JPS60176985A - Preparation of raw material for growing single crystal - Google Patents
Preparation of raw material for growing single crystalInfo
- Publication number
- JPS60176985A JPS60176985A JP59031696A JP3169684A JPS60176985A JP S60176985 A JPS60176985 A JP S60176985A JP 59031696 A JP59031696 A JP 59031696A JP 3169684 A JP3169684 A JP 3169684A JP S60176985 A JPS60176985 A JP S60176985A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- single crystal
- melt
- crystal
- crystal growth
- 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
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
Description
【発明の詳細な説明】
〔技術分野〕
本発明は原料としてアルミナ(Atiss)及びベリリ
ア(BO2)を用い、フローティングゾーン法により単
結晶を育成するための原料製造法である。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention is a raw material manufacturing method for growing a single crystal by a floating zone method using alumina (Atiss) and beryllia (BO2) as raw materials.
従来、フローティングゾーン法(以下FZ法)による特
許は新しい結晶の育成法に関するものがほとんどであり
、結晶の品質に関するものはほとんどなく、これらの方
法で育成した結晶には多数の欠陥が存在只、特に、宝石
として用いる人工結晶においては欠陥の中の1つである
気泡は、本来の光の反射、屈折を減少させ宝石としての
価値を減少させる大きな原因となっている。Until now, most of the patents for the floating zone method (hereinafter referred to as FZ method) were related to new crystal growth methods, and there were almost no patents related to the quality of the crystals, and the crystals grown by these methods had many defects. In particular, air bubbles, which are one of the defects in artificial crystals used as jewelry, are a major cause of reducing the original reflection and refraction of light, reducing the value of the crystal as a jewelry.
本発明は以上の間顯点を解決するもので、その目的とす
るところは、Ii’Z法によって育成する、コランダム
結晶及びアレキサンドライト結晶の中に気泡がないもの
を合成するための原料を製造する方法を提供することに
ある。The present invention solves the above problems, and its purpose is to produce a raw material for synthesizing corundum crystals and alexandrite crystals without air bubbles, which are grown by the Ii'Z method. The purpose is to provide a method.
本発明は融液から単結晶を育成する方法において、コラ
ンダム結晶及びアレキサンドライト結晶の原料粉末を真
空で処理することを特徴とする。The present invention is a method for growing a single crystal from a melt, and is characterized by treating raw material powders of corundum crystals and alexandrite crystals in a vacuum.
本発明に用いるアルミナはα−アルミナ、r−アルミナ
などがあるが限定されるものではない。Alumina used in the present invention includes α-alumina, r-alumina, etc., but is not limited thereto.
ベリリアにおいても同様である。The same is true for beryllia.
本発明における処理温度は800°C〜1500°Cの
範囲が最適で800℃以下では吸着ガスの解離及び脱離
が起きにくく効果が少ない。1500℃以上では2次粒
子が形成され、粒径が大きくなり、焼結性が低下するた
め上述の範囲が望ましい本発明における真空度は10−
’Torr〜1O−6TOrrが最適であり、10−1
TOrr以下では吸着ガスの除去に効果がなく、10
−’Torr以上では吸着ガスの除去に変化はみられず
、効果は同じである。よって上述の範囲が望ましい。The optimum treatment temperature in the present invention is in the range of 800° C. to 1500° C. If it is below 800° C., dissociation and desorption of the adsorbed gas are difficult to occur and the effect is small. At temperatures above 1,500°C, secondary particles are formed, the particle size increases, and sinterability deteriorates.
'Torr ~ 1O-6TOrr is optimal, and 10-1
Below TOrr, there is no effect in removing adsorbed gas, and 10
-'Torr or more, no change is observed in the removal of adsorbed gas, and the effect is the same. Therefore, the above range is desirable.
