JPS5945998A - Preparation of corundum - Google Patents

Preparation of corundum

Info

Publication number
JPS5945998A
JPS5945998A JP57151067A JP15106782A JPS5945998A JP S5945998 A JPS5945998 A JP S5945998A JP 57151067 A JP57151067 A JP 57151067A JP 15106782 A JP15106782 A JP 15106782A JP S5945998 A JPS5945998 A JP S5945998A
Authority
JP
Japan
Prior art keywords
crystal
raw material
corumdum
oxide
corundum
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
JP57151067A
Other languages
Japanese (ja)
Other versions
JPH0355436B2 (en
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 JP57151067A priority Critical patent/JPS5945998A/en
Publication of JPS5945998A publication Critical patent/JPS5945998A/en
Publication of JPH0355436B2 publication Critical patent/JPH0355436B2/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
    • 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 prepare red orange-colored jewels inexpensively, by molding and sintering a corumdum raw material blended with chromium oxide and nickel oxide as a color producing reagent into a cylindrical shape to give a raw material, heating it in infrafed rays using corumdum seed crystal. CONSTITUTION:Aluminum oxide as a main bomponent, 0.2-0.5wt% chromium oxide and 0.2-0.5wt% nickel oxide as a color producing reagent based on the total amount, respectively, are powdered, blended, packed into a rubber tube, and molded into a cylindrical rod by rubber pressing method. It is sintered in an electric furnace at 1,200-1,700 deg.C to give a raw material, and corumdum crystal or sintered corumdum is used as a seed crystal. The material rod 3 and the seed crystal 4 are molted by the artificial source lamp 2 set at one foucs of the ellipsoidal mirror 1 by a production unit for single crystal under concentrated heating by infrared rays shown by the figure, and the top and bottom shaft 5 and 6 are dropped while being rotated, to synthesize the crystal. Red orange- colored Paparachia sapphire can be prepared inexpensively.

Description

【発明の詳細な説明】 本発明は、赤外線集中加熱単結晶MJ造装置を用いたコ
ランダムの製造方法に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing corundum using an infrared concentrated heating single crystal MJ production apparatus.

コランダムの色は、発色剤として酸化クロムを用いれば
ルビーとなり、酸化チタン、酸化第2鉄を用いればブル
ーサファイアとなる。本発明では、発色剤として酸化ク
ロム、酸化ニッケルを用いたパパラチアサファイアにつ
いて述べる。
The color of corundum becomes ruby if chromium oxide is used as a coloring agent, and blue sapphire if titanium oxide or ferric oxide is used as a coloring agent. In the present invention, Padparadscha sapphire using chromium oxide or nickel oxide as a coloring agent will be described.

主成分の酸化アルミニウムに発色剤として酸化クロム及
び酸化ニッケルを各々全Llに対して02W%〜0.5
 w%、0.2 w%〜0.5 w%を乳ばちに入れ、
十分混合する。このとき酸化ニアケルが0、2 w%よ
り少くない場合は、合成時に酸化ニッケルが蒸発してし
まうため不適であり、0.5 w%より多い場合は黄色
が強くなりすぎるため不適である。また、酸化クロムが
全り目こ対しc O,2W%より少くない場合は赤色が
薄く不適であり、全組に対して0.5W%より多い場合
は赤色が強すぎて不適である。次に混合した粉末をゴム
チューブに詰め、チューブ内の空気抜きを行なう。これ
をうバープレス法により円柱状の棒に成形する。この棒
を゛電気炉中で1200℃〜1600℃で焼結する。こ
のとき1200℃以下では焼結不足で合成時に結晶内に
気泡が多針に取り込むため不適である。また1700℃
以上では焼結度が変わらない。
The main component is aluminum oxide, and chromium oxide and nickel oxide are added as coloring agents to the total Ll, each at 02W% to 0.5%.
w%, 0.2 w% to 0.5 w% is added to the milk drum,
Mix thoroughly. At this time, if the amount of nickel oxide is less than 0.2 w%, it is unsuitable because the nickel oxide will evaporate during the synthesis, and if it is more than 0.5 w%, the yellow color will become too strong, which is unsuitable. Further, if the chromium oxide content is less than cO,2W% for all sets, the red color will be weak and unsuitable, and if it is more than 0.5W% for the whole set, the red color will be too strong and unsuitable. Next, the mixed powder is packed into a rubber tube, and the air inside the tube is removed. This is formed into a cylindrical rod using the wrapper press method. This rod is sintered at 1200°C to 1600°C in an electric furnace. At this time, temperatures below 1200° C. are not suitable because sintering is insufficient and many air bubbles are incorporated into the crystal during synthesis. Also 1700℃
Above this, the degree of sintering does not change.

