JPS58190900A - Production of quartz crystal - Google Patents

Production of quartz crystal

Info

Publication number
JPS58190900A
JPS58190900A JP58005431A JP543183A JPS58190900A JP S58190900 A JPS58190900 A JP S58190900A JP 58005431 A JP58005431 A JP 58005431A JP 543183 A JP543183 A JP 543183A JP S58190900 A JPS58190900 A JP S58190900A
Authority
JP
Japan
Prior art keywords
soln
quartz crystal
solution
mixed
contg
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
JP58005431A
Other languages
Japanese (ja)
Other versions
JPS646159B2 (en
Inventor
Takashi Fujii
隆 藤井
Tsuguo Fukuda
承生 福田
Yoshihiro Kokubu
国分 義弘
Hitoshi Hirano
均 平野
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.)
Toshiba Corp
Original Assignee
Toshiba Corp
Tokyo Shibaura Electric Co Ltd
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 Toshiba Corp, Tokyo Shibaura Electric Co Ltd filed Critical Toshiba Corp
Priority to JP58005431A priority Critical patent/JPS58190900A/en
Publication of JPS58190900A publication Critical patent/JPS58190900A/en
Publication of JPS646159B2 publication Critical patent/JPS646159B2/ja
Granted 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
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • 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
    • C30B29/18Quartz

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 produce a quartz crystal easily by making use of a concn. phenomenon at an ordinary temp., by mixing a soln. contg. iron and a soln. contg. silicon dioxide, adding a seed crystal to the mixed solns. and allowing the solns. to stand. CONSTITUTION:A soln. prepd. by dissolving iron to 4-12 normal nitric acid and an aq. soln. of silicate or silica gel are mixed and a seed crystal of quartz crystal is put in the mixed soln. If the soln. is allowed to stand thereafter, the quartz crystal crystallizes in the gellike material contg. SiO2 produced in the soln. The inexpensive quartz crystal is thus obtained without using any intricate and costly device and installation.

Description

【発明の詳細な説明】 この発明は、耐火性酸化物である水晶を常温濃縮現象を
利用して製造する方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing quartz, which is a refractory oxide, by utilizing a room temperature concentration phenomenon.

水晶は研磨材や時計の軸受、宝石、レコード針等の広い
用途をもつ。従来耐火性酸化物の単結晶を得る方法とし
ては、■引上げ法、■EFG法、■熱交換法、■バクダ
ザロフ法、■ベルヌーイ法、■フラックス法などが知ら
れている。
Quartz has a wide range of uses, including abrasive materials, watch bearings, jewelry, and record needles. Conventionally known methods for obtaining single crystals of refractory oxides include (1) pulling method, (2) EFG method, (2) heat exchange method, (2) Bakdazarov method, (2) Bernoulli method, and (2) flux method.

■〜■はいずれも原材料をるつぼや容器に入れ、高温に
加熱して融解し種子結晶下に成長させる方法である。■
はるつばや容器を使用しないが、原料を高温で融解する
点で■〜■と同じである。
Methods (1) to (2) are all methods in which raw materials are placed in a crucible or container, heated to high temperatures, melted, and grown under seed crystals. ■
It is the same as ① to ③ in that it does not use a melting pot or container, but the raw materials are melted at high temperatures.

■は原材料をフラックス剤pboや水晶石(Naμ/7
6)を用いてその融点よシ低い温度で融解し、結晶を晶
出させる方法である。いずれの方法でも、少くとも10
00℃以上の高温にすることが必要となシ、従ってるつ
ぼや容器として白金、イリジューム、モリブデン等の高
融点金属材を用いなければならない。また高温融解用針
や発熱体にも特殊な材料、設備が要求される。
■The raw materials are flux agent PBO and crystal stone (Naμ/7
6) is melted at a temperature lower than its melting point, and crystals are crystallized. Either way, at least 10
It is necessary to raise the temperature to a temperature of 00° C. or higher, and therefore a high melting point metal material such as platinum, iridium, or molybdenum must be used for the crucible or container. Special materials and equipment are also required for the high-temperature melting needle and heating element.

