JPH0648889A - Production of single crystal - Google Patents
Production of single crystalInfo
- Publication number
- JPH0648889A JPH0648889A JP22074492A JP22074492A JPH0648889A JP H0648889 A JPH0648889 A JP H0648889A JP 22074492 A JP22074492 A JP 22074492A JP 22074492 A JP22074492 A JP 22074492A JP H0648889 A JPH0648889 A JP H0648889A
- Authority
- JP
- Japan
- Prior art keywords
- seed crystal
- single crystal
- iridium
- crystal
- rod
- 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
【０００１】[0001]
【産業上の利用分野】本発明は、イットリウム・アルミ
ニウム・ガーネット単結晶（以後ＹＡＧ単結晶と記載）
あるいは、イットリウム・アルミウム・ペロブスカイト
単結晶（以後はＹＡＰ単結晶と記載）または、イットリ
ウム・シリケート単結晶（以後はＹＳＯ単結晶と記載）
等の融点１７００℃以上の高融点単結晶を引上げ法によ
り育成する単結晶の製造方法に関するものである。BACKGROUND OF THE INVENTION The present invention relates to yttrium-aluminum-garnet single crystal (hereinafter referred to as YAG single crystal).
Alternatively, yttrium / aluminum / perovskite single crystal (hereinafter referred to as YAP single crystal) or yttrium / silicate single crystal (hereinafter referred to as YSO single crystal)
The present invention relates to a method for producing a single crystal in which a high melting point single crystal having a melting point of 1700 ° C. or higher is grown by a pulling method.
【０００２】[0002]
【従来の技術】従来、種結晶をサファイヤ製の種結晶支
持棒に固定する方法としては、白金・ロジウムからなる
線を使って、直接種結晶をサファイヤ製の種結晶支持棒
に縛り付けて固定していた。2. Description of the Related Art Conventionally, as a method of fixing a seed crystal to a sapphire seed crystal support rod, a wire made of platinum / rhodium is used to directly bind and fix the seed crystal to a sapphire seed crystal support rod. Was there.
【０００３】[0003]
【発明が解決しようとする課題】ところが、上述の種結
晶の固定方法により、高融点単結晶を育成すると、サフ
ァイヤ製の種結晶支持棒と種結晶が反応をおこして接触
部分から溶け落ちたり、また特に小さな種結晶を用いざ
るを得ない場合、溶融している原料に種結晶を浸ける時
の温度に十分に耐えることが出来ず、白金・ロジウムか
らなる線が溶け切れ種結晶が落下したりして、安定して
単結晶を得ることが困難であった。それ故に本発明の目
的は、白金・ロジウムからなる線の溶融切断を防止し、
また、サファイヤ製の種結晶支持棒と種結晶の反応をお
さえて、安定に単結晶を育成することを可能とする単結
晶の製造方法を提供することにある。However, when a high-melting-point single crystal is grown by the above-mentioned seed crystal fixing method, the sapphire seed crystal support rod and the seed crystal react with each other and melt down from the contact portion, Also, especially when small seed crystals are unavoidable, the temperature cannot be sufficiently high when the seed crystals are immersed in the molten raw material, the wire made of platinum / rhodium melts and the seed crystals fall. Then, it was difficult to stably obtain a single crystal. Therefore, an object of the present invention is to prevent the fusion cutting of a wire made of platinum / rhodium,
Another object of the present invention is to provide a method for producing a single crystal that suppresses the reaction between the sapphire seed crystal support rod and the seed crystal and enables stable growth of the single crystal.
【０００４】[0004]
【課題を解決するための手段】すなわち、本発明は、図
１に示すように、融液から種結晶５を用いて単結晶４を
引き上げて育成する方法において、サファイヤ製の種結
晶支持棒７にイリジウム製棒６を接続し、該イリジウム
製棒６に該種結晶５を取り付け、該イリジウム製棒６と
該種結晶５をイリジウム製ピン１３で固定して単結晶４
を引き上げて育成することを特徴とする単結晶の製造方
法である。That is, according to the present invention, as shown in FIG. 1, in a method of pulling and growing a single crystal 4 from a melt by using a seed crystal 5, a seed crystal support rod 7 made of sapphire is used. An iridium rod 6 is connected to the iridium rod 6, the seed crystal 5 is attached to the iridium rod 6, and the iridium rod 6 and the seed crystal 5 are fixed with an iridium pin 13 to obtain a single crystal 4
Is a method for producing a single crystal, which is characterized by pulling up and growing.
