JPH029791A - Production of blue rock crystal - Google Patents
Production of blue rock crystalInfo
- Publication number
- JPH029791A JPH029791A JP16233188A JP16233188A JPH029791A JP H029791 A JPH029791 A JP H029791A JP 16233188 A JP16233188 A JP 16233188A JP 16233188 A JP16233188 A JP 16233188A JP H029791 A JPH029791 A JP H029791A
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- rock crystal
- blue
- crystals
- raw materials
- 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
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title abstract description 14
- 239000011034 rock crystal Substances 0.000 title abstract 9
- 239000013078 crystal Substances 0.000 claims abstract description 73
- 239000000654 additive Substances 0.000 claims abstract description 19
- 230000000996 additive effect Effects 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000004040 coloring Methods 0.000 claims description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 11
- 239000002904 solvent Substances 0.000 abstract description 8
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract description 6
- 239000010975 amethyst Substances 0.000 abstract description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 abstract description 3
- 235000015320 potassium carbonate Nutrition 0.000 abstract description 2
- 238000005216 hydrothermal crystallization Methods 0.000 abstract 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000003086 colorant Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910021489 α-quartz Inorganic materials 0.000 description 3
- 239000010453 quartz Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 230000003716 rejuvenation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は装飾品としてよく知られているアメシスト（紫
水晶）と同質の水晶であり、同じく装飾品として価値の
ある青色水晶の製造方法に関するしのである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing blue crystal, which is a crystal similar to amethyst (amethyst), which is well known as an ornament, and is also valuable as an ornament. It's Shino.
本発明は、装飾品としてよく知られている着色水晶を人
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Ｆｅ（ＮＯ５）ｉを添
加し、結晶を育成し、育成した結晶を熱処理することに
よって青色水晶を製造する方法である。The present invention is a manufacturing method that can artificially synthesize colored crystals, which are well known as decorative items, using a hydrothermal synthesis method in which crystals are grown on seed crystals in an appropriate solvent while applying a predetermined temperature and pressure. , is a method of producing blue crystal by adding Fe(NO5)i as a coloring additive, growing crystals, and heat-treating the grown crystals.
従来、水熱合成法においては、人工水晶の育成について
の研究開発および量産化が最も盛んであり、水熱合成法
における結晶育成としては、鼓ら成功した例であるとい
える。現在までに人工水晶に関してはほとんど址産１ヒ
技術が確立している。Conventionally, in the hydrothermal synthesis method, research and development and mass production of artificial quartz crystals have been most active, and this can be said to be a successful example of crystal growth using the hydrothermal synthesis method. Until now, most of the techniques for producing artificial crystals have been established.
また、この製造技術を生かした着色水晶の製造方法につ
いても、紫水晶、黄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（Ｋ ＯＩｆ ）水溶液、あるいは炭酸
カリウム（Ｋ２ ＣＯ，）水溶液を使用し、温度範囲３
００〜４００ ’Ｃ１圧力１０００〜１５００ｋｇ／ａ
ｌｌの条件で育成が行われている。また、着色添加剤と
しては、各種金属塩が使用されている。Furthermore, research and development is being carried out on various colored crystals such as amethyst and yellow quartz regarding methods for producing colored crystals that utilize this manufacturing technology. Current colored crystals use solvents such as
Using potassium hydroxide (K OIf ) aqueous solution or potassium carbonate (K2 CO,) aqueous solution, temperature range 3
00~400'C1 pressure 1000~1500kg/a
The cultivation is carried out under the following conditions. Furthermore, various metal salts are used as coloring additives.
従来の青色水晶の水熱合成においては、着色用添加剤と
しては、ＣｏＣｊ ２− ＣＯＯ３、ＣｏＣＯ３等か用
いられていた。これｔｌの着色用添加剤を使用しても青
色結晶が育成できる（、のの以下のような問題点があっ
た。In conventional hydrothermal synthesis of blue crystal, CoCj 2-COO3, CoCO3, etc. have been used as coloring additives. Even if this TL coloring additive is used, blue crystals can be grown (there were the following problems with Nono.
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があった。When conventional coloring additives are used, there is a problem of color unevenness in which darkly colored parts and lightly colored parts are formed in the grown crystal.
また、育成部分の着色が不十分であるといった、色あい
の問題も生じていた。In addition, there was also a problem of color tone, such as insufficient coloring of the growing part.
従来の水熱合成法により着色水晶の育成についての、色
あい、色むら、透明度、あるいはクラックの発生といっ
た課題については、着色用添加剤の選択に起因している
０着色用添加剤については様々な種類があるか、Ｌ記課
題を解決するため最適な着色用添加剤としてＦ ｅ （
ＮＯｘ ） ｓを見出した。When growing colored crystals using conventional hydrothermal synthesis methods, problems such as color tone, color unevenness, transparency, or the occurrence of cracks are caused by the selection of coloring additives. There are various types of additives for coloring, and F e (
NOx)s was found.
また、育成結晶を青色にするために熱処理を行うことに
した。We also decided to perform heat treatment to turn the grown crystals blue.