この焼結体を原料とし、種子結晶としてコランダム単結
晶または、コランダム焼結体を用いて図1に示すごとく
の赤外線集中加熱単結晶製造装置により単結晶を合成す
る。合成された結晶は赤橙色の結晶となる。
Using this sintered body as a raw material and a corundum single crystal or a corundum sintered body as a seed crystal, a single crystal is synthesized using an infrared concentrated heating single crystal manufacturing apparatus as shown in FIG. The synthesized crystals are reddish-orange.

コランダム結晶の中で赤橙色の結晶は、パバラチアサフ
ァイアと呼ばれ、スリラン力だけしか産出しない非常に
珍しい宝石であり非常に高価である。本発明では、この
貴重な宝石を一般に安価に提供することを可能とした。
Among the corundum crystals, the reddish-orange crystal is called Pavaratia sapphire, and it is a very rare gemstone that only produces Srilan power, and is very expensive. The present invention has made it possible to provide this precious gemstone to the general public at a low cost.

本発明の効果をより一掃はっきりさせるために以下に実
施例を述べる。
Examples will be described below to make the effects of the present invention more clear.

〈実施例1〉 (1)原料棒作製方法 酸化アルミニウム    2988? 酸化クロム       0061i′酸化ニツケル 
     0061 上記3種類の原料粉末をアルミナ乳ばち(こ入れ十分混
合する。これをゴムチューブに詰め、チューブ内の空気
を真空ポンプで抜き、ラノく一プレスにより3000 
”F’/C/Jの圧力で10語(φ)X 120vn 
(1)の棒に成形する。この棒をケラマックス電気炉中
で1600℃で焼結する。
<Example 1> (1) Raw material rod production method Aluminum oxide 2988? Chromium oxide 0061i′ nickel oxide
0061 The above three kinds of raw material powders are thoroughly mixed in an alumina pestle. This is packed into a rubber tube, the air inside the tube is removed with a vacuum pump, and the 3000
"F'/C/J pressure 10 words (φ) x 120vn
(1) Shape into a rod. This bar is sintered in a Keramax electric furnace at 1600°C.

(2)合成方法 図1に示すような装置音用いて下記の条件により結晶を
合成する。
(2) Synthesis method Crystals are synthesized under the following conditions using the equipment sound shown in Figure 1.

種子結晶    コランダム単結晶 成長方向    (100) 成長速度    2 wn / H 上シャフト回転数 3Orpm   (上、王道回転)
下シャフト回転数 30rp+n 育成雰囲気    空気 合成時間     50時間 (3)結果 赤橙色の楕円形の棒状の単結晶が合成できた。
Seed crystal Corundum single crystal Growth direction (100) Growth rate 2 wn / H Upper shaft rotation speed 3 Orpm (Top, classic rotation)
Lower shaft rotation speed: 30 rp+n Growth atmosphere: Air Synthesis time: 50 hours (3) Result: A reddish-orange oval rod-shaped single crystal was synthesized.

〈実施例2〉 (1)原料棒作製方法 酸化アルミニウム    29.70 f酸化クロム 
        0.159酸化二ソケル      
 015v 以下の操作は〈実施例1〉に従う。
<Example 2> (1) Raw material rod production method Aluminum oxide 29.70 f Chromium oxide
0.159 disokel oxide
015v The following operations follow <Example 1>.

