JPH03183626A - Production of starting material for synthetic quartz glass crucible - Google Patents
Production of starting material for synthetic quartz glass crucibleInfo
- Publication number
- JPH03183626A JPH03183626A JP32225289A JP32225289A JPH03183626A JP H03183626 A JPH03183626 A JP H03183626A JP 32225289 A JP32225289 A JP 32225289A JP 32225289 A JP32225289 A JP 32225289A JP H03183626 A JPH03183626 A JP H03183626A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- ingot
- synthetic quartz
- particle size
- flotation
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000007858 starting material Substances 0.000 title abstract description 4
- 238000005188 flotation Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 33
- 238000010306 acid treatment Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 17
- 239000002245 particle Substances 0.000 abstract description 16
- 239000000843 powder Substances 0.000 abstract description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052742 iron Inorganic materials 0.000 abstract description 9
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910021529 ammonia Inorganic materials 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 5
- 206010027146 Melanoderma Diseases 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 239000010453 quartz Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000010299 mechanically pulverizing process Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 239000011521 glass Substances 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000006148 magnetic separator Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000010665 pine oil Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010064127 Solar lentigo Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は合成石英ガラスルツボ用原料の製造方法、特に
はゾル−ゲル法で作られた石英ガラスインゴット粉砕品
を精製してＯ）１基含有量が低く、高温粘性が高いこと
からシリコーン単結晶引上げ用ルツボ材として有用とさ
れる合成石英ガラス原料を製造する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 method for producing a raw material for a synthetic silica glass crucible, and in particular, to purifying a pulverized quartz glass ingot made by a sol-gel method. The present invention relates to a method for producing a synthetic quartz glass raw material that is useful as a crucible material for pulling silicone single crystals because of its low content and high high-temperature viscosity.
（従来の技術）
半遵体物質、特にシリコーン単結晶の引上げ用ルツボは
高温での耐熱性にすぐれていることが必要とされること
から天然の石英ガラス製のものが汎用されているが、こ
の天然の石英ガラスには不純物が多く含まれていること
から、このものは粉砕、篩別後に精製して使用されてお
り、この精製は通常磁力選鉱か浮遊選鉱で行なわれてい
る。(Prior art) Crucibles for pulling semi-conforming materials, especially silicone single crystals, are required to have excellent heat resistance at high temperatures, so crucibles made of natural quartz glass are commonly used. Since this natural quartz glass contains many impurities, it is used after being crushed and sieved and purified, and this purification is usually performed by magnetic beneficiation or flotation.
しかし最近における半導体メモリの高集積化のためにこ
の歩留りの低下が問題となり、この高純度化が要望され
てきる。However, due to the recent increase in the degree of integration of semiconductor memories, this reduction in yield has become a problem, and higher purity has been desired.
（発明が解決しようとする課題）
そのため、このルツボを純度の高い合成石英ガラスで作
ることも検討されているが、■四塩化けい素などを酸水
素火炎中で加水分解させてシリカ微粒子とし、これを溶
融して石英ガラスとする方法にはガラス中に０）１基が
１．（１００ｐｐｍも残留し、高温粘性が低く、真空中
高温では発泡するという問題点があり、■この酸水素火
炎をプラズマ炎とする方法にはコストが高く、量産化も
難しいという不利があるため、これについてはアルコキ
シシランをアルコール溶媒中で加水分解してシリカを作
り、これを溶融して合成石英を得るという、いわゆるゾ
ル−ゲル法によることも検討されており、これには高純
度品を安価に得ることができるという利益があるものの
ＯＨ基が残り易く、製造に長時間が必要とされ、高温粘
性の高いものが得られ難いという不利があり、これには
またアルコキシシランの分解で発生した炭素分が混入さ
れるためにこれから作られるルツボには泡や黒点不純物
が数多く発生するという欠点がある。(Problem to be solved by the invention) Therefore, it is being considered to make this crucible from highly pure synthetic quartz glass. In the method of melting this to make quartz glass, 0) 1 group is added to 1. (As much as 100 ppm remains, the viscosity at high temperatures is low, and foaming occurs at high temperatures in a vacuum. Regarding this, the so-called sol-gel method, in which alkoxysilane is hydrolyzed in an alcohol solvent to produce silica and then melted to obtain synthetic quartz, is being considered. However, it has the disadvantage that OH groups tend to remain, a long time is required for production, and it is difficult to obtain products with high viscosity at high temperatures. Because of the carbon content mixed in, the crucibles that will be made from now on have the disadvantage of producing a lot of bubbles and black spot impurities.