【０００５】[0005]
【作用】ＹＡＰ単結晶、ＹＡＧ単結晶及びＹＳＯ単結晶
は、原料としての酸化イットリウム（Ｙ2Ｏ3）、酸化ア
ルミニウム（Ａｌ2Ｏ3）もしくは酸化珪素（ＳｉＯ2）
をイリジウム（Ｉｒ）坩堝に溶かし込み、育成される。
融液原料にＣａ、Ｐｔ、Ｆｅ、Ｎｉ、Ｒｈ等の不純物が
混入すると５００ｎｍより短い波長領域での光吸収が増
加して光学的品質を低下させることが良く知られてい
る。従って、１７００℃以上の温度で反応する白金・ロ
ジウム線が融液原料中に落下することにより、結晶の光
学的品質を低下させる恐れがあり、また、サファイヤ製
の種結晶支持棒とＹＡＰ、ＹＡＧ単結晶及びＹＳＯ単結
晶の種結晶が反応することによって、破断して種結晶が
落下する可能性もある。そこで、直接に種結晶支持棒と
種結晶を白金・ロジウム線で縛って固定するのではな
く、図１に示すようにイリジウム製棒６を介して種結晶
５をイリジウム製ピン１３で固定することにより白金・
ロジウムの混入を防止し、また、種結晶支持棒７と種結
晶５との反応を防止することができる。[Function] YAP single crystal, YAG single crystal and YSO single crystal are used as raw materials for yttrium oxide (Y 2 O 3 ), aluminum oxide (Al 2 O 3 ) or silicon oxide (SiO 2 ).
Is dissolved in an iridium (Ir) crucible and grown.
It is well known that when impurities such as Ca, Pt, Fe, Ni, and Rh are mixed in the melt raw material, optical absorption in a wavelength region shorter than 500 nm increases and optical quality deteriorates. Therefore, the platinum / rhodium wire that reacts at a temperature of 1700 ° C. or higher may fall into the melt raw material, which may deteriorate the optical quality of the crystal. Moreover, the seed crystal support rod made of sapphire and YAP, YAG The seed crystals of the single crystal and the YSO single crystal may react with each other to break and the seed crystal may fall. Therefore, instead of directly fixing the seed crystal support rod and the seed crystal with the platinum / rhodium wire to fix, the seed crystal 5 is fixed with the iridium pin 13 via the iridium rod 6 as shown in FIG. Due to platinum
Rhodium can be prevented from mixing in, and the reaction between the seed crystal support rod 7 and the seed crystal 5 can be prevented.
【０００６】[0006]
【実施例】以下本発明の実施例を用いて、従来の単結晶
育成方法と比較しながら、本発明を説明する。図１は本
発明による単結晶の製造方法を示す。図１においてイリ
ジウム坩堝（以下Ｉｒ坩堝と称する）１の中にはイット
リウムおよび珪素の各酸化物原料が充填されており、Ｉ
ｒ坩堝１の外側に巻かれた高周波加熱コイル３によりＩ
ｒ坩堝を加熱し、ほぼ２０５０℃の温度で溶融する。溶
融原料２の液面上には、育成中の単結晶４が種結晶５を
介してイリジウム製棒６及び種結晶支持棒７に支持さ
れ、回転されながら上方へ引き上げられて成長する。Ｉ
ｒ坩堝１と坩堝保温材８の間にはジルコニア（Ｚｒ
Ｏ2）粉末９が充填され、Ｉｒ坩堝の上部は保温筒１
０、１１により２重に覆われている。EXAMPLES The present invention will be described below with reference to examples of the present invention while comparing it with a conventional method for growing a single crystal. FIG. 1 shows a method for producing a single crystal according to the present invention. In FIG. 1, an iridium crucible (hereinafter referred to as an Ir crucible) 1 is filled with oxide raw materials of yttrium and silicon.
r by the high frequency heating coil 3 wound on the outer side of the crucible 1
r The crucible is heated and melted at a temperature of approximately 2050 ° C. On the liquid surface of the molten raw material 2, the growing single crystal 4 is supported by the iridium rod 6 and the seed crystal supporting rod 7 via the seed crystal 5, and is pulled up while being rotated to grow. I
Between the crucible 1 and the crucible heat insulating material 8, zirconia (Zr
O 2 ) powder 9 is filled, and the upper part of the Ir crucible is the heat insulating cylinder 1.
It is doubly covered with 0 and 11.
【０００７】次に、直径が６ｍｍ、全長が１５０ｍｍの
サファイヤ製種結晶支持棒７の直下に、２ｍｍ×２ｍｍ
×５０ｍｍのイリジウム製棒６を白金・ロジウム線１２
で固定し、５ｍｍ×５ｍｍ×１０ｍｍの種結晶５の上端
面にφ３ｍｍのイリジウム製棒を挿入するための穴を開
け側面よりφ２ｍｍの貫通孔を２ケ所に開けφ１．５ｍ
ｍ×５ｍｍのイリジウム製ピン１３を差し込んでセット
した。Next, 2 mm × 2 mm is provided just below the sapphire seed crystal support rod 7 having a diameter of 6 mm and a total length of 150 mm.
X 50 mm iridium rod 6 with platinum / rhodium wire 12
Then, a hole for inserting a φ3 mm iridium rod is made in the upper end surface of the 5 mm × 5 mm × 10 mm seed crystal 5, and a through hole of φ2 mm is opened at two places from the side surface and φ1.5 m
An iridium pin 13 of m × 5 mm was inserted and set.
