JPS58167495A - Synthesis of artificial beryl single crystal - Google Patents

Synthesis of artificial beryl single crystal

Info

Publication number
JPS58167495A
JPS58167495A JP4797282A JP4797282A JPS58167495A JP S58167495 A JPS58167495 A JP S58167495A JP 4797282 A JP4797282 A JP 4797282A JP 4797282 A JP4797282 A JP 4797282A JP S58167495 A JPS58167495 A JP S58167495A
Authority
JP
Japan
Prior art keywords
beryl
solvent
single crystal
artificial
added
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
Application number
JP4797282A
Other languages
Japanese (ja)
Other versions
JPH0235719B2 (en
Inventor
Toshiyuki Hirose
広瀬 敏幸
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Matsushima Kogyo KK
Seiko Epson Corp
Suwa Seikosha KK
Original Assignee
Matsushima Kogyo KK
Seiko Epson Corp
Suwa Seikosha KK
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Matsushima Kogyo KK, Seiko Epson Corp, Suwa Seikosha KK filed Critical Matsushima Kogyo KK
Priority to JP4797282A priority Critical patent/JPH0235719B2/en
Publication of JPS58167495A publication Critical patent/JPS58167495A/en
Publication of JPH0235719B2 publication Critical patent/JPH0235719B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B9/00Single-crystal growth from melt solutions using molten solvents

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

PURPOSE:To obtain high-quality artificial beryl single crystal efficiently and inexpensively, by blending BeO with Al2O3, SiO2, etc. in a given ratio, adding cesium element and a solvent to the blend, heating it to form a molten salt, annealing it so that a crystal is grown. CONSTITUTION:BeO is blended with Al2O3 and SiO2 approximately in a beryl composition ratio, and, if necessary, a colorant such as chromium oxide, etc. is added to it. To the prepared raw material substance is added a solvent selected from lithium molybdate, molybdenum dioxide, vanadium pentoxide, etc., stress in the growing crystal is released, in order to prevent the occurrence of cracks, cesium element is previously added to the solvent. The blend is heated to a temperature >= the melting point of the solvent to form a molten salt, after a given time, a beryl seed crystal is added to the salt, which is annealed to grow an artificial beryl single crystal. The prepared single crystal is used as a jewel such as emerald, etc.

Description

【発明の詳細な説明】 本発明は溶剤(7ラツクス)を用いた人工ベリル単結晶
の合成方法に関し、詳しくは溶融塩より良質なベリル単
結晶を効率よく且つ経済的に合成する方法に関するもの
である。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for synthesizing an artificial beryl single crystal using a solvent (7 lux), and more specifically to a method for efficiently and economically synthesizing beryl single crystals of better quality than molten salt. be.

エメラルドに代表される単結晶ベリルは近年需要も増大
の傾向、にある、大工ベリルの合成方法としては水熱法
、fm剤を用いた溶融塩法が知られているが本発明は、
この溶融塩法の改良に属する。
The demand for single-crystal beryl, represented by emerald, has been increasing in recent years. Hydrothermal methods and molten salt methods using FM agents are known as methods for synthesizing carpenter beryl, but the present invention
This belongs to an improvement of the molten salt method.

溶融塩法は、はぼベリルの組成比を示す、酸化ベリリウ
ム、II化ア、8−イエつム及び二酸化ケイ素必要に応
じて酸化り四ム及び酸化ニッケル、酸化鉄、酸化コパル
)$m化マンガンその他の補助着色剤もしくはドープ剤
からなる原料物質に溶剤としての五酸化バナジウム、モ
リブデン酸リチウム、三酸化モリブデン等の溶剤から選
ばれた1種もしくは2種以上を加え、これを上記溶剤の
溶融温度以上に加熱して溶融塩を形成して、この溶融塩
を一定温度で長時間保持するか、一定時間保持後、ゆる
やかな濃度勾配をもって除冷するかいずれかの操作で溶
融塩中にベリル種子結晶を配置することによりこの種子
結晶の囲りに人工ベリルを生成又は育成する方法である
The molten salt method shows the composition ratio of beryl, beryllium oxide, aluminum II oxide, 8-yetum, and silicon dioxide (as required, tetramuth oxide and nickel oxide, iron oxide, copal oxide). Add one or more solvents selected from vanadium pentoxide, lithium molybdate, molybdenum trioxide, etc. as a solvent to the raw material consisting of manganese and other auxiliary colorants or doping agents, and melt the above solvent. Beryl is added to the molten salt by heating it above temperature to form a molten salt, and then holding the molten salt at a constant temperature for a long time, or by holding it for a certain period of time and gradually cooling it with a gentle concentration gradient. This is a method of generating or growing artificial beryl around seed crystals by arranging them.

