JPH04132695A - Production of single crystal of alumina-based oxide having high melting point - Google Patents
Production of single crystal of alumina-based oxide having high melting pointInfo
- Publication number
- JPH04132695A JPH04132695A JP25393190A JP25393190A JPH04132695A JP H04132695 A JPH04132695 A JP H04132695A JP 25393190 A JP25393190 A JP 25393190A JP 25393190 A JP25393190 A JP 25393190A JP H04132695 A JPH04132695 A JP H04132695A
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- single crystal
- melting point
- high melting
- based high
- 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
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 16
- 238000002844 melting Methods 0.000 title claims description 10
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 230000008018 melting Effects 0.000 title claims description 7
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 125000004430 oxygen atom Chemical group O* 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000005231 Edge Defined Film Fed Growth Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、融液からザファイヤ等高品質なアルミナ系高
融点酸化物単結晶を育成する製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a manufacturing method for growing high-quality alumina-based high-melting point oxide single crystals such as zaphire from a melt.
［従来の技術および課題］
融液からサファイヤ等アルミナ系高融点酸化物単結晶を
育成する方法としては、ベルヌーイ法、チョクラルスキ
法、バクダサロフ法、熱交換法、ＥＦＧ法等が知られて
いる。大型アルミナ系高融点酸化物単結晶を育成する方
法としては、チョクラルスキ法、バクダサロフ法、熱交
換法、Ｅ、ＦＧ法によるルツボを用いた方法があり、量
産化されている。しかしながらルツボを用いるとチョク
ラルスキ法やＥＦＧ法においては結晶中に気泡が入りや
すく、高品質化することができない。この気泡を除去す
る方法としては、結晶成長速度を遅くしたり、原材料の
前処理として粉末原料を溶融固化させることが行なわれ
ている。しかしながら結晶成長速度を遅くすることは量
産性において不利であり、原材料粉末を溶融固化させる
ことは原料単価を引上げる要因となり、高品質なアルミ
ナ系高融点酸化物単結晶を低価格で供給することはでき
ない。[Prior Art and Problems] Known methods for growing single crystals of alumina-based high melting point oxides such as sapphire from melts include the Bernoulli method, Czochralski method, Bakudasarov method, heat exchange method, and EFG method. Methods for growing large alumina-based high-melting-point oxide single crystals include the Czochralski method, Bakdasarov method, heat exchange method, and methods using crucibles such as E and FG methods, which have been mass-produced. However, when a crucible is used, air bubbles tend to enter the crystal in the Czochralski method or the EFG method, making it impossible to achieve high quality. Methods for removing these bubbles include slowing down the crystal growth rate and melting and solidifying the powder raw material as a pretreatment of the raw material. However, slowing the crystal growth rate is disadvantageous in terms of mass production, and melting and solidifying the raw material powder increases the raw material unit price, making it difficult to supply high-quality alumina-based high-melting point oxide single crystals at low prices. I can't.
本発明はこの点を鑑みて、気泡のない大型で高品質な単
結晶を低価格で供給することを目的とする。In view of this point, the present invention aims to supply a large, high-quality single crystal without bubbles at a low cost.
［課題を解決するための手段コ
アルミナ系高融点酸化物単結晶をルツボを用いて育成す
る方法において、気泡の発生する原因が高温でアルミナ
（／Ｖ２０：ｉ）が分解して生成する酸素原子（０）お
よび酸素分子（０２）が融液中に過飽和に存在し、それ
が析出することによることを見出した。そのため本発明
は融液中に過飽和に存在する酸素原子および酸素分子の
除去方法としては還元性ガスを用いるものであり、水素
および一酸化炭素が有効である。[Means for Solving the Problems] In the method of growing core-alumina-based high-melting point oxide single crystals using a crucible, the cause of bubble generation is oxygen atoms (which are generated by the decomposition of alumina (/V20:i) at high temperatures). 0) and oxygen molecules (02) are present in the melt in a supersaturated state, and it has been found that this is caused by precipitation. Therefore, the present invention uses a reducing gas as a method for removing supersaturated oxygen atoms and oxygen molecules in the melt, and hydrogen and carbon monoxide are effective.
還元性ガスはルツボとの反応性があるが、不活性ガスに
より希釈することで防止でき、容量比が１／１００未満
であると融液中に過飽和に存在するＯおよびｏ２を除去
することができないので、１／１００以上必要である。Reducing gas has reactivity with the crucible, but this can be prevented by diluting it with an inert gas, and if the volume ratio is less than 1/100, O and O2 present in supersaturation in the melt cannot be removed. Since this is not possible, 1/100 or more is required.
