JPS63260894A - Synthesis method of chrysoberyl cat's eye single crystal - Google Patents
Synthesis method of chrysoberyl cat's eye single crystalInfo
- Publication number
- JPS63260894A JPS63260894A JP26121987A JP26121987A JPS63260894A JP S63260894 A JPS63260894 A JP S63260894A JP 26121987 A JP26121987 A JP 26121987A JP 26121987 A JP26121987 A JP 26121987A JP S63260894 A JPS63260894 A JP S63260894A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- single crystal
- rod
- zone
- melt zone
- 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.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 61
- 229910001602 chrysoberyl Inorganic materials 0.000 title claims description 27
- 241000282326 Felis catus Species 0.000 title description 5
- 238000001308 synthesis method Methods 0.000 title 1
- 239000002994 raw material Substances 0.000 claims abstract description 50
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000423 chromium oxide Inorganic materials 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 9
- 150000002367 halogens Chemical class 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000010453 quartz Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 7
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 20
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 5
- 125000005843 halogen group Chemical group 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- 239000000155 melt Substances 0.000 abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 7
- 229910052724 xenon Inorganic materials 0.000 abstract description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 3
- 238000000034 method Methods 0.000 description 14
- 239000000843 powder Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 9
- 238000005245 sintering Methods 0.000 description 5
- 239000003086 colorant Substances 0.000 description 4
- 238000004040 coloring Methods 0.000 description 4
- 230000004907 flux Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000010437 gem Substances 0.000 description 2
- 229910001751 gemstone Inorganic materials 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- QXYJCZRRLLQGCR-UHFFFAOYSA-N molybdenum(IV) oxide Inorganic materials O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
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ＢｅＡｌｚｏａ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，Ｐｂ０−ＰｂＦｚ系、ＰｂＯＰｂＦｚ Ｂ
ｚＯｉ系、ＬｉｔＭＯＯ，−ＭｏＯ２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とは難しく、又
、この様な方法で作製した結晶は、双晶になり易く、単
結晶は困難であった。Chrysoberyl has the composition BeAlzoa, and natural cat's eye stones, 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, Pb0-PbFz system, PbOPbFz B
Several methods have been carried out using fluxes such as zOi-based, LitMOO, and -MoO2-based fluxes. However, it is difficult to obtain large crystals by these methods, and crystals produced by such methods tend to form twins, making it difficult to produce single crystals.
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。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. .
第１図にＢｅ０−Ａｌ□０．系の状態図を示す。Figure 1 shows Be0-Al□0. The state diagram of the system is shown.
図から明らかな如く、ＡＩ！、□０．の重量割合が７５
％から８５％の高温度にＢｅＯ，Ａ！！ｚ ０３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３ＢｅＯ，Ａｆ□０．又は、Ｂ ｅ Ｏ，，
３ｋＨｚ ＣｈとＢ ｅ Ｏ、Ａ ｌ ｚ Ｏｓの混晶
が生成するのみで、Ｂｅｄ、Ａｎｔ Ｏｘ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。As is clear from the diagram, AI! ,□0. The weight percentage of
% to 85% of BeO, A! ! There is a region where z 03 and melt coexist. Even if it is simply cooled and solidified from this region, 3BeO, Af□0. Or B e O,,
Only mixed crystals of 3kHz Ch, B e O, and Al z Os are generated, and single crystals of Bed and Ant Ox are not obtained. However, by using the method of the present invention, chrysoberyl single crystals were easily obtained.
本発明の原理を第２図に示す。The principle of the invention is shown in FIG.
棒状原料１の部分に赤外線ＩＲにより溶融帯２を形成す
る。溶融帯２の組成からＡＩ！、□０３の重量割合が７
５％から８５％の間にあるとする。溶融帯の温度を１８
７０°Ｃ以上に保ち、溶融帯を原料枠中上方に移動せし
めると、溶解帯下部は１８７０℃以下となり、Ｂ ｅ
Ｏ，Ａ１１ｚ Ｏｓと融液が共存する領域が生成する。A molten zone 2 is formed in a portion of the rod-shaped raw material 1 by infrared IR. AI from the composition of melt zone 2! , the weight ratio of □03 is 7
Suppose it is between 5% and 85%. The temperature of the melting zone is 18
If the temperature is maintained at 70°C or above and the melting zone is moved upward in the raw material frame, the lower part of the melting zone becomes below 1870°C, and B e
A region where O, A11z Os and the melt coexist is generated.
