JPS60191098A - Manufacture of corundum - Google Patents

Manufacture of corundum

Info

Publication number
JPS60191098A
JPS60191098A JP59047715A JP4771584A JPS60191098A JP S60191098 A JPS60191098 A JP S60191098A JP 59047715 A JP59047715 A JP 59047715A JP 4771584 A JP4771584 A JP 4771584A JP S60191098 A JPS60191098 A JP S60191098A
Authority
JP
Japan
Prior art keywords
raw material
corundum
rod
sapphire
crystal
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
JP59047715A
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 JP59047715A priority Critical patent/JPS60191098A/en
Publication of JPS60191098A publication Critical patent/JPS60191098A/en
Pending 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
    • C30B13/00Single-crystal growth by zone-melting; Refining by zone-melting
    • 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
    • C30B29/20Aluminium 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 synthesize the titled blue corundum doped with cobalt by sintering a raw material rod consisting of aluminum oxide and cobalt oxide, using said sintered rod as the raw material, and using a corundum crystal as the seed crystal. CONSTITUTION:Aluminum oxide as the essential component and cobalt oxide as the colorant are mixed and pulverized, and the amt. of the cobalt oxide to about 3.0-5.0wt%. The mixed powder is packed into a rubber tube, and the air in the tube is let out. The mixed powder is molded into a columnar rod with the rubber press method, and sintered at about 1,300-1,600 deg.C to obtain the raw material rod. The sapphire is synthesized with the beam-condensing floating zone method by using said raw material rod as the raw material and a ruby or a sapphire single crystal as the seed crystal. The blue corundum crystal in a shade different from the existing blue sapphire can be manufactured in this way.

Description

【発明の詳細な説明】 〔技術分野〕 本発明は、集光FZ法を用いたコランダムの製造方法に
関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method for producing corundum using a condensing FZ method.

〔従来技術〕[Prior art]

従来青色のコランダムは、ブルーサファイアと呼ばれ、
着色剤として酸化鉄、酸化チタンが使用されていた。こ
れに対してコバルトを着色剤とした青色のコ・ランダム
は現在まで合成されていなかった0 C本発明の目的〕 本発明の目的は、従来合成されたことがなかった、コバ
ルトドープの青色のコランダムの合成を行なうことであ
る。
Traditionally blue corundum is called blue sapphire.
Iron oxide and titanium oxide were used as colorants. On the other hand, blue corundum using cobalt as a coloring agent has not been synthesized to date. The goal is to synthesize corundum.

〔発明の概要〕[Summary of the invention]

主成分の酸化アルミニウム粉末及び、着色剤である酸化
コバルト粉末を乳ばちに秤り取り、十分に混合する。こ
のときの酸化コバルトの量は、五〇〜5.0W%とする
。次に上i己原料をゴムチューブに詰め、チーーブ内の
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1600℃〜1j00℃で焼結し原料棒と
する。これを原料とし、種子結晶にルビー、サファイア
等のコランダム単結茜を用いて、図1に示すような装置
により合成を行なう、成長方向としては、イ:意の方向
に成長させることが可能である。その11の合成条件は
、従来集光FZ法で行なわれていイルビー、サファイア
の合成条件に従う。
Aluminum oxide powder, the main component, and cobalt oxide powder, the coloring agent, are weighed into a mortar and mixed thoroughly. The amount of cobalt oxide at this time is 50 to 5.0 W%. 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 1600°C to 1j00°C to obtain a raw material rod. This is used as a raw material, and synthesis is carried out using a device as shown in Figure 1, using single corundum madder such as ruby or sapphire as a seed crystal. be. The 11 synthesis conditions follow the synthesis conditions of Ilby and Sapphire, which have been conventionally carried out using the condensing FZ method.

〔実施例〕〔Example〕

以下、本発明の効果をはっきりさせるため実H例を述べ
る。
Hereinafter, a practical example will be described in order to clarify the effects of the present invention.

〈実施例1〉 O原料組成 Al、、0. 29.15’ Oo OO,9f O原料棒作製 上記原料粉末をアルミナの乳ばちGこ入れ士多混介する
。これをφ1a鰭のゴムチューブに言め、空気抜きを行
なった後ラバープレス法にユリφ8mmX 80in 
(t)の棒に成形する。こ才を1600°Cで4時間電
気炉中で焼結し、原津棒とした。
<Example 1> O raw material composition Al, 0. 29.15' Oo OO, 9f Preparation of O raw material rod The above raw material powder is mixed in an alumina milk drum. Apply this to the rubber tube of the φ1a fin, and after removing the air, use the rubber press method to attach the lily φ8mm x 80in.
Form into a bar (t). The kosai was sintered in an electric furnace at 1600°C for 4 hours to obtain a Harazu bar.

O結晶合成 上記で作製した原料棒を原料とし、種子結晶にルビーを
用いて図1に示す装置を使用して下L 記の育成条件に
より結晶合成を行なった。
O Crystal Synthesis Using the raw material rod prepared above as a raw material and using ruby as a seed crystal, crystal synthesis was carried out using the apparatus shown in FIG. 1 under the growth conditions shown below.

