JP3095504B2 - Method for producing compound sintered body - Google Patents
Method for producing compound sintered bodyInfo
- Publication number
- JP3095504B2 JP3095504B2 JP04013033A JP1303392A JP3095504B2 JP 3095504 B2 JP3095504 B2 JP 3095504B2 JP 04013033 A JP04013033 A JP 04013033A JP 1303392 A JP1303392 A JP 1303392A JP 3095504 B2 JP3095504 B2 JP 3095504B2
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- compound
- prgao
- compound sintered
- producing
- 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 - Fee Related
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、(希土類系ガレート)
化合物焼結体の製造方法に関するものであり、特に、P
rGaO3 単結晶を製造する際又はPrGaO3 薄膜形
成用のPrGaO3 ターゲットを製造する際に使用する
母原料であるPrGaO3 化合物焼結体の製造方法に関
するものである。The present invention relates to a (rare earth gallate)
The present invention relates to a method for producing a compound sintered body,
The present invention relates to a method for producing a PrGaO 3 compound sintered body, which is a base material, used when producing an rGaO 3 single crystal or producing a PrGaO 3 target for forming a PrGaO 3 thin film.
【0002】[0002]
【従来の技術】現在幅広く使用されている酸化物単結晶
の製造方法としては、融液から単結晶を育成する高周波
加熱型引上げ方法があるが、この方法においては融液の
母原料としては製造しようとする酸化物単結晶と同一の
化合物で出来た焼結体を使用する。また、酸化物薄膜を
形成にスパッタ法やレーザ蒸着法等を用いる場合のター
ゲットを製造する際にも、製造しようとする酸化物薄膜
と同一の化合物を主とする焼結体を使用する。2. Description of the Related Art A high-frequency heating type pulling method for growing a single crystal from a melt has been used as a method for manufacturing an oxide single crystal which is widely used at present. A sintered body made of the same compound as the oxide single crystal to be used is used. Also, when manufacturing a target when a sputtering method, a laser deposition method, or the like is used for forming an oxide thin film, a sintered body mainly containing the same compound as the oxide thin film to be manufactured is used.
【0003】従来、これらの酸化物単結晶の製造又は酸
化物薄膜形成用ターゲットの製造に用いる母原料である
化合物焼結体の製造方法としては、Gellerら(M
at.Res.Bull.9(1974)637)、水
野ら(窯業協会誌 93(1985)26)の報告に代
表れるように、希土類系ガレートLnGaO3 (Lnは
希土類,以下同様)化合物を製造する場合を例にとる
と、Ln2 O3 とGa2 O3 の二種類の酸化物を出発原
料として等モル秤量し、これらをかいらい機により混成
しプレス機により圧縮成型する。この圧縮成型したもの
を大気中で1100°C以上で焼結する。次にこの焼結
物をかいらい機により再度混成しプレス機により再度圧
縮成型する。その後この再圧縮成型したものを、今度は
最初の焼結温度よりさらに高い1400°C以上の温度
で大気中で再焼結する。このように、従来では二回の混
成・成形・焼結工程を行い所望の希土類系ガレートLn
GaO3 を製造する方法がとられていた。Conventionally, as a method for producing a compound sintered body which is a base material used for producing these oxide single crystals or a target for forming an oxide thin film, Geller et al.
at. Res. Bull. 9 (1974) 637) and Mizuno et al. (Journal of the Ceramic Society of Japan 93 (1985) 26), a case where a rare earth gallate LnGaO 3 (Ln is a rare earth, the same applies hereinafter) compound is taken as an example. , Ln 2 O 3 and Ga 2 O 3 are weighed equimolarly as starting materials, mixed with a grinder and compression-molded with a press. This compression molded product is sintered at 1100 ° C. or higher in the atmosphere. Next, this sintered product is mixed again by a grinder and compression-molded again by a press. Thereafter, the recompressed product is resintered in air at a temperature of 1400 ° C. or higher, which is higher than the initial sintering temperature. As described above, conventionally, two hybridizing, forming, and sintering steps are performed to obtain a desired rare earth gallate Ln.
A method of producing GaO 3 has been adopted.
【0004】この従来の生成過程においては、二回の混
成・成形・焼結工程を必要とするため、工程が複雑で時
間がかかる欠点があった。また、再焼結工程での高温中
の焼結にはカンタルスーパー製の高価な超高温炉を使用
しなければならないため、希土類系ガレートLnGaO
3 化合物からなる母原料を作製する際のコストが高価に
なるという欠点があった。[0004] In this conventional production process, two hybridizing, forming and sintering steps are required, so that the steps are complicated and time-consuming. In addition, an expensive ultrahigh temperature furnace manufactured by Kanthal Super must be used for sintering at a high temperature in the resintering process.
There was a drawback that the cost for producing a mother material composed of three compounds was high.