この領域に於て、ＢｅＯ，Ａ１．ｔ Ｏｘは下部原料中
に残り、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、Ａｌ！０３単結晶のみが残る。下部
原料棒即ち、１３ ｅ Ｏ−Ａ １□０．が育成される
領域にＢｅｏ、Ａ／！□０．の種子結晶が存在すると結
晶化は容易となり、完全なる単結晶が生成が行なわれる
。In this region, BeO, A1. Since tOx remains in the lower raw material and the melt moves upward along the melting zone, Beo, Al! Only the 03 single crystal remains. Lower raw material rod, 13 e O-A 1□0. Beo, A/! □0. The presence of a seed crystal facilitates crystallization, and a perfect single crystal is formed.
尚クリソベリル単結晶の緑色を析出させるために着色剤
として酸化クロムを用いる。酸化クロムは酸化ベリリウ
ムと酸化アルミニウムの合１重１に対して、重量比で１
．５４〜３．００％混入する。Note that chromium oxide is used as a coloring agent to precipitate the green color of the chrysoberyl single crystal. Chromium oxide has a weight ratio of 1 to 1 of beryllium oxide and aluminum oxide.
．． Contains 54 to 3.00%.
第３図に於て、本発明を実施する装置について説明する
。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
。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
、真空あるいは加圧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を移動させ
ることができる。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. 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 in a transparent quartz tube 8, so that the atmosphere can be controlled freely, and it is also possible to apply a vacuum or pressurization. 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 melting zone 9 can be moved over the rod-shaped raw material by moving the rotating shaft 6.7 up and down.
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った。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。The present invention will be described below with reference to Examples.
実施例１
酸化ベリリウム粉末２５ｇ１ガンマアルミナ粉末７５ｇ
、酸化クロム粉末３ｇをボールミルにて混合した後、棒
状に圧縮成型し１２００°Ｃで焼成した。この原料棒を
赤外線集中加熱炉にセットし溶融帯を５閣／ｈｒの速度
で移動させることにより暗緑色のアレキサンドライトの
完全結晶を得た。Example 1 25 g of beryllium oxide powder 1 75 g of gamma alumina powder
After mixing 3 g of chromium oxide powder in a ball mill, the mixture was compression molded into a rod shape and fired at 1200°C. This raw material rod was set in an infrared concentrated heating furnace and the melting zone was moved at a speed of 5 min/hr to obtain a dark green perfect crystal of alexandrite.
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ソベリル単結晶をセ
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０本方法により径１０鵬長さ８ｃｍのアレキサ
ンドライト結晶を得た。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, the seed chrysoberyl single crystal is set on the lower rotating shaft, and the upper and lower rotating shafts are connected. rotate in the opposite direction,
After the molten zone was formed, an alexandrite crystal with a diameter of 10 cm and a length of 8 cm was obtained by the zero method in which a seed crystal was brought into contact with the seed crystal and the molten zone was moved.
実施例３
酸化アルミニウム６０ｇ、酸化ベリリウム５ｇ酸化クロ
ム１ｇ、酸化チタン０．５ｇをボールミル混合し、８０
０°Ｃ，３０ｋｇ／ａｌＴでホットプレス成型して棒状
とした後、赤外線集中加熱装置にセットし、４ ｋｇ／
ｃｆｆｌの酸素圧下で結晶成長を行ないキャッツアイ状
の光条の生ずるクリソベリルを得た。Example 3 60 g of aluminum oxide, 5 g of beryllium oxide, 1 g of chromium oxide, and 0.5 g of titanium oxide were mixed in a ball mill.
After hot press molding at 0°C and 30 kg/alT into a rod shape, it was set in an infrared concentrated heating device and the weight was 4 kg/alT.
Crystal growth was performed under oxygen pressure of cffl to obtain chrysoberyl with cat's-eye striations.
