JPH0416583A - Production of blue rock crystal - Google Patents

Production of blue rock crystal

Info

Publication number
JPH0416583A
JPH0416583A JP12100690A JP12100690A JPH0416583A JP H0416583 A JPH0416583 A JP H0416583A JP 12100690 A JP12100690 A JP 12100690A JP 12100690 A JP12100690 A JP 12100690A JP H0416583 A JPH0416583 A JP H0416583A
Authority
JP
Japan
Prior art keywords
crystal
growth
blue
additives
coloring
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.)
Pending
Application number
JP12100690A
Other languages
Japanese (ja)
Inventor
Hiroshi Kuroda
浩 黒田
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.)
Seiko Instruments Inc
Original Assignee
Seiko Instruments Inc
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 Seiko Instruments Inc filed Critical Seiko Instruments Inc
Priority to JP12100690A priority Critical patent/JPH0416583A/en
Publication of JPH0416583A publication Critical patent/JPH0416583A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To obtain the blue rock crystal which is substantially free from unequal colors, is free from microcracks and has extremely good transparency by using AlPO4 and CoSO4 as additives in a hydrothermal crystallization method. CONSTITUTION:AlPO4 and CoSO4 are added as additives for coloring to the blue rock crystal in the growth of the blue rock crystal by the hydrothermal crystallization method. For example, a raw material 4 for growth and the AlPO4 and CoSO4 8 which are additives for coloring are installed in the bottom of a pressure vessel body 1 subjected to pressure sealing with a cover 3 via a sealing ring 2. A seed crystal 6 is then disposed on the raw material 4 for growth via a seed crystal supporting frame 5 and a baffle plate 7 is installed via the frame 5 therebetween. The growth of the blue rock crystal is thereafter executed. An aq. soln. of Na2CO3 is used as a solvent and is packed into the vessel 1 at such a packing rate at which the prescribed pressure is obtd. at a prescribed temp.

Description

【発明の詳細な説明】[Detailed description of the invention]

[産業上の利用分野] 本発明は、装飾品としてよく用いられている、アメシス
ト(紫水晶)と同質の水晶であり、アメシストと同様に
装飾品として価値のある、青色の人工水晶の製造方法に
関するものである。 [発明の概要] 本発明は、装飾品としてよく知られている青色の水晶を
人工的に合成できる製造方法において。 所定の温度、圧力を与え、適当な溶媒中で種子結晶上に
結晶を育成する水熱合成法により、着色添加剤として、
Al2PO4及びCo S O4を添加し青色の人工水
晶を育成するものである。 〔従来の技術1 従来、水熱合成法においては、人工水晶の育成について
の研究開発が最も盛んであり、水熱合成法における結晶
育成としては、最も成功した例であるといえる。現在ま
でに1人工水晶に関してはほとんど量産化技術が確立し
ている。また、この技術を生かした着色水晶の製造方法
についても、紫水晶など各種着色水晶について研究開発
がなされている。現在の着色水晶は、溶媒として、水酸
化カリウム(KOH)水溶液、あるいは炭酸カリウム(
K、Co、)水溶液を使用し、温度範囲300〜400
℃、圧力1000〜1500kg/cm”の条件で育成
が行われている。また、着色添加剤としては、各種金属
イオンが使用されている。 〔発明が解決しようとする課題1 従来の着色用添加剤を添加した、人工水晶の結晶成長に
おいては、結晶が育成できるものの以下のような問題点
があった。 従来の着色用添加剤を使用した場合、育成結晶中に、濃
く着色された部分と、薄く着色された部分ができてしま
うといった色むらの問題、あるいは、育成部分の着色が
不十分であるといった色あいの問題があった。また、着
色によるマイクロクラックの発生といった問題も生じて
いた。
[Industrial Application Field] The present invention is a method for producing blue artificial crystal, which is a crystal of the same quality as amethyst (amethyst), which is often used as an ornament, and is valuable as an ornament like amethyst. It is related to. [Summary of the Invention] The present invention relates to a manufacturing method that can artificially synthesize blue crystal, which is well known as a decorative item. As a coloring additive, it is produced using a hydrothermal synthesis method in which crystals are grown on seed crystals in an appropriate solvent by applying a predetermined temperature and pressure.
Blue artificial quartz is grown by adding Al2PO4 and CoSO4. [Prior Art 1] Conventionally, in the hydrothermal synthesis method, research and development on growing artificial quartz has been most active, and it can be said that this is the most successful example of crystal growth in the hydrothermal synthesis method. To date, mass production technology for most of the artificial quartz crystals has been established. Furthermore, research and development is being conducted on various colored crystals such as amethyst as well as methods for producing colored crystals using this technology. Current colored crystals are produced using an aqueous solution of potassium hydroxide (KOH) or potassium carbonate (
K, Co, ) aqueous solution, temperature range 300-400
℃ and a pressure of 1000 to 1500 kg/cm''. Various metal ions are used as coloring additives. [Problem to be solved by the invention 1 Conventional coloring additives] When growing artificial quartz crystals using additives, although crystals can be grown, there are the following problems: When conventional coloring additives are used, darkly colored areas may appear in the grown crystals. There were problems with color unevenness, such as the formation of lightly colored areas, and problems with color tone, such as insufficient coloring of the growing areas.Additionally, there were also problems such as the generation of microcracks due to the coloring.

