JPH09165214A - Production of synthetic quartz powder - Google Patents

Production of synthetic quartz powder

Info

Publication number
JPH09165214A
JPH09165214A JP33019995A JP33019995A JPH09165214A JP H09165214 A JPH09165214 A JP H09165214A JP 33019995 A JP33019995 A JP 33019995A JP 33019995 A JP33019995 A JP 33019995A JP H09165214 A JPH09165214 A JP H09165214A
Authority
JP
Japan
Prior art keywords
powder
silica gel
synthetic quartz
rotary kiln
temperature
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
JP33019995A
Other languages
Japanese (ja)
Inventor
Yoshio Suguro
芳雄 勝呂
Masaru Shimoyama
勝 下山
Shoji Oishi
昭二 大石
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.)
Mitsubishi Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
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 Mitsubishi Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP33019995A priority Critical patent/JPH09165214A/en
Publication of JPH09165214A publication Critical patent/JPH09165214A/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/10—Forming beads
    • C03B19/1005—Forming solid beads
    • C03B19/106—Forming solid beads by chemical vapour deposition; by liquid phase reaction
    • C03B19/1065—Forming solid beads by chemical vapour deposition; by liquid phase reaction by liquid phase reactions, e.g. by means of a gel phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/10—Forming beads
    • C03B19/1095—Thermal after-treatment of beads, e.g. tempering, crystallisation, annealing

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Silicon Compounds (AREA)
  • Muffle Furnaces And Rotary Kilns (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

PROBLEM TO BE SOLVED: To decrease the amount of residual carbon by continuously supplying silica gel powder from an end of a furnace core tube of a rotary kiln rotating at a specific speed and heat-treating the powder. SOLUTION: A tetraalkoxysilane is hydrolyzed by adding 1-10 times equivalent of water based on the alkoxy group of the alkoxysilane and the product is dried at 50-200 deg.C to obtain silica gel powder having particle diameter of 10-1,000μm and an impregnation rate of 1-30wt.%. The silica gel powder is supplied through a dry gel hopper 6 and a table feeder 7 to the feeding port 9 of a furnace core tube 8 of a rotary kiln rotating at a circumferential speed of 2-12m/min, heated to 50-300 deg.C by the 1st heater 15 to evaporate water, heated to 300-600 deg.C by the 2nd to the 4th heaters 16-18 to burn out the residual carbon and finally heated at 900-1,100 deg.C by the 5th heater 19 to seal the pores of the silica gel and obtain the objective synthetic quartz powder having a tap bulk density of 1.0-1.2g/mL and a carbon concentration of 50-1,000ppm.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【発明の属する技術分野】本発明は、合成石英粉の効率
的な製造方法に関するものである。近年、光通信分野、
半導体産業等で使用されるガラス製品に於いては、その
微量不純物及び製品中の微小泡に関し非常に厳しい管理
が行われている。このような高品質のガラスは主に、
天然石英を精製する方法、四塩化珪素の酸水素炎中で
の分解で発生したヒュームを基体に付着・成長させる方
法、シリコンアルコキシド等の加水分解・ゲル化によ
り得たシリカゲルを焼成してガラス化する方法等によっ
て生成される。しかしながら、の方法では、微量不純
物含有率の低減に限界があり、の方法では、極めて製
造コストが高い等の問題点がある。一方、の、シリカ
ゲルを用いる方法、特に原料としてシリコンアルコキシ
ドを用いる方法では、の方法に比べると安価に微量不
純物含有率が低い合成石英粉が得られるが、要求レベル
を必ずしも満足しているとは言えないし、このシリコン
アルコキシドを用いる方法では、最終製品の成形体中
に、場合によっては、微小泡が発生すると言う問題点が
ある。TECHNICAL FIELD The present invention relates to a method for efficiently producing synthetic quartz powder. In recent years, the optical communication field,
In glass products used in the semiconductor industry and the like, very strict control is carried out regarding trace impurities and micro bubbles in the products. Such high quality glass is mainly
A method for purifying natural quartz, a method for attaching and growing fumes generated by decomposition of silicon tetrachloride in an oxyhydrogen flame to a substrate, and a method for sintering silica gel obtained by hydrolysis and gelation of silicon alkoxide and the like. Generated by such a method. However, the method (1) has a limit in reducing the content of trace impurities, and the method (2) has problems such as extremely high manufacturing cost. On the other hand, in the method using silica gel, in particular, the method using silicon alkoxide as a raw material, a synthetic quartz powder having a low trace impurity content can be obtained at a lower cost than the method, but it does not necessarily satisfy the required level. In other words, the method using the silicon alkoxide has a problem that, in some cases, microbubbles are generated in the molded product of the final product.

【０００２】[0002]

【発明が解決しようとする課題】本発明者らの鋭意検討
により、シリコンアルコキシドを用いる合成石英粉の製
造方法で、従来に比べ安価で、かつ成形体を製造する際
に微小泡の発生が極めて少ない合成石英粉を工業的に製
造するには、次に示す課題を解決すればよいことが判っ
た。The inventors of the present invention have earnestly studied, and in the method for producing synthetic quartz powder using a silicon alkoxide, it is cheaper than the conventional method, and very small bubbles are generated when a molded body is produced. It was found that the following problems should be solved in order to industrially produce a small amount of synthetic quartz powder.

【０００３】即ち、シリカゲルの焼成は、容器からの不
純物のコンタミを排除するために、石英製の容器にシリ
カゲルを仕込み、電気炉等で加熱する方法が採用され
る。特に、工業的製造を図る場合には、大容量の石英容
器、例えば大口径の石英るつぼを使用することになる。
しかしながら、シリカゲルは石英粉に比べ嵩密度が低い
ために、焼成に用いる容器を効率的に利用できず、生産
性が悪く、製造コストが高くなっている。従って、生産
性の向上にはるつぼに仕込む粉体の嵩密度アップが重要
な課題となる。That is, in the firing of silica gel, in order to eliminate the contamination of impurities from the container, a method of charging silica gel in a quartz container and heating it in an electric furnace or the like is adopted. In particular, for industrial production, a large capacity quartz container, for example, a large diameter quartz crucible is used.
However, since silica gel has a lower bulk density than quartz powder, a container used for baking cannot be used efficiently, productivity is poor, and production cost is high. Therefore, increasing the bulk density of the powder charged in the crucible is an important issue for improving productivity.

