to 1 ° C.
Bake at 300 ℃.
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,
Bake at 1200 ℃ -1700 ℃.
第１工程において、Zr溶液、Sn溶液、Ti溶液としては、
オキシ塩化ジルコニウム、硝酸ジルコニウム、金属ジル
コニウム、塩化スズ、臭化スズ、フッ化スズ、硫酸ス
ズ、塩化チタン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, as the Zr solution, Sn solution, and Ti solution,
Aqueous or alcoholic solutions of zirconium oxychloride, zirconium nitrate, metallic zirconium, tin chloride, tin bromide, tin fluoride, tin sulfate, titanium chloride and the like can be used.
加水分解反応は混合液を100℃程度に加熱保持すること
によりなされる。ゾルを仮焼したものは容易に粉砕する
ことができ、サブミクロン級の微細粉末が得られる。The hydrolysis reaction is performed by heating and holding the mixed liquid at about 100 ° C. The calcinated sol can be easily pulverized to obtain fine powder of submicron grade.
（ZrｘSn１−ｘ）とTi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 (Zr x Sn 1-x ) to Ti is 1.0 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。Then, in the first step, by calcining the coprecipitate, a fine powder of submicron class having 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 calcined powder is mixed with the powder of the remaining components necessary to form the desired ceramic composition, and calcined. It is desirable to use the powders of the remaining components having the same particle size as that of 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、Al、S
n、As、Bi、Zn、La、Ce、Sr等が用いられ得る。In addition, a small amount of a sintering aid can be added in the manufacturing process. As the sintering aid, Zr, Mg, Sc, Hf, Th,
W, Nb, Ta, Cr, Mo, Ti, Mn, Fe, Co, Ni, Cd, Al, S
n, As, Bi, Zn, La, Ce, Sr and the like can be used.
本発明の第１工程において、ゾルの仮焼温度は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, if the calcination temperature of the sol is lower than 700 ° C, agglomeration occurs, and if it 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℃〜1
300℃が望ましい。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。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 where significant particle growth does not occur.
300 ° C is desirable. The firing temperature in the third step is 1200
If the temperature is lower than ℃, the whole sintering is insufficient, and if it exceeds 1700 ℃, the particles become coarse and the constituents 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（Zr、Sn）
TiO4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。[Effects] In the present invention, however, a submicron-class metamorphic raw material powder having extremely good dispersibility is obtained in the first step, and the raw material powder is mixed with another raw material powder to form a desired composition raw material. By firing, it is dense and has high dielectric constant and Q value (Zr, Sn)
TiO 4 -based ceramics can be obtained and can be suitably used as a dielectric resonator material.
［実施例］ 塩化チタン水溶液（1.3317/mol 濃度）43.57ccと、
オキシ塩化ジルコニウム水溶液（1.146/mol 濃度）1
50ccしを混合した。この水溶液を、100℃で100時間保持
することで加水分解を行ない、Ti4+とZr4+を含むゾルを
得た。これを洗浄、乾燥した後、1100℃で仮焼して（Zr
0.8Ti0.2）O2粉末を得た。粉末の平均粒径は0.32μｍで
あった。[Example] 43.57 cc of titanium chloride aqueous solution (1.3317 / mol concentration),
Zirconium oxychloride aqueous solution (1.146 / mol concentration) 1
50cc were mixed. This aqueous solution was hydrolyzed by keeping it at 100 ° C. for 100 hours to obtain a sol containing Ti 4+ and Zr 4+ . This is washed and dried, then calcined at 1100 ° C (Zr
0.8 Ti 0.2 ) O 2 powder was obtained. The average particle size of the powder was 0.32 μm.
上記により得られた粉末3.5779gと、市販のTiO2微粉末
1.9963g、SnO2微粉末4.7065gとを混合して（Zr0.8S
n0.2）TiO4組成となるように配合し、ボールミルで一昼
夜混合した後、1000℃で１時間仮焼して（Zr0.8Sn0.2）
TiO4粉末を作成した。平均粒径は0.36μｍであった。3.5779 g of the powder obtained above and a commercially available TiO 2 fine powder
1.9963 g and SnO 2 fine powder 4.7065 g are mixed (Zr 0.8 S
n 0.2 ) TiO 4 composition, mixed all day and night in a ball mill, and then calcined at 1000 ° C. for 1 hour (Zr 0.8 Sn 0.2 ).