還元性ガスにより融液中に過飽和に存在するＯおよび０
２を化学反応により除去するため、希釈ガスを用いた場
合においては、引き上げる結晶およびルツボに仕込んだ
原材料に依存する。O and 0 present in supersaturation in the melt due to reducing gas
Since 2 is removed by a chemical reaction, when a diluent gas is used, it depends on the crystal to be pulled and the raw material charged in the crucible.
［実施例１］
原料として純度９９９９％のアルミナを使用し、ルツボ
としてモリブデンを採用した。チョクラルスキ法により
溶融し、育成雰囲気としては静２０ｖｏ１％Ｈ２とし、
育成条件としては引上げ方位＜００１＞ 、回転数３Ｏ
ｒｐｍ 、引上げ速度４ｍｍ／ｈｒで、仕込み重量の約
７５％の単結晶を得た。得られた結晶は、直径約２５〜
２０悶φで、長さが直胴部で約１００Ｍである。結晶の
色は無色透明であり、気泡は観察されなかった。[Example 1] Alumina with a purity of 9999% was used as a raw material, and molybdenum was used as a crucible. It was melted by the Czochralski method, and the growth atmosphere was static 20 vol 1% H2.
The growth conditions are pulling direction <001> and rotation speed 3O.
rpm and a pulling speed of 4 mm/hr, a single crystal weighing about 75% of the charged weight was obtained. The obtained crystals have a diameter of about 25~
It has a diameter of 20 mm and a length of about 100 m at the straight body. The crystals were colorless and transparent, and no bubbles were observed.
［実施例２］
原料として純度９９．９９％のアルミナを使用し、ルツ
ボとしてモリブデンを採用した。チョクラルスキ法によ
り溶融し、育成雰囲気としてはＡｒ−１０ｖｏ１％Ｈ２
とし、育成条件としては引上げ方位＜００１＞ 、回転
数３Ｏｒｐｍ 、引上げ速度４ｍ／ｈｒで、仕込み重量
の約１５％の単結晶を得た。得られた結晶は、直径約２
５〜２０摩φで、長さが直胴部で約１００＃である。結
晶の色は無色透明であり、気泡は観察されなかった。[Example 2] Alumina with a purity of 99.99% was used as a raw material, and molybdenum was used as a crucible. It is melted by the Czochralski method, and the growth atmosphere is Ar-10vo1%H2.
The growth conditions were a pulling direction <001>, a rotational speed of 3 rpm, and a pulling speed of 4 m/hr, and a single crystal weighing about 15% of the charged weight was obtained. The resulting crystal has a diameter of approximately 2
The diameter is 5 to 20, and the length of the straight body is about 100#. The crystals were colorless and transparent, and no bubbles were observed.
［実施例３］
原料として純度９９．９９％のアルミナを使用し、ルツ
ボとしてモリブデンを採用した。チョクラルスキ法によ
り溶融し、育成雰囲気としては酵５ｖｏｌＸＣＯとし、
育成条件としては引上げ方位＜００１＞ 、回転数３Ｏ
ｒｐｍ 、引上げ速度４ｍ＋／ｈｒで、仕込み重量の約
７５％の単結晶を得た。得られた結晶は、直径的２５〜
２０ｍｍφで、長さが直胴部で約ｉ ００Ｍである。結
晶の色は無色透明であり、気泡は観察されなかった。[Example 3] Alumina with a purity of 99.99% was used as a raw material, and molybdenum was used as a crucible. It was melted by the Czochralski method, and the growth atmosphere was 5volXCO of fermentation.
The growth conditions are pulling direction <001> and rotation speed 3O.
rpm and a pulling speed of 4 m+/hr, a single crystal weighing about 75% of the charged weight was obtained. The obtained crystals have a diameter of 25~
It has a diameter of 20 mm and a length of approximately i00M at the straight body. The crystals were colorless and transparent, and no bubbles were observed.
［発明の効果］
本発明により、アルミナ系高融点酸化物単結晶をルツボ
を用いて育成する方法において、気泡の発生する原因で
ある融液中の過飽和な酸素原子および酸素分子を水素お
よび一酸化炭素等還元性ガスにより除去し、高品質なア
ルミナ系高融点酸化物大型単結晶を低価格において製造
する方法を確立することができた。[Effects of the Invention] According to the present invention, in a method for growing an alumina-based high melting point oxide single crystal using a crucible, supersaturated oxygen atoms and oxygen molecules in the melt, which are the cause of bubble generation, are replaced with hydrogen and monoxide. We were able to establish a method for producing high-quality, large-sized single crystals of high-melting-point alumina oxides at low cost by removing them with a reducing gas such as carbon.
