JPS60176994A - Preparation of corundum - Google Patents

Preparation of corundum

Info

Publication number
JPS60176994A
JPS60176994A JP59031698A JP3169884A JPS60176994A JP S60176994 A JPS60176994 A JP S60176994A JP 59031698 A JP59031698 A JP 59031698A JP 3169884 A JP3169884 A JP 3169884A JP S60176994 A JPS60176994 A JP S60176994A
Authority
JP
Japan
Prior art keywords
raw material
single crystal
rod
corundum
production unit
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
JP59031698A
Other languages
Japanese (ja)
Inventor
Hitoshi Miyasaka
均 宮坂
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 Epson Corp
Suwa Seikosha KK
Original Assignee
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 Seiko Epson Corp, Suwa Seikosha KK filed Critical Seiko Epson Corp
Priority to JP59031698A priority Critical patent/JPS60176994A/en
Publication of JPS60176994A publication Critical patent/JPS60176994A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-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
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides

Landscapes

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

Abstract

PURPOSE:To control freely an atmosphere gas and to obtain easily green corundum, by doping aluminum oxide with cobalt oxide, synthesizing corundum by the use of a production unit of infrared concentrated heating for single crystal. CONSTITUTION:Aluminum oxide powder is fully blended with cobalt oxide as a colorant. An amount of the colorant is 1.0-5.0wt% based on the total amount. The raw material is then packed into a rubber tube, air in the tube is taken out, and molded into a column rod by rubber press method. The rod is sintered at 1,000-1,700 deg.C to give a raw material rod, and corumdum is synthesized by using corumdum single crystal and a sintered material of it as seed crystal by a production unit of infrared concentrated heating for single crystal in a reducing atmosphere. The production unit shown by the fig. is provided with the rotary elliptic face mirror 1, the halogen lamp 2, the quartz pipe 3, the inlet and the outlets 4 and 5 of atomsphere gas. the raw material 6, the seed crystal 7, and the melt zone part 8.

Description

【発明の詳細な説明】 〔技術分野〕 本発明は、緑色のコランダム単結晶の製造に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to the production of green corundum single crystals.

〔従来技術〕[Prior art]

従来々−１緑色のコランダムは、ベルヌーイ法及び引き
上げ法により合成されているが、雰囲気制御が困難であ
り、目的の緑色を出すことが非常に難しい。Conventionally, -1 green corundum has been synthesized by the Bernoulli method and the pulling method, but it is difficult to control the atmosphere and it is very difficult to produce the desired green color.

〔目　的〕〔the purpose〕

本発明の目的は、雰囲気制御が容易なＦ、Ｚ。 The object of the present invention is to provide F and Z with easy atmosphere control.

装置を用いて緑色のコランダムを合成することである。The purpose is to synthesize green corundum using a device.

〔発明の要約〕[Summary of the invention]

本発明では、主成分の酸化アルミニウム粉末及び着色剤
である酸化コバルトを乳ばちに秤り取り十分混合する。In the present invention, aluminum oxide powder, which is the main component, and cobalt oxide, which is a coloring agent, are weighed in a milk pestle and mixed thoroughly.

このときの着色剤の量は、全量に対して１．０〜５．０
Ｗ％とする。１．０Ｗ％より少ない場合は着色されず、
Ｓ、ＯＷ％より多い場合は、偏析を起こすため不適であ
る。次に上ｈピ原料をゴムチューブに詰め、チューブ内
の空気を抜き、ラバープレス法により円柱状の棒に成型
する。この棒を１０００℃〜１７００℃で焼結し原料棒
とする。これを原料とし、種子結晶にコランダム単結晶
及びその焼結体を用いて図１に示すような装置により合
成を行なう。成長方向は、任意の方向ｉ選ぶことが可能
である。育成雰囲気は、還元雰囲気とし、任意の還元性
ガスを用いることができる。例えば、水素ガス、−酸化
炭素ガス、またそれと不活性ガスとの混合ガス等がこれ
に用いることが可能である。その他の合成条件は、従来
Ｆ、Ｚ、装置によって合成されているルビー、サファイ
ア等の合成条件Ｇこ従う。The amount of colorant at this time is 1.0 to 5.0 to the total amount.
Let it be W%. If it is less than 1.0W%, it will not be colored,
If it exceeds S and OW%, it is unsuitable because it causes segregation. Next, the raw materials are packed into a rubber tube, the air inside the tube is removed, and the tube is molded into a cylindrical rod using a rubber press method. This rod is sintered at 1000°C to 1700°C to obtain a raw material rod. Using this as a raw material and a corundum single crystal and its sintered body as a seed crystal, synthesis is carried out using an apparatus as shown in FIG. Any direction i can be selected as the growth direction. The growth atmosphere is a reducing atmosphere, and any reducing gas can be used. For example, hydrogen gas, -carbon oxide gas, or a mixed gas of these and an inert gas can be used. Other synthesis conditions follow the synthesis conditions G for ruby, sapphire, etc. synthesized by conventional F, Z, and equipment.

〔実施例〕〔Example〕

以下に本発明の効果をはっきりさせるため、実施例を述
べる。Examples will be described below in order to clarify the effects of the present invention.

