JPS60226485A - Production of corundum - Google Patents

Production of corundum

Info

Publication number
JPS60226485A
JPS60226485A JP59084492A JP8449284A JPS60226485A JP S60226485 A JPS60226485 A JP S60226485A JP 59084492 A JP59084492 A JP 59084492A JP 8449284 A JP8449284 A JP 8449284A JP S60226485 A JPS60226485 A JP S60226485A
Authority
JP
Japan
Prior art keywords
raw material
sulfate
golden
sapphire
chloride
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
JP59084492A
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 JP59084492A priority Critical patent/JPS60226485A/en
Publication of JPS60226485A publication Critical patent/JPS60226485A/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
    • C30B13/16—Heating of the molten zone
    • C30B13/22—Heating of the molten zone by irradiation or electric discharge
    • C30B13/24—Heating of the molten zone by irradiation or electric discharge using electromagnetic waves
    • 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)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

PURPOSE:To produce a high-quality corundum crystal free from voids, by sintering powdery mixture composed of an Al salt, etc., Cr hydroxide, etc., and Ni chloride, etc. at specific ratios, and synthesizing the objective corundum from the obtained sintered material by the focused floating zone melting process. CONSTITUTION:An Al compound selected from the ammonium carbonate, ammonium hydroxide sulfate and sulfate, a Cr compound selected from the hydroxide, nitrate, sulfate and chloride, and an Ni compound selected from the chloride, nitrate and sulfate are mixed together at a ratio close to the compositional ratio of golden sapphire, and the mixture is thermally decomposed at about 800- 1,200 deg.C to obtain the raw material powder. The powder is formed to a columnar rod by a rubber-press, and is sintered at about 1,300 deg.C-1,600 deg.C to obtain a raw material rod. The rod is used as the raw material, and a golden sapphire is grown from the raw material by the focused floating zone process using a corundum crystal as the seed crystal. A golden sapphire free from voids and colored uniformly in golden color can be produced by this process.

Description

【発明の詳細な説明】 〔技術分野〕 本発明は、竿先Ｆ、Ｚ（７０−ティングゾーン）法によ
るコランダムの合成に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to the synthesis of corundum by the tip F, Z (70-ting zone) method.

〔従来技術〕[Prior art]

従来ゴールデンサファイアの原料に市販の酸化アルミニ
ウム、酸化クロム、酸化ニッケルを用いて原料棒を作製
した場合、合成した結晶に多用の気泡を含有するという
問題点があった。これは宝石部材としてのゴールデンサ
ファイアの価値を著しく低下させる原因となる。Conventionally, when raw material rods were produced using commercially available aluminum oxide, chromium oxide, and nickel oxide as raw materials for golden sapphire, there was a problem in that the synthesized crystal contained a large number of air bubbles. This causes a significant decrease in the value of golden sapphire as a jewelry component.

〔目　的〕〔the purpose〕

本発明の目的は気泡のない良質のゴールデンサファイア
の結晶を合成することにより宝石部材としての価値を高
めることである。The purpose of the present invention is to increase its value as a jewelry member by synthesizing high-quality golden sapphire crystals without bubbles.

〔概　要〕〔overview〕

本発明では、ゴールデンサファイアの原料粉末をアルミ
ニウムのアンモニウム炭酸塩、水酸化物アンモニウム硫
酸塩、硫酸塩のいずれが１つ及びクロムの水酸化物、硝
酸塩、硫酸塩、塩化物のいずれか１つ及びニッケルの塩
化物、硝酸塩、硫酸塩のいずれか１つをボールミル、又
は乳ばちで混合し電気炉中で熱分解して得る。このとき
クロムの水酸化物、硝酸塩、硫酸塩、塩化物の量は、酸
化物に換算して金星に対し００１〜００５Ｗ％とする。In the present invention, the raw material powder of golden sapphire is combined with one of aluminum ammonium carbonate, hydroxide, ammonium sulfate, and sulfate, and one of chromium hydroxide, nitrate, sulfate, and chloride. It is obtained by mixing any one of nickel chloride, nitrate, and sulfate in a ball mill or pestle and thermally decomposing the mixture in an electric furnace. At this time, the amount of chromium hydroxide, nitrate, sulfate, and chloride is 001 to 005 W% relative to Venus in terms of oxide.

