JPS61163184A - Production of single crystal - Google Patents
Production of single crystalInfo
- Publication number
- JPS61163184A JPS61163184A JP537185A JP537185A JPS61163184A JP S61163184 A JPS61163184 A JP S61163184A JP 537185 A JP537185 A JP 537185A JP 537185 A JP537185 A JP 537185A JP S61163184 A JPS61163184 A JP S61163184A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- y3fe5o12
- flux
- fe2o3
- bao
- 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
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はＹ、Ｆ・、０８．単結晶の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention is directed to Y, F., 08. This invention relates to a method for producing a single crystal.
ＹＨＦ ｅ Ｂ Ｏｌ！ （以下ＹｒＧと略す）は、酸
化物強磁性体であり、光アイソレータ等の光材機１目素
子として巾広い実用上の用途が見い出されている。YHF e B Ol! YrG (hereinafter abbreviated as YrG) is an oxide ferromagnetic material, and has been found to have a wide range of practical uses as a primary element for optical materials such as optical isolators.
このＹＩＧ単結晶は、十数百度でペロブスカイト＜ＹＦ
・０．〉とＦ＠１０ｇとに分解するため、直接溶融法で
製造するのは困難である。そのため通常、フラックス法
による製造が用いられており、大型のものが製造、販売
されている。This YIG single crystal has perovskite<YF
・0. ) and F@10g, it is difficult to produce by direct melting method. For this reason, a flux method is usually used, and large-sized products are manufactured and sold.
しかし従来の７ラツクス法によるＹＩＧ単結晶の製造で
は、かなり大きい単結晶が製造できるようになった利点
はあるが、■大型単結晶を得るのに長期間かかる ■フ
ラックスが混入する ■単結晶育成後に方位決定をする
操作が必要になるという問題点があった。そこで本発明
は、このような問題点を解決するもので、その目的は、
高品質の大型ＹＩＧ単結晶を短時間に製造する方法を提
供することにある。However, the production of YIG single crystals using the conventional 7-lux method has the advantage of being able to produce fairly large single crystals, but ■It takes a long time to obtain large single crystals.■Flux is mixed in.■Single crystal growth There was a problem in that an operation for determining the orientation was required later. Therefore, the present invention is intended to solve these problems, and its purpose is to:
The object of the present invention is to provide a method for manufacturing high-quality large-sized YIG single crystals in a short time.
本発明は、ＹＩＧ単結晶の製造方法としてＢ＆０−Ｂ、
０３系を用いた７ラツクスひきあげ法を利用することを
特徴とする。The present invention provides B&0-B,
It is characterized by the use of the 7-lux pull-up method using the 03 system.
本発明の上記の構成によれば、ＹＩＧ種結晶の方位を任
意に選ぶことにより望みの方向の単結晶が得られ、また
結晶径は、ひきあげ速度と降温速度の調整により望みの
大きさの単結晶が得られる。According to the above structure of the present invention, a single crystal in a desired direction can be obtained by arbitrarily selecting the orientation of the YIG seed crystal, and the crystal diameter can be adjusted to a desired size by adjusting the pulling rate and cooling rate. Crystals are obtained.
一般に７ラツクスひきあげ法では、ふたをすることかで
きないので、フラツクス法による蝋性酸化物単結晶の製
造に最も使用されているｐｂｏおよび（または）ＰｂＦ
！のように蒸気圧が高いフラックスは、不適である。ま
たＰｂ０−ＰｂＦ、系を用いたフラックス法の場合には
、Ｐｂイオンが１０８〜ＬＬ７２％も混入してしまい、
ＹＩＧ単結晶の光吸収系数を劣化してしまう。In general, in the 7-lux pulling method, it is only possible to put a lid on, so pbo and/or PbF, which are most used in the production of waxy oxide single crystals by the flux method, are
! Fluxes with high vapor pressure, such as , are unsuitable. In addition, in the case of the flux method using the Pb0-PbF system, Pb ions are mixed in as much as 108 to LL72%,
This will deteriorate the light absorption coefficient of the YIG single crystal.
一方、不発明の上記の構成で用いる１１ａＯＢｔｕｓ系
７ラツクスは、ガーネットと比重差が小さく、また粘性
も大きい。その上不揮発性であるのでＹＩＧ単結晶の７
ラツクスひきあげ法による製造上鏝も適している。On the other hand, the 11aOBtus type 7 lux used in the above-mentioned configuration of the invention has a small difference in specific gravity from garnet and also has a high viscosity. Moreover, since it is non-volatile, YIG single crystal 7
A trowel is also suitable for manufacturing by the Lux drawing method.