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７１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
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Ｆｅ＜Ｎｏ５）３を用いた。育成された結晶
は、色に着色しているが、この育成結晶をさらに熱処理
することにより青色水晶を得ることかできる。In the hydrothermal synthesis method, the starting material 71 is dissolved in an aqueous solution of an appropriate solvent at an appropriate temperature and pressure, and crystals are grown on a seed crystal by slow cooling or by transporting nutrients using the temperature difference. to develop. 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. Fe<No5)3 was used as the coloring additive. The grown crystals are colored, but blue crystals can be obtained by further heat-treating the grown crystals.
以下、実施例に従い詳しく説明する。Hereinafter, a detailed explanation will be given according to examples.
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１はシールリング２を介してカバー３によ
り圧力シールかされている。以Ｅ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Ｆｅ （ＮＯｌ）３８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次に種結晶支持枠５を介して種
結晶６が育成川原′ｆ１４の上に配置されている。FIG. 1 shows a cross-sectional view schematically showing the configuration of this embodiment.
The pressure vessel main body 1 is pressure-sealed by a cover 3 via a seal ring 2. In the pressure vessel having the following configuration E, the growth raw material 4 and the coloring additive Fe (NOl) 38 are installed at the bottom of the pressure vessel main body. The seed crystal 6 is placed on the growth riverbed 14 via the seed crystal support frame 5, which uses a natural crystal raw stone (lath force) crushed into an appropriate size as the raw material 4 for growth. has been done.
種結晶５としては、天然あるいは人工の水晶を用いる。As the seed crystal 5, natural or artificial crystal is used.
種結晶の結晶面としては各種の面（例えば、２面、Ｙ面
、Ｒ面など）か用いられているが、今回は２面のもの（
Ｚ板）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、クラッ
ク転位などの少ない種結晶が必要である。このように育
成用原料４および種結晶６を配置し、その間に同じく種
結晶支持枠５を介してバッフル板７が設置されている。Various types of crystal planes (for example, 2 planes, Y planes, R planes, etc.) are used as the crystal planes of the seed crystals, but this time we used 2 planes (2 planes, etc.).
Z plate) was used. In addition, a seed crystal with particularly few internal inclusions, crack dislocations, etc. is required so as not to cause defects in the single crystal to be grown. The growth raw material 4 and the seed crystal 6 are arranged in this way, and a baffle plate 7 is installed between them via the seed crystal support frame 5 as well.
このような構成の圧力容器中で着色水晶の育成を行った
。溶媒としては、Ｋ２ＣＯ３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。Colored crystals were grown in a pressure vessel with such a configuration. A K2CO3 aqueous solution was used as the solvent, and the pressure vessel was filled at a filling rate such that a predetermined pressure was obtained at a predetermined temperature.
以上の設定で水熱合成を行った。このようにして得られ
た結晶は淡い褐色をしている。この結晶を所定の温度、
時間で、大気中で熱処理することによって青色水晶が得
られた。詳しい育成条件は以下の通りである。Hydrothermal synthesis was performed with the above settings. The crystals thus obtained have a light brown color. This crystal is heated to a specified temperature,
Blue crystals were obtained by heat treatment in air for an hour. The detailed growth conditions are as follows.
実施例１
種結晶６の温度・・・３２０°Ｃ
育成用原料４の温度・・・３４０°Ｃ
溶媒・・・０．５モルＫ ２ＣＯｓ水溶液着色用添加剤
量・・Ｆｅ（Ｎｏ３）ｓ１重足％圧力・・・８００ｋｌ
ｒ／′−
育成期間・・・１０日間
熱処理温度・・・４００°Ｃ
熱処理時間・・・８時間
この結果、種結晶６の上に以下の様な青色水晶か育成さ
れた。Example 1 Temperature of seed crystal 6...320°C Temperature of growing raw material 4...340°C Solvent...0.5 mol K Amount of additive for coloring 2COs aqueous solution...Fe(No3)s 1 weight Foot % pressure...800kl
r/'- Growth period: 10 days Heat treatment temperature: 400°C Heat treatment time: 8 hours As a result, blue crystals as shown below were grown on the seed crystal 6.
成長した層の厚み・・・７．４市
成長速度・・・７４０μｍ／日
育成、熱処理後の結晶の性質・・・α−水晶（Ｘ線回折
法により同定）、インクルージヨン、マイクロクラック
の非常に少ない色むらのない青色の結晶が得られた。Thickness of grown layer: 7.4 Growth rate: 740 μm/day Crystal properties after growth and heat treatment: α-quartz (identified by X-ray diffraction), inclusions, and microcracks. Blue crystals with little color unevenness were obtained.