本発明における処理原料はFZ法による単結晶育成に用
いるものである。コランダム結晶の場合アルミナを主原
料とし、着色剤として、ルビーは酸化クロム、パパラチ
アは酸化クロムと酸化ニッケル、プx−サファイヤは酸
化鉄と酸化チタンを加え、丸棒状に焼結して原料とする
が、上述の処理原料を用いることによって、これら着色
剤の種類及び量に影響なく、気泡のない結晶を合成する
ことができる。The raw material to be treated in the present invention is used for single crystal growth by the FZ method. In the case of corundum crystals, alumina is the main raw material, and as a coloring agent, chromium oxide for ruby, chromium oxide and nickel oxide for padparadsia, iron oxide and titanium oxide for px-sapphire, and the raw material is sintered into a round rod shape. However, by using the above-mentioned processing raw materials, bubble-free crystals can be synthesized without affecting the type and amount of these colorants.
アレキサンドライト結晶の場合も同様に上述の処理原料
であるアルミナとベリリアを用い、着色剤として、酸化
クロムと酸化鉄を加え、原料棒に成形したものを用いて
FZ法によって結晶を育成すると、着色剤の毎に影響な
く気泡のない結晶が合成できる。In the case of alexandrite crystals, the above-mentioned processing raw materials alumina and beryllia are similarly used, chromium oxide and iron oxide are added as colorants, and the crystals are grown by the FZ method using the raw material rods formed. Bubble-free crystals can be synthesized without any effects.
本発明におけるJ東料は上述の着色剤を加え、よく混合
してゴムチューブに詰め、ラバープレスを行ない、その
後電気炉で焼結して長さ10 mm 、直径8−〜10
y++mの棒状に成形する。ぞしてこの原 ゛料俸をF
Z装置(赤外線加熱単結晶製造装置)の上部シャフトに
吊るし、下部シャフトに種子結晶を設置して加熱を行な
い、原料と種子の間に溶融体を形成して、との両方を同
時に一定の速度で下方に移動させて押子結晶上に結晶を
育成させる。J Toryo in the present invention adds the above-mentioned coloring agent, mixes well, packs into a rubber tube, performs a rubber press, and then sinters in an electric furnace to obtain a length of 10 mm and a diameter of 8 to 10 mm.
Form into a bar shape of y++m. So this field, the fee is F.
It is suspended from the upper shaft of the Z equipment (infrared heating single crystal production equipment), and the seed crystal is placed on the lower shaft to perform heating, forming a molten body between the raw material and the seed, and simultaneously heating both at a constant speed. to grow the crystal on the pusher crystal.
、この時の下方への移動速度つまり成長速度が五〇mm
/ H以上では結晶の中に気泡が含まれてしまい、3
.0晒/H未満が望ましい。, the downward movement speed, that is, the growth speed at this time, is 50 mm.
/ H or higher, air bubbles are included in the crystal, and 3
.. Desirably less than 0 exposure/H.
〔実施例1〕
試薬特級(純度999%以上)のα−アルミナ40rを
白金るつぼに入れ、真空焼結炉で、温度1500℃、真
空度10=Torrで2時間処理した原料に3wt%の
酸化クロムを加え、乳針中でダイフロンを加えてよく混
合する。乾燥後、該混合物20rを内径101rfnの
ゴムチューブに詰め、一端を密封して、ラバープレスに
てj ton / crl (D圧力で約15分間、成
形した。さらに該成形原料棒を電気炉で1700°C−
20時間焼結を行なった。該焼結原料棒を用いてFZ装
置により、ルビー単結晶を育成した。育成条件を以下に
示す。[Example 1] Reagent grade (999% or higher purity) α-alumina 40r was placed in a platinum crucible and treated in a vacuum sintering furnace at a temperature of 1500°C and a vacuum level of 10 Torr for 2 hours.The raw material was oxidized at 3 wt%. Add chromium, add Diflon in milk needle and mix well. After drying, 20r of the mixture was packed into a rubber tube with an inner diameter of 101rfn, one end was sealed, and molded using a rubber press at a pressure of J ton/crl (D) for about 15 minutes.The raw material rod was then heated in an electric furnace at a pressure of 1700 °C-
Sintering was carried out for 20 hours. A ruby single crystal was grown using the sintered raw material rod using an FZ apparatus. The growing conditions are shown below.