（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ガラスルツ
ボ用原料の製造方法に関するものであり、これはゾル−
ゲル法により製造した石英ガラスインゴットを機械的に
粉砕し、篩別してから、ａ）磁力選鉱工程、ｂ）浮遊選
鉱工程、Ｃ）熱処理工程、ｄ）酸処理工程のいずれか、
またはこれらの２工程あるいは２工程以上を組合せて処
理し精製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 producing raw materials for synthetic silica glass crucibles that solves these disadvantages.
The quartz glass ingot produced by the gel method is mechanically crushed and sieved, and then subjected to one of a) magnetic beneficiation process, b) flotation process, C) heat treatment process, d) acid treatment process,
Alternatively, it is characterized by processing and purifying these two steps or a combination of two or more steps.
すなわち、本発明者らはシリコン！ｌ−結晶の引上げ用
ルツボ材として使用し得る合成石英ガラスの製造方法に
ついて種々検討した結果、メチルシリケートをメタノー
ル溶媒中でアンモニアを触媒として加水分解すると粒径
が２００〜３，０００ ｒ＋ｍのシリカが得られること
、このシリカを固液分離後、濃縮し、乾燥してから加熱
酸化するとＯＨ基の少ない石英ガラスインゴットの得ら
れること、このインゴットを粉砕したのち、磁力選鉱な
どで精製し、ついで高温に加熱して透明ガラス化すると
黒点不純物がなく、高温粘性も高いことがらルツボ用原
料として有用とされる石英ガラスの得られることを見出
して本発明を完成させた。In other words, the inventors used silicon! As a result of various studies on the manufacturing method of synthetic quartz glass that can be used as a crucible material for pulling l-crystals, we found that when methyl silicate is hydrolyzed in methanol solvent using ammonia as a catalyst, silica with a particle size of 200 to 3,000 r+m is produced. After solid-liquid separation, this silica is concentrated, dried, and then heated and oxidized to obtain a quartz glass ingot with few OH groups.This ingot is crushed, purified by magnetic beneficiation, etc., and then heated at high temperature. The inventors have completed the present invention by discovering that quartz glass, which is free of sunspot impurities and has high high-temperature viscosity and is useful as a raw material for crucibles, can be obtained by heating the glass to transparent glass.
［作用］ 以下にこれをさらに詳述する。[Effect] This will be explained in further detail below.
本発明はゾル−ゲル法で製造したシリカを加熱酸化して
石英ガラスインゴットとし、粉砕後に精製するものであ
る。The present invention heats and oxidizes silica produced by the sol-gel method to form a quartz glass ingot, which is then purified after being crushed.
本発明の方法はゾル−ゲル法によるものであるが、本発
明の方法では始発材としてメチルシリケートが使用れる
。すなわち、従来公知のゾル−ゲル法では通常エチルシ
リケートを始発材とし、これをエタノール溶媒中でアン
モニアまたは塩酸を触媒として加水分解させており、こ
の場合も５００ｎｍ程度の粒径をもつシリカが得られ、
これを乾燥後１，０５０℃で焼結し、さらに１．５００
℃で溶融ガラス化すれば透明な石英ガラスを得ることが
できるけれども、この石英ガラスはＯＨ基含有量が多く
、高温粘性も低いという不利があることが判った。Although the method of the present invention is based on a sol-gel method, methyl silicate is used as the starting material in the method of the present invention. That is, in the conventionally known sol-gel method, ethyl silicate is usually used as a starting material and this is hydrolyzed in an ethanol solvent using ammonia or hydrochloric acid as a catalyst, and in this case as well, silica with a particle size of about 500 nm can be obtained. ,
After drying, this was sintered at 1,050°C, and further heated to 1.500°C.
Although transparent quartz glass can be obtained by melting and vitrifying it at .degree. C., it has been found that this quartz glass has the disadvantages of having a high OH group content and low high-temperature viscosity.