〈実施例１〉 ０原料組成 Ａｔ、０．　３９．６ｒ Ｏｏ　ＯＯ，４ｔ Ｏ原料棒作製 上記粉末をアルミナの乳ばちに入れ十分混合する。これ
をφ１０叫のゴムチューブに詰め、空気抜きを行なった
後ラバープレス法により４８ｍｍＸ８０嘔（Ａ）の棒に
成型する。これを１６００℃で４時間電気炉中で焼結し
、原料棒とすＯ結晶合成 上記で作成した原料棒を原料とし、種子結晶にルビーを
用いて図１に示す装置を用いて下記の育成条件により結
晶合成を行なった。<Example 1> 0 raw material composition At, 0. 39.6r Oo OO, 4t Preparation of O raw material rod Place the above powder in an alumina mortar and mix thoroughly. This was packed into a rubber tube with a diameter of 10 mm, and after air was removed, it was molded into a rod of 48 mm x 80 mm (A) using a rubber press method. This was sintered in an electric furnace at 1,600°C for 4 hours, and used as a raw material rod for O crystal synthesis. Using the raw material rod created above as a raw material and using ruby as a seed crystal, the following growth was performed using the apparatus shown in Figure 1. Crystal synthesis was carried out under certain conditions.

成長方向　（００１） シャフトの回転数（上下に逆・方向）３０ｒｐｍ育成雰
囲気　：　水素 育成速度　１．０　ｍｍ／　Ｈ Ｏ結　果 緑色のコランダム単結晶が合成できた。また結晶全体に
均一に着色した。Growth direction (001): Rotation speed of shaft (inverted vertically/direction): 30 rpm Growth atmosphere: Hydrogen growth rate: 1.0 mm/H O Results: A green corundum single crystal was synthesized. Furthermore, the entire crystal was colored uniformly.

〈実施例２〉 Ｏ原料組成 Ａｔ、０．　３８．Ｏｆ ＯＱ　Ｏ２，Ｏｒ Ｏ原料作製 〈実施例１〉に従う Ｏ結晶合成 〈実施例１〉に従う。<Example 2> O raw material composition At, 0. 38. Of OQ O2, Or O raw material preparation According to <Example 1> O crystal synthesis According to <Example 1>.

Ｏ結　果 緑色のコランダムの単結晶が合成された。また結晶全体
に均一に着色された。Results: A green corundum single crystal was synthesized. In addition, the entire crystal was uniformly colored.

〈実施例５〉 ０原料組成 Ａｚ、ｏ３　３９．Ｏｆ Ｏｏ　Ｏ１，Ｏｆ Ｏ原料棒作製 〈実施例１〉に従う。<Example 5> 0 raw material composition Az, o3 39. Of Oo　O1,Of O raw material rod production According to <Example 1>.

Ｏ結晶合成 雰囲気ガス　Ｈ，（５０％）−１−Ａｒ（５０％）その
他の条件は、〈実施例１〉に従う。O crystal synthesis atmosphere gas H, (50%) -1-Ar (50%) Other conditions are in accordance with <Example 1>.

Ｏ結　果 緑色のコランダムの単結晶が合成できた。また結晶全体
に均一に着色した。Result: A green corundum single crystal was synthesized. Furthermore, the entire crystal was colored uniformly.

〔発明の効果〕〔Effect of the invention〕

以上より、本発明の効果は、図１に示すようなＦ、Ｚ、
装置を用いて、雰囲気ガスを自由にコントロールするこ
とにより容易に緑色のコランダムを合成することが可能
になった。From the above, the effect of the present invention is that F, Z, as shown in FIG.
Using this equipment, it has become possible to easily synthesize green corundum by freely controlling the atmospheric gas.

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

第１図に赤外線加熱単結晶製造装置の概略を示す。 １・・・・・・・・・回転楕円面鏡 ２−’−−−−−゛°ハロゲンランプ ３・・・・・・・・・石英管 ４・・・・・・・・・雰囲気ガス入口 ５・・・・・・・・・雰囲気ガス出口 ６・・・・・・・・・原料棒 ７・・・・・・・・・種子結晶 ８・・・・・・・・・融帯部 ９・・・・・・・・・上シャフト １０・・・・・・下シャフト 以　上 FIG. 1 shows an outline of the infrared heating single crystal manufacturing apparatus. 1・・・・・・・・・Spheroidal mirror 2−’−−−−−゛°Halogen lamp ３・・・・・・・・・Quartz tube 4・・・・・・Atmosphere gas inlet 5・・・・・・Atmosphere gas outlet 6・・・・・・・・・Raw material rod 7... Seed crystal 8・・・・・・・・・Fluid zone 9・・・・・・・・・Upper shaft １０・・・Lower shaft that's all

Claims (2)

【特許請求の範囲】[Claims] （１）酸化アルミニウムに着色剤として酸化コバルトを
ドープし、図１に示す赤外線集中加熱単結晶製造装置を
用いることを特徴とするコランダムの製造方法。(1) A method for producing corundum, which comprises doping aluminum oxide with cobalt oxide as a coloring agent and using an infrared concentrated heating single crystal production apparatus shown in FIG. （２）前記組成の結晶の育成雰囲気を還元雰囲気とする
ことを特徴とする特許請求の範囲第１項記載のコランダ
ムの製造方法。(2) The method for producing corundum according to claim 1, characterized in that the atmosphere for growing crystals having the above composition is a reducing atmosphere.
JP59031698A 1984-02-22 1984-02-22 Preparation of corundum Pending JPS60176994A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59031698A JPS60176994A (en) 1984-02-22 1984-02-22 Preparation of corundum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59031698A JPS60176994A (en) 1984-02-22 1984-02-22 Preparation of corundum

Publications (1)

Publication Number Publication Date
JPS60176994A true JPS60176994A (en) 1985-09-11

Family

ID=12338288

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59031698A Pending JPS60176994A (en) 1984-02-22 1984-02-22 Preparation of corundum

Country Status (1)

Country Link
JP (1) JPS60176994A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100497968B1 (en) * 2002-06-05 2005-07-01 김창경 A and therefore

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100497968B1 (en) * 2002-06-05 2005-07-01 김창경 A and therefore

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