JPS632899A - Production of alexandrite single crystal - Google Patents
Production of alexandrite single crystalInfo
- Publication number
- JPS632899A JPS632899A JP5826387A JP5826387A JPS632899A JP S632899 A JPS632899 A JP S632899A JP 5826387 A JP5826387 A JP 5826387A JP 5826387 A JP5826387 A JP 5826387A JP S632899 A JPS632899 A JP S632899A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- sintered
- single crystal
- alexandrite
- boundary face
- 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 44
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002994 raw material Substances 0.000 claims abstract description 35
- 238000002844 melting Methods 0.000 claims abstract description 19
- 230000008018 melting Effects 0.000 claims abstract description 19
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 10
- 150000002367 halogens Chemical class 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 24
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 10
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 10
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 claims description 7
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- KQHXBDOEECKORE-UHFFFAOYSA-L beryllium sulfate Chemical compound [Be+2].[O-]S([O-])(=O)=O KQHXBDOEECKORE-UHFFFAOYSA-L 0.000 abstract description 6
- 230000002706 hydrostatic effect Effects 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 2
- 229910052593 corundum Inorganic materials 0.000 abstract 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229940037003 alum Drugs 0.000 description 2
- FOJJCOHOLNJIHE-UHFFFAOYSA-N aluminum;azane Chemical group N.[Al+3] FOJJCOHOLNJIHE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052614 beryl Inorganic materials 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は棒状焼結体に赤外線を回転楕円面鏡により集中
して溶融帯を形成し、溶融帯の一界面で溶融を行ない、
他方の界面でＣ軸方向に育成させて得られる変色性を示
すアレキサンドライト単結晶の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention focuses infrared rays on a rod-shaped sintered body using a spheroidal mirror to form a molten zone, and performs melting at one interface of the molten zone.
The present invention relates to a method for producing an alexandrite single crystal that exhibits discoloration and is grown in the C-axis direction at the other interface.
本発明の目的は双晶や包含物がなく自然光下で暗緑色、
人工光下で赤色を呈する変色性の顕著な高品質アレキサ
ンドライト単結晶を提供することにある。The purpose of the present invention is to produce a dark green color under natural light without twins or inclusions.
The object of the present invention is to provide a high-quality alexandrite single crystal with remarkable discoloration that exhibits a red color under artificial light.
本発明の他の目的は低コストでしかも短期間で大型アレ
キサンドライト単結晶を提供することにある。Another object of the present invention is to provide large alexandrite single crystals at low cost and in a short period of time.
アレキサンドライトはベリリウムとアルミニウムの２成
分酸化物（ＢｅＡＱ２０４ ）中に酸化クロムや酸化鉄
、等が固溶したクリンベリルの一種であり、高い硬度、
高融点、化学耐久性を示す斜方晶系の結晶である。自然
光下では暗緑色を呈し。Alexandrite is a type of green beryl in which chromium oxide, iron oxide, etc. are dissolved in a binary oxide of beryllium and aluminum (BeAQ204), and it has high hardness and
It is an orthorhombic crystal with a high melting point and chemical durability. It appears dark green under natural light.
人工打丁では赤色を呈する代表的な宝石として著名であ
る。レーザーのホスト材料としても注目されている。こ
れを人工的に得ようとする試みは古来種々性なわれてお
り、フラックス法、引き上げ法により試みられているが
高品質大皿単結晶を得るまでには至っていない、即ちフ
ラックス法の場合双晶が生じやすく、添加物が固溶し難
く、又育成に長期間を要する。引き上げ法の場合にはア
レキサンドライトが１８７０℃の融点である為にイリジ
ウム等の高価格貴金属を用いなければならず、このルツ
ボ材料が抱合物として結晶中に入り込む等の不都合が生
じやすく良品質単結晶は得られていない。It is famous as a typical red-colored gemstone in artificially carved knives. It is also attracting attention as a host material for lasers. There have been various attempts to obtain this artificially since ancient times, and attempts have been made using the flux method and the pulling method, but they have not reached the point of obtaining a high-quality large plate single crystal.In other words, in the case of the flux method, twin crystals It is difficult for additives to form a solid solution, and it takes a long time to grow. In the case of the pulling method, since alexandrite has a melting point of 1870°C, expensive precious metals such as iridium must be used, and this crucible material tends to enter the crystal as conjugates, resulting in problems such as high-quality single crystals. has not been obtained.
