JPH04310530A - Production of synthetic quartz crucible - Google Patents
Production of synthetic quartz crucibleInfo
- Publication number
- JPH04310530A JPH04310530A JP10386091A JP10386091A JPH04310530A JP H04310530 A JPH04310530 A JP H04310530A JP 10386091 A JP10386091 A JP 10386091A JP 10386091 A JP10386091 A JP 10386091A JP H04310530 A JPH04310530 A JP H04310530A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- synthetic quartz
- heating element
- powder
- carbon
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000010453 quartz Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 8
- 229910002804 graphite Inorganic materials 0.000 abstract description 10
- 239000010439 graphite Substances 0.000 abstract description 10
- 238000011109 contamination Methods 0.000 abstract description 7
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 abstract description 3
- 239000012774 insulation material Substances 0.000 abstract description 2
- 238000003980 solgel method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910000953 kanthal Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- -1 etc. Inorganic materials 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
- C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は合成石英ルツボの製造方
法、特には非晶質合成石英粉から表面汚染のない、高純
度の合成石英ルツボを製造する方法に関するものである
。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing synthetic quartz crucibles, and more particularly to a method for manufacturing synthetic quartz crucibles of high purity free from surface contamination from amorphous synthetic quartz powder.
【０００２】0002
【従来の技術】石英ルツボの製造は従来、天然水晶粉を
回転する金型あるいはカーボン型中において遠心力によ
りルツボ型に成形し、ついでこれを単相あるいは三相の
アーク焔で２，４００℃まで加熱し溶融するという方法
で作られているが、天然水晶粉から作られた石英ルツボ
は純度的に問題があるために半導体シリコン単結晶引上
げ用ルツボの成形のために最近は天然水晶粉の代わりに
合成石英粉を使用し同様の方法で合成石英ルツボを製造
する方法も開発されているけれども、ルツボの大口径化
の傾向からこの加熱に強い火力が必要とされるというこ
とから、この加熱はアーク焔を用いるものが主流となっ
ており、アーク焔以外のものは使用されていない。[Prior Art] Conventionally, quartz crucibles have been manufactured by forming natural quartz powder into a crucible shape by centrifugal force in a rotating mold or carbon mold, and then heating it to 2,400°C using a single-phase or three-phase arc flame. However, since quartz crucibles made from natural quartz powder have purity issues, recently natural quartz powder has been used to form crucibles for pulling semiconductor silicon single crystals. Although a method of manufacturing synthetic quartz crucibles in a similar manner using synthetic quartz powder instead has been developed, this heating method requires strong heat due to the trend toward larger diameter crucibles. The mainstream is to use an arc flame, and nothing other than an arc flame is used.
【０００３】0003
【発明が解決しようとする課題】しかし、このアーク焔
による加熱には、アーク焔に使用される電極が黒鉛とさ
れていることから、この黒鉛がアーク焔の衝撃で飛び散
り、これがルツボの表面に落ちるためにルツボが汚染さ
れるという不利がある。そして、この黒鉛自体はこのル
ツボを酸化性雰囲気で加熱すれば酸化されて後かたもな
くなるけれども、黒鉛中の不純物がそのまま表面に残る
ためにこれが汚染として残ることになり、この汚染はル
ツボが天然水晶粉から作られたものである場合には
することで削除できるのであまり問題
にはならないけれども、このルツボが合成石英粉から作
られたものであるときにはこれを削除することができず
、この対策が大きな問題点とされている。[Problem to be Solved by the Invention] However, since the electrode used in the arc flame is made of graphite, this graphite is scattered by the impact of the arc flame, and this spreads onto the surface of the crucible. The disadvantage is that the crucible is contaminated due to falling. Although this graphite itself is oxidized and disappears when the crucible is heated in an oxidizing atmosphere, the impurities in the graphite remain on the surface and remain as contamination. If it is made from natural crystal powder
However, if this crucible is made from synthetic quartz powder, this cannot be removed, and this countermeasure is considered to be a major problem.
【０００４】0004
【課題を解決するための手段】本発明はこのような不利
を解決した合成石英ルツボの製造方法に関するものであ
り、これは非晶質石英粉を回転する金型またはカーボン
型内で遠心力によりルツボ状に成形し、ついで炭素発熱
体、炭化けい素発熱体、酸化物発熱体または金属発熱体
を用いて加熱し、焼結することを特徴とするものである
。[Means for Solving the Problems] The present invention relates to a method for manufacturing a synthetic quartz crucible that solves the above-mentioned disadvantages.This invention involves manufacturing amorphous quartz powder in a rotating mold or carbon mold by centrifugal force. It is characterized in that it is formed into a crucible shape, and then heated and sintered using a carbon heating element, a silicon carbide heating element, an oxide heating element, or a metal heating element.