【０００４】一方、石英粉を用いた成形体の製造に於い
て、成形体を製造する際の微小泡の発生は、石英粉製造
時の焼成工程の昇温過程が影響を及ぼす。シリコンアル
コキシドの加水分解により得たシリカゲル粉末は、副生
したアルコールを乾燥により除去しても、未反応のアル
コキシ基及び副生したアルコールの一部が残存する。実
際、乾燥を施したシリカゲル粉末中のカーボン濃度を測
定すると、乾燥条件によっても異なるが、１〜３％であ
る。このシリカゲル粉末を酸素含有ガス中で焼成を行う
と、大部分のカーボンは、昇温過程で燃焼除去される
が、一部が未燃カーボンとして合成石英粉中に閉じ込め
られることがある。この未燃カーボンを含有する合成石
英粉を用いると、溶融成形の際にＣＯやＣＯ2ガスとな
り、泡発生の原因となる。従って、シリカゲルの封孔前
に、未燃カーボンを実質的に全量除去することが必要と
なり、昇温過程における昇温速度が重要となるわけであ
る。On the other hand, in the production of a molded body using quartz powder, the generation of microbubbles during the production of the molded body is affected by the heating process in the firing step in the production of quartz powder. The silica gel powder obtained by hydrolyzing the silicon alkoxide retains unreacted alkoxy groups and a part of the by-produced alcohol even if the by-produced alcohol is removed by drying. Actually, when the carbon concentration in the dried silica gel powder is measured, it is 1 to 3% depending on the drying conditions. When this silica gel powder is calcined in an oxygen-containing gas, most of the carbon is burned and removed in the course of raising the temperature, but part of the carbon is sometimes trapped as unburned carbon in the synthetic quartz powder. When this synthetic quartz powder containing unburned carbon is used, it becomes CO or CO 2 gas at the time of melt molding and causes bubbles. Therefore, it is necessary to remove substantially all of the unburned carbon before sealing the silica gel, and the rate of temperature increase during the temperature increase process is important.

【０００５】ところが、先述の様に、合成石英粉を工業
的に製造する場合、大口径の石英るつぼが使用され、昇
温過程に於ける、るつぼ内の温度は不均一となるので、
容器内の全ての部分を所定の温度パターンで昇温するの
は困難である。その結果、場合によっては、カーボンが
残存した合成石英粉が部分的に生成しその合成石英粉を
用いた成形体中に、微小泡が発生するという現象が見ら
れるのである。However, as described above, in the case of industrially producing synthetic quartz powder, a large-diameter quartz crucible is used, and the temperature inside the crucible becomes uneven during the temperature rising process.
It is difficult to raise the temperature of all parts in the container in a predetermined temperature pattern. As a result, in some cases, a phenomenon is observed in which synthetic quartz powder in which carbon remains is partially generated, and microbubbles are generated in a molded body using the synthetic quartz powder.

【０００６】[0006]

【課題を解決するための手段】本発明者らは、上記課題
に鑑み、更に鋭意検討を行った結果、シリカゲルを焼成
前に適当な条件及び操作で加熱処理することにより、焼
成に供する粉体の嵩密度を焼成後と同等にすることがで
き、なおかつ、アルコキシ基及び水酸基を十分に除去す
ることができる事を見いだし、本発明を完成するに到っ
た。即ち、本発明は、シリカゲル粉末を、ロータリーキ
ルンの片端より連続的に供給しつつ、流動させながら加
熱処理することにより合成石英粉を製造する方法であっ
て、ロータリーキルンの炉心管を周速２ｍ／分〜１２ｍ
／分で回転させることを特徴とする合成石英粉の製造方
法、にある。Means for Solving the Problems In view of the above-mentioned problems, the present inventors have made further studies, and as a result, by heating silica gel under appropriate conditions and operations before firing, the powder to be subjected to firing It was found that the bulk density of (1) can be made equal to that after firing and the alkoxy group and hydroxyl group can be sufficiently removed, and the present invention has been completed. That is, the present invention is a method for producing synthetic quartz powder by heat-treating while flowing silica gel powder continuously from one end of a rotary kiln, in which the furnace core tube of the rotary kiln has a peripheral speed of 2 m / min. ~ 12m
The method for producing a synthetic quartz powder is characterized by rotating at a speed of 1 / min.

【０００７】以下、本発明を詳細に説明する。本発明で
対象となる合成石英粉は、シリカゲル粉末を、焼成する
ことにより無孔化してなる合成石英粉である。シリカゲ
ル粉末の製造法は特に限定されず、種々の公知方法を採
用できるが、高純度を容易に達成できる等の観点からア
ルコキシシラン等の加水分解・ゲル化による、いわゆる
ゾルゲル法によるものが好ましい。ゾルゲル法によるア
ルコキシシランの加水分解は、公知の方法にしたがっ
て、アルコキシシランと水を反応させることによって行
われる。Hereinafter, the present invention will be described in detail. The synthetic quartz powder targeted by the present invention is a synthetic quartz powder obtained by firing silica gel powder to make it non-porous. The method for producing the silica gel powder is not particularly limited, and various known methods can be adopted, but from the viewpoint of easily achieving high purity, the so-called sol-gel method by hydrolysis / gelation of alkoxysilane or the like is preferable. Hydrolysis of alkoxysilane by the sol-gel method is carried out by reacting alkoxysilane with water according to a known method.

【０００８】原料として用いられるアルコキシシランと
しては、テトラメトキシシラン、テトラエトキシシラン
等のＣ１〜Ｃ４の低級アルコキシシラン或いはそのオリ
ゴマーが好ましい。水の使用量は、通常、アルコキシシ
ラン中のアルコキシ基の１倍等量以上から１０倍等量以
下の範囲から選択される。この際、必要に応じて、水と
相溶性のあるアルコール類やエーテル類等の有機溶媒を
混合して使用してもよい。使用されるアルコールの代表
例としては、メタノール・エタノール等の低級脂肪族ア
ルコールが挙げられる。As the alkoxysilane used as a raw material, C1 to C4 lower alkoxysilane such as tetramethoxysilane and tetraethoxysilane or an oligomer thereof is preferable. The amount of water used is usually selected from the range of 1 to 10 equivalents of the alkoxy group in the alkoxysilane. At this time, if necessary, an organic solvent such as an alcohol or an ether which is compatible with water may be mixed and used. Representative examples of the alcohol used include lower aliphatic alcohols such as methanol and ethanol.