Claims (3)
の育成方法において、還元性ガス雰囲気内にて行なうこ
とを特徴としたアルミナ系高融点酸化物単結晶の製造方
法。(1) A method for producing an alumina-based high-melting-point oxide single crystal, which is characterized in that the growth method of an alumina-based high-melting-point oxide single crystal is carried out in a reducing gas atmosphere using a melt growth method.
混合比が少なくとも容量比で、１／１００以上である請
求項（１）記載のアルミナ系高融点酸化物単結晶の製造
方法。(2) The method for producing an alumina-based high melting point oxide single crystal according to claim (1), wherein the reducing gas atmosphere contains hydrogen gas, and the hydrogen mixing ratio is at least 1/100 or more by volume.
、一酸化炭素混合比が少なくとも容量比で、１／１００
以上である請求項（１）記載のアルミナ系高融点酸化物
単結晶の製造方法。(3) Contains carbon monoxide gas as a reducing gas atmosphere, and the carbon monoxide mixing ratio is at least 1/100 by volume.
The method for producing an alumina-based high melting point oxide single crystal according to claim (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25393190A JP2962795B2 (en) | 1990-09-21 | 1990-09-21 | Method for producing alumina-based high melting point oxide single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25393190A JP2962795B2 (en) | 1990-09-21 | 1990-09-21 | Method for producing alumina-based high melting point oxide single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04132695A true JPH04132695A (en) | 1992-05-06 |
| JP2962795B2 JP2962795B2 (en) | 1999-10-12 |
Family
ID=17258011
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25393190A Expired - Fee Related JP2962795B2 (en) | 1990-09-21 | 1990-09-21 | Method for producing alumina-based high melting point oxide single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2962795B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06199597A (en) * | 1992-10-15 | 1994-07-19 | Natl Inst For Res In Inorg Mater | Production of aluminum oxide single crystal |
| US6788026B2 (en) | 2001-08-30 | 2004-09-07 | Yamaha Corporation | Battery charger, including an amplifier for audio signals, for portable audio devices |
| JP2007197230A (en) * | 2006-01-24 | 2007-08-09 | Sumitomo Metal Mining Co Ltd | Method for manufacturing aluminium oxide single crystal and aluminium oxide single crystal obtained by using the method |
| JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
| JP2013095611A (en) * | 2011-10-28 | 2013-05-20 | Sumco Corp | Method for producing sapphire single crystal |
| CN103194791A (en) * | 2013-04-24 | 2013-07-10 | 哈尔滨工业大学 | Horizontal directional region melt-crystallization preparation method of large-dimension plate-like sapphire mono-crystal |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4844429B2 (en) * | 2007-02-26 | 2011-12-28 | 日立化成工業株式会社 | Method for producing sapphire single crystal |
-
1990
- 1990-09-21 JP JP25393190A patent/JP2962795B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06199597A (en) * | 1992-10-15 | 1994-07-19 | Natl Inst For Res In Inorg Mater | Production of aluminum oxide single crystal |
| US6788026B2 (en) | 2001-08-30 | 2004-09-07 | Yamaha Corporation | Battery charger, including an amplifier for audio signals, for portable audio devices |
| JP2007197230A (en) * | 2006-01-24 | 2007-08-09 | Sumitomo Metal Mining Co Ltd | Method for manufacturing aluminium oxide single crystal and aluminium oxide single crystal obtained by using the method |
| JP2011195423A (en) * | 2010-03-24 | 2011-10-06 | Sumitomo Metal Mining Co Ltd | Method of manufacturing sapphire single crystal |
| JP2013095611A (en) * | 2011-10-28 | 2013-05-20 | Sumco Corp | Method for producing sapphire single crystal |
| CN103194791A (en) * | 2013-04-24 | 2013-07-10 | 哈尔滨工业大学 | Horizontal directional region melt-crystallization preparation method of large-dimension plate-like sapphire mono-crystal |
| CN103194791B (en) * | 2013-04-24 | 2016-05-04 | 哈尔滨工业大学 | The horizontal orientation district clinkering crystal preparation method of the tabular sapphire monocrystal of large scale |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2962795B2 (en) | 1999-10-12 |
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