Ｙ、Ｏ，、Ｆ・ＷａＳをＹ、Ｆ・、０□の組成比となる
よう秤量し、加剰Ｆ・、０３をＦ・ｔｏｓ ： Ｙ Ｉ
Ｇ＝＝１ ：５で加えたものを原料とした。フラック
スとしては、ＢａＯは水と反応して発熱したり、空気中
の炭酸ガスと化合したりするため、安定な１３ａｃｏ３
を用いてＢａＯ：Ｂ！０３”＝５ ： １となるよう秤
量した、これらをフラックス：原料−６０：４Ｑに十分
１合した後、順次溶融しつつ白金るつぼに充填し、種結
晶を液面真上につるした後に１２５００で２４時間保持
した。炉床部と炉上部で温度差を２５Ｃつけて徐冷し、
１１００ＣになったところでＹＩＧ橿結晶を６０ｒＰｍ
で回転しつつ、液面下はぼ５ｍの溶液中へ入れ、１−０
ｍ／ｄａｙで育成・ひきあげを行った。この時の成長固
液界面の温度は、はぼ１０８０Ｃであった。１０５０Ｃ
までの徐冷が終了したら単結晶を溶液から離し、熱衝撃
を緩和するために１００Ｃ／ｈの速度で室温まで徐冷し
た。この育成中に蒸発したフラックスの量は、はぼ８％
であった。育成されたＹＩＧ単結晶への７ラツクスの混
入量をスベワトル分析で調べたところ、１００１％以下
と高品質であった。また（１１０）面を鏡面研摩し、熱
リン酸および塩酸溶液による腐食ｆ象を観察した。熱リ
ン酸による腐食の場合には、１０μ程度のエッチピット
が偏在し、そのエッチピット濃度の平均値は１０３〜１
０４個／−であった。一方、塩酸溶液による腐食の場合
には１μ以下のエッチピットが１ａＳ〜１０４個／ｃｄ
の濃度で全体に平均して覗祭された。Weigh Y, O,, F・WaS so that the composition ratio becomes Y, F・, 0□, and calculate the additive F・,03 as F・tos : Y I
The material added at a ratio of G==1:5 was used as the raw material. As a flux, BaO reacts with water to generate heat and combines with carbon dioxide gas in the air, so it is a stable 13aco3.
Using BaO:B! 03" = 5:1. After mixing these with flux: raw material - 60:4Q, they were sequentially melted and filled into a platinum crucible, and after suspending the seed crystal directly above the liquid level, 12,500 It was held for 24 hours at a temperature difference of 25C between the hearth and the upper part of the furnace, and then slowly cooled.
When the temperature reaches 1100C, turn the YIG crystal to 60rPm.
While rotating with
They were raised and raised on a m/day basis. The temperature of the growing solid-liquid interface at this time was approximately 1080C. 1050C
After the slow cooling was completed, the single crystal was removed from the solution and slowly cooled to room temperature at a rate of 100 C/h to alleviate thermal shock. The amount of flux evaporated during this growth was approximately 8%.
Met. When the amount of 7 lux mixed into the grown YIG single crystal was investigated by subewattle analysis, it was found to be of high quality with less than 1001%. The (110) plane was also mirror-polished and the corrosion phenomenon caused by hot phosphoric acid and hydrochloric acid solutions was observed. In the case of corrosion by hot phosphoric acid, etch pits of about 10μ are unevenly distributed, and the average value of the etch pit concentration is 103 to 1.
It was 04/-. On the other hand, in the case of corrosion by hydrochloric acid solution, the number of etch pits of 1μ or less is 1aS ~ 104 pieces/cd.
The overall average concentration was peep festival.
樽られたＹＩＧ単債晶の強磁性をｏｆ１認するため、マ
イクロ表面磁力弾性波を用い反射法で室温における特性
を測定した。四角棒状に切り出されたＹｒＧ単結晶の磁
化された方向に対して、横断方向に、１２５０Ｍｈｚの
磁力弾性反射波が測定され、その減衰の遅延時間は、１
０ｄｂ／μｓｅｃ程度であり念。In order to confirm the ferromagnetism of the barreled YIG single bond crystal, its characteristics at room temperature were measured by a reflection method using micro surface magnetoelastic waves. A magnetoelastic reflected wave of 1250 MHz was measured in the transverse direction to the magnetized direction of a YrG single crystal cut into a rectangular bar shape, and the delay time of its decay was 1.
Please note that it is about 0db/μsec.
また、強磁性共鳴の全半値幅を測定するためて、ポンド
法により球状試料を作成した。そのＸバンドの周波数（
９２ｏｏＭｈｚ）での強磁性共鳴の測定において、吸収
線の幅は、（Ｌ５ｆｉφの大きさの試料で五ＯＱｅエル
ステッドであった。In addition, in order to measure the full width at half maximum of ferromagnetic resonance, a spherical sample was prepared using the Pond method. Its X-band frequency (
In the ferromagnetic resonance measurements at 92 ooMhz), the width of the absorption line was 5 OQe Oersteds for a sample of size L5fiφ.
以上述べたように本発明によれば、フラックスひきあげ
法においてフラックスとしてＢａＯＪ０８系を用いるこ
とにより、高品質強磁性体である大型ＹＩＧ単結晶が短
時間上製造できるという効果を有する。As described above, according to the present invention, by using BaOJ08-based flux as a flux in the flux pulling method, a large YIG single crystal, which is a high-quality ferromagnetic material, can be produced in a short time.
以上that's all
Claims (1)
晶を育成・ひきあげるフラツクスひきあげ法において、
フラツクスとしてＢａＯ−Ｂ＿２Ｏ＿３系を用いること
を特徴とする単結晶の製造方法In the flux pulling method, a seed crystal is used to grow and pull up a single crystal from flux while lowering the temperature.
A method for producing a single crystal characterized by using BaO-B_2O_3 system as a flux
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP537185A JPS61163184A (en) | 1985-01-16 | 1985-01-16 | Production of single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP537185A JPS61163184A (en) | 1985-01-16 | 1985-01-16 | Production of single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS61163184A true JPS61163184A (en) | 1986-07-23 |
Family
ID=11609307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP537185A Pending JPS61163184A (en) | 1985-01-16 | 1985-01-16 | Production of single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61163184A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8132835B2 (en) | 2008-09-30 | 2012-03-13 | Fanuc Ltd | Workpiece gripping device |
-
1985
- 1985-01-16 JP JP537185A patent/JPS61163184A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8132835B2 (en) | 2008-09-30 | 2012-03-13 | Fanuc Ltd | Workpiece gripping device |
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