本発明では原料棒の焼結温度を８００ ’Ｃ以上として
いるが、焼結温度が８００°Ｃ以下になると合成単結晶
の中に気泡が残ることがあり、光学的性質や装飾性を著
しく劣化させる。また着色剤として添加する酸化クロム
は酸化ベリリウムと酸化アルミニウムの合算重量の１．
５４〜３．００％の添加量であるが、３．００％を超え
ると酸化クロムの偏析を生じ単結晶の割れ等の惧れがあ
り、また１、５４％より少ないと十分な着色が得られな
い。In the present invention, the sintering temperature of the raw material rod is set to 800°C or higher, but if the sintering temperature is lower than 800°C, air bubbles may remain in the synthesized single crystal, significantly degrading the optical properties and decorativeness. let The amount of chromium oxide added as a coloring agent is 1.0% of the total weight of beryllium oxide and aluminum oxide.
The amount added is 54 to 3.00%, but if it exceeds 3.00%, there is a risk of segregation of chromium oxide and cracking of the single crystal, and if it is less than 1.54%, sufficient coloring may not be obtained. I can't.
本発明によれば材質が均一でしかも着色むらのない大型
の単結晶を提供したものであり、光学的にも装飾的にも
優れたクリソベリル単結晶が得られた。According to the present invention, a large single crystal with uniform material and no uneven coloring was provided, and a chrysoberyl single crystal which was excellent both optically and decoratively was obtained.
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である。
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
以上
出願人 セイコーエプソン株式会社
第１図
第２図
第３図
手続補正書（方式）
１．事件の表示
３、補正する者
事件との関係 出願人
東京都新宿区西新宿２丁目４番１号
（２３６）セイコーエプソン株式会社
代表取締役 中 村 恒 也
手続補正書く自発）
２、発明の名称
クリソベリル単結晶製造法
３、補正する者
本件との関係 出願人
東京都新宿区西新宿２丁目４番１号
（２３６）セイコーエプソン株式会社
代表取締役 中 村 恒 也
４、代理人
〒１０４ 東京都中央区京橋２丁目６番２１号連Ｍｔ
先 ５６３−２１１１ 内線６３１〜６３５ 担当
林明細書
１、発明の名称
クリソベリル単結晶製造法
２、特許請求の範囲
回転楕円鏡体と、その中で各々逆方向に回転し又上下動
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、少くとも酸化ベリリウ
ム粉末とガンマアルミナ粉末及び酸化クロム粉末を混合
して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回転軸間に前記棒状原料
を固定し、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
って移動させ、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
前記溶融帯にお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！ｆ％
、酸化アルミニウム７５〜８５重量％であり、且つ前記
酸化クロムが前記酸化ベリリウムと前記酸化アルミニウ
ムの合算重量に対して１．５４〜３．００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。
３、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。
・一本発明の目的は、容易に大型
クリソベリル単結晶を得ることにある。
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。
クリソベリルはＢｅＡ／！□０４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
試みはＰ ｂ Ｏ−Ｐ ｂ ０＝ＰｂＦｘ系、ＰｂＯＰ
ｂＦｔ Ｂｚ Ｏｓ系、Ｌｌ、ＭＯＯ，−ＭＯＯ□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わ
れてきた。しかし、これらの方法では大結晶を得ること
は難しく、又、この様な方法で作製した結晶は、双晶に
なり易く、単結晶は困難であった。
本発明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Ｂ ｅ ０−Ａｌ１！、 Ｏ，系の状態図を示
す。
図から明らかな如く、Ａｌｔｏｓの重量割合が７５％か
ら８５％の高温度にＢｅＯ・Ａｎｔ’ｓ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３ＢｅＯ・Ａ１□Ｏ５又は、Ｂｅ０・３Ａｌｚ Ｏｓ
とＢ ｅ ０−Ａｊ！ｔ Ｏｘの混晶が生成するのみで
、Ｂｅｄ−Ａｌｅ Ｏｓ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。
棒状原料１の部分に赤外線ＩＲにより溶融帯２を形成す
る。溶融帯２の組成からＡｕｔｏｓ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
°Ｃ以上に保ち、溶融帯を原料枠中上方に移動せしめる
と、溶解帯下部は１８７０’Ｃ以下となり、Ｂｅ０−Ａ
ｆ、０．と融液が共存するＭ域が生成する。この領域に
於て、ＢｅＯ・Ａ／！、Ｏ，は下部原料中に残り、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Ｂ
ｅｏ−Ａ１．ｏ、単結晶のみが残る。下部原料捧即ち、
ＢｅＯＡｌｔｏｓが育成される領域にＢｅＯ・Ａ２□０
．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われる。
尚クリソベリル単結晶の緑色を析出させるために着色剤
として酸化クロムを用いる。酸化クロムは酸化ベリリウ
ムと酸化アルミニウムの合算重量に対して、重量比で１
．５４〜３．００％混入する。
第３図に於て、本発明を実施する装置について説明する
。
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
。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
、真空あるいは加圧することも可能である。棒状原料５
中で温度の上が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を移動させ