本発明は全く新規なる方法で高品質大工アレキサンドラ
イト単結晶を得るものである。The present invention provides a completely new method for obtaining high quality carpenter alexandrite single crystals.
本発明の要旨は酸化アルミニウムと酸化ベリリウムのほ
ぼ等モル割合の組成の棒状高密度焼結体原料にハロゲン
ランプかキセノンランプより発せられる赤外線を回転楕
円面鏡により集光して原料棒の先端に溶融帯を形成し、
この溶融帯に種子結晶を接触させ、徐々に溶融帯を原料
棒中を移動させて種子結晶側の界面で結晶化を行ない、
他方の界面で原料の溶融を行なって結晶育成に伴う溶融
液の減少をおぎなう操作を継続していく育成製造法であ
る。棒状高密度焼結体の出発原料は酸化アルミニウムに
ついてはアンモニウムアルミニウムミョウバンを９００
℃乃至１２００”Ｃで焼結し、酸化ベリリウムについて
は硫酸ベリリウムを９００℃乃至１２００℃で焼成した
ものを用い、更に酸化クロムもしくは酸化鉄の少なくと
も一方を０゜０５重量パーセント乃至５重量パーセント
添加して用いられる。焼成温度が９００℃に達しない場
合には反応が完全に終了せず未反応成分が高密度焼結体
の中に混入し結晶化を妨げる。又焼成温度が１２００℃
を超える場合は原料粉末の粒子径が大きく成長しすぎ高
密度焼結体が得られなくなる。The gist of the present invention is to focus infrared rays emitted from a halogen lamp or a xenon lamp onto a rod-shaped high-density sintered raw material with a composition of approximately equimolar proportions of aluminum oxide and beryllium oxide, and direct it to the tip of the raw material rod. forming a molten zone,
A seed crystal is brought into contact with this molten zone, and the molten zone is gradually moved through the raw material rod to cause crystallization at the interface on the seed crystal side.
This is a growth production method in which the raw material is melted at the other interface and the operation is continued to reduce the amount of melt that accompanies crystal growth. The starting material for the rod-shaped high-density sintered body is ammonium aluminum alum at 900% for aluminum oxide.
℃ to 1200"C, and for beryllium oxide, beryllium sulfate sintered at 900℃ to 1200℃ is used, and at least one of chromium oxide or iron oxide is added from 0.05% by weight to 5% by weight. If the firing temperature does not reach 900°C, the reaction will not complete and unreacted components will mix into the high-density sintered body, hindering crystallization.Also, if the firing temperature does not reach 1200°C
If it exceeds this, the particle size of the raw material powder will grow too large, making it impossible to obtain a high-density sintered body.