(2)合成方法 〈実施例1〉に従う。(2) Synthesis method According to <Example 1>.

(3)   結  果 〈実施例1〉より濃い赤橙色の結晶が合成された。また
結晶は楕円形の棒状のものとなった。
(3) Results Crystals with a deeper reddish-orange color than in Example 1 were synthesized. In addition, the crystals were oval and rod-shaped.

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

第1図に示すように回転楕円面鏡(1)の一方の焦点に
人工ゲンランプ(2)を置き、もう一方の焦点に集光さ
せてそこに置かれた原料棒(3)及び種子結晶(4)を
溶融させ、ゾーンを形成させる。そして、上下シャ7 
ト(5) 、 (a)を回転させながら下降することに
より結晶を合成する。また石英管内(7)に適当なガス
を流すことにより育成雰囲気を変えることが可能である
。 以  上 出願人  株式会社諏訪精工舎 代理人  弁理士 最上  務
As shown in Fig. 1, an artificial generator lamp (2) is placed at one focal point of the spheroidal mirror (1), and the light is focused at the other focal point, and the raw material rod (3) and seed crystals ( 4) is melted to form a zone. And upper and lower shaft 7
(5) and (a) are lowered while rotating to synthesize crystals. Furthermore, it is possible to change the growth atmosphere by flowing an appropriate gas into the quartz tube (7). Applicant Suwa Seikosha Co., Ltd. Patent Attorney Tsutomu Mogami

Claims (1)

【特許請求の範囲】[Claims] (1)酸化アルミニウムを主成分とし、発色剤として酸
化クロム及び酸化ニッケルを加えてなるコランダム原料
を、ゴムチューブに詰め、ラバープレス法により円柱状
の棒に成形する。 これを電気炉中で1200℃〜1700℃で焼結する。 この棒を原料とし、種子結晶としてコランダム結晶また
は、コランダムの焼結体を用いて図1に示すような赤外
線集中加熱単結晶製造装置を用いて合成することを特徴
とするコランダムの製造方法。 (2、特許請求の範囲第1項において、発色剤である酸
化クロム及び酸化ニッケルが全量に対して各々0.2 
w%〜0.5 w%、0.2 w%〜0.5W%とする
ことよりなる同項記載の方法。
(1) A corundum raw material containing aluminum oxide as a main component and chromium oxide and nickel oxide as coloring agents is packed into a rubber tube and formed into a cylindrical rod by a rubber press method. This is sintered at 1200°C to 1700°C in an electric furnace. A method for producing corundum, which comprises using this rod as a raw material, using a corundum crystal or a sintered body of corundum as a seed crystal, and using an infrared concentrated heating single crystal production apparatus as shown in FIG. (2. In claim 1, each of chromium oxide and nickel oxide as coloring agents is 0.2% of the total amount.
The method according to the same item, which comprises setting the content to w% to 0.5 w% and 0.2 w% to 0.5 W%.
JP57151067A 1982-08-31 1982-08-31 Preparation of corundum Granted JPS5945998A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP57151067A JPS5945998A (en) 1982-08-31 1982-08-31 Preparation of corundum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP57151067A JPS5945998A (en) 1982-08-31 1982-08-31 Preparation of corundum

Publications (2)

Publication Number Publication Date
JPS5945998A true JPS5945998A (en) 1984-03-15
JPH0355436B2 JPH0355436B2 (en) 1991-08-23

Family

ID=15510575

Family Applications (1)

Application Number Title Priority Date Filing Date
JP57151067A Granted JPS5945998A (en) 1982-08-31 1982-08-31 Preparation of corundum

Country Status (1)

Country Link
JP (1) JPS5945998A (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5556093A (en) * 1978-10-16 1980-04-24 Seiko Epson Corp Production of star ruby or star sapphire

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5556093A (en) * 1978-10-16 1980-04-24 Seiko Epson Corp Production of star ruby or star sapphire

Also Published As

Publication number Publication date
JPH0355436B2 (en) 1991-08-23

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