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った。
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２５ｇ、ガンマアルミナ粉末７５ｇ
、酸化クロム粉末３ｇをボールミルにて混合した後、棒
状に圧縮成型し１２０６°Ｃで焼成した。この原料棒を
赤外線集中加熱炉にセットし溶融帯を５ｍｍ／ｈｒの速
度で移動させることにより暗緑色のアレキサンドライト
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
にセットシ、下部回転軸に種子クリソベリル単結晶をセ
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０本方法により径１０ａｍ長さ８０のアレキサ
ンドライト結晶を得た。
実施例３
酸化アルミニウム６０ｇ、酸化ベリリウム５ｇ、酸化ク
ロム１ｇ１酸化チタン０．５ｇをポールミル混合し、８
００°Ｃ，３０ｋｇ／ｃ艷でホットプレス成型して棒状
とした後、赤外線集中加熱装置にセットし、４ｋｇ／ｃ
４の酸素圧下で結晶成長を行いキャッツアイ状の光条の
生ずるクリソベリルを得た。
本発明では原料棒の焼結温度をｓ ｏ ｏ ’ｃ以上と
しているが、焼結温度が８００°Ｃ以下になると合成単
結晶の中に気泡が残ることがあり、光学的性質や装飾性
を著しく劣化させる。また着色剤として添加する酸化ク
ロムは酸化ベリリウムと酸化アルミニウムの合算重量の
１．５４〜３．００％の添加量であるが、３．００％を
超えると酸化クロムの偏析を生じ単結晶の割れ等の慣れ
があり、また１、５４％より少ないと十分な着色が得ら
れない。
本発明によれば材質が均一でしかも着色むらのない大型
の単結晶を提供したものであり、光学的にも装飾的にも
優れたクリソベリル単結晶が得られた。又ガンマアルミ
ナ粉末を原料棒に使用することによって原料棒が緻密に
なり反応性が高くなるので、種子同士が着き易くなり、
原料棒段階での空気の取り込みが少なく、気泡の発生が
少なくなるメリットを持つ。
４、図面の簡単な説明
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である。
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
回転輪 ８・・・透明石英管９・・・溶融帯
以上FIG. 1 is a detailed state diagram illustrating the present invention. FIG. 2 is a diagram explaining the present 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... Melting 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 or above Applicant Seiko Epson Corporation Figure 1 Figure 2 Figure 3 Procedural amendment (method) 1. Indication of the case 3, Person making the amendment Relationship with the case Applicant: 2-4-1 Nishi-Shinjuku, Shinjuku-ku, Tokyo (236) Tsuneya Nakamura, Representative Director, Seiko Epson Corporation (Voluntary action to write the amendment) 2. Name of the invention: Chrysoberyl Single crystal manufacturing method 3, Person making the amendment Relationship to the case Applicant: 2-4-1 Nishi-Shinjuku, Shinjuku-ku, Tokyo (236) Representative Director of Seiko Epson Corporation Tsuneya Nakamura 4, Agent: 104 Chuo-ku, Tokyo Kyobashi 2-6-21 Mt.
563-2111 Extension 631-635 Person in charge Hayashi Specification 1, Name of the invention Process for producing chrysoberyl single crystal 2, Claims A spheroidal mirror body, and an upper rotating body that can rotate in opposite directions and move up and down within it. In a single crystal manufacturing method using an infrared concentrated heating furnace having a shaft, a lower rotating shaft, a transparent quartz tube surrounding and sealing the upper and lower rotating shafts, and a halogen lamp or a heating lamp consisting of a halogen lamp, at least beryllium oxide powder and gamma A rod-shaped raw material is formed by mixing and sintering alumina powder and chromium oxide powder, and the heating lamp is placed at one focal point in the spheroidal body, and the rod-shaped raw material is placed at the other focal point on the upper surface of the spheroidal body. The rod-shaped raw material is fixed between rotating shafts, a molten zone is formed on the rod-shaped raw material using infrared rays from the heating lamp, and the molten zone is formed along the rod-shaped raw material by moving the rod-shaped raw material in the longitudinal direction. 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! f%
, aluminum oxide is 75 to 85% by weight, and the chromium oxide is 1.54 to 3.00% by weight based on the total weight of the beryllium oxide and the aluminum oxide. . 3. 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.