【０００９】この加水分解反応には、触媒として塩酸・
酢酸等の酸や、アンモニア等のアルカリを触媒として添
加してもよい。なお、当然のことながら、ここで使用す
る水・触媒等の、反応系に導入される物質はすべて高純
度であることが必要である。加水分解生成物のゲル化
は、加熱下あるいは常温で実施される。加熱を行うと、
ゲル化の速度を向上することができるので、加熱の程度
を調節することにより、ゲル化時間を調節することがで
きる。In this hydrolysis reaction, hydrochloric acid is used as a catalyst.
An acid such as acetic acid or an alkali such as ammonia may be added as a catalyst. It is needless to say that all substances to be introduced into the reaction system, such as water and catalyst used here, need to be of high purity. Gelation of the hydrolysis product is performed under heating or at room temperature. When heating,
Since the speed of gelation can be improved, the gelation time can be adjusted by adjusting the degree of heating.

【００１０】得られたゲルは水分及び加水分解により生
成したアルコールを多量に含むウェットシリカゲルであ
り、これを細分化してから乾燥してもよいし、乾燥して
から細分化してもよい。いずれにしても、乾燥後の粒径
が、１０〜１０００μｍ、好ましくは、１００〜６００
μｍと成るように細分化を行う。乾燥は、常圧、或い
は、減圧下で加熱しつつ行われる。加熱温度は、条件に
よっても異なるが、通常、５０〜２００℃である。ま
た、操作は、回分・連続のいずれによっても行うことが
できる。乾燥の程度は、通常、含液率が１〜３０重量％
まで行われる。ここで言う含液率とは、１６０℃におい
て恒量に達した時の重量減少率である。The obtained gel is wet silica gel containing a large amount of water and alcohol produced by hydrolysis, and may be subdivided and dried, or may be dried and subdivided. In any case, the particle size after drying is 10 to 1000 μm, preferably 100 to 600 μm.
Subdivision is performed to a size of μm. Drying is performed while heating under normal pressure or reduced pressure. The heating temperature varies depending on the conditions, but is usually 50 to 200 ° C. The operation can be performed either batchwise or continuously. The degree of drying is usually 1 to 30% by weight.
Done until. The liquid content referred to here is the weight reduction rate when a constant weight is reached at 160 ° C.

【００１１】このようにして得られた乾燥シリカゲル粉
末を、以下に述べる特定の条件下で加熱処理する。即
ち、シリカゲル粉末をロータリーキルン内で特定の温度
条件下でロータリーキルンを回転してシリカゲル粉末を
流動させながら加熱処理する。この加熱処理は、複数の
ロータリーキルンを用いて加熱処理を行ってもよい。こ
こで言う「粉体の流動」とは、例えば粉体を仕込んだ回
転状態のロータリーキルンの断面を示す図２を用い静止
状態のロータリーキルンの断面を示す図１と比較して説
明すると、粉体（１）と炉心管（２）壁の接粉面（３）
との間には実質的に滑りが生じておらず、炉心管壁で持
ち上げられ、安息角以上で粉体が壁面を離れて炉心管壁
下部に流下している状態（図２中の黒矢印方向）をい
う。The dried silica gel powder thus obtained is heat-treated under the following specific conditions. That is, the silica gel powder is heated in the rotary kiln under specific temperature conditions by rotating the rotary kiln to cause the silica gel powder to flow. This heat treatment may be performed using a plurality of rotary kilns. The "flow of powder" referred to here is, for example, as shown in FIG. 2 which shows a cross section of a rotary kiln in a rotating state in which powder is charged, in comparison with FIG. 1 which shows a cross section of a rotary kiln in a stationary state. 1) and core tube (2) wall contact surface (3)
There is substantially no slippage between the core and the core, the core is lifted by the core wall, and the powder leaves the wall above the angle of repose and flows down to the bottom of the core wall (black arrow in Fig. 2). Direction).

【００１２】炉心管の材質は、処理を行った粉への材質
のコンタミが発生しないものを選択する必要があり、石
英製が好ましい。石英製の場合、製作上、炉心管のサイ
ズに限界があるので、条件によっては、多段のロータリ
ーキルンを用いて加熱処理を行うこととなる。加熱処理
を行う温度領域は、５０〜１１００℃である。通常、加
熱はヒーターによって行われる。ここで、粉体を流動さ
せるための、ロータリーキルンの炉心管の回転速度を周
速２ｍ／分〜１２ｍ／分とすることが本発明の要件であ
る。周速２ｍ／分未満では、加熱処理後の粉体中の黒色
粒子の数が増加し、また溶融成形して得られる成形体中
の微小泡の発生が増加する。この理由は必ずしも明らか
ではないが、周速２ｍ／分未満の場合、粉体の混合状態
が特定レベル以下となり、粉体の混合状態が特定のレベ
ル以下となると酸素との接触が急速に悪化し未燃の残存
カーボンが増加するためと考えられる。一方、１２ｍ／
分を超えると黒色粒子の発生数、成形体の微小泡量に差
はなくなり、また、炉心管の強度の面から１２ｍ／分を
超えた場合には炉心管肉厚を厚くする必要が生じるの
で、好ましくない。It is necessary to select a material for the furnace tube that does not cause contamination of the material to the treated powder, and is preferably made of quartz. In the case of quartz, there is a limit in the size of the furnace tube in terms of manufacturing, so that heat treatment is performed using a multi-stage rotary kiln depending on conditions. The temperature range in which the heat treatment is performed is 50 to 1100 ° C. Usually, heating is performed by a heater. Here, it is a requirement of the present invention that the rotation speed of the core tube of the rotary kiln for flowing the powder is set to a peripheral speed of 2 m / min to 12 m / min. If the peripheral speed is less than 2 m / min, the number of black particles in the powder after heat treatment will increase, and the generation of fine bubbles in the molded product obtained by melt molding will increase. The reason for this is not clear, but when the peripheral speed is less than 2 m / min, the powder mixing state becomes a specific level or less, and when the powder mixing state becomes a specific level or less, the contact with oxygen rapidly deteriorates. It is considered that unburned residual carbon increases. On the other hand, 12m /
If it exceeds 12 minutes, there will be no difference in the number of black particles generated and the amount of minute bubbles in the molded body. If it exceeds 12 m / minute from the viewpoint of the strength of the core tube, it will be necessary to increase the thickness of the core tube. , Not preferable.

