JPS6042195B2 - Chrysoberyl single crystal manufacturing method - Google Patents
Chrysoberyl single crystal manufacturing methodInfo
- Publication number
- JPS6042195B2 JPS6042195B2 JP7248577A JP7248577A JPS6042195B2 JP S6042195 B2 JPS6042195 B2 JP S6042195B2 JP 7248577 A JP7248577 A JP 7248577A JP 7248577 A JP7248577 A JP 7248577A JP S6042195 B2 JPS6042195 B2 JP S6042195B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- rod
- shaped raw
- rotating shaft
- single crystal
- 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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- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明は酸化ベリリウム、酸化アルミニウム混合粉末を
棒状に成型した原料に、赤外線を焦光して溶融帯を形成
し、かつその溶融帯を移動せしめることによりクリソベ
リル単結晶を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention produces chrysoberyl single crystals by focusing infrared rays on a raw material made of a mixed powder of beryllium oxide and aluminum oxide molded into a rod shape to form a molten zone, and then moving the molten zone. Relating to a method of manufacturing.
本発明の目的は、容易に大型クリソベリル単結晶を得る
ことにある。An object of the present invention is to easily obtain large chrysoberyl single crystals.
本発明の他の目的は、安価にクリソベリル単結晶を得る
ことにある。Another object of the present invention is to obtain chrysoberyl single crystals at low cost.
クリソベリルはＢｅＡ１。Chrysoberyl is BeA1.
ｏ。なる組成を持ち、天然には猫目石、アレキサンドラ
イトなどが宝石として著名である。近年、その光物性か
らレーザーホスト材料として有望視されている。これを
人工的に製造しようとする試はＰｂＯ、ＰｂＯ−ＰｂＦ
２系、ＰｂＯ−ＰｂＦ２−Ｂ２Ｏ３系、Ｌｉ２ＭＯＯ４
−ＭＯＯ３系などの融剤をフラックスとして用いる方法
が幾つか行なわれてきた、しかし、これらの方法では大
結晶を得るこは難しく、又、この様な方法で作業した結
晶は、双晶になり易く、単結晶は困難であつた。本発明
者は赤外線を集光することにより得られる高温によりあ
らかじめ棒状に成型した原料中に溶融帯を形成し、かつ
その溶融帯を移動せしめることにより容易にクリソベリ
ル単結晶が得られる’ことを見出した第１図にＢｅ０−
Ａ１。o. Naturally, cat's eye stone, alexandrite, etc. are famous as gemstones. In recent years, it has been viewed as a promising laser host material due to its optical properties. Attempts to artificially produce this are PbO, PbO-PbF
2 system, PbO-PbF2-B2O3 system, Li2MOO4
- Several methods have been carried out using fluxes such as MOO3-based fluxes, but it is difficult to obtain large crystals with these methods, and crystals produced using such methods tend to become twinned. However, it was difficult to make a single crystal. The present inventor has discovered that chrysoberyl single crystals can be easily obtained by forming a molten zone in a raw material that has been previously formed into a rod shape using high temperatures obtained by concentrating infrared rays, and by moving the molten zone. In Figure 1, Be0-
A1.
Ｏ。系の状態図を示す。図から明らかな如く、Ａ１。Ｏ
ａの重合割合が７５％から８５％の高温度にＢｅ０、Ａ
１２Ｏ、と融液が共存する領域が存在する。この領域か
ら単純に冷却固化させても、３Ｂｅ０、Ａｌ２Ｏａ又は
ＢｅＯ、３Ａｌ２Ｏ。とＢｅ０、Ａｌ２（）、の混晶が
生成するのみで、Ｂｅ０、Ａ１。への単結晶は得られな
い。しかし、本発明方法を用いることにより容易にクリ
ソベリル単結晶が得られた。本発明の原理を第２図に示
す。O. The state diagram of the system is shown. As is clear from the figure, A1. O
Be0, A at a high temperature where the polymerization ratio of a is 75% to 85%.
There is a region where 12O and the melt coexist. Even if it is simply cooled and solidified from this region, 3Be0, Al2Oa, BeO, 3Al2O. Only mixed crystals of Be0, Al2(), and Be0, Al2() are generated. Single crystals cannot be obtained. However, by using the method of the present invention, chrysoberyl single crystals were easily obtained. The principle of the invention is shown in FIG.