この発明は、複雑かつ高価な設備を用いることなく、常
温濃縮現象を利用して簡便に水晶を製造する方法を提供
するものである。
The present invention provides a method for easily producing crystal using a room-temperature concentration phenomenon without using complicated and expensive equipment.

この発明の方法は、鉄(Fe )を含む溶液と二酸化硅
素(8102)を含む溶液を混合し、この混合溶液に種
子結晶を入れて放置することにより、常温濃縮現象で水
晶を成長させることを特徴としている。
The method of this invention is to mix a solution containing iron (Fe) and a solution containing silicon dioxide (8102), add seed crystals to this mixed solution, and leave it to grow crystals by concentration at room temperature. It is a feature.

゛例えば、Feを4〜12規程の硝酸に溶解した溶解液
と、硅酸塩捷たはシリカダルの水溶液を混合して放置す
ると、溶液中に生じた5to2’i含むケ゛ル状物質中
に水晶が晶出する。この結晶成長には、溶液中のF e
 (OH)3または5i02ダルが触媒として作用して
いるもの考えられる。
For example, if you mix a solution of Fe in 4-12 nitric acid and an aqueous solution of silicate or silica dal and leave it to stand, crystals will form in the shell-like substance containing 5to2'i produced in the solution. Crystallizes. This crystal growth requires Fe in solution.
It is thought that (OH)3 or 5i02 Dal acts as a catalyst.

この発明の方法は、従来法のような高温を要せず、常温
付近で簡単に実施できることが基本的に優れている点で
ある。得られる水晶の大きさや成長速度は、溶液の一濃
度、温度、過飽和度等の制御により、また種子結晶を入
れることによシ、制御される。
The basic advantage of the method of this invention is that it does not require high temperatures unlike conventional methods and can be easily carried out at around room temperature. The size and growth rate of the resulting crystals are controlled by controlling the concentration of the solution, temperature, degree of supersaturation, etc., and by introducing seed crystals.

以下この発明の詳細な説明する。100CCのビーカー
を2個用意し、一方のビーカーに8規程の硝酸を約50
CC入れ、これに三価のFeを含む鉄の棒(2団φX 
30 +mn )を入れた。更にPH濃度調整のためN
aOHを約5cc入れた。他方のビーカーには水50C
Cを入れこれにシリカケ゛ルを溶かして5IO2濃度5
0 ppmのシリカ溶液を作った。これらの溶液を交互
に少しずつ混合して最終的に3− ル成長も可能である。
This invention will be described in detail below. Prepare two 100CC beakers, and add about 50% of 8-regulation nitric acid to one beaker.
CC is inserted, and an iron rod containing trivalent Fe (2 groups φX
30+mn) was added. Furthermore, N was added to adjust the pH concentration.
Approximately 5 cc of aOH was added. In the other beaker, add 50C water.
Add C and dissolve silica gel to make 5IO2 concentration 5
A 0 ppm silica solution was made. It is also possible to mix these solutions little by little alternately to finally achieve 3-hole growth.

一方のビーカーに全部を入れ、これに水晶の種子結晶を
入れて5日間放置した。これによシ、種子結晶上に水晶
結晶が生成された。
Put everything into one beaker, add quartz seed crystals to it, and leave it for 5 days. As a result, quartz crystals were formed on the seed crystals.