又酸化鉄もしくは酸化クロムが０．０５重量パーセント
に達しない場合はほとんど着色がみられず又、赤外線の
吸収能が悪くなる為に結晶化が妨げられる。この場合、
酸化クロム、酸化鉄は着色剤として作用するが、これら
酸化クロム、酸化鉄が少ないと溶融部分は透明状となり
集中照射される赤外線の吸収が悪くなり溶融が均一に、
良質に行なえないものである。従って本発明の如き赤外
線照射が集中して溶融帯域が形成される製造方法におい
ては発色剤としての酸化クロム、酸化鉄が０゜０５重量
パーセント以上含有することはアレキサンドライトの美
麗な色調をもたらす上において、赤外線の集中照射によ
る良質な溶融帯域な形成する上においても極めて重要な
ことである。又、酸化クロム、酸化鉄が５重量パーセン
トを超えると結晶中に偏析を起して混在物として結晶性
を劣化させてしまう、成製はゴム製袋に粉末を充填し静
水圧でバインダーを用いずにラバープレスして棒状に作
製する。焼結は通常鹸化性雰囲気中で１３００℃乃至１
７００℃で行なわれる。この場合１３００℃未満である
と各原料（酸化アルミニウム、酸化ベリリウム、融化ク
ロム、酸化鉄）同士は完全な同相反応が起こらなくなり
、原料棒の各原料が均一状態とならないことから、均−
買のアレキサンドライトが得られなくなる。−方、１７
００℃を超えると各原料が還元されやすくなり原料棒か
ら７レキサンドライトが形成される際気泡が生じやすく
、又電気炉の耐久性が劣ることになる。Further, if the amount of iron oxide or chromium oxide is less than 0.05% by weight, almost no coloring is observed and crystallization is hindered due to poor infrared absorbing ability. in this case,
Chromium oxide and iron oxide act as coloring agents, but if there is little of these chromium oxide and iron oxide, the melted part will become transparent and the absorption of concentrated infrared rays will be poor, resulting in uniform melting.
It cannot be done in good quality. Therefore, in the production method of the present invention in which infrared rays are concentrated to form a melting zone, it is important to contain 0.05% by weight or more of chromium oxide and iron oxide as coloring agents in order to obtain a beautiful color tone of alexandrite. This is extremely important in forming a high-quality melting zone by concentrated infrared irradiation. In addition, if chromium oxide or iron oxide exceeds 5% by weight, they will segregate in the crystal and deteriorate crystallinity as inclusions.For production, fill a rubber bag with powder and use a binder with hydrostatic pressure. Rubber press to make a rod shape. Sintering is usually carried out at 1300°C to 1°C in a saponifying atmosphere.
It is carried out at 700°C. In this case, if the temperature is below 1300°C, a complete in-phase reaction will not occur between the raw materials (aluminum oxide, beryllium oxide, fused chromium, iron oxide), and the raw materials in the raw material rod will not be in a uniform state.
Buy Alexandrite will no longer be available. - direction, 17
If the temperature exceeds 00°C, each raw material is likely to be reduced, bubbles are likely to be generated when lexandrite is formed from the raw material rod, and the durability of the electric furnace is deteriorated.
従って原料棒を得るだめの焼結温度は１３００℃乃至１
７００℃が好適である。−方、この原料棒の焼結時の雰
囲気は酸化性雰囲気とすることにより良質なアレキサン
ドライトが得られる。即ち、非酸化性雰囲気中でこの焼
結を行なうと、各原料は酸化物であるから各原料が還元
されやすくなり原料棒の溶解状態から結晶化される際に
その結晶物中に気泡が生じ、良質なアレキサンドライト
が得られないことになる。又、原料棒の溶解、結晶化を
空気などの酸化性雰囲気中で行なうことも上記の如く原
料棒を還元化させることがなく、従って気泡のない良質
なアレキサンドライトが得られるものである。−方、種
子結晶は望ましくはＣ軸方向に長い棒状のものが良いが
必ずしもこだわる必要はないが最大育成方向は種子結晶
のＣ軸方向に一致させると円柱状の完全なる単結晶を得
ることができる。他の方向に育成させるとＣ軸に垂直な
る面が生じ偏平状の結晶となってしまう、この様にして
均一に着色した包含物のない円柱棒状の大皿単結晶が得
られた。Therefore, the sintering temperature for obtaining the raw material rod is 1300℃ to 1
700°C is preferred. - On the other hand, good quality alexandrite can be obtained by setting the atmosphere during sintering of this raw material rod to an oxidizing atmosphere. That is, when this sintering is performed in a non-oxidizing atmosphere, each raw material is an oxide, so each raw material is easily reduced, and when the raw material rod is crystallized from the melted state, bubbles are generated in the crystal. , good quality alexandrite cannot be obtained. Further, melting and crystallizing the raw material rod in an oxidizing atmosphere such as air does not reduce the raw material rod as described above, and therefore, good quality alexandrite without bubbles can be obtained. - On the other hand, it is preferable that the seed crystal be long in the C-axis direction, but it is not necessary to be particular about this, but if the maximum growth direction is aligned with the C-axis direction of the seed crystal, it is possible to obtain a complete cylindrical single crystal. can. If grown in any other direction, a plane perpendicular to the C-axis would be produced, resulting in a flat crystal.In this way, a uniformly colored, cylindrical, rod-shaped, large plate single crystal without inclusions was obtained.