棒状原料１の部分に赤外線１Ｒにより溶融帯２を形成す
る。A molten zone 2 is formed in a portion of the rod-shaped raw material 1 by infrared rays 1R.
溶融帯２の組成からＡｌ．Ｏ３の重量割合が７５％から
８５％の間にあるとする。溶融帯の温度を１８７０℃以
上に保ち、溶融帯を原料棒中上方に移動せしめると、溶
解帯下部は１８７０℃以下となり、ＢｅＯ．Ａｌ２Ｏ３
と融液が共存する領域が発生する。この領域に於いて、
ＢｅＯ．Ａｌ２Ｏ３は下部原料中に幾り、融液は溶融帯
を共に上方に移動する為に、下部原料中にはＢｅＯ．Ａ
Ｉ２Ｏ３単結晶のみが残る。下部原料棒即ち、ＢｅＯ．
Ａｌ２Ｏ３が育生される領域にＢｅＯ．Ａｌ２Ｏ３の種
子結晶が存在すると結晶化は容易となり、完全なる単結
晶の生成が行なわれる。第３図に於て、本発明を実施す
る装置について説明する。From the composition of molten zone 2, Al. Assume that the weight percentage of O3 is between 75% and 85%. When the temperature of the melting zone is kept at 1870°C or higher and the melting zone is moved upward in the raw material rod, the lower part of the melting zone becomes lower than 1870°C, and BeO. Al2O3
A region occurs where both the melt and the melt coexist. In this area,
BeO. Since Al2O3 is present in the lower raw material and the melt moves upward along the melting zone, BeO. A
Only the I2O3 single crystal remains. Lower raw material rod, BeO.
BeO. The presence of Al2O3 seed crystals facilitates crystallization and results in the formation of a perfect single crystal. Referring to FIG. 3, an apparatus for implementing the present invention will be described.
回転楕円鏡体３内の一焦点にハロゲンランプ４又はクセ
ノンランプを配置し、他の焦点に棒状原料５を配置する
。A halogen lamp 4 or a xenon lamp is placed at one focal point within the spheroidal body 3, and a rod-shaped raw material 5 is placed at the other focal point.
棒状原料５は上部回転軸６、下部回転軸７により支持さ
れている。原料棒５と回転軸６，７は透明石英管８内に
密封されており雰囲気を自由にコントロールでき、又、
真空あるいは加熱することも可能である。棒状原料５中
で温度の上るのは焦点に完全に一致した部分のみであり
、この部分が溶融帯９である。溶融帯９は、回−転軸６
，７を上下動させることにより棒状原料上移動させるこ
とができる。本発明方法を用いることにより双晶のない
大型完全クリソベリル単結晶の製造が可能となつた。The rod-shaped raw material 5 is supported by an upper rotating shaft 6 and a lower rotating shaft 7. The raw material rod 5 and the rotating shafts 6 and 7 are sealed inside a transparent quartz tube 8, so that the atmosphere can be controlled freely.
Vacuum or heating is also possible. In the rod-shaped raw material 5, the temperature rises only in the part that completely coincides with the focal point, and this part is the melting zone 9. The molten zone 9 is connected to the rotating shaft 6
, 7 can be moved up and down to move the rod-shaped raw material. By using the method of the present invention, it has become possible to produce a large perfect chrysoberyl single crystal without twins.
以下に本発明を実施例について説明する。実施例１
酸化ベリリウム粉末２５ｙ１ガンマアルミナ粉末７５ｙ
１酸化クロム粉末３ｙをボールミルにて混合した後、棒
状に圧縮成型し１２００℃で焼成した。The present invention will be described below with reference to Examples. Example 1 Beryllium oxide powder 25y1 Gamma alumina powder 75y
After mixing chromium monoxide powder 3y in a ball mill, it was compression molded into a rod shape and fired at 1200°C.