【００１３】加熱処理により、まず、シリカゲルが含有
する水及びアルコールが揮発する。この際、ロータリー
キルン内の粉体の温度は、通常、５０〜３００℃とな
る。この温度領域に於いて、粉体より発生するガスの量
を５００N-リットル／Ｋｇ・Hr以下とすることが好まし
い。発生量が、５００N-リットル／Ｋｇ・Hrより高い
と、粉体内で突沸現象が発生し、粉体の流動性が消失す
ることがある。理由は、明らかではないが、突沸により
揮発成分のガスが大量に発生して粉体を浮上させること
により、壁面での摩擦力が減少し、粉体が炉心管壁で持
ち上げられ難くなる為と考えられる。[0013] By the heat treatment, first, water and alcohol contained in the silica gel are volatilized. At this time, the temperature of the powder in the rotary kiln is usually 50 to 300 ° C. In this temperature range, the amount of gas generated from the powder is preferably 500 N-liter / Kg · Hr or less. When the amount generated is higher than 500 N-liter / Kg · Hr, bumping phenomenon may occur in the powder, and the fluidity of the powder may disappear. The reason is not clear, but because a large amount of volatile component gas is generated by bumping and the powder is levitated, the frictional force on the wall surface is reduced and it becomes difficult for the powder to be lifted by the core tube wall. Conceivable.

【００１４】続いて、残存するカーボン成分の燃焼温度
領域に昇温される。この温度領域は、３００〜６００℃
である。しかしながら、本発明者らの検討によって、３
００〜４３０℃で、残存するカーボン成分を燃焼するた
めの加熱をロータリーキルンで行うと、ロータリーキル
ン内の粉体の流動性が極めて悪いことが判明した。そこ
で、残存するカーボン成分の燃焼は４５０℃以上の温度
で行われる。Then, the temperature is raised to the combustion temperature range of the remaining carbon component. This temperature range is 300-600 ℃
It is. However, according to the study by the present inventors, 3
It was found that the fluidity of the powder in the rotary kiln was extremely poor when the heating for burning the remaining carbon component was carried out in the rotary kiln at 00 to 430 ° C. Therefore, the combustion of the remaining carbon component is performed at a temperature of 450 ° C. or higher.

【００１５】ところが、実際に、この加熱処理を、ロー
タリーキルンの片端より連続的に供給しつつ、流動させ
ながら行うと、当然ながら、昇温過程に相当する３００
〜４３０℃の温度ゾーンが発生する。この、温度ゾーン
の長さが５ｃｍ以上、１３５ｃｍ以下となるように熱供
給を調節するとよい。温度ゾーンの長さが１３５ｃｍよ
り長いと粉体の流動性が悪化する部分が発生する。一
方、５ｃｍ未満では流動性が悪化する部分は発生しない
が、極めて狭い領域で強烈な加熱を行う必要があるため
である。However, in practice, if this heat treatment is carried out while being continuously supplied from one end of the rotary kiln and flowing, 300 which corresponds to the temperature raising process is naturally obtained.
A temperature zone of ˜430 ° C. occurs. The heat supply may be adjusted so that the length of the temperature zone is 5 cm or more and 135 cm or less. When the length of the temperature zone is longer than 135 cm, there are portions where the fluidity of the powder deteriorates. On the other hand, if it is less than 5 cm, the portion where the fluidity deteriorates does not occur, but it is necessary to perform intense heating in an extremely narrow region.

【００１６】この、３００〜４３０℃の温度領域で、粉
体の流動性が低下する理由は、明らかではないが、こ
の温度領域で、シリカゲルの嵩密度が低下する、この
温度領域のシリカゲルは静電気を発生しやすい等の物理
的な性質があり、これらが合い重なって壁面での摩擦力
が減少し、粉体が炉心管壁で持ち上げられ難くなる為と
考えられる。The reason why the fluidity of the powder decreases in the temperature range of 300 to 430 ° C. is not clear, but the bulk density of the silica gel decreases in this temperature range. It is considered that there is a physical property such as that the powder is easily generated, and when these are combined, the frictional force on the wall surface is reduced, and it becomes difficult for the powder to be lifted by the core tube wall.

【００１７】４５０℃以上の温度領域に加熱された粉体
は、残存カーボンの減少が進行する。粉体温度が、６０
０℃以上となるとシリカゲルの封孔が開始するので、こ
の温度領域に到達するまでに、残存するカーボンのほぼ
全量を消失させておかなければならない。さもなけれ
ば、得られた合成石英粉中に未燃カーボンが残存し、溶
融成形の際に泡が発生する。In the powder heated to a temperature range of 450 ° C. or higher, the reduction of residual carbon proceeds. If the powder temperature is 60
When the temperature reaches 0 ° C. or higher, sealing of the silica gel starts, so that almost all of the remaining carbon must be eliminated before the temperature reaches this temperature range. Otherwise, unburned carbon remains in the obtained synthetic quartz powder, and bubbles are generated during melt molding.

【００１８】そのために、粉体が４５０〜５５０℃の温
度領域を通過する時間を適切に制御するのがよい。ロー
タリーキルンでは、粉体は進行方向に対し、ほぼピスト
ンフロー的に移動する。従って、所定温度ゾーンの通過
時間は、ロータリーキルン内の所定温度ゾーンの長さと
粉体の進行方向に対する移動速度からおのずと求められ
る。例えば、所定温度ゾーンの長さが１ｍで、粉体の進
行方に対する移動速度が０．５ｍ／Ｈｒであると、通過
時間は２Ｈｒとなる。Therefore, it is preferable to properly control the time during which the powder passes through the temperature range of 450 to 550.degree. In a rotary kiln, powder moves in a piston flow substantially in the traveling direction. Therefore, the passage time in the predetermined temperature zone is naturally determined from the length of the predetermined temperature zone in the rotary kiln and the moving speed in the traveling direction of the powder. For example, when the length of the predetermined temperature zone is 1 m and the moving speed of the powder in the traveling direction is 0.5 m / Hr, the passage time is 2 Hr.