成長方向 (001) シャフトの回転数 30rpm(上、下逆回転) 1 有成雰囲気 空気 育成速度 2. Q晒/H O結果及び所見 色むらのない青色の結晶が合成できた。Growth direction (001) Shaft rotation speed: 30 rpm (up and down reverse rotation) 1 Formed atmosphere air Growth speed 2. Q exposure/H OResults and findings Blue crystals with no uneven color were synthesized.

〈実施例2〉 offi、料組成 At20. 3a5f! ト o o o 1. 5 ≦− 5o原料棒作製 〈実施例1〉に従う。<Example 2> offi, material composition At20. 3a5f! G o o o 1. 5≦− 5o raw material rod production According to <Example 1>.

し O結晶合成 十 育成速度をt Omm/ Hとする以外は〈実施例
1〉に従う。
Example 1 was followed except that the growth rate was set to t Omm/H.

0結果及び所見 色むらのない青色の結晶が合成できた。0 results and findings Blue crystals with no uneven color were synthesized.

〈実施例3〉 0jら(料組成 Al、、Oa 29.15’ Co OO,9V O原料)・;Σ作製 く実施例1〉に従う。<Example 3> 0j et al. Al,,Oa 29.15' Co OO,9V O raw material)・;Σ production Example 1 was followed.

0結晶子ヤ成 成長方向を(100)とする以外はに実施例1 )+こ
 fY う 。 ・ Q結果及び所見 色むらのない青色の結晶が合成できた。
Example 1) + fY except that the growth direction of 0 crystallites was set to (100).・Q results and findings Blue crystals with no color unevenness were synthesized.

〔う自明の効果〕[Obvious effect]

以上のように、本発明によれば、着色剤として15マ化
コバルトを用いることにより従N〔のブルーサファイア
とは異なる青色のコランダム結晶の合成が可能となった
As described above, according to the present invention, by using cobalt 15meride as a coloring agent, it has become possible to synthesize a blue corundum crystal that is different from the conventional blue sapphire.

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

第1図は本発明に用いた実験装置の概略図である。 1・・・・・・回転楕円面鏡 2・・・・・・ハロゲンランプ 5・・・・・・石莢管 4・・・・・・算囲気ガス導入口 5・・・・・・雰囲気ガス出口 6・・・・・・原料体 7・・・・・・種子結晶 8・・・・・・融 帯 9・・・・・・主4’j+ Jニシャフト10・・°主
軸下シャフト 以 上 出願人 株式会社諏訪1jl’を工舎 代理人 弁理士 最上 務 第1図
FIG. 1 is a schematic diagram of the experimental apparatus used in the present invention. 1...Spheroidal mirror 2...Halogen lamp 5...Stone capsule tube 4...Internal air gas inlet 5...Atmosphere Gas outlet 6... Raw material body 7... Seed crystal 8... Melting zone 9... Main 4'j+ J Nishaft 10...° Below the shaft below the main axis Applicant: Suwa 1JL Co., Ltd., agent of Kosha, patent attorney, Tsutomu Mogami Figure 1

Claims (1)

【特許請求の範囲】[Claims] ri12化アルミニウムを主成分とし、着色剤として酸
化コバルトからなるコランダムの原料粉末をゴムチュー
ブに詰め、ラバープレス法により棒状に成形し、焼結し
て原料棒とし、これを原料とし種子結晶にルビー、サフ
ァイア等のコランダム結晶を用いて、集光フローティン
グゾーン法により合成を行なうことを特徴とするコラン
ダムの製造方法も
Raw material powder of corundum, which is mainly composed of aluminum ri12 and cobalt oxide as a coloring agent, is packed into a rubber tube, formed into a rod shape by a rubber press method, and sintered to form a raw material rod. There is also a method for producing corundum characterized by synthesis using a condensing floating zone method using corundum crystals such as sapphire.
JP59047715A 1984-03-13 1984-03-13 Manufacture of corundum Pending JPS60191098A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59047715A JPS60191098A (en) 1984-03-13 1984-03-13 Manufacture of corundum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59047715A JPS60191098A (en) 1984-03-13 1984-03-13 Manufacture of corundum

Publications (1)

Publication Number Publication Date
JPS60191098A true JPS60191098A (en) 1985-09-28

Family

ID=12783001

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59047715A Pending JPS60191098A (en) 1984-03-13 1984-03-13 Manufacture of corundum

Country Status (1)

Country Link
JP (1) JPS60191098A (en)

Cited By (3)

* 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
JP5729569B2 (en) * 2010-03-31 2015-06-03 国立研究開発法人産業技術総合研究所 Method for producing metal compound crystal and method for producing decorative article
WO2017187647A1 (en) * 2016-04-25 2017-11-02 株式会社信光社 Blue-colored aluminum oxide single crystal and method for producing aluminum oxide single crystal

Cited By (4)

* 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
JP5729569B2 (en) * 2010-03-31 2015-06-03 国立研究開発法人産業技術総合研究所 Method for producing metal compound crystal and method for producing decorative article
WO2017187647A1 (en) * 2016-04-25 2017-11-02 株式会社信光社 Blue-colored aluminum oxide single crystal and method for producing aluminum oxide single crystal
JPWO2017187647A1 (en) * 2016-04-25 2018-08-30 株式会社信光社 Aluminum oxide single crystal exhibiting blue color and method for producing the aluminum oxide single crystal

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