TiO 4 powder was created. The average particle size was 0.36 μm.
得られた粉末を1t/cm2で成形し、1450℃で２時間焼成し
た。The obtained powder was molded at 1 t / cm 2 and fired at 1450 ° C. for 2 hours.
得られたセラミックス焼結体の密度は4.79g/cm3、9G K
Hzにおける誘電率は37.0、Ｑ値は6000であった。The density of the obtained ceramic sintered body was 4.79 g / cm 3 , 9G K
The dielectric constant in Hz was 37.0 and the Q value was 6000.
［比較例］ 市販のZrO2、SnO2、TiO2粉末を（Zr0.8Sn0.2）TiO4の組
成となるように、ZrO29.858g、SnO23.014g、TiO27.990g
を配合し、ボールミルで一昼夜混合した後1200℃で１時
間仮焼した。仮焼粉末の平均粒径は約2.1μｍであっ
た。Comparative Example A commercially available ZrO 2, SnO 2, TiO 2 powder (Zr 0.8 Sn 0.2) so as to have the composition of TiO 4, ZrO 2 9.858g, SnO 2 3.014g, TiO 2 7.990g
Was mixed with a ball mill for one day and then calcined at 1200 ° C. for 1 hour. The average particle size of the calcined powder was about 2.1 μm.
この粉末を1t/cm2で成形し、上記実施例と同じ条件下で
焼成した。This powder was molded at 1 t / cm 2 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は4.22g/cm3、誘電
率は27.2、Ｑ値は2000であった。The obtained ceramic sintered body had a density of 4.22 g / cm 3 , a dielectric constant of 27.2 and a Q value of 2000.
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（Zr、S
n）TiO4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。Thus, according to the present invention, the density is higher and the permittivity is higher than in the conventional method, and the Q value is particularly high (Zr, S
n) TiO 4 ceramics can be obtained. The ceramics obtained in the present invention are suitable for use as a dielectric resonator material that requires a high Q value.
Claims (1)
O4系セラミックス（但し0.6＜ｘ＜1.0）を製造する方法
であって、 （１）Zr以外の少なくとも１成分とZr溶液との混合液、
およびSn以外の少なくとも１成分とSn溶液とのひ混合液
のいずれかを作り、加水分解反応を行なってゾルを生成
せしめ、乾燥後700℃〜1300℃で仮焼する第一工程、 （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℃〜1700℃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。1. (Zr x Sn 1-x ) Ti for a dielectric resonator material
A method for producing O 4 -based ceramics (where 0.6 <x <1.0), which is (1) a mixed solution of at least one component other than Zr and a Zr solution,
And a first step of preparing a mixed solution of at least one component other than Sn and a Sn solution, performing a hydrolysis reaction to generate a sol, and calcination at 700 ° C to 1300 ° C after drying, (2) The step of mixing the obtained calcined powder and the powder of the remaining components of the desired composition and firing at 700 ° C to 1300 ° C, (3) molding the obtained calcined powder to 1200 ° C to 1700 ° C A method of manufacturing a dielectric resonator material, which comprises:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30089786A JPH0729848B2 (en) | 1986-12-17 | 1986-12-17 | Method for manufacturing dielectric resonator material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30089786A JPH0729848B2 (en) | 1986-12-17 | 1986-12-17 | Method for manufacturing dielectric resonator material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63153871A JPS63153871A (en) | 1988-06-27 |
| JPH0729848B2 true JPH0729848B2 (en) | 1995-04-05 |
Family
ID=17890439
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30089786A Expired - Lifetime JPH0729848B2 (en) | 1986-12-17 | 1986-12-17 | Method for manufacturing dielectric resonator material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0729848B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7094596B1 (en) * | 2021-10-15 | 2022-07-04 | 庄司電気株式会社 | Healthcare tableware for pets |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118026666A (en) * | 2023-12-26 | 2024-05-14 | 成都宏科电子科技有限公司 | Microwave ceramic material with medium-high dielectric constant and preparation method and application thereof |
-
1986
- 1986-12-17 JP JP30089786A patent/JPH0729848B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7094596B1 (en) * | 2021-10-15 | 2022-07-04 | 庄司電気株式会社 | Healthcare tableware for pets |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63153871A (en) | 1988-06-27 |
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