【０００８】原料となる酸化イットリウム（Ｙ2Ｏ3）と
酸化珪素（ＳｉＯ2）を１：１の割合で秤量、混合し、
φ５０ｍｍ×５０Hｍｍ×１．５tｍｍのＩｒ坩堝に充填
し焼成を行い焼成体を３個作る。これを出発原料とし、
窒素流量が１リットル／分の雰囲気中で昇温、溶融させ
る。その後種結晶５を融液につけて１０〜２０ｒｐｍの
速度で回転させ、１．５〜２．５ｍｍ／Ｈｒの速度で引
き上げて結晶を育成した。本発明による種結晶支持法に
よると種結晶５が落下せず再現性良く単結晶が得られ
た。イリジウム製棒６およびイリジウム製ピン１３を使
用することなく、従来法で行った場合、３回が３回とも
白金・ロジウム線１２が溶融切断して、種結晶５が落下
し育成続行不可能となった。Yttrium oxide (Y 2 O 3 ) as a raw material and silicon oxide (SiO 2 ) were weighed and mixed at a ratio of 1: 1,
Filling an Ir crucible of φ50 mm × 50 H mm × 1.5 t mm and firing, three firing bodies are prepared. With this as the starting material,
The temperature is raised and melted in an atmosphere with a nitrogen flow rate of 1 liter / min. After that, the seed crystal 5 was immersed in the melt, rotated at a speed of 10 to 20 rpm, and pulled up at a speed of 1.5 to 2.5 mm / Hr to grow a crystal. According to the seed crystal supporting method of the present invention, the single crystal was obtained with good reproducibility without dropping the seed crystal 5. When the conventional method is used without using the iridium rod 6 and the iridium pin 13, the platinum / rhodium wire 12 melts and cuts three times, and the seed crystal 5 falls and the growth cannot be continued. became.
【０００９】[0009]
【発明の効果】以上述べた通り本発明によれば、種結晶
支持棒の直下にイリジウムからなる棒を介して種結晶を
取り付けイリジウム製棒と種結晶をイリジウムからなる
ピンで固定することにより、高融点温度の単結晶を安定
に得ることが出来るようになった。As described above, according to the present invention, the seed crystal is attached directly below the seed crystal support rod through the rod made of iridium, and the rod made of iridium and the seed crystal are fixed by the pin made of iridium. It has become possible to stably obtain a single crystal having a high melting point temperature.
【図１】図１は本発明による単結晶の製造方法の説明図
である。FIG. 1 is an explanatory view of a method for producing a single crystal according to the present invention.
１ イリジウム坩堝 ２ 溶融原料 ３ 高周波加熱コイル ４ 単結晶 ５ 種結晶 ６ イリジウム製棒 ７ 種結晶支持棒 ８ 坩堝保温材 ９ ジルコニア粉末 １０、１１ 保温筒 １２ 白金・ロジウム線 １３ イリジウム製ピン 1 Iridium crucible 2 Melting raw material 3 High-frequency heating coil 4 Single crystal 5 Seed crystal 6 Iridium rod 7 Seed crystal support rod 8 Crucible heat insulating material 9 Zirconia powder 10, 11 Heat insulating tube 12 Platinum / Rhodium wire 13 Iridium pin
Claims (1)
て育成する方法において、サファイヤ製の種結晶支持棒
にイリジウム製棒を接続し、該イリジウム製棒に種結晶
を取り付け、該イリジウム製棒と該種結晶をイリジウム
製ピンで固定して単結晶を引き上げて育成することを特
徴とする単結晶の製造方法。1. A method for pulling and growing a single crystal from a melt using a seed crystal, wherein a sapphire seed crystal supporting rod is connected to an iridium rod, and the iridium rod is attached with the seed crystal. A method for producing a single crystal, which comprises fixing a rod and the seed crystal with an iridium pin and pulling the single crystal to grow it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22074492A JPH0648889A (en) | 1992-07-27 | 1992-07-27 | Production of single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22074492A JPH0648889A (en) | 1992-07-27 | 1992-07-27 | Production of single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0648889A true JPH0648889A (en) | 1994-02-22 |
Family
ID=16755856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22074492A Pending JPH0648889A (en) | 1992-07-27 | 1992-07-27 | Production of single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0648889A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012110009A1 (en) * | 2011-02-17 | 2012-08-23 | Crytur Spol.S R.O. | Preparation of doped garnet structure single crystals with diameters of up to 500 mm |
| CN103014843A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Clamp for mounting seed crystal for growing sapphire crystal with kyropoulos method |
-
1992
- 1992-07-27 JP JP22074492A patent/JPH0648889A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012110009A1 (en) * | 2011-02-17 | 2012-08-23 | Crytur Spol.S R.O. | Preparation of doped garnet structure single crystals with diameters of up to 500 mm |
| US9499923B2 (en) | 2011-02-17 | 2016-11-22 | Crytur Spol S.R.O. | Method for the preparation of doped garnet structure single crystals with diameters of up to 500 mm |
| CN103014843A (en) * | 2013-01-10 | 2013-04-03 | 苏州巍迩光电科技有限公司 | Clamp for mounting seed crystal for growing sapphire crystal with kyropoulos method |
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