第１図に本発明方法の概要を示す。FIG. 1 shows an outline of the method of the present invention.
回転楕円面鏡体１は二つの焦点を持っている。The spheroidal mirror body 1 has two focal points.
−焦点にハロゲンランプ又はキセノンランプを配置し、
他方の焦点には棒状原料３を配置する。棒状原料３は上
部回転４により保持されている。又種子結晶５は下部回
転軸６にセットされている、棒状原料３、種子結晶５、
上下回転軸４，６は透明石英管７内に封入されており雰
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３中で瀧度が上がり溶融
帯８の形成されるのは焦点に完全に一致した部分のみで
ある。溶融帯８は回転軸４，６を上方あるいは下方に移
動させることにより相対的に移動される。操作はまず原
料棒３の先端に赤外線を集中させて溶融帯８を形成し、
しかるのちに種子結晶５を上方に移動して溶融帯８を接
触させる。平衡状態になったのを確認した後回転軸４，
６を移動すると種子結晶５が成長した状態で透明単結晶
が得られる。即ち溶融帯８と原料棒３の界面での原料の
溶融が起り、溶融帯８と結晶５の界面では結晶化が行な
われている。- placing a halogen or xenon lamp at the focal point;
A rod-shaped raw material 3 is placed at the other focal point. The rod-shaped raw material 3 is held by an upper rotation 4. Further, the seed crystal 5 is set on the lower rotating shaft 6, and includes a rod-shaped raw material 3, a seed crystal 5,
The upper and lower rotating shafts 4 and 6 are enclosed in a transparent quartz tube 7, so that the atmosphere can be freely controlled, and it is also possible to use vacuum or pressurization. In the rod-shaped raw material 3, the degree of melting increases and a molten zone 8 is formed only in a portion that completely coincides with the focal point. The melting zone 8 is relatively moved by moving the rotating shafts 4 and 6 upward or downward. The operation begins by concentrating infrared rays on the tip of the raw material rod 3 to form a molten zone 8.
Thereafter, the seed crystal 5 is moved upward to contact the molten zone 8. After confirming that the equilibrium state has been reached, rotate the rotating shaft 4,
6, a transparent single crystal is obtained with the seed crystal 5 grown. That is, melting of the raw material occurs at the interface between the melting zone 8 and the raw material rod 3, and crystallization occurs at the interface between the melting zone 8 and the crystals 5.
この方法は次の様な数々の特徴及びメリットを持ってい
る。This method has a number of features and advantages, including:
１、高温が容易に得られる為に操作上の安全性が非常に
高い０例えばベルヌーイ法の場合には酸素ガスと水素ガ
スを用いる為に高度のテクニックが必要であり、爆発の
危険に常にさらされているが末法では操作は容易で特別
な経験或いはテクニックを必要とせず、又危険性は全く
ない。1. Operational safety is very high because high temperatures can be easily obtained. For example, in the Bernoulli method, advanced techniques are required because oxygen gas and hydrogen gas are used, and there is always a risk of explosion. However, the final method is easy to operate, does not require any special experience or technique, and is completely free of danger.
２、雰囲気及び圧力のコントロールが可能である為に分
解しやすい化合物あるいは酸化されやすい化合物も結晶
化が容易である。2. Since the atmosphere and pressure can be controlled, compounds that are easily decomposed or easily oxidized can be easily crystallized.