【０００５】すなわち、本発明者らはアーク焔による汚
染を防止した合成石英ルツボの製造方法を開発すべく種
々検討した結果、ルツボの成形自体は従来法と同様の方
法で成形したのち、この成形されたルツボの焼結をアー
ク焔を使用せず、他の発熱体、例えば炭素発熱体、炭化
けい素発熱体、酸化物発熱体または金属発熱体を用いて
行えば、これらの発熱体から炭素が遊離されることもな
いし、他の不純物によってルツボから汚染されることも
ないので、目的とする合成石英ルツボを汚染のない高純
度のものとして得ることができることを見出して本発明
を完成させた。以下にこれをさらに詳述する。That is, the present inventors have conducted various studies to develop a method for manufacturing synthetic quartz crucibles that prevents contamination from arc flames. If the crucible is sintered without using an arc flame but with another heating element, such as a carbon heating element, a silicon carbide heating element, an oxide heating element, or a metal heating element, carbon can be removed from these heating elements. The present invention was completed based on the discovery that the desired synthetic quartz crucible can be obtained as a high-purity product free from contamination, since the crucible is not liberated and the crucible is not contaminated by other impurities. . This will be explained in further detail below.
【０００６】[0006]
【作用】本発明は合成石英ガラスルツボの製造方法に関
するものであり、これは非晶質合成石英粉末から遠心力
でルツボを成形し、これを発熱体を用いて焼結すること
を要旨とするものである。[Operation] The present invention relates to a method for manufacturing a synthetic silica glass crucible, and the gist of this invention is to form a crucible from amorphous synthetic quartz powder by centrifugal force and sinter the crucible using a heating element. It is something.
【０００７】本発明による合成石英ルツボの製造は非晶
質合成石英粉末を始発材として行なわれる。この非晶質
合成石英粉末は例えばメチルシリケートをメタノール溶
媒中でアンモニアを用いて加水分解し、乾燥後、閉孔し
、ガラス化するという、いわゆるゾル−ゲル法によって
得ることができるが、このものは結晶質合成石英粉のよ
うに結晶化していないけれども、ＯＨ基含有量が極めて
低く、高純度で高い粘性をもっているので、これから作
られた合成石英ルツボは半導体シリコン単結晶引上げ用
ルツボとして有用とされる。The synthetic quartz crucible according to the present invention is manufactured using amorphous synthetic quartz powder as a starting material. This amorphous synthetic quartz powder can be obtained, for example, by the so-called sol-gel method, in which methyl silicate is hydrolyzed using ammonia in a methanol solvent, dried, closed, and vitrified. Although it is not crystallized like crystalline synthetic quartz powder, it has an extremely low OH group content, high purity, and high viscosity, so synthetic quartz crucibles made from it are useful as crucibles for pulling semiconductor silicon single crystals. be done.
【０００８】本発明による合成石英ルツボの製造はこの
非晶質合成石英粉末からルツボを成形し、これを焼成す
ることによって行なわれるが、このルツボの成形は従来
公知の方法にしたがって、この非晶質合成石英粉末を回
転する金型またはカーボン型に装入し、この型を回転さ
せ、遠心力によって成形すればよい。The synthetic quartz crucible according to the present invention is manufactured by molding the crucible from the amorphous synthetic quartz powder and firing the crucible. The synthetic quartz powder may be charged into a rotating metal mold or a carbon mold, and the mold may be rotated to form the powder by centrifugal force.
【０００９】また、このようにして成形されたルツボ状
の成形体はついで高温で焼結させることによって石英ル
ツボとされるのであるが、本発明においてはこの加熱が
アーク焔ではなく、発熱体を用いて行なわれる。この発
熱体としては黒鉛電極を使用する炭素発熱体、炭化けい
素を使用する炭化けい素発熱体、ジルコニアなどを使用
する酸化物発熱体、タングステン、モリブデンなどを使
用する金属発熱体が例示されるが、本発明ではこれらの
発熱体を使用して上記で得た成形体を１，６００〜１，
８００℃に加熱して焼結させればよく、これによればア
ーク焔によるような炭素粉の付着による汚染が全く行な
われないので、目的とする合成石英ルツボを高純度なも
のとして容易に得ることができる。[0009] Furthermore, the crucible-shaped compact formed in this manner is then sintered at high temperature to form a quartz crucible, but in the present invention, this heating is not done with an arc flame but with a heating element. It is done using Examples of this heating element include a carbon heating element using graphite electrodes, a silicon carbide heating element using silicon carbide, an oxide heating element using zirconia, etc., and a metal heating element using tungsten, molybdenum, etc. However, in the present invention, the molded body obtained above using these heating elements has a temperature of 1,600 to 1,
All you have to do is heat it to 800°C and sinter it. This way, there will be no contamination due to adhesion of carbon powder like that caused by arc flames, so you can easily obtain the desired synthetic quartz crucible with high purity. be able to.