この様に溶融塩法は融点以上、通常700℃〜1200
℃の温度範囲において生成又は育成することができるが
、結晶中にインクルージ1ンを含まない良質のベリル単
結晶育成となるとルツボ炉の温度プロファイル、成長ス
ピード、溶剤のmm等いくつかの管理すべきlインドが
ある。またインクルージ璽ンには大きくわけて溶融塩を
とり込んだもの、すなわちフェザ−インクルージーンと
、7−エナヤイト等同−ルツボ内でベリルと同様に生成
する結晶物岬をとり込んだものがあり、宝石としても最
も主要なポイントである透明度低下の主原因になってい
る。これらのインクルージ。
In this way, the molten salt method uses temperatures above the melting point, usually 700°C to 1200°C.
Although it can be produced or grown in the temperature range of ℃, in order to grow a high-quality beryl single crystal that does not contain inclusions in the crystal, there are several controls such as the temperature profile of the crucible furnace, growth speed, and the mm of solvent. There is India. In addition, there are two main types of Incluge capes: those that incorporate molten salts, namely, those that incorporate molten salts, and those that incorporate crystalline capes that are produced in the same crucible as 7-enayaite in the same way as beryl. This is the main cause of the decrease in transparency, which is the most important point in jewelry. These include.

ンは溶融塩法による人工ベリル単結晶合成においては現
段階まではさけられないことであり、これが人工ベリル
単結晶の品質上最大の問題となっている。なぜフェザ−
インクルージ曹ンが発生するかその原因は結晶成長中に
ディスロケーシ璽ンを起し結果的には歪が発生しある時
点までいくと歪が解放させる歪が解放された部分はりラ
ックとなり、クラック部分に7ラツクスが流入すること
によりフェザ−インクルージ冒ンとなるためである、ク
ラックを押える方法としては、成長スピードのコントロ
ール及び、歪解放剤の添加によりインクルージ曹ンの発
生管防止することができる。本発明は、曽に応力解鰍を
しクラックを発生させないために、溶剤中にセシウムを
添加したことを特徴としたものであり、本発明の効果な
より一層明確にするために実施例をまじえて詳細に説明
する実施例1 (1)原料物質、溶剤ならびに配合 ベリル粉末  10F VxOi    100 f MOon    10 Of LitMOO畠 100f yH8・     3t OrlOl     (L 2 f (2)装置及び方法 上記物質を白金ルツボ内に充填し加熱は図1の装置を用
い950℃昇温し950℃になりてから24H後に種子
結晶を投入しその後−夕月後に取り出し観察した。
This is unavoidable at this stage in the synthesis of artificial beryl single crystals by the molten salt method, and this is the biggest problem in terms of the quality of artificial beryl single crystals. why feather
The cause of occurrence of inclusion cracks is that dislocation occurs during crystal growth, resulting in distortion, and when it reaches a certain point, the distortion releases.The released part becomes a beam rack, and cracks occur. This is due to the inflow of 7 lux into the part, which causes feather inclusion damage.The way to suppress cracks is to control the growth speed and prevent the occurrence of inclusion carbon by adding a strain release agent. Can be done. The present invention is characterized in that cesium is added to the solvent in order to relieve stress and prevent the occurrence of cracks.In order to further clarify the effects of the present invention, Examples are included. Example 1 (1) Raw material, solvent, and blended beryl powder 10F VxOi 100 f MOon 10 Of LitMOO Hatake 100 f yH8・3t OrlOl (L 2 f) (2) Apparatus and method The above materials were placed in a platinum crucible. For filling and heating, the temperature was raised to 950° C. using the apparatus shown in FIG. 1, and 24 hours after the temperature reached 950° C., seed crystals were put in, and then taken out and observed after sunset.

(3)結果 ベリル単結晶が2swa〜5■成長しておりかつインク
ルージ請′ンの発生が見られない良質なものが得られた
(3) As a result, a good quality product was obtained in which the beryl single crystal had grown from 2 to 5 cm and no inclusion defects were observed.