しかし、このエチルシリケートをメチルシリケートとす
るとコスト的に有利であることのほか、これをメタノー
ル溶媒中でアンモニアを触媒として加水分解させるとこ
の加水分解反応はメチルシリケート注加直後に始まって
瞬時にシリカの生成が行われるという有利性が与えられ
る。この加水分解で得られたシリカの粒径はここに使用
するメタノール、アンモニア、メチルシリケートの重量
比、反応温度、攪拌速度によって制御可能とされるが、
ＯＨ基含有量の少ないシリカ粉を製造するためには平均
粒径が２０Ｏｎ１１１以上のものとする必要が・あるし
、乾燥して塊状とするためにはある程度の微粉であるこ
とが必要とされるので本発明の方法ではここに得られる
シリカは平均粒径が２００〜３．０００ｎｍのものとす
ることがよい。However, if this ethyl silicate is replaced with methyl silicate, it is advantageous in terms of cost, and when this is hydrolyzed in a methanol solvent using ammonia as a catalyst, this hydrolysis reaction starts immediately after the methyl silicate is added, and the silica is instantly converted into methyl silicate. The advantage is that the generation of The particle size of the silica obtained by this hydrolysis can be controlled by the weight ratio of methanol, ammonia, and methyl silicate used here, the reaction temperature, and the stirring speed.
In order to produce silica powder with a low OH group content, it is necessary to have an average particle size of 20 On111 or more, and in order to dry it into a lump, it needs to be a certain amount of fine powder. Therefore, in the method of the present invention, the silica obtained here preferably has an average particle size of 200 to 3.000 nm.
このようにして得られたシリカは遠心分離器またはフィ
ルタープレスで固液分離したのち、真空中あるいは窒素
ガス雰囲気中で濃縮、乾燥し、ついで空気中あるいは酸
素雰囲気で５００℃程度に加熱すると有機物が除去され
たものとなるので、つぎにこれを真空中、ヘリウムガス
中または水素ガス中において１，５００℃程度に加熱す
るとこのものはシリカが閉孔化されガラス化されて、透
明で通常の石英ガラスと同等の比重を有する塊状体とな
るが、このシリカが粒径３，００Ｏｒ＋ｍ以下のものと
されているので上記における閉孔化は容易に進行し、泡
を含まないガラス塊が容易に得られる。このようにして
得られたガラス塊はついでボールミル、ロールミル、ロ
ッドセルなとで粉砕して平均粒径が５０から２００メツ
シユのものに粒度を調整するのであるが、この粉砕は粉
砕時の摩耗によって目的とする石英ガラス粉中に混入さ
れるものが鉄であると爾後における磁力選鉱法で除去し
易いということから、鉄系の媒体を用いて行なうことが
よく、したがってこれは例えばライニングボールが鉄系
のものであるボールミルや、歯が鉄系のもので作られて
いるインペラーブレーカ−やディスクミルを用いて行な
うことがよいし、篩別網も鉄系のものとすることがよい
。The silica thus obtained is subjected to solid-liquid separation using a centrifuge or filter press, concentrated and dried in a vacuum or nitrogen gas atmosphere, and then heated to about 500°C in air or an oxygen atmosphere to remove organic matter. When this is heated to about 1,500°C in vacuum, helium gas, or hydrogen gas, the silica becomes pore-closed and vitrified, making it transparent and normal quartz. The resulting silica has a specific gravity equivalent to that of glass, but since the particle size of this silica is 3,00 Or+m or less, the above pore closure progresses easily, making it easy to obtain a glass lump that does not contain bubbles. It will be done. The glass lumps obtained in this way are then crushed in a ball mill, roll mill, or rod cell to adjust the particle size to an average particle size of 50 to 200 mesh. If iron is mixed in the quartz glass powder to be used, it is easy to remove it later using the magnetic beneficiation method, so it is often carried out using an iron-based medium. It is preferable to use a ball mill, an impeller breaker, or a disc mill whose teeth are made of iron, and it is also preferable to use an iron-based sieve screen.
このように粉砕された石英ガラスインゴットはついで精
製されるが、この精製はａ）磁力選鉱工程、ｂ）浮遊選
鉱工程、Ｃ）熱処理工程、ｄ）酸処理工程のいずれか、
またはこれらの組合せによって行えばよく、これによれ
ば泡や黒点不純物が除去されるので外観上もすぐれた超
高純度の石英ガラスインゴット粉を得ることができる。The quartz glass ingot crushed in this way is then purified, and this purification is performed by any one of a) magnetic beneficiation process, b) flotation process, C) heat treatment process, d) acid treatment process,
Alternatively, a combination of these may be used. According to this method, since bubbles and black spot impurities are removed, ultra-high purity quartz glass ingot powder with excellent appearance can be obtained.