またニッケルについても同様に全量に対してｉ、　ｏ　
ｗ％〜２．　Ｄ　ｗ％とする。また熱分解の温度は、８
００℃〜１２００℃とする。次に上記原料をゴムチー−
ブに詰め・チーープ内の空気を抜キラバープレス法によ
り円柱状の棒に成型する。この棒を１３００℃〜１６０
０℃で焼結し原料棒とする。これを原料とし種子結晶に
コランダム単結晶を用いて図１に示すような装置により
ゴールデンサファイアの結晶を合成する◇成長方向とし
ては、任意の方向に成長させることか可能である。Similarly, for the total amount of nickel, i, o
w%~2. D w%. In addition, the temperature of thermal decomposition is 8
00°C to 1200°C. Next, add the above raw materials to rubber
Fill it in a cheep, remove the air inside the cheep, and mold it into a cylindrical rod using the rubber press method. This rod is heated to 1300℃~160℃
It is sintered at 0°C to form a raw material rod. Using this as a raw material and a corundum single crystal as a seed crystal, golden sapphire crystals are synthesized using an apparatus as shown in FIG. 1. ◇Growth in any direction is possible.

その他の合成条件は、従来の集光Ｆ、Ｚ、法によるゴー
ルデンサファイアの合成条件に従う。Other synthesis conditions follow the conventional synthesis conditions for golden sapphire using the condensing F, Z method.

〔実施例〕〔Example〕

〈実施例１〉 ０原料組成 ＮＨ，ＡｆｉＯ（ＯＨ）ＨＣ！０３　１０７９９３９１
０ｒ（ＯＨ）３　・２Ｈ２００，００７３ＰＨ１ａｆ１
２・６Ｈ２０１，２７２７グ０原料棒作製 上記原料粉末をボールミルにより２４時間混合した後白
金ルツボに入れ１０００℃で１時間電気炉中で仮焼する
。これをアルミナ乳ばちに入れ粉砕する。次にこれをφ
１０語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φ８鮎・×８０鵡（２）の棒に成型
する０これを１６００℃４時間電気炉中で焼結し原料棒
とした。<Example 1> 0 Raw material composition NH, AfiO(OH)HC! 03 10799391
0r(OH)3 ・2H200,0073PH1af1
2.6H201,2727g0 Production of raw material rod The above raw material powder was mixed in a ball mill for 24 hours, then placed in a platinum crucible and calcined in an electric furnace at 1000°C for 1 hour. Place this in an alumina mortar and crush. Next, add this to φ
The mixture was packed into 10 rubber tubes, air removed, and then molded into rods of φ8 Ayu x 80 Ayu (2) using a rubber press method.This was sintered in an electric furnace at 1600° C. for 4 hours to obtain a raw material rod.

０結晶合成 上記で作製した原料棒を原料とし、種子結晶にルビーの
単結晶を用いて、図１に示すような装置により下記の合
成条件で結晶合成を行なった。0 Crystal Synthesis Using the raw material rod prepared above as a raw material and using a ruby single crystal as a seed crystal, crystal synthesis was carried out under the following synthesis conditions using an apparatus as shown in FIG. 1.

成長方向　：（００１） シャフトの回転数　：３０ｒｐｍ（上、下、逆回転）育
成雰囲気　：空気 育成速度　：　ｔ　Ｏｍ、　／　Ｈ Ｏ結果及び所見 気泡を含有しない黄金色の結晶が合成できた。Growth direction: (001) Shaft rotation speed: 30 rpm (upward, downward, reverse rotation) Growth atmosphere: Air Growth rate: t Om, /H O Results and findings Golden crystals containing no bubbles were synthesized.

また結晶全体に均一に着色していた。In addition, the entire crystal was uniformly colored.

〈実施例２〉 ０原料組成 ＡＱ２（Ｎｏ４）３・１８Ｈ２０２５６，０８２６ｆＯ
ｒ（Ｎｏ３）３瞼９Ｈ，００，１０５２１ｉ’Ｎｔ（Ｎ
ｏ、、）２・６ｎ、、ｏ　３．５８８３ｆＯ原料棒作製 〈実施例１〉に従う。<Example 2> 0 Raw material composition AQ2 (No4) 3.18H20256,0826fO
r (No 3) 3 eyelids 9H, 00, 10521i'Nt (N
o, ,)2・6n,,o 3.5883fO raw material rod production according to <Example 1>.

〇結晶合成 〈実施例１〉に従う。〇Crystal synthesis According to <Example 1>.