-An object of the present invention is to easily obtain large chrysoberyl single crystals. Another object of the present invention is to obtain chrysoberyl single crystals at low cost. Chrysoberyl is BeA/! It has a composition of □04, and cat's eye stone, alexandrite, etc. are famous natural 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 based on PbO-Pb0=PbFx system, PbOP
Several methods have been carried out using fluxes such as bFt Bz Os series, Ll, MOO, -MOO□ series, etc. as fluxes. However, it is difficult to obtain large crystals by these methods, and crystals produced by such methods tend to form twins, making it difficult to produce single crystals. The present invention forms a molten zone in a raw material that has been previously formed into a rod shape using high temperature obtained by concentrating infrared rays,
We also discovered that chrysoberyl single crystals can be easily obtained by moving the melted zone. In Figure 1, B e 0-Al1! , O, shows the state diagram of the system. As is clear from the figure, there is a region where BeO.Ant's and the melt coexist at high temperatures where the weight percentage of Altos is 75% to 85%. Even if it is simply cooled and solidified from this region, 3BeO・A1□O5 or Be0・3Alz Os
and B e 0-Aj! Only a mixed crystal of tOx was generated, and a single crystal of Bed-Ale Os was not obtained. However, by using the method of the present invention, a chrysoberyl single crystal was easily obtained. The principle of the invention is shown in FIG. A molten zone 2 is formed in a portion of the rod-shaped raw material 1 by infrared IR. From the composition of melting zone 2, the weight percentage of Autos is 75%.
Assume that it is between 85% and 85%. The temperature of the melting zone is 1870
When the temperature is kept above °C and the melting zone is moved upward in the raw material frame, the lower part of the melting zone becomes below 1870'C, and Be0-A
f, 0. An M region is formed in which the melt and the melt coexist. In this area, BeO・A/! , O, remain in the lower raw material, and since the melt moves upward along the melting zone, B remains in the lower raw material.
eo-A1. o, only single crystal remains. Lower raw material supply, i.e.
BeO・A2□0 in the area where BeOAltos is grown
．． The presence of a seed crystal facilitates crystallization and results in the formation of a perfect single crystal. Note that chromium oxide is used as a coloring agent to precipitate the green color of the chrysoberyl single crystal. Chromium oxide has a weight ratio of 1 to the total weight of beryllium oxide and aluminum oxide.
．． Contains 54 to 3.00%. Referring to FIG. 3, an apparatus for implementing the present invention will be described. 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. 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 shaft 6.7 are sealed in a transparent quartz tube 8, so that the atmosphere can be controlled freely, and it is also possible to apply a vacuum or pressurization. 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 melting zone 9 can be moved over the rod-shaped raw material by moving the rotating shaft 6.7 up and down. By using the method of the present invention, it has become possible to produce a large perfect chrysoberyl single crystal without twins. The present invention will be described below with reference to Examples. Example 1 25g of beryllium oxide powder, 75g of gamma alumina powder
After mixing 3 g of chromium oxide powder in a ball mill, the mixture was compression molded into a rod shape and fired at 1206°C. This raw material rod was set in an infrared concentrated heating furnace and the melting zone was moved at a speed of 5 mm/hr to obtain a dark green perfect crystal of alexandrite. Example 2 From beryllium oxide, aluminum oxide, and chromium oxide,
Only the part that will become the molten zone at one end of the raw material rod is made of 80% aluminum oxide and 20% beryllium oxide, and a chrysoberyl single crystal is set on the upper rotating shaft and the seed chrysoberyl single crystal is set on the lower rotating shaft. rotate in the opposite direction,
After the molten zone was formed, an alexandrite crystal having a diameter of 10 am and a length of 80 mm was obtained by the 0-line method in which a seed crystal was brought into contact with the seed crystal and the molten zone was moved. Example 3 60 g of aluminum oxide, 5 g of beryllium oxide, 1 g of chromium oxide, 0.5 g of titanium oxide were mixed in a pole mill,
After hot press molding at 00°C and 30kg/c to form a rod, it was set in an infrared concentrated heating device and heated to 4kg/c.