この精製は上記したａ）〜ｄ）の工程のいずれか１つで
行えばよいが、工業的に充分精製された石英ガラスイン
ゴットを得るためにはこれらをすべて組合せたものとす
ることがよく、したがってこれについては例えば上記で
得た石英ガラスインゴットをまず磁力選鉱機に通して大
粒の鉄分を除去したのち、インゴット粉に付着している
微粉状の鉄分を除去するためにこれを濃度が１５〜２５
重量％の塩酸水溶液で酸処理し、ついで酸性のまま浮遊
選鉱槽に移してパイン油を入れ、泡沫浮遊選鉱を行なっ
てルツボ成形時の泡の発生原因となるゴムと他の有機物
を除去したのちに脱水し、８００〜１，０００℃の温度
で仮焼してパイン油を分解、酸化除去してから、濃度が
２〜５重量％のフッ酸水溶液で洗浄して粒子表面の汚れ
を除去すると共にその純度を上げ、乾燥してから、最後
に再度磁力選鉱機を通すという方法で行なえばよい。This purification may be carried out in any one of the above steps a) to d), but in order to obtain a quartz glass ingot that is industrially sufficiently purified, it is best to use a combination of all of these steps. Therefore, regarding this, for example, the quartz glass ingot obtained above is first passed through a magnetic ore separator to remove large grains of iron, and then the ingot powder is passed through a magnetic ore separator to remove the fine iron particles adhering to the ingot powder. 25
After acid treatment with an aqueous hydrochloric acid solution of % by weight, the material was transferred to a flotation tank while still acidic, and pine oil was added thereto to perform foam flotation to remove rubber and other organic substances that cause bubbles during crucible molding. The particles are dehydrated and calcined at a temperature of 800 to 1,000°C to decompose and oxidize the pine oil, and then washed with a hydrofluoric acid aqueous solution with a concentration of 2 to 5% by weight to remove dirt on the particle surface. At the same time, the purity can be increased, dried, and finally passed through the magnetic separator again.
この精製工程を経た石英粉は真空中あるいは不活性ガス
存在下で１，７００℃以上に加熱し、溶融すれば合成石
英ガラスとすることができるが、ここに得られた合成石
英ガラス粉はＯＨ基含有量が例えば１ ｐｐＩ１１以下
というように低いし、これはまた上記方法で作られたシ
リカが極めて規則正しい構造をもつものであり、上記し
た加熱溶融時にもこの構造が不規則になることもないの
で高温粘性が例えば１，４００℃において１〜４ Ｘ
１０”ボイズと高い値を示すという特性をもっているの
で、このものは特にシリコン単結晶引上げ用ルツボ材と
して有用とされるという工業的な有利性をもつものにな
る。The quartz powder that has gone through this purification process can be heated to 1,700°C or higher in a vacuum or in the presence of an inert gas and melted to produce synthetic quartz glass. The group content is low, for example, 1 ppI11 or less, and this also means that the silica produced by the above method has an extremely regular structure, and this structure does not become irregular even when heated and melted as described above. Therefore, the high temperature viscosity is, for example, 1 to 4 X at 1,400°C.
Since it has the property of exhibiting a high value of 10'' voids, it has an industrial advantage, particularly as it is useful as a crucible material for pulling silicon single crystals.
（実施例） つぎに本発明方法による実施例をあげる。(Example) Next, examples using the method of the present invention will be given.
実施例
反応容器にメタノール１５０モル、純水１２０モル、ア
ンモニア５０モルを入れて２０℃に保ち、ここにメチル
シリケート１０モルを１２０分で滴下して加水分解反応
させ、反応終了後生成したシリカを自然沈降させてから
沈降物を取り出し、真空中で１５０℃に加熱して乾燥し
たところ、平均粒径が７００ｎｍであるシリカ粉が得ら
れた。Example: 150 moles of methanol, 120 moles of pure water, and 50 moles of ammonia were placed in a reaction vessel and kept at 20°C. 10 moles of methyl silicate was added dropwise over 120 minutes to cause a hydrolysis reaction. After the reaction, the silica produced was After natural sedimentation, the precipitate was taken out and dried by heating at 150° C. in vacuum to obtain silica powder with an average particle size of 700 nm.