【００１９】通過時間は、通常、０．５〜１０時間、好
ましくは、１〜５時間である。この範囲より短いと、十
分に未燃カーボンを減少させるのは困難であり、また、
これ以上の通過時間では、未燃カーボン量に差が見られ
ず、装置が大型化し経済的ではないためである。次に、
これまで述べた加熱処理の制御方法について説明する。The passage time is usually 0.5 to 10 hours, preferably 1 to 5 hours. If it is shorter than this range, it is difficult to sufficiently reduce unburned carbon, and
This is because if the passage time is longer than this, there is no difference in the amount of unburned carbon, and the size of the device is large, which is not economical. next,
The control method of the heat treatment described above will be described.

【００２０】本発明では、操作を連続で行うので、処理
粉体の進行方向に従い炉心管の加熱ゾーンを複数個に分
割し、粉体の温度が所定領域になるように、各々のゾー
ンのヒーターの加熱強度を調節することにより達成され
る。具体的には、炉心管の片端より清浄な空気あるい
は、酸素含有ガスを供給し、他端より排出する方法がと
られる。ガスの供給量は、通常、連続的に供給する粉体
１ｋｇ当たり、酸素換算で３０〜３００リットル／Ｈｒ
である。ロータリーキルンを用い粉体を流動させつつ行
うことにより、カーボンの減少が促進されるとともに、
均質な処理粉体が得られる。In the present invention, since the operation is carried out continuously, the heating zone of the core tube is divided into a plurality of zones according to the traveling direction of the treated powder, and the heater of each zone is arranged so that the temperature of the powder falls within a predetermined region. It is achieved by adjusting the heating intensity of. Specifically, a method of supplying clean air or oxygen-containing gas from one end of the core tube and discharging it from the other end is adopted. The gas supply amount is usually 30 to 300 liters / Hr in terms of oxygen per 1 kg of powder continuously supplied.
It is. By using a rotary kiln while flowing the powder, the reduction of carbon is promoted and
A homogeneous treated powder is obtained.

【００２１】この処理により、シリカゲル中のカーボン
濃度は、５０〜１０００ｐｐｍ程度に減少する。残存す
るカーボンがほぼ消失した処理粉体は、引き続き加熱さ
れ、最終的な粉体の温度は、９００〜１１００℃、好ま
しくは９５０〜１０５０まで高められる。この際の昇温
速度は通常、１００〜１０００℃／Ｈｒである。ロータ
リーキルンでは、粉体は進行方向に対し、ほぼピストン
フロー的に流れるので、供給した粉体はロータリーキル
ン内を進行方向に移動するに従い昇温されることとな
る。従って、粉体の昇温速度は、ロータリーキルン内の
温度分布と粉体の進行方向に対する移動速度からおのず
と求められる。例えば、温度測定点間の距離が１ｍで温
度差が２００℃であり、粉体の進行方向に対する移動速
度が０．５ｍ／Ｈｒであると、昇温速度は４００℃／Ｈ
ｒとなる。By this treatment, the carbon concentration in silica gel is reduced to about 50 to 1000 ppm. The treated powder in which the residual carbon has almost disappeared is subsequently heated, and the temperature of the final powder is increased to 900 to 1100 ° C, preferably 950 to 1050. The heating rate at this time is usually 100 to 1000 ° C./Hr. In the rotary kiln, the powder flows substantially in a piston flow in the traveling direction, so that the temperature of the supplied powder increases as it moves in the rotary kiln in the traveling direction. Therefore, the temperature rising rate of the powder is naturally obtained from the temperature distribution in the rotary kiln and the moving speed of the powder in the traveling direction. For example, if the distance between the temperature measurement points is 1 m, the temperature difference is 200 ° C., and the moving speed of the powder in the traveling direction is 0.5 m / Hr, the heating rate is 400 ° C./H.
r.

【００２２】この温度領域に於ける加熱処理も、清浄な
空気あるいは、酸素含有ガス雰囲気下で行われる。具体
的には、炉心管の片端より清浄な空気あるいは、酸素含
有ガスを供給し、他端より排出する方法がとられる。ガ
スの供給量は、通常、連続的に供給する粉体１ｋｇ当た
り、酸素換算で３〜５０リットル／Ｈｒである。またこ
の温度領域に於ける加熱処理もロータリーキルンを用い
粉体を流動させつつ行う事が望ましい。ロータリーキル
ンを用い粉体を流動させつつ行うことにより、均一な加
熱が行われ、均質な処理粉体が得られる。この処理によ
りシリカゲルの封孔はほぼ終了し、０．７〜０．８ｇ／
ｍｌ程度であった粉体のタップ嵩密度（以後、嵩密度と
称す）は、１．０〜１．２ｇ／ｍｌ程度まで上昇する。The heat treatment in this temperature range is also performed in a clean air or oxygen-containing gas atmosphere. Specifically, a method of supplying clean air or oxygen-containing gas from one end of the core tube and discharging it from the other end is adopted. The supply amount of gas is usually 3 to 50 liter / Hr in terms of oxygen per 1 kg of powder continuously supplied. Further, it is desirable that the heat treatment in this temperature range is also carried out by using a rotary kiln while flowing the powder. By performing the process while the powder is flowing using a rotary kiln, uniform heating is performed, and a uniform processed powder is obtained. With this treatment, the sealing of the silica gel was almost completed, and 0.7-0.8 g /
The tap bulk density (hereinafter referred to as bulk density) of the powder, which was about ml, rises to about 1.0 to 1.2 g / ml.