０結果及び所見 気泡を含有しない黄金色の結晶が合成できた０また結晶
全体に均一に着色していた。0Results and ObservationsA golden yellow crystal containing no bubbles was synthesized.The entire crystal was uniformly colored.

〈実施例６〉 ０原料組成 （ＮＨ，Ｌ　５ｏ４−ｈＱ２（ｓｏ、　）３−２４Ｈ，
０３５２、０９３８ｆ ＯｒＣｆ）、３・６Ｈ，００，０１４０１ｉ’Ｎ　ｉ　
Ｓ　Ｏ，・６Ｈ２０１，４０７３ｆＯ原料棒作製 上記原料粉末をボールミルにより混合し、白金ルツボに
入れ１２００℃で１時間電気炉中で仮焼する。以下の繰
作は〈実施例１〉に従う。<Example 6> 0 raw material composition (NH,L 5o4-hQ2(so, )3-24H,
0352, 0938f OrCf), 3・6H, 00, 01401i'N i
S O,.6H201,4073fO raw material rod production The above raw material powders were mixed in a ball mill, placed in a platinum crucible, and calcined in an electric furnace at 1200° C. for 1 hour. The following operations are in accordance with <Example 1>.

０結晶合成 〈実施例１〉に従う０ ０結果及び所見 気泡を含有しない黄金色の結晶が合成できた。0 crystal synthesis 0 according to <Example 1> 0 results and findings Golden crystals containing no bubbles were synthesized.

また結晶全体に均一に着色していた・ 〔効　果〕 本発明の効果は集光Ｆ、ｚ　、Ｑにより気泡のないゴー
ルデンサファイアを合成することが可能となったことで
ある０In addition, the entire crystal was uniformly colored. [Effect] The effect of the present invention is that it became possible to synthesize bubble-free golden sapphire by focusing light F, z, and Q.

【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ｐンランプ ６・・・・・・石英管 ４・・・・・雰囲気ガス導入口 ５・・・・・・雰囲気ガス出口 ６・・・・・・原料棒 ７・・・・・・種子結晶 ８・・・・・・融帯 ９・・・・・・主軸上シャフト １０・・・・・・主軸下シャフト 以　上 出願人　株式会社諏訪精工自 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... Halo pn lamp 6...Quartz tube 4... Atmosphere gas inlet 5... Atmosphere gas outlet 6... Raw material rod 7...Seed crystal 8...Tender zone 9... Main spindle shaft 10... Main spindle lower shaft that's all Applicant: Suwa Seiko Co., Ltd. Agent Patent Attorney Mogami Figure 1

Claims (1)

【特許請求の範囲】[Claims] アルミニウムのアンモニウム炭酸塩、又は、水酸化物ア
ンモニウム硫酸塩、又は、硫酸塩のいずれか１つ、及び
クロムの水酸化物、又は硝酸塩、又は硝酸塩、又は塩化
物のいずれか１つ、及びニッケルの塩化物、硝酸塩、硫
酸塩のいずれか１つをほぼゴールデンサファイアの組成
比を示すように混合し、熱分解して原料粉末とし、これ
を円柱状の棒に成型し電気炉中で焼結し、これを原料と
し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。Any one of ammonium carbonate, hydroxide, ammonium sulfate, or sulfate of aluminum, and any one of chromium hydroxide, nitrate, or nitrate, or chloride, and nickel. Any one of chloride, nitrate, and sulfate is mixed in a composition ratio approximately equal to that of golden sapphire, thermally decomposed to obtain a raw material powder, which is formed into a cylindrical rod and sintered in an electric furnace. , a method for producing corundum, which is characterized in that the synthesis is carried out by a light-concentrating floating zone method using this as a raw material.
JP59084492A 1984-04-26 1984-04-26 Production of corundum Pending JPS60226485A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59084492A JPS60226485A (en) 1984-04-26 1984-04-26 Production of corundum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59084492A JPS60226485A (en) 1984-04-26 1984-04-26 Production of corundum

Publications (1)

Publication Number Publication Date
JPS60226485A true JPS60226485A (en) 1985-11-11

Family

ID=13832144

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59084492A Pending JPS60226485A (en) 1984-04-26 1984-04-26 Production of corundum

Country Status (1)

Country Link
JP (1) JPS60226485A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI403623B (en) * 2010-08-10 2013-08-01 Method for coating crystal

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI403623B (en) * 2010-08-10 2013-08-01 Method for coating crystal

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