３、赤外線により加熱が行なわれるので高周波誘導加熱
のできない酸化物等の単結晶の育成ができる。ルツボを
用いない為に当然不純物の混入が非常に少ない、溶融帯
の形成はハロゲンランプでは１９００℃、キセノンラン
プでは２８００ ’Ｃまで行なえるので、本発明では主
にハロゲンランプが用いられる。3. Since heating is performed by infrared rays, it is possible to grow single crystals such as oxides that cannot be heated by high frequency induction heating. Since a crucible is not used, naturally there is very little contamination of impurities, and a molten zone can be formed at temperatures up to 1900° C. with a halogen lamp and 2800° C. with a xenon lamp, so halogen lamps are mainly used in the present invention.
４、ハロゲンランプ、キセノンランプは非常に出力が安
定しており、又コントロールも非常に容易である。その
為に溶融帯も非常に安定しており。4. Halogen lamps and xenon lamps have very stable output and are very easy to control. Therefore, the molten zone is also very stable.
必ずしも種子単結晶を用いなくても結晶化が行なえる。Crystallization can be carried out without necessarily using a seed single crystal.
５、溶融状態を監視できる為、結晶成長の様子が観察で
きる。5. Since the melting state can be monitored, the state of crystal growth can be observed.
以下に本発明について更に詳しく述べる。The present invention will be described in more detail below.
棒状原料は結晶の品質を良くする為にはできるだけ高密
度に焼結されていなければならない、その為には酸化ア
ルミニウム、酸化ベリリウムはできるだけ粒子径の細か
い粉末が用いられる。セの為にアンモニウムアルミニウ
ムミョウバン、硫酸ベリリウムを９００℃乃至１２００
℃で焼結したものが用いられる。この酸化アルミニウム
、酸化ベリリウムに酸化クロムあるいは酸化鉄のいずれ
か一方もしくは両方を０．０５重量パーセント乃至５重
量パーセント添加し、ラバープレス法で成製し、電気炉
で１３００℃乃至１７００℃で焼結する。装置はハロゲ
ンランプを２個装着した双楕円型赤外線集中加熱装置を
用いることにより大聖の単結晶が得られる。育成条件は
上下回転軸の回転数がそれぞれ４０〜６０ｒｐｍで逆方
向に回転し、成長速度は２〜５ ｍｍ ／ Ｈで雰囲気
は空気である０種子結晶の方位は背面ラウ加工もしくは
プリセッシ璽ン法で決められる。In order to improve the quality of the crystals, the rod-shaped raw material must be sintered as densely as possible, and for this purpose aluminum oxide and beryllium oxide powders with as fine particle size as possible are used. ammonium aluminum alum and beryllium sulfate at 900°C to 1200°C.
The material sintered at ℃ is used. 0.05% to 5% by weight of either chromium oxide or iron oxide or both is added to the aluminum oxide or beryllium oxide, produced by a rubber press method, and sintered at 1300°C to 1700°C in an electric furnace. do. The device uses a bielliptical infrared concentrated heating device equipped with two halogen lamps to obtain a single crystal of Daisei. The growth conditions are that the upper and lower rotational axes rotate in opposite directions at 40 to 60 rpm, the growth rate is 2 to 5 mm/H, and the atmosphere is air.The orientation of the seed crystal is back-row processing or precession method. It can be determined by
以下に実施例について本発明を説明する。The invention will be explained below with reference to examples.
［実施例］
酸化アルミニウムと酸化ベリリウムがモル割合でｌ：１
の粉末に０．５重量パーセントの酸化クロム、３．０重
量パーセントの酸化鉄を添加し。[Example] Aluminum oxide and beryllium oxide in a molar ratio of 1:1
0.5 weight percent chromium oxide and 3.0 weight percent iron oxide were added to the powder.