以上、実施例を説明したが、この発明の方法は単純な溶
液からの濃縮に限らず、圧力下で約200℃程度の熱水
合成によってもよい。更に上記実施例ではFeを溶解す
るのに硝酸を用いたが、硝酸と他の酸の混液等を用いて
もよい。更にまた、5i02を含む溶液についても、N
a 2 S i O3やに2SiO3等、Feを含む溶
液と混合したときに5I02rルを生ずるような硅酸塩
を溶かした水溶液を用いることができる。
Although the embodiments have been described above, the method of the present invention is not limited to simple concentration from a solution, but may also be hydrothermal synthesis at about 200° C. under pressure. Further, in the above embodiment, nitric acid was used to dissolve Fe, but a mixture of nitric acid and other acids may also be used. Furthermore, for solutions containing 5i02, N
An aqueous solution containing a silicate such as a 2 Si O 3 or 2 SiO 3 which produces 5I02r when mixed with a solution containing Fe can be used.

この発明の効果を列記すれば次のとbBである。(1)
従来、少くとも1000℃以上の高温でなければ結晶成
長できなかった水晶を常温付近できわめて簡便に作るこ
とができる。(2)耐熱容器。
The effects of this invention can be listed as follows. (1)
Quartz crystal, which conventionally could only be grown at a high temperature of at least 1000° C., can be produced extremely easily at room temperature. (2) Heat-resistant container.

高温溶解設備など、複雑かつ高価な装置や設備を要せず
、従って安価な水晶を提供できる。(3)結晶成長は種
子結晶上に行うことができ、溶液のpH8度の制御等に
よシ、水晶のエビタキシャ4− 出願人代理人  弁理士 鈴 江 武 彦5−
Complex and expensive devices and equipment such as high-temperature melting equipment are not required, and therefore inexpensive crystal can be provided. (3) Crystal growth can be performed on seed crystals by controlling the pH of the solution to 8 degrees, etc.

Claims (2)

【特許請求の範囲】[Claims] (1)鉄を含む溶液と二酸化硅素を含む溶液を混合し、
この混合溶液に種子結晶を入れて放置することを特徴と
する水晶の製造方法。
(1) Mix a solution containing iron and a solution containing silicon dioxide,
A method for producing crystals, which comprises adding seed crystals to this mixed solution and leaving it to stand.
(2)鉄を含む溶液は鉄を4〜12規程の硝酸に溶解し
た溶液であシ、二酸化硅素を含む溶液は硅酸塩またはシ
リカグルを水に溶解した溶液である特許請求の範囲第1
項記載の水晶の製造方法。
(2) The solution containing iron is a solution in which iron is dissolved in 4-12 nitric acid, and the solution containing silicon dioxide is a solution in which silicate or silica glu is dissolved in water.Claim 1
2. Method for producing crystals described in Section 1.
JP58005431A 1983-01-17 1983-01-17 Production of quartz crystal Granted JPS58190900A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP58005431A JPS58190900A (en) 1983-01-17 1983-01-17 Production of quartz crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP58005431A JPS58190900A (en) 1983-01-17 1983-01-17 Production of quartz crystal

Related Parent Applications (1)

Application Number Title Priority Date Filing Date
JP11875880A Division JPS5854119B2 (en) 1980-08-28 1980-08-28 Production method of α-alumina single crystal

Publications (2)

Publication Number Publication Date
JPS58190900A true JPS58190900A (en) 1983-11-07
JPS646159B2 JPS646159B2 (en) 1989-02-02

Family

ID=11610997

Family Applications (1)

Application Number Title Priority Date Filing Date
JP58005431A Granted JPS58190900A (en) 1983-01-17 1983-01-17 Production of quartz crystal

Country Status (1)

Country Link
JP (1) JPS58190900A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0693580A1 (en) * 1994-07-18 1996-01-24 Sumitomo Electric Industries, Ltd. Oxide thin film having quartz crystal structure and process for producing the same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0693580A1 (en) * 1994-07-18 1996-01-24 Sumitomo Electric Industries, Ltd. Oxide thin film having quartz crystal structure and process for producing the same
US5879811A (en) * 1994-07-18 1999-03-09 Sumitomo Electric Industries, Ltd. Oxide thin film having quartz crystal structure

Also Published As

Publication number Publication date
JPS646159B2 (en) 1989-02-02

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