実施例２
種結晶６の温度・・・３２０℃
育成用原料４の温度・・・３４０°Ｃ
溶媒・・・０．５モルに２ Ｃｏ、水溶液若色用添加削
址・・Ｆｅ （ＮＯｓ ）３１重量％Ｊ王力・・・５０
０ｋｆ／Ｊ
育成期間・・・１０日間
熱処理温度・・・１１００℃
熱処理時間・・・８時間
この結果、種結晶６の上に以下の様な青色の水晶が育成
された。Example 2 Temperature of seed crystal 6: 320°C Temperature of growing raw material 4: 340°C Solvent: 0.5 mol of 2 Co, aqueous solution rejuvenation additive: Fe (NOs) 31% by weight J Royal Power...50
0 kf/J Growth period: 10 days Heat treatment temperature: 1100°C Heat treatment time: 8 hours As a result, blue crystals as shown below were grown on the seed crystal 6.
成長した層の厚み・・・５．８１ｗ１１成長速度・・・
５８０μｍ／′日
育成、熱処理後の結晶の性質・・・α−水晶（Ｘ線回折
法により同定）、インクルージヨン、マイクロクラック
の非常に少ない色むらのない４色の結晶か得られた。実
施例ａで得られた結晶とくらべて、淡い青色の結晶が得
られた。Thickness of grown layer...5.81w11 Growth rate...
Properties of crystals after growth at 580 μm/'day and heat treatment: Four-color crystals with very few α-quartz crystals (identified by X-ray diffraction), inclusions, and microcracks and no color unevenness were obtained. A pale blue crystal was obtained compared to the crystal obtained in Example a.
実施例３
種結晶６の温度・・・３００″Ｃ
育成用原料４の温度・・・３２０℃
溶媒・・・０．５モルに２Ｃ０３水溶液着色用添加剤量
・・・Ｆｅ（ＮＯｓ ）３ １．５重藍％圧力・・・１
０００ ｋ２．／’ａｉｆｆ育成期間・・・１０日間
熱処理温度・・・５００℃
熱処理時間・・・８時間
この結果、種結晶６の上に以下の様な青色水晶が育成さ
れた。Example 3 Temperature of seed crystal 6: 300″C Temperature of growing raw material 4: 320°C Solvent: 0.5 mol 2C03 aqueous solution coloring additive amount: Fe(NOs)3 1 .5 heavy indigo% pressure...1
000 k2. /'aiff Growth period: 10 days Heat treatment temperature: 500° C. Heat treatment time: 8 hours As a result, blue crystals as shown below were grown on the seed crystal 6.
成長した層の厚み・・・７．１間
成長速度・・・７１０μ／ｍ
育成、熱処理後の結晶の性質・・・α−水晶（Ｘ線回折
法により同定）、インクルージヨン、マイクロクラック
の非常に少ない色むらのない青色の結晶か得られた。Thickness of grown layer: 7.1 Growth rate: 710μ/m Properties of crystals after growth and heat treatment: α-quartz (identified by X-ray diffraction), inclusions, and microcracks. A blue crystal with little color unevenness was obtained.
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Ｆ ｅ （ＮＯ３） ３を用いかつ熱処理を行うこと
により、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。As detailed above, according to the present invention, by using Fe (NO3) 3 as a coloring additive and performing heat treatment, it is possible to grow blue crystals with very good transparency and almost no color unevenness. . Furthermore, it becomes possible to grow blue crystals that have sufficient value as ornaments, and the effect is extremely large.
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
種結晶支持枠
種結晶
バッフル板
着色用添加剤
以上
出願人 セイコー電子工業株式会社
代理人 弁理士 林 敬 之 動圧力客器の、構
凸Σ表）＋−）す右面図第１図FIG. 1 is a sectional view showing the structure of a pressure vessel. Pressure vessel main body Seal ring cover Raw material for growing Seed crystal support frame Seed crystal baffle plate Additive for coloring Applicant Seiko Electronics Co., Ltd. Agent Patent attorney Takashi Hayashi Structure convex Σ table of dynamic pressure passenger equipment) +-) Right side view Figure 1
Claims (1)
おいて、着色用添加剤としてＦｅ（ＮＯ＿３）＿３を加
え、水晶を育成した後に熱処理することを特徴とする青
色水晶の製造方法。A method for producing blue crystal, which is characterized by adding Fe(NO_3)_3 as a coloring additive in a hydrothermal synthesis method of growing a crystal by applying a predetermined temperature and pressure, and heat-treating the crystal after growing the crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16233188A JPH029791A (en) | 1988-06-28 | 1988-06-28 | Production of blue rock crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16233188A JPH029791A (en) | 1988-06-28 | 1988-06-28 | Production of blue rock crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH029791A true JPH029791A (en) | 1990-01-12 |
Family
ID=15752515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16233188A Pending JPH029791A (en) | 1988-06-28 | 1988-06-28 | Production of blue rock crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH029791A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924289A (en) * | 2014-05-07 | 2014-07-16 | 台州市原本光电科技有限公司 | Growing method of medical optical crystals |
-
1988
- 1988-06-28 JP JP16233188A patent/JPH029791A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103924289A (en) * | 2014-05-07 | 2014-07-16 | 台州市原本光电科技有限公司 | Growing method of medical optical crystals |
| CN103924289B (en) * | 2014-05-07 | 2016-07-06 | 台州市原本光电科技有限公司 | A kind of growing method of medical optical crystal |
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