成長速度 : 2.Omm/H
上部シャフト回転数 : 45rpm
下部シャフト回転数 : 15rpm
種 子 : コランダム単結晶
雰囲気 : 空 気
育成時間 : 20時間
上記方法で育成した結晶は長さ40闘、径aO調の丸棒
状で、全体に気泡のない良質のルビー単結晶であった。Growth rate: 2. Omm/H Upper shaft rotation speed: 45 rpm Lower shaft rotation speed: 15 rpm Seed: Corundum single crystal Atmosphere: Air Growth time: 20 hours The crystal grown by the above method is a round rod with a length of 40cm and a diameter of aO. It was a high quality ruby single crystal with no bubbles throughout.
〔実施例2〕
試薬特級(純度999%以上)のα−アルミナ409を
白金るつぼに入れ、真空焼結炉で、温度900℃、真空
度10−’Torrで2時間処理した原料に0.2 w
t%の酸化クロムと0,4W%の酸化ニッケルを加え
、以下〔実施例1〕と同様な方法により焼結原料を作り
、〔実施例1〕と同様な育成条件により、パパラチア単
結晶の育成を行なった。[Example 2] Reagent grade (999% or higher purity) α-alumina 409 was placed in a platinum crucible and treated in a vacuum sintering furnace at a temperature of 900°C and a vacuum of 10-' Torr for 2 hours. lol
A sintering raw material was prepared by adding t% of chromium oxide and 0.4W% of nickel oxide in the same manner as in [Example 1], and a Padparadscha single crystal was grown under the same growth conditions as in [Example 1]. I did it.
上記方法で育成した結晶は長さ40m+n、径aO胴の
丸棒状で、全体に気泡のない良質のパパラチア単結晶で
あった。The crystal grown by the above method had a round bar shape with a length of 40 m+n and a diameter of aO, and was a high-quality Padparadscha single crystal without air bubbles throughout.
〔実施例3〕
〔実施例1〕と同様な方法で温度1200℃真空度10
−”Torrで2時間処理したアルミナ2五12と、試
薬特級(純度995%以上)のベリリアをアルミナの場
合と同様に温度1200℃、真空度10”””Torr
で2時間処理したべIJ IJア5.67 rを乳鉢中
に入れ、さらに着色剤として酸化クロム0.14 rと
酸化鉄1.09 rを入れ、以下〔実施例1〕と同様な
方法により焼結原料棒を作り、〔実施例1〕と同様な育
成条件により、アレキサンドライト単結晶の育成を行な
った。[Example 3] Using the same method as [Example 1], the temperature was 1200°C and the degree of vacuum was 10.
- Alumina 2512 treated for 2 hours at Torr and beryllia of special reagent grade (995% or higher purity) were treated at a temperature of 1200°C and a vacuum of 10 Torr as in the case of alumina.
5.67 r of IJ IJ treated for 2 hours was placed in a mortar, 0.14 r of chromium oxide and 1.09 r of iron oxide were added as coloring agents, and the following was carried out in the same manner as in [Example 1]. A sintered raw material rod was prepared, and alexandrite single crystal was grown under the same growth conditions as in [Example 1].
上記方法で育成した結晶は長さ40++++n、径aO
<間の丸棒状で、全体に気泡のない良質のアレキサンド
ライト単結晶であった。The crystal grown by the above method has a length of 40+++n and a diameter of aO.
It was a high quality alexandrite single crystal with a round bar shape and no bubbles throughout.
以上述べたように本発明によれば、融液からの単結晶育
成において、コランダム結晶とアレキサンドライト結晶
の原料粉末であるアルミナとベリリアを温度800°C
〜1500℃かつ真空度1O−1Torr−10−’
To rrにおいて処理することによって、着色剤の種
類とにに関係なく、Fz法によって成長速度5 rrr
m / H未満で育成したコランダム結晶とアレキサン
ドライト結晶には気泡がなく人工宝石用として、さらに
電子材料として品質の向上、生産性の向上などに多大の
効果を有するものである。As described above, according to the present invention, when growing a single crystal from a melt, alumina and beryllia, which are raw material powders for corundum crystals and alexandrite crystals, are grown at a temperature of 800°C.