Crystal growth was performed under an oxygen pressure of 4 to obtain chrysoberyl with cat's eye-shaped striations. In the present invention, the sintering temperature of the raw material rod is set to be above 800°C, but if the sintering temperature is below 800°C, air bubbles may remain in the synthesized single crystal, which may deteriorate the optical properties and decorative properties. cause significant deterioration. In addition, the amount of chromium oxide added as a coloring agent is 1.54 to 3.00% of the total weight of beryllium oxide and aluminum oxide, but if it exceeds 3.00%, segregation of chromium oxide may occur, causing cracks in the single crystal. If the amount is less than 1.54%, sufficient coloring cannot be obtained. According to the present invention, a large single crystal with uniform material and no uneven coloring was provided, and a chrysoberyl single crystal which was excellent both optically and decoratively was obtained. In addition, by using gamma alumina powder in the raw material rod, the raw material rod becomes denser and more reactive, making it easier for seeds to stick to each other.
It has the advantage of less air being taken in at the raw material rod stage, which reduces the generation of air bubbles. 4. Brief Description of the Drawings FIG. 1 is a state diagram illustrating the present invention in detail. FIG. 2 is a diagram explaining the present 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... Melting zone 3...
Spheroidal mirror body 4...Halogen lamp 5...
Rod-shaped raw material 6... Upper rotating shaft 7... Lower rotating wheel 8... Transparent quartz tube 9... Above the molten zone
Claims (1)
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、少くとも酸化ベリリウ
ムと酸化アルミニウム及び酸化クロムを混合して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回転軸間に前記棒状
原料を固定し、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
に沿って移動させ、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、
且つ前記溶融帯にお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％であり、且つ
前記酸化クロムが前記酸化ベリリウムと前記酸化アルミ
ニウムの合算重量に対して１．５４〜３．００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。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 body, a transparent quartz tube that surrounds and seals the vertical rotating shaft, and a halogen lamp or a heating lamp that is a halogen lamp. In a single crystal manufacturing method using an infrared concentrated heating furnace having
A rod-shaped raw material is sintered at a temperature of 0.degree. is fixed, a molten zone is formed on the rod-shaped raw material using infrared rays of the heating lamp, and the molten zone is moved along the rod-shaped raw material by moving the rod-shaped raw material in the longitudinal direction, and at the same time, the lower part of the molten zone is moved. a single crystal is formed in the molten metal, and further the melting zone temperature 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 and 75 to 85% by weight of aluminum oxide, and the chromium oxide is added to the total weight of the beryllium oxide and the aluminum oxide. A method for producing a chrysoberyl single crystal, characterized in that the amount is 1.54 to 3.00% by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26121987A JPS63260894A (en) | 1987-10-16 | 1987-10-16 | Synthesis method of chrysoberyl cat's eye single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26121987A JPS63260894A (en) | 1987-10-16 | 1987-10-16 | Synthesis method of chrysoberyl cat's eye single crystal |
Related Parent 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 |
|---|---|
| JPS63260894A true JPS63260894A (en) | 1988-10-27 |
| JPH0329758B2 JPH0329758B2 (en) | 1991-04-25 |
Family
ID=17358796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26121987A Granted JPS63260894A (en) | 1987-10-16 | 1987-10-16 | Synthesis method of chrysoberyl cat's eye single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63260894A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS546900A (en) * | 1977-06-17 | 1979-01-19 | Seiko Epson Corp | Production of clean beryl single crystal |
| JPS60260495A (en) * | 1985-04-05 | 1985-12-23 | Seiko Epson Corp | Preparation of single crystal of chrysoberyl |
-
1987
- 1987-10-16 JP JP26121987A patent/JPS63260894A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS546900A (en) * | 1977-06-17 | 1979-01-19 | Seiko Epson Corp | Production of clean beryl single crystal |
| JPS60260495A (en) * | 1985-04-05 | 1985-12-23 | Seiko Epson Corp | Preparation of single crystal of chrysoberyl |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0329758B2 (en) | 1991-04-25 |
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