JPS6050760B2 - Oxide single crystal pulling method - Google Patents
Oxide single crystal pulling methodInfo
- Publication number
- JPS6050760B2 JPS6050760B2 JP7440377A JP7440377A JPS6050760B2 JP S6050760 B2 JPS6050760 B2 JP S6050760B2 JP 7440377 A JP7440377 A JP 7440377A JP 7440377 A JP7440377 A JP 7440377A JP S6050760 B2 JPS6050760 B2 JP S6050760B2
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- crystals
- single crystal
- seed crystal
- seed
- 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
Links
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- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 この発明はＬｉＴａＯ。[Detailed description of the invention] This invention is LiTaO.
、ＬｉＮｂＯ。からなる酸化物単結晶の引上げ方法に関
する。従来引上げ方法により単結晶を製造する場合、転
位等の欠陥の少くない高品質の単結晶を得る方法として
、種子結晶を融液につけ、該融液によくなじませた後、
引上げ開始し最初は種子結晶の直径から少しづつ細く結
晶化させる事により種子結晶に存在していた欠陥や種子
結晶を融液につけた時に発生した欠陥を取りのそいた後
結晶を太らせていく方法がとられている。, LiNbO. The present invention relates to a method for pulling an oxide single crystal consisting of. When producing a single crystal using the conventional pulling method, as a method of obtaining a high quality single crystal with few defects such as dislocations, a seed crystal is immersed in a melt, and after being well adapted to the melt,
When pulling begins, the diameter of the seed crystal is first crystallized little by little to remove defects that existed in the seed crystal and defects that occurred when the seed crystal was immersed in the melt, and then the crystal becomes thicker. A method is being taken.
このような結晶成長の前記種子結晶の直径より細く結晶
化することをネツキングといいほとんどすべての単結晶
引上げ法に用いられている。しかしながらＬｉＮｂ０。
、ＬｉＴａＯ。結晶の場合、このネツキングにより一番
細い部分が直径２−以下〜１ｗｌ程度までなつた場合非
常に高い確率で双晶が生じ、ネツキング以後−１↓ｌ」
一 −’３↓口上口↓することを見出した。This process of crystallization in which the seed crystal grows thinner than the diameter of the seed crystal is called netting, and is used in almost all single crystal pulling methods. However, LiNb0.
, LiTaO. In the case of crystals, if the thinnest part becomes smaller than 2 to 1 wl in diameter due to this netting, there is a very high probability that twinning will occur, and after netting, -1↓l.
I found out that 1-'3↓pronunciation↓.
さらにこの異つた方位の結晶は成長陵の出方等の外見上
種子結晶の方位て成長する結晶と非常によく似ており、
結晶を量産する場合大きなトラブルの原因となりやすい
。従つてこのような双晶の発生を零にする事が要求され
る。本発明は上記点に鑑みなされたもので、ＬｉＮｂＯ
。、ＬｉＴａＯ。からなる酸化物単結晶引上げの際に種
子結晶の方位のまま酸化物単結晶を確実に成長させる事
の出来る酸化物単結晶引上げ方法を提供するにある。す
なわち、少くなくとも３−以上の直径を持つ所定の方位
の種子結晶を用いてネツキングを直径２７７！７７１以
上におさえる事により双晶の発生を防止し、種子結晶と
同一方位て酸化物結晶成長させる単結晶引上け方法を提
供するものである。以下具体的な実施例にもとついて本
発明方法の詳細を説明する。Furthermore, these crystals with different orientations are very similar to crystals that grow in different orientations of seed crystals in appearance, such as the appearance of growth ridges.
When mass producing crystals, this can easily cause major trouble. Therefore, it is required to reduce the occurrence of such twins to zero. The present invention has been made in view of the above points, and is based on LiNbO
. , LiTaO. An object of the present invention is to provide a method for pulling an oxide single crystal that can reliably grow the oxide single crystal while keeping the orientation of the seed crystal when pulling the oxide single crystal. In other words, by using a seed crystal with a diameter of at least 3- or more in a predetermined orientation and suppressing netting to a diameter of 277!771 or more, generation of twins can be prevented and oxide crystals can grow in the same direction as the seed crystal. The purpose of the present invention is to provide a method for pulling a single crystal. The details of the method of the present invention will be explained below based on specific examples.