１５００℃で焼結した原料棒を用い、ｌ、５ｋＷのハロ
ゲンランプを２個用いた双楕円製回転楕円面鏡体で育成
した０種子結晶としてＣ軸に長い単結晶を回転軸の延長
方向にセットした０回転速度は４Ｏｒｐｍで成長速度は
５ ｍ＋ａ ／ Ｈで行なうと個溶限以上の酸化鉄包含
物となったリフラックが生じたが２ ＋ｎ ／ Ｈで行
なうと透明な完全な単結晶が得られた。この単結晶は自
然光でやや茶色を帯びた暗緑色で、電灯光下で赤色を呈
した。Using a raw material rod sintered at 1500°C, a single crystal long along the C axis is grown as a zero-seed crystal grown in a bielliptic spheroid mirror using two 5kW halogen lamps in the direction of extension of the rotation axis. When the 0 rotation speed was set to 4 Orpm and the growth rate was 5 m+a/H, reflux occurred which resulted in iron oxide inclusions exceeding the solubility limit, but when carried out at 2+n/H, a transparent perfect single crystal was obtained. It was done. This single crystal was dark green with a slight brown tinge under natural light, and red under electric light.
第１図は本発明方法の原理を説明する図である。 １・・・・・・回転楕円面鏡体 ２・・・…ハロゲンランプ ３・・・・・・棒状原料 ４・・・・・・上部回転軸 ５・・・・・・種子結晶 ６・・・・・・下部回転軸 ７・・・・・・石英管 ８・・・・・・溶融帯 以 上 FIG. 1 is a diagram explaining the principle of the method of the present invention. 1...Spheroidal mirror body 2...Halogen lamp 3... Rod-shaped raw material 4... Upper rotating shaft 5...Seed crystal 6...Lower rotating shaft 7...Quartz tube ８・・・・・・Melting zone that's all
Claims (1)
割合の組成物に酸化クロムもしくは酸化鉄の少なくとも
一方を０．０５重量パーセントないし５重量パーセント
添加し酸化性雰囲気中で１３００℃乃至１７００℃の温
度範囲で焼結した棒状高密度焼結体原料に、ハロゲンラ
ンプもしくはキセノンアークランプから発する赤外線を
回転楕円面鏡により集中して空気中にて溶融帯域を形成
し、かつ前記原料を移動させることにより、該溶融帯域
の一方の界面において原料の溶融を行ない、他方の界面
において種子結晶上に結晶育成を行なうことを特徴とす
るアレキサンドライト単結晶の製造法。(1) 0.05% to 5% by weight of at least one of chromium oxide or iron oxide is added to a composition containing aluminum oxide and beryllium oxide in approximately equimolar proportions, and the temperature range is from 1300°C to 1700°C in an oxidizing atmosphere. By concentrating infrared rays emitted from a halogen lamp or xenon arc lamp on a rod-shaped high-density sintered raw material sintered with a spheroidal mirror to form a molten zone in the air, and moving the raw material, A method for producing an alexandrite single crystal, characterized in that a raw material is melted at one interface of the melting zone, and crystals are grown on a seed crystal at the other interface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5826387A JPS632899A (en) | 1987-03-13 | 1987-03-13 | Production of alexandrite single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5826387A JPS632899A (en) | 1987-03-13 | 1987-03-13 | Production of alexandrite single crystal |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13432578A Division JPS5562890A (en) | 1978-10-31 | 1978-10-31 | Production of alexandrite single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS632899A true JPS632899A (en) | 1988-01-07 |
| JPH0361635B2 JPH0361635B2 (en) | 1991-09-20 |
Family
ID=13079275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5826387A Granted JPS632899A (en) | 1987-03-13 | 1987-03-13 | Production of alexandrite single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS632899A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912521A (en) * | 1973-04-30 | 1975-10-14 | Creative Crystals Inc | Synthetic crystal and method of making same |
| JPS5562890A (en) * | 1978-10-31 | 1980-05-12 | Seiko Epson Corp | Production of alexandrite single crystal |
-
1987
- 1987-03-13 JP JP5826387A patent/JPS632899A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3912521A (en) * | 1973-04-30 | 1975-10-14 | Creative Crystals Inc | Synthetic crystal and method of making same |
| JPS5562890A (en) * | 1978-10-31 | 1980-05-12 | Seiko Epson Corp | Production of alexandrite single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0361635B2 (en) | 1991-09-20 |
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