【課題を解決するための手段】[Means to solve the problem]

従来の水熱合成法による着色水晶の育成についての色あ
い、色むら、透明度、あるいはマイクロクラックの発生
といった問題については、着色用添加剤の選択に起因し
ている。 着色用添加剤については様々な種類があるが、上記課題
を解決するための最適な着色用添加剤としてAlpo、
及びCo S O4を見出した。 [作用] 水熱合成法においては、適当な温度と圧力のもとで出発
原料を適当な溶媒の水溶液に溶解させ。 徐冷するまたは温度差を利用して養分を輸送することに
より結晶を種子結晶上に育成する。この結晶育成の際に
、着色用添加剤を添加する。これにより、着色用添加剤
は水溶液中で金属イオンとなり、結晶中に取り込まれる
。この着色用添加剤として、Alpo、及びCo S 
O4を用いた。青色の人工水晶を育成する際、AlPO
4及びCO3O4は理想的な添加剤である。 〔実施例〕 第1図に本実施例の構成を模式的に表す断面図を示す、
圧力容器本体lはシールリング2を介してカバー3によ
り圧力シールがされている0以上の構成の圧力容器にお
いて圧力容器本体の底部に育成用原料4及び着色用添加
剤のAlPO4。 CoSO48を設置する。この育成用原料4としては、
天然水晶原石(ラス力)を適当な大きさに砕いたものを
使用した0次に種子結晶支持枠5を介して種子結晶6が
育成用原料4の上に配置されている1種子結晶5として
は、天然あるいは人工の水晶を用いる0種子結晶の結晶
面としては各種(例えば、2面、Y面、R面など)の面
のものが用いられているが、今回は2面のものを使用し
た。また、育成する単結晶の欠陥の原因とならないよう
に特に内部のインクルージヨン、転位などの少ない種子
結晶が必要である。このように育成用原料4及び種子結
晶6を配置し、その間に同じく種子結晶支持枠5を介し
てバッフル板7が設置されている。このような構成の圧
力容器中で青色水晶の育成を行った。溶媒としては、N
 a zCOs水溶液を用い、所定の温度で所定の圧力
が得られるような充填率で圧力容器中へ充填した。 以上の設定で水熱合成を行った。すなわち以下の通りで
ある。 実施例1 種子結晶6の温度・・・310℃ 育成用原料4の温度・・・340℃ 溶媒・・・1.0モルNag COs水溶液着色用添加
剤量・・・AlPO40,5重量%Co50.0.5重
量% 圧力・・・800 kg/cm” 育成期間・・・10日間 この結果、種子結晶6の上に以下の様な青色の水晶が育
成された。 成長した層の厚み・・・7.0mm 成長速度・・・700μm/日 成長した層の性質・・・α−水晶(X線回折法により固
定)、インクルージヨンおよびクラック等の欠陥の非常
に少ない色むらのない結晶が得られた。 実施例2 種子結晶6の温度・・・320℃ 育成用原料4の温度・・・340℃ 溶媒・・・1.0モルNag COs水溶液着色用添加
剤量・・・AlPO,0,5重量%CoSO40,5重
量% 圧力・・・800 kg/cが 育成期間・・・lO日日 間の結果、種子結晶6の上に以下の様な青色の水晶が育
成された。 成長した層の厚み・・・6.2s+n+成長速度・・・
620um/日 成長した層の性質・・・a−水晶(X線回折法により固
定)、インクルージヨンおよびクラック等の欠陥の非常
に少ない色むらのない結晶が得られた。 実施例3 種子結晶6の温度・・・340℃ 育成用原料4の温度・・・360℃ 溶媒・・・1.0モルNag Cow水溶液着色用添加
剤量・・・AβPO41,0重量%Co50.1.0重
量% 圧力・−−1000kg/cm” 育成期間・・・10日間 この結果、種子結晶6の上に以下の様な青色の水晶が育
成された。 成長した層の厚み・・・6.5mm 成長速度・・・650μm/日 成長した層の性質・・・α−水晶(X線回折法により固
定)、インクルージヨンおよびクラック等の欠陥の非常
に少ない色むらのない結晶が得られた。 [発明の効果] 以上詳述したように本発明によれば、着色用添加剤とし
てAlPO4、Co50.を用いることにより1色むら
のほとんどない、透明度の非常によい青色水晶の育成が
可能である。また、装飾品としての価値を十分に持った
青色水晶の育成が可能となり、その効果は極めて大きい
Problems with the growth of colored crystals by conventional hydrothermal synthesis methods, such as color tone, color unevenness, transparency, or the occurrence of microcracks, are caused by the selection of coloring additives. There are various types of coloring additives, but the best coloring additives to solve the above problems are Alpo,
and Co SO4 were found. [Operation] In the hydrothermal synthesis method, starting materials are dissolved in an aqueous solution of an appropriate solvent under appropriate temperature and pressure. Crystals are grown on seed crystals by slow cooling or by transporting nutrients using temperature differences. A coloring additive is added during this crystal growth. As a result, the coloring additive becomes a metal ion in the aqueous solution and is incorporated into the crystal. As the coloring additive, Alpo and CoS
O4 was used. When growing blue artificial quartz, AlPO
4 and CO3O4 are ideal additives. [Example] FIG. 1 shows a cross-sectional view schematically showing the configuration of this example.
The pressure vessel main body 1 is pressure-sealed by a cover 3 via a seal ring 2. In a pressure vessel having a configuration of 0 or more, a growth raw material 4 and a coloring additive AlPO4 are placed at the bottom of the pressure vessel main body. Install CoSO48. As this raw material 4 for growth,