この原料棒を赤外線集中加熱炉にセツし溶融帯を５３朗
１ｈｒの速度て移動させることにより暗縁色のアレキサ
ンドラの完全結晶を得た。実施例２
酸化ベリリウム、酸化アルミニウム、酸化クロムより、
原料棒の一方の先端の溶融帯となる部分クのみ酸化アル
ミニウム８０％酸化ベリリウム２０％ととし、上部回転
軸にセットし、下部回転軸に種子クリンベリル単結晶を
セットし、上部回転軸と下部回転軸を反対方向に回転し
、溶融帯が形成して後、種子結晶を接触させ、溶融帯を
移動させた。This raw material rod was placed in an infrared concentrated heating furnace and the melting zone was moved at a speed of 53 to 1 hour to obtain a dark-rimmed alexandra perfect crystal. Example 2 From beryllium oxide, aluminum oxide, and chromium oxide,
Only the part that will become the melting zone at one end of the raw material rod is made of 80% aluminum oxide and 20% beryllium oxide, and is set on the upper rotating shaft, and the seed criberyl single crystal is set on the lower rotating shaft, and the upper rotating shaft and lower rotating shaft are set. The axis was rotated in the opposite direction, and after the molten zone had formed, the seed crystals were brought into contact and the molten zone was moved.
本方法により径１―長さ８αのアレキサドライト結晶を
得た。実施例３
酸化アルミニウム６０ｑ１酸化ベリリウム５ｙ１ノ酸化
クロム１ｙ１酸化チタン０．５ｙをボールミル混合し、
８００′Ｃｌ３Ｏｋ９ｌｃＩｔでホットブレス成型して
棒状とした後、赤外線集中加熱装置にセットして、４ｋ
ｇＩｃＦ１！に酸素圧下で結晶成長を行ないキヤツツア
イ状の光条の生ずるクリソベリルを得た。By this method, alexadorite crystals having a diameter of 1 and a length of 8α were obtained. Example 3 60q of aluminum oxide, 5y of beryllium oxide, 1y of chromium oxide, 0.5y of titanium oxide were mixed in a ball mill,
After hot-breath molding with 800'Cl3Ok9lcIt into a rod shape, it was set in an infrared concentrated heating device and heated to 4k.
gIcF1! Crystal growth was performed under oxygen pressure to obtain chrysoberyl with cat's-eye striations.
以上の如く本発明では、二元化合物を成する原料以外に
着色剤として酸化クロムを用い、酸化アルミニウムと酸
化ベリリウムと酸化クロムの各各の粉末を混合して８０
０℃以上の温度で焼結して棒状原料を構成することによ
り、着色剤を幅射線吸収加熱剤として作用させ、赤外線
集中加熱炉によつて二元化合物ＢｅＯ．Ａｌ。Ｏ３を極
めて効率良く製造し得るようにした。また着色剤となる
酸化クロムが結晶速度を制御し、インクルージヨンのな
い単結晶育成が可能となつた。また棒状材料には酸化ベ
リリウムと酸化アルミニウムと酸化クロムの粉末を混合
し、８００゜Ｃ以上の温度て焼結してあるので、溶融帯
の中の組成が常に均一に保つことができ、色ムラのない
透明度の均質な単結晶が得られるものであり、装飾品、
光学的手段として価値を著しく高めるものてある。As described above, in the present invention, chromium oxide is used as a coloring agent in addition to the raw materials forming the binary compound, and powders of aluminum oxide, beryllium oxide, and chromium oxide are mixed and
By sintering at a temperature of 0°C or higher to form a rod-shaped raw material, the colorant acts as a radiation absorbing heating agent, and the binary compound BeO. Al. O3 can be produced extremely efficiently. In addition, chromium oxide, which serves as a colorant, controls the crystallization rate, making it possible to grow single crystals without inclusions. In addition, the rod-shaped material is made of a mixture of beryllium oxide, aluminum oxide, and chromium oxide powders and sintered at a temperature of 800°C or higher, so the composition in the molten zone can always be kept uniform and color unevenness can be maintained. A homogeneous single crystal with no transparency can be obtained, and it can be used for decorations,
There are things that can significantly increase the value of optical tools.
第１図は本発明の詳細な説明する状態図である。
第２図は本発明の詳細な説明する図てある。第３図は本
発明に用いる赤外線集中加熱装置の説明図である。１・
・・・・・棒状原料、２・・・・・・溶融帯、３・・・
・・・回転楕円鏡体、４・・・・・・ハロゲンランプ、
５・・・・・・棒状原料、６・・・・・・上部回転軸、
７・・・・・・下部回転軸、８・・・・・・透明石英管
、９・・・・・・溶融帯。FIG. 1 is a detailed state diagram illustrating the present invention. FIG. 2 is a diagram for explaining the invention in detail. FIG. 3 is an explanatory diagram of an infrared concentrated heating device used in the present invention. 1・
... Rod-shaped raw material, 2 ... Melt zone, 3 ...