実施例2 (1)原料物質、溶剤ならびに配合 実施例1に同じ (Z)装置及び方法 950℃昇温度24後に種子結晶投入 その後α1℃/Hrasocまで除冷 (3)結果 実施例1に同じ 実施例& (1)原料物質、溶剤ならびに配合 ベリル粉末     10F vlol       500 ? Lion        50 f NH8・       30f OrlOl        (L  2  f(z)装
置及び方法 実施例1に同じ (II)結果 ベリル単結晶は2■〜5m成長している。
Example 2 (1) Raw material, solvent, and formulation Same as Example 1 (Z) Apparatus and method 950°C temperature increase 24 hours later, seed crystals were added and then slowly cooled to α1°C/Hrasoc (3) Results Same implementation as Example 1 Examples & (1) Raw material, solvent and blended beryl powder 10F vlol 500? Lion 50 f NH8 30 f OrlOl (L 2 f(z) Apparatus and method Same as Example 1 (II) Result Beryl single crystal grows 2~5 m.

特色としてはatlwiJ−の成長が大きいインクルー
ジ謬ンはなく良質の単結晶が得られた。
As a special feature, a high-quality single crystal was obtained without any inclusion defects due to the large growth of atlwiJ-.

本発明ではその他の溶剤、補色剤として実施例以外のも
のを用いることも可能であり、本発明の実施例の範囲に
限定させることなく取捨選択出来るものである。
In the present invention, it is also possible to use other solvents and complementary color agents other than those in the examples, and these can be selected without being limited to the scope of the examples of the present invention.

以上の実施例等より理解された様に本発明によれば人工
ベリル単結晶の合成に用いる溶剤にセシウムを添加する
ごとにより、従来の溶融塩法の有する本質的利益留保し
た上で品質向上ならびに歩留りの向上が可能となり大巾
なコストダウンを図れるので、本発明は人工ベリル単結
晶の製造方法として極めて有意義である。
As understood from the above examples, according to the present invention, by adding cesium to the solvent used to synthesize artificial beryl single crystals, the quality can be improved while retaining the essential benefits of the conventional molten salt method. The present invention is extremely meaningful as a method for producing artificial beryl single crystals, since the yield can be improved and costs can be significantly reduced.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明に用いた加熱装置及び、ルツメ内のレイ
アウトを示すものである。 く符号の説明〉 1・・・加熱装置    2・・・ヒーター3・・・白
金ルツボ   4・・・種子結晶5・・・溶融塩   
  6・・・バックル以  上 第1図
FIG. 1 shows the heating device used in the present invention and the layout inside the nut. Explanation of symbols> 1... Heating device 2... Heater 3... Platinum crucible 4... Seed crystal 5... Molten salt
6...buckle and above Figure 1

Claims (1)

【特許請求の範囲】[Claims] はぼベリル組成比を示す酸化ベリリウム、#I化アルミ
ーウム、二酸化ケイ素及び必要に応じて酸化クロムその
他の着色を加えてなる原料物質に溶剤としての、モリブ
デン酸リチウム、二酸化モリブデン、五酸化バナジウム
等の中から選ばれた一種又は二種以上を加えてこれを上
記溶剤の溶融温度以上に加熱して溶融塩を形成して人工
ベリル単結晶を合成又は育成する方法において上記溶剤
中にセシウム元素を添加し、ベリル単結晶を合成又は育
成せしめることな特徴とする溶融塩法による人工ベリル
単結晶の合成方法。
Lithium molybdate, molybdenum dioxide, vanadium pentoxide, etc. as a solvent are used as a solvent to a raw material obtained by adding beryllium oxide, aluminum #I, silicon dioxide, and other colorings such as chromium oxide as necessary. Adding cesium element to the above solvent in a method of synthesizing or growing an artificial beryl single crystal by adding one or more selected from among them and heating it above the melting temperature of the above solvent to form a molten salt. A method for synthesizing an artificial beryl single crystal by a molten salt method, which is characterized in that the beryl single crystal is synthesized or grown.
JP4797282A 1982-03-25 1982-03-25 JINKOBERIRUTANKETSUSHONOGOSEIHOHO Expired - Lifetime JPH0235719B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4797282A JPH0235719B2 (en) 1982-03-25 1982-03-25 JINKOBERIRUTANKETSUSHONOGOSEIHOHO

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4797282A JPH0235719B2 (en) 1982-03-25 1982-03-25 JINKOBERIRUTANKETSUSHONOGOSEIHOHO

Publications (2)

Publication Number Publication Date
JPS58167495A true JPS58167495A (en) 1983-10-03
JPH0235719B2 JPH0235719B2 (en) 1990-08-13

Family

ID=12790225

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4797282A Expired - Lifetime JPH0235719B2 (en) 1982-03-25 1982-03-25 JINKOBERIRUTANKETSUSHONOGOSEIHOHO

Country Status (1)

Country Link
JP (1) JPH0235719B2 (en)

Also Published As

Publication number Publication date
JPH0235719B2 (en) 1990-08-13

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