As a seed crystal 5, a seed crystal 6 is placed on a growing raw material 4 via a seed crystal support frame 5 using a natural crystal rough stone (lath force) crushed into an appropriate size. Various types of crystal planes (e.g., 2-sided, Y-plane, R-plane, etc.) are used as the crystal planes of 0-seed crystals using natural or artificial crystals, but this time we used 2-sided crystals. did. In addition, a seed crystal with particularly few internal inclusions and dislocations is required so as not to cause defects in the single crystal to be grown. The growing raw material 4 and the seed crystal 6 are arranged in this manner, and a baffle plate 7 is also installed between them via the seed crystal support frame 5. Blue crystal was grown in a pressure vessel with such a configuration. As a solvent, N
A pressure vessel was filled with an azCOs aqueous solution at a filling rate such that a predetermined pressure was obtained at a predetermined temperature. Hydrothermal synthesis was performed with the above settings. That is, as follows. Example 1 Temperature of seed crystal 6: 310°C Temperature of growing raw material 4: 340°C Solvent: 1.0 mol Nag COs aqueous solution coloring additive amount: AlPO40, 5% by weight Co50. 0.5% by weight Pressure: 800 kg/cm" Growth period: 10 days As a result, blue crystals as shown below were grown on the seed crystal 6. Thickness of the grown layer... 7.0 mm Growth rate: 700 μm/day Properties of the grown layer: α-quartz (fixed by X-ray diffraction method), crystals with very few defects such as inclusions and cracks and no uneven color are obtained. Example 2 Temperature of seed crystal 6: 320°C Temperature of growing raw material 4: 340°C Solvent: 1.0 mol Nag COs aqueous solution coloring additive amount: AlPO, 0,5 Weight% CoSO40.5% by weight Pressure: 800 kg/c Growth period: 10 days As a result, the following blue crystals were grown on top of the seed crystal 6.Thickness of the grown layer ...6.2s+n+growth rate...
Properties of the layer grown at 620 um/day: a-quartz crystal (fixed by X-ray diffraction method), a crystal with very few defects such as inclusions and cracks and without uneven color was obtained. Example 3 Temperature of seed crystal 6: 340°C Temperature of growing raw material 4: 360°C Solvent: 1.0 mol Nag Cow aqueous solution Coloring additive amount: AβPO4 1.0% by weight Co50. 1.0% by weight Pressure: --1000kg/cm" Growth period: 10 days As a result, blue crystals as shown below were grown on the seed crystal 6. Thickness of the grown layer: 6 .5mm Growth rate: 650 μm/day Properties of the grown layer: α-quartz (fixed by X-ray diffraction method), crystals with very few defects such as inclusions and cracks and no uneven color were obtained. [Effects of the Invention] As detailed above, according to the present invention, by using AlPO4 and Co50 as coloring additives, it is possible to grow blue crystal with very good transparency and almost no single color unevenness. In addition, it has become possible to grow blue crystals that have sufficient value as ornaments, and the effect is extremely large.