...Spheroidal mirror body, 4...Halogen lamp,
5... Rod-shaped raw material, 6... Upper rotating shaft,
7... Lower rotating shaft, 8... Transparent quartz tube, 9... Molten zone.
Claims (1)
下動しうる上回転軸と下回転軸、前記上下回転軸を包囲
密封する透明石英管、及びハロゲンランプもしくはハロ
ゲンランプからなる加熱ランプを有する赤外線集中加熱
炉を用いた単結晶製造方法において、少なくとも酸化ベ
リリウムと酸化アルミニウム及び着色剤として酸化クロ
ムの各々の粉末を混合して８００℃以上で焼結した棒状
原料を形成し、前記回転楕円鏡体内の１焦点に前記加熱
ランプを配置し、他の焦点に前記棒状原料が配置される
ように前記上下回転軸に前記棒状原料を支持し、前記加
熱ランプの赤外線を用いて前記棒状原料に溶融帯を形成
するとともに、前記棒状原料を長手方向に移動させるこ
とにより前記溶融帯を前記棒状原料に沿つて移動させ、
同時に溶融帯下部に単結晶を形成して成り、更に前記溶
融帯温度は１８７０℃以上であり、且つ前記溶融帯にけ
る前記酸化ベリリウムと前記酸化アルミニウムの混合割
合が酸化ベリリウム２５〜１５重量％、酸化アルミニウ
ム７５〜８５重量％であることを特徴とするクリソベリ
ル単結晶製造法。1. A spheroidal mirror body, an upper rotating shaft and a lower rotating shaft that can each rotate in opposite directions and move up and down within the mirror, a transparent quartz tube that surrounds and seals the vertical rotating shaft, and a halogen lamp or a heating device consisting of a halogen lamp. In a single crystal manufacturing method using an infrared concentrated heating furnace equipped with a lamp, a rod-shaped raw material is formed by mixing powders of at least beryllium oxide, aluminum oxide, and chromium oxide as a coloring agent and sintering at 800 ° C. or higher, and The heating lamp is placed at one focal point in the spheroidal body, and the rod-shaped raw material is supported on the vertical rotating shaft so that the rod-shaped raw material is placed at the other focal point, and the rod-shaped raw material is heated using the infrared rays of the heating lamp. forming a molten zone in the raw material and moving the molten zone along the rod-shaped raw material by moving the rod-shaped raw material in the longitudinal direction;
At the same time, a single crystal is formed in the lower part of the melting zone, and further, the temperature of the melting zone is 1870° C. or higher, and the mixing ratio of the beryllium oxide and the aluminum oxide in the melting zone is 25 to 15% by weight of beryllium oxide, A method for producing a chrysoberyl single crystal, characterized in that the content of aluminum oxide is 75 to 85% by weight.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7248577A JPS6042195B2 (en) | 1977-06-17 | 1977-06-17 | Chrysoberyl single crystal manufacturing method |
| US05/915,847 US4218282A (en) | 1977-06-17 | 1978-06-15 | Method of preparation of chrysoberyl and beryl single crystals |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7248577A JPS6042195B2 (en) | 1977-06-17 | 1977-06-17 | Chrysoberyl single crystal manufacturing method |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7288185A Division JPS60260495A (en) | 1985-04-05 | 1985-04-05 | Preparation of single crystal of chrysoberyl |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS546900A JPS546900A (en) | 1979-01-19 |
| JPS6042195B2 true JPS6042195B2 (en) | 1985-09-20 |
Family
ID=13490665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7248577A Expired JPS6042195B2 (en) | 1977-06-17 | 1977-06-17 | Chrysoberyl single crystal manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6042195B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60260495A (en) * | 1985-04-05 | 1985-12-23 | Seiko Epson Corp | Preparation of single crystal of chrysoberyl |
| JPS63260894A (en) * | 1987-10-16 | 1988-10-27 | Seiko Epson Corp | Synthesis method of chrysoberyl cat's eye single crystal |
| CN108060456A (en) * | 2017-12-12 | 2018-05-22 | 中国科学院上海光学精密机械研究所 | The Bridgman-Stockbarger method of beryllium aluminate crystal |
| CN113403679A (en) * | 2021-03-15 | 2021-09-17 | 青岛海泰光电技术有限公司 | Method for growing emerald gem crystal by Czochralski method |
-
1977
- 1977-06-17 JP JP7248577A patent/JPS6042195B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS546900A (en) | 1979-01-19 |
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