ついで、このシリカ粉を空気中において５ｏｏ℃に加熱
して有機物を酸化除去したのち、真空中で１．５００℃
に加熱してこのシリカを閉孔化し、ガラス化したところ
、粒径が１〜５ｍｍである透明な合成石英ガラスインゴ
ット３０ｋｇを収率９８％で得ることができたので、こ
のインゴットをハンマーで砕き、粉砕歯が５Ｓ−４１で
作られているディスクよルで粉砕してから、円型振動篩
で粒度を５ＯＮ１５０メツシユに揃えたところ、合成石
英ガラス粉２５ｋｇが得られた。Next, this silica powder was heated to 50°C in air to oxidize and remove organic matter, and then heated to 1.500°C in vacuum.
When this silica was heated to close the pores and vitrified, we were able to obtain 30 kg of transparent synthetic quartz glass ingots with a particle size of 1 to 5 mm at a yield of 98%.This ingot was crushed with a hammer. After crushing with a disc mill whose crushing teeth were made of 5S-41, the particles were adjusted to a 5ON150 mesh using a circular vibrating sieve, yielding 25 kg of synthetic quartz glass powder.
ついでこの合成石英ガラス粉を磁力選鉱機・ＣＧ−５０
型（ダルトン社製商品名）に通して脱鉄したのち、濃度
２０重量％の塩酸水溶液中に入れ、１時間ローラーで攪
拌して酸処理を行ない、浮遊選鉱槽に入れ、パイン油５
０ｃ、ｃ、を添加しエアでバブリングさせながらオーバ
ーフローさせ、脱水してから酸素雰囲気中において１，
０００℃に１時間保持し、冷却後濃度３重量％のフッ酸
水溶液中で３０分間攪拌し、脱水後６００℃で乾燥し、
再度前記した磁力選鉱機に通したところ、精製された合
成石英ガラス粉２０ｋｇが得られた。Next, this synthetic quartz glass powder is passed through a magnetic separator, CG-50.
After passing it through a mold (trade name manufactured by Dalton Co., Ltd.) to remove iron, it was placed in an aqueous solution of hydrochloric acid with a concentration of 20% by weight, stirred with a roller for 1 hour for acid treatment, placed in a flotation tank, and mixed with pine oil 5.
Add 0c, c, overflow while bubbling with air, dehydrate, and then add 1,
After cooling, it was stirred for 30 minutes in a hydrofluoric acid aqueous solution with a concentration of 3% by weight, and after dehydration, it was dried at 600°C.
When it was passed through the magnetic separator again, 20 kg of purified synthetic quartz glass powder was obtained.
つぎにこの合成石英ガラス粉について化学分かを行なっ
てその不純物を測定したところ、これ１ｉＡｕ３５ｐｐ
ｂ、 Ｆｅ ５２ｐｐｂ、 Ｎａ１８ ｐｐｂ、 ８２
０ ｐｐｂ、Ｃ５５ｐｐｂという純度の高いもので、こ
のもののＯＨＪは＜ １ ｐｐｍで、これをアーク溶融
して成形した）Ｌツボは泡、黒色不純物のない良好なも
のであり、このものをファイバーエロンゲーション法で
測方した１、４０［） ｔにおける粘性は７．５ Ｘｌ
０１０ボイズてあった。Next, this synthetic quartz glass powder was subjected to chemical separation to measure its impurities, and it was found that 1iAu35pp
b, Fe 52ppb, Na18ppb, 82
It has a high purity of 0 ppb and C55 ppb, and the OHJ of this product is < 1 ppm, and it was molded by arc melting). The viscosity at 1,40 [) t measured by the method is 7.5 Xl
There was a 010 voice.