【００１０】なお、この焼結はどのような雰囲気で行な
ってもよいが、これを不活性ガス雰囲気とするときには
炭素発熱体、炭化けい素発熱体を使用し、還元性雰囲気
とするときには金属発熱体を使用することがよいが、量
産性を向上させるために酸化性雰囲気とするときにはカ
ンタルスーパー１，９００［カンタル社製商品名］やモ
リシリ発熱体、ジルコニア発熱体を使用することがよい
。[0010] This sintering may be carried out in any atmosphere, but when an inert gas atmosphere is used, a carbon heating element or a silicon carbide heating element is used, and when a reducing atmosphere is used, a metal heating element is used. However, when creating an oxidizing atmosphere to improve mass productivity, it is preferable to use Kanthal Super 1,900 (trade name, manufactured by Kanthal), Morishiri heating element, or zirconia heating element.
【００１１】つぎにこれを添付の図面について説明する
が、図１は本発明において使用される石英ルツボ製造装
置の縦断面図を示したものである。この装置はカーボン
型１が水冷チャンバー３を有する黒鉛断熱材２で囲まれ
ているが、このカーボン型１はモーター４で回転するよ
うにされており、これにはその中心部にルツボ状成形体
５を焼結するための熱源となる発熱体６が上部から懸吊
されていて、これは昇降装置７によって上下されるよう
にされている。Next, this will be explained with reference to the accompanying drawings. FIG. 1 shows a longitudinal sectional view of a quartz crucible manufacturing apparatus used in the present invention. In this device, a carbon mold 1 is surrounded by a graphite insulating material 2 having a water-cooled chamber 3, and this carbon mold 1 is rotated by a motor 4, which has a crucible-shaped molded body in its center. A heating element 6, which serves as a heat source for sintering the heating element 5, is suspended from the top, and is raised and lowered by a lifting device 7.
【００１２】この装置を使用した合成石英ルツボの製造
はこのカーボン型１に始発材となる非晶質合成石英粉を
充填し、モーター４を作動してカーボン型１を回転させ
、遠心力によってルツボ状成形体５を成形させたのち、
発熱体６に通電してルツボ状成形体５を１，６００〜１
，８００℃に加熱し焼成すればよく、これによれば炭素
などの汚染なく、高純度の合成石英ルツボを容易に得る
ことができる。To manufacture a synthetic quartz crucible using this device, the carbon mold 1 is filled with amorphous synthetic quartz powder as a starting material, the motor 4 is activated to rotate the carbon mold 1, and the crucible is moved by centrifugal force. After molding the shaped body 5,
The heating element 6 is energized to heat the crucible-shaped molded body 5 to 1,600 to 1
. , 800° C. and sintering. Accordingly, a high-purity synthetic quartz crucible can be easily obtained without contamination with carbon or the like.
【００１３】[0013]
【実施例】つぎに本発明の実施例、比較例をあげる。
実施例、比較例
メタノール１５０モル、純水１２０モル、アンモニア５
０モルを入れた容器にメチルシリケート１０モルを滴下
して加水分解させ、得られたシリカを１５０℃で乾燥し
たのち１，５００℃に加熱して閉孔化し、ガラス化して
透明ガラス塊を作り、ボールミルで粉砕し、篩別して合
成シリカ粉を作った。[Examples] Next, examples of the present invention and comparative examples will be given. Examples, Comparative Examples Methanol 150 mol, pure water 120 mol, ammonia 5
10 moles of methyl silicate is dropped into a container containing 0 moles and hydrolyzed, the resulting silica is dried at 150°C, heated to 1,500°C to close the pores, and vitrified to create a transparent glass lump. , ground in a ball mill and sieved to produce synthetic silica powder.
【００１４】ついでこのようにして得た６０〜８０メッ
シュの非晶質合成シリカ粉２３ｋｇを１８インチルツボ
製造用のカーボン型に充填し、このカーボン型を２００
ｒｐｍで回転させてルツボ状成形体を作成し、窒素ガス
雰囲気において純化処理したカーボン電極に通電して１
，８００℃で焼結し、その後１，２００℃に降温して３
０分間保持し、通電を止めて４００℃まで放冷したのち
取り出したところ、合成石英ルツボが得られたので、こ
のルツボの表面層１ｍｍを削り取り、化学分析したとこ
ろ、後記する表１に示したとおりの結果が得られた。Next, 23 kg of amorphous synthetic silica powder of 60 to 80 mesh obtained in this manner was filled into a carbon mold for manufacturing an 18-inch crucible, and this carbon mold was
A crucible-shaped molded body was created by rotating at rpm, and electricity was applied to the purified carbon electrode in a nitrogen gas atmosphere.