ＬｉＮｂＯ３、およびＬｉＴａＯ。結晶をそれぞれＸ軸
、Ｙ軸、Ｚ軸方位の種子結晶を用いて結晶作成を行うと
通常第１図に夫々ａ、ｂ、ｃに示すような（１０２）面
からなる成長陵が観察される。しかしながら、ａ図はＸ
軸引上げ、を図はＹ軸引上げ、ｃ図はＺ軸引上げである
。種子結晶から結晶を成長させてネツキングを〜２ｗＬ
φ以下まで細くした後太らせ結晶作成を行うと、非常に
高い確率（〜７０％）で（１０２）双晶形成により平行
部分の結晶は第２図のように一見第１図の各軸に対応し
た成長陵が観察されるが、別の方位の結晶が成長する。
第３図に各軸種子結晶を用いた場合の双晶形成による異
方位成長結晶のステレオ投影図を示した。中央の点が引
上げ方向を示す。この原因に２順φ以下にネツキングを
行つた時、結晶径が小さい為表面の曲率が小さく結晶に
大きな成長応力がかかりその為（１０２）双晶が形成さ
れ、それがそのまま成長する為と考えられる。そこで本
発明に基づき次のようにネツキングを２Ｔｍφ以上で行
つた。実施例１
炭酸リチユームと五酸化タンタルよりコングルエント組
成のＬｉ／Ｔａ＝０．９５のＬｉＴａＯ３原料２ｋ９を
用意し、８０φ８０ｈＲｈ２０〜４０％含有したＰｔる
つぼに加熱溶融し、周知の高周波加熱方式の引上げ機に
より第４図に示すようにＸ軸方位の５Ｔ！Ｒｌｎφの種
子結晶を用いて次のようにして結晶作成を行つた。LiNbO3, and LiTaO. When crystals are prepared using seed crystals oriented along the X, Y, and Z axes, growth ridges consisting of (102) planes as shown in a, b, and c in Figure 1 are usually observed. . However, diagram a is
The figure shows Y-axis pull-up, and the figure c shows Z-axis pull-up. Grow crystals from seed crystals and netsking ~2wL
If you thin the crystal to less than φ and then make it thicker, there is a very high probability (~70%) that the parallel portion of the crystal will appear along each axis in Figure 1 due to the formation of (102) twins, as shown in Figure 2. Corresponding growth ridges are observed, but crystals with different orientations grow.
FIG. 3 shows a stereo projection view of a crystal grown in different orientations due to twinning when each axis seed crystal is used. The center point indicates the pulling direction. The reason for this is thought to be that when netting is performed below 2-order φ, the crystal diameter is small, the surface curvature is small, and a large growth stress is applied to the crystal, resulting in the formation of (102) twins, which continue to grow. It will be done. Therefore, based on the present invention, netting was performed at 2Tmφ or more as follows. Example 1 2k9 LiTaO3 raw materials with a congruent composition of Li/Ta=0.95 were prepared from lithium carbonate and tantalum pentoxide, heated and melted in a Pt crucible containing 20 to 40% of 80φ80hRh, and heated using a well-known high-frequency heating type pulling machine. As shown in Figure 4, 5T in the X-axis direction! Crystals were prepared as follows using seed crystals of Rlnφ.
まづ溶融物を融点より若干高目の温度にして、種子結晶
４０を溶融物につけ種子結晶４０が若干溶一け気味の条
件に定めた後種子結晶４０を５Ｔｍｍ時で引上げ開始す
る。成長結晶が前記種子結晶４０より細い３〜４ｗＬφ
程度まで細くなつたら、それ以上細くならないように溶
融液の温度を調整しながら第４図に示すように〜５悶引
上げてネツキング部分４１を形成する。その後溶融液の
温度を少しづつ降下させ結晶を太らせる所定の直径例え
ば３５φになつたら通常の自動径制御装置につなぎ１０
０′結晶４２を作成した。この方法により１００％種子
結晶４０と同一方位の結晶４２作成が達成できた。実施
例１に述べた本発明のネツキング方法によりＬｉＮｂＯ
３，ＬｉＴａＯ３のＸ軸、Ｙ軸、Ｚ軸方位種子結晶によ
り各軸方位引上げ結晶作成が１００％達成した。First, the temperature of the molten material is raised to slightly higher than the melting point, and the seed crystal 40 is immersed in the molten material. After setting the conditions such that the seed crystal 40 is slightly melted, the seed crystal 40 is pulled up at 5 Tmm. The growing crystal is 3 to 4 wLφ thinner than the seed crystal 40.