【００２３】本発明に従いシリカゲル粉末に加熱処理を
施すと合成石英粉が得られるが、通常、シラノールが１
０００ｐｐｍ以上残存している。そこで、更に高められ
た温度領域での焼成を行う。焼成に用いる容器は、合成
石英粉への不純物のコンタミを発生させない材質、例え
ば、石英製のるつぼを用いる。この焼成に於いては、す
でに、焼成に用いる粉体中のカーボンは実質的に全量除
去されているので、昇温速度に特別な注意を払う必要は
ない。従って、容器内での昇温速度のばらつきが品質に
影響を与えないので、均質な製品が得られ、従来に比
べ、大容量の容器の使用も可能となる。また、予め、粉
体の嵩密度が十分に高められており、焼成前の粉体の嵩
密度と焼成後の粉体の嵩密度に大きな変化がなく、容器
を効率的に利用できるので、生産性の向上が計られる。When silica gel powder is subjected to heat treatment according to the present invention, synthetic quartz powder is obtained.
000 ppm or more remains. Therefore, firing is performed in a further elevated temperature range. As a container used for firing, a material that does not generate contamination of the synthetic quartz powder with impurities, for example, a crucible made of quartz is used. In this firing, it is not necessary to pay special attention to the heating rate because substantially all of the carbon in the powder used for firing has already been removed. Therefore, since the variation in the heating rate in the container does not affect the quality, a homogeneous product can be obtained, and a container having a larger capacity can be used as compared with the related art. In addition, since the bulk density of the powder has been sufficiently increased in advance, there is no significant change in the bulk density of the powder before firing and the bulk density of the powder after firing, and the container can be used efficiently, so production It is possible to improve the sex.

【００２４】焼成温度は、通常、１１００〜１３００℃
である。昇温速度は特に限定されず、１００〜２０００
℃／Ｈｒの範囲から適宜選択さる。焼成時間は、焼成温
度にもよるが、通常１０〜１００時間で、合成石英粉中
のシラノール濃度が１００ｐｐｍ以下、好ましくは、６
０ｐｐｍ以下となるまで継続される。また、加熱の際に
実質的に水分を含有しない空気、あるいは、不活性ガス
を流通しつつ行うとシラノール基の減少速度が加速され
るので好ましい。当然ながら、焼成後の合成石英粉中に
は、実質的にカーボンは存在しない。The firing temperature is usually 1100 to 1300 ° C.
It is. The heating rate is not particularly limited, and is 100 to 2000.
It is appropriately selected from the range of ° C / Hr. Although the firing time depends on the firing temperature, it is usually 10 to 100 hours, and the silanol concentration in the synthetic quartz powder is 100 ppm or less, preferably 6 hours.
It is continued until it becomes 0 ppm or less. Further, it is preferable that the heating is carried out while flowing air containing substantially no water or an inert gas, because the rate of reduction of silanol groups is accelerated. Naturally, carbon does not substantially exist in the synthetic quartz powder after firing.

【００２５】このようにして得られた合成石英粉は、成
形体に成形される。その、成形方法は、成形体の用途に
よって異なるが、例えば、用途がるつぼで有る場合には
アークメルト法が、ＩＣ用治具である場合には、一旦、
酸・水素炎によるベルヌーイ法でインゴットに成形する
方法や、炭素製の鋳型を用い真空下で加熱溶融するヒュ
ージョン法等が挙げられる。The synthetic quartz powder thus obtained is molded into a compact. The molding method differs depending on the use of the molded body. For example, when the use is a crucible, the arc melt method is used.
Examples thereof include a method of forming an ingot by a Bernoulli method using an acid / hydrogen flame, and a fusion method of heating and melting under a vacuum using a carbon mold.

【００２６】いずれにしても、本発明方法によって得ら
れた合成石英粉を用いると、泡の発生が極めて少ない成
形体が得られるので、成形体の品質及び製品歩留りが大
きく向上する。In any case, when the synthetic quartz powder obtained by the method of the present invention is used, a molded product with extremely few bubbles is obtained, so that the quality of the molded product and the product yield are greatly improved.

【００２７】[0027]

〔実施例１〕[Example 1]

（ドライシリカゲルの作成）高純度テトラメトキシシラ
ンを水と反応させ、塊状のウェットゲルを得た。続い
て、この塊状のウェットゲルを網式粉砕機で粉砕した
後、減圧下で加熱乾燥し、粉状のドライシリカゲルを得
た。この粉状のドライシリカゲルを、振動篩別機で分級
し５００μｍ以下及び１００μｍ以上の粒子を取得し
た。この粉状のドライシリカゲルを分析したところ、含
液率は１９．５重量％で、カーボン濃度は１．１重量％
であった。また、この粉状のドライシリカゲルの嵩密度
は、０．９２ｇ／ｍｌであった。(Preparation of dry silica gel) High-purity tetramethoxysilane was reacted with water to obtain a lump wet gel. Subsequently, the lump-shaped wet gel was pulverized by a net pulverizer and then dried by heating under reduced pressure to obtain powdery dry silica gel. This powdery dry silica gel was classified with a vibration sieving machine to obtain particles of 500 μm or less and 100 μm or more. Analysis of this powdery dry silica gel showed a liquid content of 19.5% by weight and a carbon concentration of 1.1% by weight.
Met. The powdery dry silica gel had a bulk density of 0.92 g / ml.