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

第1図は圧力容器の構造を表わす断面図である。 圧力容器本体 シールリング カバー 育成用原料 種子結晶支持枠 種子結晶 バッフル板 看色用添加剤 FIG. 1 is a sectional view showing the structure of a pressure vessel. Pressure vessel body Seal ring cover Raw materials for growing seed crystal support frame seed crystal baffle plate Color viewing additive

Claims (1)

【特許請求の範囲】[Claims] 所定の温度、圧力を与え結晶を成長させる水熱合成法に
おいて、添加剤として、AlPO_4及びCoSO_4
を加えることにより、青色の人工水晶を育成したことを
特徴とする青色水晶の製造方法。
In the hydrothermal synthesis method in which crystals are grown by applying a predetermined temperature and pressure, AlPO_4 and CoSO_4 are used as additives.
A method for producing blue crystal, characterized in that blue artificial crystal is grown by adding.
JP12100690A 1990-05-10 1990-05-10 Production of blue rock crystal Pending JPH0416583A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP12100690A JPH0416583A (en) 1990-05-10 1990-05-10 Production of blue rock crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP12100690A JPH0416583A (en) 1990-05-10 1990-05-10 Production of blue rock crystal

Publications (1)

Publication Number Publication Date
JPH0416583A true JPH0416583A (en) 1992-01-21

Family

ID=14800458

Family Applications (1)

Application Number Title Priority Date Filing Date
JP12100690A Pending JPH0416583A (en) 1990-05-10 1990-05-10 Production of blue rock crystal

Country Status (1)

Country Link
JP (1) JPH0416583A (en)

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