Once it is thinned to a certain extent, the necking portion 41 is formed by pulling it up by 5 degrees as shown in FIG. 4 while adjusting the temperature of the melt so that it does not become thinner any further. After that, the temperature of the melt is gradually lowered and the crystal is thickened.When the crystal reaches a predetermined diameter, for example 35φ, it is connected to a normal automatic diameter control device.
0' crystal 42 was created. By this method, 100% crystal 42 with the same orientation as the seed crystal 40 could be produced. By the netting method of the present invention described in Example 1, LiNbO
3. Creation of crystals pulled in each axis direction was achieved 100% by using LiTaO3 X-axis, Y-axis, and Z-axis oriented seed crystals.
第１図はＬｉＮｌ）０３、ＬｉＴａＯ３の各軸引上げ結
晶に見られる成長陵を種子結晶側から見た概念図、（第
１図において１はいわゆる肩部のみに見られる成長陵で
２は肩部および平行部の両方に見られる成長陵である）
、第２図は双晶形成により異方位の結晶成長した場合の
種子結晶側から見た概念図、（第２図において５，５，
６はそれぞれＸ，Ｙ，Ｚ軸方位の種子結晶を用いた場合
である）、第３図は第２図の５，５，８のステレオ投影
図、（第３図において９，２は（１０２）面である）、
第４図は本発明方法の実施例説明図である。Figure 1 is a conceptual diagram of the growth ridges seen in each axis-pulled crystal of LiNl)03 and LiTaO3, viewed from the seed crystal side. (growth ridges seen in both the and parallel parts)
, Figure 2 is a conceptual diagram viewed from the seed crystal side when crystals with different orientations grow due to twin formation.
6 is the case where seed crystals are oriented in the X, Y, and Z axes, respectively), FIG. 3 is a stereo projection view of 5, 5, and 8 in FIG. 2, (9 and 2 in FIG. 3 are (102 ) surface),
FIG. 4 is an explanatory diagram of an embodiment of the method of the present invention.
Claims (1)
、その種子結晶に結晶成長させる酸化物単結晶引上げ方
法において、初期の結晶成長部に種子結晶より小さく、
直径２ｍｍ以上のネツキング部をもたせたことを特徴と
する酸化物単結晶引上げ方法。1. In an oxide single crystal pulling method in which a seed crystal with a diameter of 3 mm or more is brought into contact with a melt and crystals are grown on the seed crystal, a seed crystal smaller than the seed crystal is formed in the initial crystal growth area.
A method for pulling an oxide single crystal, characterized by having a netting part with a diameter of 2 mm or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7440377A JPS6050760B2 (en) | 1977-06-24 | 1977-06-24 | Oxide single crystal pulling method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7440377A JPS6050760B2 (en) | 1977-06-24 | 1977-06-24 | Oxide single crystal pulling method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS549171A JPS549171A (en) | 1979-01-23 |
| JPS6050760B2 true JPS6050760B2 (en) | 1985-11-09 |
Family
ID=13546179
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7440377A Expired JPS6050760B2 (en) | 1977-06-24 | 1977-06-24 | Oxide single crystal pulling method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6050760B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS604599B2 (en) * | 1976-03-17 | 1985-02-05 | 株式会社東芝 | Method for producing lithium tantalate single crystal |
| JPS56109900A (en) * | 1980-02-06 | 1981-08-31 | Nec Corp | Growing method for rare earth element aluminate single crystal |
| US4439265A (en) * | 1981-07-17 | 1984-03-27 | Bell Telephone Laboratories, Incorporated | Fabrication method for LiNbO3 and LiTaO3 integrated optics devices |
| US5336801A (en) * | 1992-09-15 | 1994-08-09 | E. I. Du Pont De Nemours And Company | Processes for the preparation of 2,2,3,3-tetrafluoropropionate salts and derivatives thereof |
-
1977
- 1977-06-24 JP JP7440377A patent/JPS6050760B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS549171A (en) | 1979-01-23 |
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