【００２８】概略を図３に示すロータリーキルンを用
い、以下の加熱処理を行った。図３中、６はドライゲル
ホッパー、７はテーブルフィーダー、８は炉心管、９は
供給口、１０は供給口ドーナツ状堰、１１は空気供給
管、１２は排出口、１３は排出口ドーナツ状堰、１４は
処理粉受器、１５は第１加熱ヒーター、１６は第２加熱
ヒーター、１７は第３加熱ヒーター、１８は第４加熱ヒ
ーター、１９は第５加熱ヒーターである。炉心管は材質
が石英で、長さ（加熱ゾーン）：２ｍ、内径：２００ｍ
ｍ、供給口ドーナツ状堰開口径：２０ｍｍ、排出口ナツ
状堰開口径： ４０ｍｍの寸法とし、最大層高が８０ｍ
ｍとなるように設定した。また、炉心管は、傾斜角度が
０．２°になるように調節した。 （加熱処理）まず、加熱ヒーターを昇温し（第１加熱ヒ
ーター：３３０℃、第２加熱ヒーター：３３０℃、第３
加熱ヒーター：４５５℃、第４加熱ヒーター：４５５
℃、第５加熱ヒーター：４５５℃）、炉心管を周速５．
０ｍ／分で回転させつつ粉状のドライシリカゲルを１１
ｋｇ／時で、空気を１００リットル／分で供給口より供
給した。The following heat treatment was performed using a rotary kiln whose outline is shown in FIG. In FIG. 3, 6 is a dry gel hopper, 7 is a table feeder, 8 is a furnace tube, 9 is a supply port, 10 is a supply port donut-shaped weir, 11 is an air supply pipe, 12 is a discharge port, and 13 is a donut-shaped discharge port. Weir, 14 is a processing powder receiver, 15 is a first heater, 16 is a second heater, 17 is a third heater, 18 is a fourth heater, and 19 is a fifth heater. The furnace tube is made of quartz, length (heating zone): 2m, inner diameter: 200m
m, opening diameter of doughnut-shaped weir at supply port: 20 mm, opening diameter of doughnut-shaped weir at discharge port: 40 mm, maximum bed height 80 m
It was set to be m. The core tube was adjusted so that the inclination angle was 0.2 °. (Heat treatment) First, the temperature of the heater is raised (first heater: 330 ° C, second heater: 330 ° C, third heater
Heater: 455 ° C, 4th heater: 455
℃, 5th heater: 455 ℃), the peripheral speed of the core tube 5.
While rotating at 0 m / min, powdery dry silica gel 11
Air was supplied at 100 l / min from the supply port at kg / hr.

【００２９】炉心管内の粉体は、連続して、終始流動し
ていた。各加熱ゾーンの粉体の温度は、第１加熱ヒータ
ー部：１１０℃、第２加熱ヒーター部：１３５℃、第３
加熱ヒーター部：２６５℃、第４加熱ヒーター部：４３
３℃、第５加熱ヒーター部：４６４℃であった。粉体温
度が３００℃以下のゾーンの、ガスの発生量は、３１０
N-リットル／Ｋｇ・Hrであった。また、粉体温度が３０
０〜４３０℃のゾーンの長さは、３０ｃｍであった。さ
らに、粉体温度が４５０〜４６４℃のゾーンの通過時間
は、0.6時間であった。次に、供給操作開始後、４、
６、８時間目に排出された粉を分析したところ、表１に
示す値であった。The powder in the core tube was continuously flowing all the time. The temperature of the powder in each heating zone is as follows: 1st heating heater part: 110 ° C, 2nd heating heater part: 135 ° C, 3rd
Heating heater part: 265 ° C, 4th heating heater part: 43
It was 3 degreeC and the 5th heater part: 464 degreeC. The amount of gas generated in the zone where the powder temperature is 300 ° C. or lower is 310
It was N-liter / Kg · Hr. Also, the powder temperature is 30
The length of the zone from 0 to 430 ° C was 30 cm. Further, the passage time through the zone where the powder temperature was 450 to 464 ° C. was 0.6 hours. Next, after starting the supply operation,
When the powder discharged at 6th and 8th hours was analyzed, the values shown in Table 1 were obtained.

【００３０】[0030]

【表１】 [Table 1]

【００３１】表１から判るように、粉体の分析値は安定
していた。続いて、同じロータリーキルンを用い、上記
操作で得られた粉を、以下に示件で加熱処理した。第１
加熱ヒーター：５００℃、第２加熱ヒーター：５００
℃、第３加熱ヒーター：５００℃、第４加熱ヒーター：
１０００℃、第５加熱ヒーター：１０３０℃に昇温し、
炉心管を周速５．０ｍ／分で回転させつつ、粉体を９．
２ｋｇ／Ｈｒで、空気を１１０リットル／分で供給口よ
り供給した。As can be seen from Table 1, the analytical values of the powder were stable. Then, using the same rotary kiln, the powder obtained by the above operation was heat-treated under the following conditions. First
Heating heater: 500 ° C, Second heating heater: 500
℃, 3rd heater: 500 ℃, 4th heater:
1000 ° C, 5th heater: heated to 1030 ° C,
While rotating the core tube at a peripheral speed of 5.0 m / min, the powder was mixed with 9.
Air was supplied from the supply port at 110 kg / min at 2 kg / hr.

【００３２】加熱処理の粉体の最終温度は、１０２０℃
であった。炉心管内の粉体は、連続して、終始流動して
いた。供給操作開始後、４、６、８時間目に排出された
合成石英粉を分析したところ、表２に示す値であった。The final temperature of the heat-treated powder is 1020 ° C.
Met. The powder in the furnace tube was flowing continuously and continuously. When the synthetic quartz powder discharged at 4, 6, and 8 hours after the start of the supply operation was analyzed, the values shown in Table 2 were obtained.

【００３３】[0033]

【表２】 [Table 2]

【００３４】（焼成）加熱処理で得られた合成石英粉１
３０ｋｇを直径５５０ｍｍの石英るつぼに仕込み、電気
炉内で加熱し焼成を行った。炉は昇温速度 ２００℃／
Ｈｒで到達温度１２００℃まで昇温後、同温度で４０時
間保持した。この際、るつぼに、露点が−６０℃の清浄
な乾燥空気を７８０リットル／Ｈｒで流通した。保持終
了後、加熱を停止し、室温まで冷却した。冷却の際にも
清浄な乾燥空気は流通した。焼成後られた合成石英粉
は、１１２ｋｇであった。得られた合成石英粉を、サン
プリング場所毎に分析したところ表３に示す値であっ
た。(Baking) Synthetic quartz powder 1 obtained by heat treatment
30 kg was charged into a quartz crucible having a diameter of 550 mm, and heated and fired in an electric furnace. Furnace heating rate 200 ℃ /
After the temperature was increased to an ultimate temperature of 1200 ° C. with Hr, the temperature was maintained at the same temperature for 40 hours. At this time, clean dry air having a dew point of −60 ° C. was passed through the crucible at 780 liters / hr. After the completion of the holding, the heating was stopped and the temperature was cooled to room temperature. During the cooling, clean dry air circulated. The calcined synthetic quartz powder weighed 112 kg. When the obtained synthetic quartz powder was analyzed for each sampling location, the values shown in Table 3 were obtained.