（発明の効果）
本発明は合成石英ガラスルツボ用原料の製造方７去に関
するもので、これは前記したようにメチルシリケートか
らソ゛ルーゲル
加熱酸化して石英ガラスインゴットとし、ついでこれを
＄１械的に粉砕し、篩別してから、ａ）６７３力選鉱工
程、ｂ）浮遊選鉱工程、Ｃ）熱処理工程、 ｄ）酸処理
工程のいずれか、またはこれらの組合せで精製するもの
であるが、これによればＯＨ基が少なく、高温粘性が高
く、ざらには黒点不純物も含有されていない合成石英ガ
ラス粉末が容易に得られるし、この合成石英ガラス粉末
は」二足したような物性をもっているのでこれを溶融し
てルツボを成形すれば得られたルツボは外観的にも、物
性上からもすぐれたものになるという有利性が与えられ
る。(Effects of the Invention) The present invention relates to a method for producing a raw material for a synthetic quartz glass crucible, which involves heating and oxidizing a solid gel from methyl silicate to obtain a quartz glass ingot, which is then mechanically oxidized for $1, as described above. After crushing and sieving, it is purified by one of a) 673 force beneficiation process, b) flotation process, C) heat treatment process, d) acid treatment process, or a combination thereof. Synthetic quartz glass powder with few OH groups, high high-temperature viscosity, and no black spot impurities can be easily obtained. If the crucible is molded using this method, the resulting crucible has the advantage of being excellent in both appearance and physical properties.
Claims (1)
を機械的に粉砕し、篩別してから、ａ）磁力選鉱工程、
ｂ）浮遊選鉱工程、ｃ）熱処理工程、ｄ）酸処理工程の
いずれか、またはこれらの２工程あるいは２工程以上を
組合わせて処理して精製することを特徴とする合成石英
ガラスルツボ用原料の製造方法。 ２、精製工程がａ）磁力選鉱工程、ｄ）酸処理工程、ｂ
）浮遊選鉱工程、ｃ）熱処理工程、ｄ）酸処理工程、ａ
）磁力選鉱工程の順に行なわれる請求項１に記載の合成
石英ガラスルツボ用原料の製造方法。[Claims] 1. After mechanically crushing and sieving a quartz glass ingot produced by the sol-gel method, a) magnetic beneficiation step;
A raw material for a synthetic quartz glass crucible that is purified by any one of b) flotation process, c) heat treatment process, d) acid treatment process, or a combination of two or more of these processes. Production method. 2. The refining process is a) magnetic beneficiation process, d) acid treatment process, b
) Flotation process, c) Heat treatment process, d) Acid treatment process, a
2. The method for producing a raw material for a synthetic quartz glass crucible according to claim 1, wherein the magnetic beneficiation step is performed in this order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32225289A JPH03183626A (en) | 1989-12-12 | 1989-12-12 | Production of starting material for synthetic quartz glass crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32225289A JPH03183626A (en) | 1989-12-12 | 1989-12-12 | Production of starting material for synthetic quartz glass crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03183626A true JPH03183626A (en) | 1991-08-09 |
| JPH0563416B2 JPH0563416B2 (en) | 1993-09-10 |
Family
ID=18141590
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32225289A Granted JPH03183626A (en) | 1989-12-12 | 1989-12-12 | Production of starting material for synthetic quartz glass crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03183626A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0803469A1 (en) * | 1995-01-12 | 1997-10-29 | Mitsubishi Chemical Corporation | Silica gel, synthetic quartz glass powder, quartz glass molding, and processes for producing these |
| JP2017061413A (en) * | 2016-12-28 | 2017-03-30 | 株式会社Sumco | Method of manufacturing silica glass crucible for silicon single crystal lifting, method of manufacturing silicon single crystal, and silicon single crystal |
-
1989
- 1989-12-12 JP JP32225289A patent/JPH03183626A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0803469A1 (en) * | 1995-01-12 | 1997-10-29 | Mitsubishi Chemical Corporation | Silica gel, synthetic quartz glass powder, quartz glass molding, and processes for producing these |
| EP0803469A4 (en) * | 1995-01-12 | 1997-11-19 | ||
| US6071838A (en) * | 1995-01-12 | 2000-06-06 | Mitsubishi Chemical Corporation | Silica gel, synthetic quartz glass powder, quartz glass shaped product molding, and processes for producing these |
| JP2017061413A (en) * | 2016-12-28 | 2017-03-30 | 株式会社Sumco | Method of manufacturing silica glass crucible for silicon single crystal lifting, method of manufacturing silicon single crystal, and silicon single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0563416B2 (en) | 1993-09-10 |
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