【0005】[0005]
【発明が解決しようとする課題】本発明が解決しようと
する課題は、単結晶製造及びターゲット製造の母原料と
して使用できる高品質なPrGaO3 化合物焼結体を、
プラセオディウム酸化物とガリウム酸化物を原料とし
て、簡単かつ安価に製造する方法を実現することにあ
る。An object of the present invention is to provide a high-quality PrGaO 3 compound sintered body that can be used as a base material for single crystal production and target production.
An object of the present invention is to realize a simple and inexpensive manufacturing method using praseodymium oxide and gallium oxide as raw materials.
【0006】[0006]
【課題を解決するための手段】本発明の化合物焼結体の
製造方法は、Ln6 O11(Lnは希土類)とGa2 O 3
とをモル比1:3で混成した後、焼結することを特徴と
する。Ln6 O11としてはPr6 O11を用いることが好
適であり、焼結は大気中で1200°C以下の温度で行
うことが好適である。The compound sintered body of the present invention is
The manufacturing method is Ln6O11(Ln is a rare earth) and GaTwoO Three
Is mixed at a molar ratio of 1: 3 and then sintered.
I do. Ln6O11As Pr6O11It is preferable to use
Suitable for sintering at temperatures below 1200 ° C in air.
Is preferred.
【0007】[0007]
【実施例】図1は、本発明の実施例の一つを示す図であ
る。出発原料として、Pr6 O11とGa2 O3 とを用い
る。これらをモル比でPr6 O11:Ga2 O3 =1:3
となるように等モル秤量する。ついで、等モル秤量した
出発原料をかいらい機で4時間の混成を行う。その後大
気中で1200°C以下の温度、例えば1150°Cで
15時間の焼結を行う。FIG. 1 is a diagram showing one embodiment of the present invention. Pr 6 O 11 and Ga 2 O 3 are used as starting materials. These were mixed in a molar ratio of Pr 6 O 11 : Ga 2 O 3 = 1: 3.
Weigh equimolar so that Next, the equimolarly weighed starting materials are mixed for 4 hours with a grinder. Thereafter, sintering is performed in the atmosphere at a temperature of 1200 ° C. or less, for example, 1150 ° C. for 15 hours.
【0008】このようにして製造したPrGaO3 化合
物焼結体のX線回折パターンを図2に示す。このX線回
折パターンには、後述する比較例のような同定不可能な
2θ=31.76°のピークが存在せず、得られたPr
GaO3 化合物焼結体が極めて高品質なものであること
がわかる。FIG. 2 shows an X-ray diffraction pattern of the PrGaO 3 compound sintered body thus manufactured. This X-ray diffraction pattern does not include an unidentifiable peak at 2θ = 31.76 ° as in a comparative example described later, and the obtained Pr
It can be seen that the GaO 3 compound sintered body is of extremely high quality.
【0009】本発明で製造したPrGaO3 化合物焼結
体が極めて高品質であることは、次のような結果からも
確認された。即ち、実施例の方法で製造したPrGaO
3 化合物焼結体を母原料として、白金又はイリジウム製
の坩堝内で溶融し高周波加熱型引上げ法でPrGaO3
単結晶を育成したところ、次に述べる比較例で作製した
焼結体を母原料として育成した単結晶に比べ、本発明で
製造した焼結体を使用した育成単結晶はクラック等がな
い良質の単結晶であった。更に、実施例の方法で製造し
たPrGaO3 化合物焼結体をスパッタ用ターゲットと
して用い、LnGaO3 基板,SrTiO3 基板,Mg
O基板等の上にスパッタ法でPrGaO 3 薄膜を形成し
たところ、次に述べる比較例で作製した焼結体をスパッ
タ用ターゲットとして形成した薄膜に比べ、本発明で製
造した焼結体をターゲットに使用した薄膜は均質で結晶
性のよい薄膜であった。The PrGaO produced by the present inventionThreeCompound sintering
The extremely high quality of the body is based on the following results:
confirmed. That is, PrGaO manufactured by the method of the embodiment
ThreePlatinum or iridium made from compound sintered body as base material
Melted in a crucible made of PrGaOThree
When a single crystal was grown, it was produced in the comparative example described below.
Compared with a single crystal grown from a sintered body as a base material,
The grown single crystal using the manufactured sintered body has no cracks.
It was a good single crystal. Furthermore, it is manufactured by the method of the embodiment.
PrGaOThreeThe compound sintered body is used as a sputtering target.
LnGaOThreeSubstrate, SrTiOThreeSubstrate, Mg
PrGaO on O substrate by sputtering ThreeForming a thin film
Then, the sintered body produced in the comparative example
Compared to a thin film formed as a target for
The thin film using the produced sintered body as the target is homogeneous and crystalline
It was a good thin film.