~1500℃ and vacuum level 1O-1Torr-10-'
By processing at Torr, the growth rate is 5 rrr by the Fz method, regardless of the type of colorant.
Corundum crystals and alexandrite crystals grown at less than m/H have no bubbles and are useful for artificial jewelry, and have great effects in improving quality and productivity as electronic materials.
以 上that's all
Claims (3)
融液の原料粉末を高温及び真空状態で処理することを特
徴とする単結晶育成用原料製造法。(1) In the method of growing a single crystal from a melt, the above-mentioned
A method for producing a raw material for single crystal growth, characterized by processing a raw material powder of a melt at high temperature and in a vacuum state.
びべIJ IJア(BO2)である特許請求の範囲第1
5項に記載の単結晶育成用原料製造法。(2) - Claim 1, wherein the raw material powder is alumina (Attos) and BO2.
The method for producing raw materials for single crystal growth according to item 5.
10−ITorr−10″″IITorrとする特許請
求の範囲第1項に記載の単結晶育成用原料製造法(4)
前記原料製造法が赤外線集光式フローティングゾーン
法による単結晶育成用のものであり、結晶の成長速度が
3. Ottrm / H未満で育成を行なうことを特
徴とする特許請求の範囲第1項記載の単結晶育成用原料
製造法。(3) The method for producing a raw material for single crystal growth according to claim 1, wherein the high temperature is 8003 to 1500°C and the degree of vacuum is 10-ITorr-10'''' IITorr (4)
The raw material manufacturing method is for single crystal growth using an infrared condensing floating zone method, and the crystal growth rate is 3. The method for producing a raw material for single crystal growth according to claim 1, characterized in that the growth is performed at a temperature lower than Ottrm/H.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP59031696A JPS60176985A (en) | 1984-02-22 | 1984-02-22 | Preparation of raw material for growing single crystal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP59031696A JPS60176985A (en) | 1984-02-22 | 1984-02-22 | Preparation of raw material for growing single crystal |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS60176985A true JPS60176985A (en) | 1985-09-11 |
Family
ID=12338236
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP59031696A Pending JPS60176985A (en) | 1984-02-22 | 1984-02-22 | Preparation of raw material for growing single crystal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS60176985A (en) |
-
1984
- 1984-02-22 JP JP59031696A patent/JPS60176985A/en active Pending
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP3092675B2 (en) | Oxynitride glass and method for producing the same | |
JPS60176985A (en) | Preparation of raw material for growing single crystal | |
JPH0254318B2 (en) | ||
JPH06279174A (en) | Production of oxide single crystal | |
JPS58115095A (en) | Synthesis of artificial beryl single crystal | |
JPS6065735A (en) | Production of quartz glass | |
JPS60227830A (en) | Manufacture of raw material for growing single crystal | |
JPH04338167A (en) | Production of sintered rod | |
JPS61186294A (en) | Production of star sapphire | |
JPS6144720A (en) | Production of quartz glass | |
JPS6287494A (en) | Production of alexandrite single crystal | |
JPS59162197A (en) | Production of artificial crystal of ruby by f.z. process | |
JPH04338191A (en) | Production of single crystal | |
JPS58120597A (en) | Chrysoberyl single crystal showing luster effect and its production | |
JPS60112700A (en) | Synthesizing method of corundum | |
JPH038708A (en) | Production of silica feedstock | |
JPS60226498A (en) | Preparation of starting material for single crystal | |
JPS6140825A (en) | Preparation of quartz glass | |
JPS60226482A (en) | Preparation of raw material for growth of single crystal | |
JPS60231487A (en) | Manufacture of raw material for growing single crystal | |
JPS6197112A (en) | Manufacture of zirconium nitride | |
JPS60176994A (en) | Preparation of corundum | |
JPS6081097A (en) | Synthesis method of single crystal of artificial beryl | |
JPS61101484A (en) | Production of single crystal ferrite | |
JPS60239394A (en) | Synthesis of single crystal of ruby |