, sintered at 800℃, then lowered the temperature to 1,200℃
After holding the crucible for 0 minutes, turning off the electricity and allowing it to cool to 400°C, it was taken out, and a synthetic quartz crucible was obtained. 1 mm of the surface layer of this crucible was scraped off and chemically analyzed, and the results are shown in Table 1 below. The exact results were obtained.
【００１５】しかし、比較のために上記における炭素発
熱体による焼結をアーク焔を用いて２，３００〜２，５
００℃で焼結したところ、合成石英ルツボを得ることが
できたが、このルツボの表面層を１ｍｍ削り取り、化学
分析したところ、後記する表１に示したとおりの結果が
得られ、この場合には実施例のものにくらべて純度の劣
るものであることが確認された。However, for comparison, the sintering using the carbon heating element described above was performed using an arc flame, and the temperature was 2,300 to 2,5
By sintering at 00°C, a synthetic quartz crucible could be obtained, but when the surface layer of this crucible was scraped off by 1 mm and chemically analyzed, the results shown in Table 1 below were obtained. It was confirmed that the purity was inferior to that of the example.
【００１６】[0016]
【表１】[Table 1]
【００１７】[0017]
【発明の効果】本発明は合成石英ルツボの製造方法に関
するものであり、これは前記したように非晶質合成石英
粉を回転する金型またはカーボン型内で遠心力によりル
ツボ状に成形し、炭素発熱体、炭化けい素発熱体、酸化
物発熱体または金属発熱体により加熱し焼結することを
特徴とするものであるが、これによればルツボ状成形体
の焼結がアーク焔でない発熱体で行なわれるので、この
焼結で得られる合成石英ルツボが黒鉛で汚染されること
なく、高純度のものとして得ることができるという有利
性が与えられる。The present invention relates to a method for manufacturing a synthetic quartz crucible, which involves forming amorphous synthetic quartz powder into a crucible shape by centrifugal force in a rotating mold or carbon mold, as described above. It is characterized by heating and sintering with a carbon heating element, a silicon carbide heating element, an oxide heating element, or a metal heating element, but according to this, the sintering of the crucible-shaped compact does not generate heat using an arc flame. Since the sintering is carried out in a body, the synthetic quartz crucible obtained by this sintering has the advantage that it is not contaminated with graphite and can be obtained in high purity.
【図１】本発明で使用される合成石英ルツボの製造装置
の縦断面図。FIG. 1 is a longitudinal cross-sectional view of a synthetic quartz crucible manufacturing apparatus used in the present invention.
１ カーボン型 ２ 黒鉛断熱材 ３ 水冷チャンバー ４ モーター ５ ルツボ状成形体 ６ 発熱体 ７ 昇降装置 ８ 不活性ガス導入口 ９ ガス排出口 １０ 温度管理用窓 1 Carbon type 2 Graphite insulation material 3 Water cooling chamber 4 Motor 5 Crucible-shaped molded body 6 Heating element 7 Lifting device 8 Inert gas inlet 9 Gas outlet 10 Temperature control window
Claims (1)
はカーボン型内で遠心力によりルツボ状に成形し、炭素
発熱体、炭化けい素発熱体、酸化物発熱体または金属発
熱体を用いて加熱し、焼結することを特徴とする合成石
英ルツボの製造方法。[Claim 1] Amorphous synthetic quartz powder is formed into a crucible shape by centrifugal force in a rotating mold or carbon mold, and a carbon heating element, a silicon carbide heating element, an oxide heating element, or a metal heating element is used. A method for producing a synthetic quartz crucible, which comprises heating and sintering the crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10386091A JPH04310530A (en) | 1991-04-09 | 1991-04-09 | Production of synthetic quartz crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10386091A JPH04310530A (en) | 1991-04-09 | 1991-04-09 | Production of synthetic quartz crucible |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04310530A true JPH04310530A (en) | 1992-11-02 |
Family
ID=14365206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10386091A Pending JPH04310530A (en) | 1991-04-09 | 1991-04-09 | Production of synthetic quartz crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04310530A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6546754B1 (en) * | 2000-10-27 | 2003-04-15 | General Electric Company | Apparatus for silica crucible manufacture |
-
1991
- 1991-04-09 JP JP10386091A patent/JPH04310530A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6546754B1 (en) * | 2000-10-27 | 2003-04-15 | General Electric Company | Apparatus for silica crucible manufacture |
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