【0010】[0010]
【比較例】比較のために、出発原料として、Pr2 O3
とGa2 O3 とを用いて、実施例と同様の方法で焼結体
を作製した場合のX線回折パターンを図3に示す。Pr
2 O3 とGa2 O3 とを等モル秤量し、かいらい機によ
る4時間の混成後、大気中で1150°Cで15時間の
焼結を行って作製した焼結体は、図3に示すように、P
rGaO3 化合物の生成を示唆するピークはあるものの
2θ=31.76°に同定不可能なピークを持ってい
る。このことは、Pr2 O3 とGa2 O3 を出発原料と
した場合にはPrGaO3 化合物の生成が完全には行わ
れていないことを示している。更に、念のために焼結温
度を変化させてみたが1200°Cの焼結温度では製造
される焼結体には上に述べた同定不可能なピークが存在
し、高品質なPrGaO3 化合物焼結体を得ることが出
来なかった。Comparative Example For comparison, Pr 2 O 3 was used as a starting material.
And by using the Ga 2 O 3, the X-ray diffraction pattern in the case of producing a sintered body in the same manner as in Example 3. Pr
And 2 O 3 and Ga 2 O 3 and an equimolar weighed, after mixture of 4 hours by puppet machine, sintered bodies were produced by performing the sintering for 15 hours at 1150 ° C in the atmosphere, in FIG. 3 As shown, P
Although there is a peak suggesting the formation of an rGaO 3 compound, it has an unidentifiable peak at 2θ = 31.76 °. This indicates that when Pr 2 O 3 and Ga 2 O 3 were used as starting materials, the formation of the PrGaO 3 compound was not completely performed. Furthermore, although the sintering temperature was changed just in case, at a sintering temperature of 1200 ° C., the above-mentioned unidentifiable peaks existed in the sintered body, and a high quality PrGaO 3 compound was obtained. A sintered body could not be obtained.
【0011】[0011]
【発明の効果】上述した実施例に示したように、本発明
では混成・焼結工程が一回で済むのでPrGaO3 化合
物焼結体を簡単に製造することができる。また、出発原
料としてLn6 O11及びGa2 O3 を用いるので、高品
質のPrGaO3 化合物焼結体を製造できると共に、焼
結体工程での温度を低く抑えることができ又通常の焼結
炉を使用できてPrGaO3 化合物焼結体を安価に製造
することができる。As described in the above embodiment, in the present invention, the hybrid and sintering steps can be performed only once, so that a PrGaO 3 compound sintered body can be easily manufactured. In addition, since Ln 6 O 11 and Ga 2 O 3 are used as starting materials, a high-quality PrGaO 3 compound sintered body can be manufactured, and the temperature in the sintered body process can be suppressed to a low level. The furnace can be used, and the PrGaO 3 compound sintered body can be manufactured at low cost.
【図1】本発明の実施例を示す図である。FIG. 1 is a diagram showing an embodiment of the present invention.
【図2】本発明で製造したPrGaO3 化合物焼結体の
X線回折パターンを示す図である。FIG. 2 is a view showing an X-ray diffraction pattern of a PrGaO 3 compound sintered body manufactured by the present invention.
【図3】比較例で製造した化合物焼結体のX線回折パタ
ーンを示す図である。FIG. 3 is a view showing an X-ray diffraction pattern of a compound sintered body manufactured in a comparative example.
1 出発原料の選定工程 2 等モル秤量工程 3 混成工程 4 焼結工程 1 Starting material selection process 2 Equimolar weighing process 3 Hybridization process 4 Sintering process
───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) C04B 35/42 - 35/50 CA(STN) REGISTRY(STN) WPI(DIALOG)──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. 7 , DB name) C04B 35/42-35/50 CA (STN) REGISTRY (STN) WPI (DIALOG)
Claims (3)
3 とをモル比1:3で混成した後、焼結することを特徴
とする化合物焼結体の製造方法1. Ln 6 O 11 (Ln is a rare earth) and Ga 2 O
3. A method for producing a compound sintered body, comprising: mixing 3 with a molar ratio of 1: 3, followed by sintering.
ることを特徴とする化合物焼結体の製造方法2. The method for producing a compound sintered body according to claim 1, wherein Ln 6 O 11 is Pr 6 O 11.
で1200°C以下の温度で行うことを特徴とする化合
物焼結体の製造方法3. The method for producing a compound sintered body according to claim 1, wherein the sintering is performed at a temperature of 1200 ° C. or lower in the atmosphere.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04013033A JP3095504B2 (en) | 1992-01-28 | 1992-01-28 | Method for producing compound sintered body |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP04013033A JP3095504B2 (en) | 1992-01-28 | 1992-01-28 | Method for producing compound sintered body |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH05201761A JPH05201761A (en) | 1993-08-10 |
JP3095504B2 true JP3095504B2 (en) | 2000-10-03 |
Family
ID=11821817
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP04013033A Expired - Fee Related JP3095504B2 (en) | 1992-01-28 | 1992-01-28 | Method for producing compound sintered body |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3095504B2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113831141A (en) * | 2021-09-15 | 2021-12-24 | 先导薄膜材料(广东)有限公司 | Oxide rotary target and preparation method thereof |
-
1992
- 1992-01-28 JP JP04013033A patent/JP3095504B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPH05201761A (en) | 1993-08-10 |
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Legal Events
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---|---|---|---|
LAPS | Cancellation because of no payment of annual fees |