【００３５】[0035]

【表３】 [Table 3]

【００３６】（成形）焼成で得られた合成石英粉を、ベ
ルヌーイ法でインゴットに成形した。インゴット１０ｇ
中に、１０μｍの泡が４個検出された。 〔実施例２〕炉心管の回転速度を２．５ｍ／分にした以
外は実施例１と同様に操作を行った。加熱処理で得られ
た粉体中の黒色粒子数は、２個／１０ｇであった。ま
た、ベルヌーイ法で成形したインゴット１０ｇ中に、１
０μｍ以上まの泡が６個検出された。 〔比較例１〕炉心管の回転速度を１．３ｍ／分にした以
外は、実施例１と同様に操作を行った。加熱処理で得ら
れた粉体中の黒色粒子数は６個／１０ｇであった。ま
た、ベルヌーイ法で成形したインゴット１０ｇ中に１０
μｍ以上の泡が３０個検出された。(Molding) The synthetic quartz powder obtained by firing was molded into an ingot by the Bernoulli method. Ingot 10g
Four 10 μm bubbles were detected therein. [Example 2] The same operation as in Example 1 was performed except that the rotation speed of the core tube was set to 2.5 m / min. The number of black particles in the powder obtained by the heat treatment was 2/10 g. Moreover, in 10 g of the ingot formed by the Bernoulli method, 1
Six bubbles of 0 μm or more were detected. [Comparative Example 1] The same operation as in Example 1 was performed except that the rotational speed of the core tube was set to 1.3 m / min. The number of black particles in the powder obtained by the heat treatment was 6/10 g. Also, 10 in 10g of the ingot formed by Bernoulli method
30 bubbles having a size of μm or more were detected.

【００３７】[0037]

【発明の効果】本発明により、溶融時に発泡の原因とな
る残存カーボン量の少ない合成石英粉を容易に得ること
ができる。According to the present invention, it is possible to easily obtain a synthetic quartz powder having a small amount of residual carbon which causes foaming during melting.

【図面の簡単な説明】[Brief description of the drawings]

【図１】粉体を仕込んだ静止状態のロータリーキルンの
断面図FIG. 1 is a cross-sectional view of a stationary rotary kiln charged with powder.

【図２】仕込んだ粉体が流動状態にある、回転状態のロ
ータリーキルンの断面図FIG. 2 is a cross-sectional view of a rotating rotary kiln in which charged powder is in a flowing state.

【図３】本発明に用いることのできるロータリーキルン
の概略を示す図FIG. 3 is a diagram schematically showing a rotary kiln that can be used in the present invention.

【符号の説明】[Explanation of symbols]

１：粉体 ２：炉心管 ３：接粉面 ４：炉心管内の空隙 ５：粉体表面 ６：ドライゲルホッパー ７：テーブルフィーダー ８：炉心管 ９：供給口 １０：供給口ドーナツ状堰 １１：空気供給管 １２：排出口 １３：排出口ドーナツ状堰 １４：処理粉受器 １５：第１加熱ヒーター １６：第２加熱ヒーター １７：第３加熱ヒーター １８：第４加熱ヒーター １９：第５加熱ヒーター 1: powder 2: furnace tube 3: powder contact surface 4: void in furnace tube 5: powder surface 6: dry gel hopper 7: table feeder 8: furnace tube 9: supply port 10: supply port donut weir 11: Air supply pipe 12: Outlet 13: Outlet donut-shaped weir 14: Processing powder receiver 15: First heater 16: Second heater 17: Third heater 18: Fourth heater 19: Fifth heater

Claims (6)

【特許請求の範囲】[Claims] 【請求項１】 シリカゲル粉末を、ロータリーキルンの
片端より連続的に供給しつつ、流動させながら加熱処理
することにより合成石英粉を製造する方法であって、ロ
ータリーキルンの炉心管を周速２ｍ／分〜１２ｍ／分で
回転させることを特徴とする合成石英粉の製造方法。1. A method for producing synthetic quartz powder by continuously supplying silica gel powder from one end of a rotary kiln and heating while flowing, wherein the furnace core tube of the rotary kiln has a peripheral speed of 2 m / min. A method for producing synthetic quartz powder, which comprises rotating at 12 m / min. 【請求項２】 加熱処理の最終温度が９００〜１１００
℃である請求項１記載の合成石英粉の製造方法。2. The final temperature of the heat treatment is 900 to 1100.
The method for producing a synthetic quartz powder according to claim 1, wherein the temperature is 0 ° C. 【請求項３】 加熱処理を１１００℃以下で行った後、
更に１１００℃を超える温度で焼成する請求項１又は２
に記載の合成石英粉の製造方法。3. After the heat treatment is performed at 1100 ° C. or lower,
Further, firing is performed at a temperature exceeding 1100 ° C.
The method for producing the synthetic quartz powder according to 1. 【請求項４】 多段のロータリーキルンを用いて行う請
求項１乃至３のいずれかに記載の製造方法。4. The manufacturing method according to claim 1, which is carried out using a multistage rotary kiln. 【請求項５】 ロータリーキルンの炉心管材質が石英で
ある請求項１乃至４のいずれかに記載の合成石英粉の製
造方法。5. The method for producing synthetic quartz powder according to claim 1, wherein the material of the core tube of the rotary kiln is quartz. 【請求項６】 シリカゲル粉末がテトラアルコキシシラ
ンの加水分解により得られたものである請求項１乃至５
のいずれかに記載の合成石英粉の製造方法。6. The silica gel powder is obtained by hydrolysis of tetraalkoxysilane.
5. The method for producing synthetic quartz powder according to any one of 1.
JP33019995A 1995-12-19 1995-12-19 Production of synthetic quartz powder Pending JPH09165214A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP33019995A JPH09165214A (en) 1995-12-19 1995-12-19 Production of synthetic quartz powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP33019995A JPH09165214A (en) 1995-12-19 1995-12-19 Production of synthetic quartz powder

Publications (1)

Publication Number Publication Date
JPH09165214A true JPH09165214A (en) 1997-06-24

Family

ID=18229950

Family Applications (1)

Application Number Title Priority Date Filing Date
JP33019995A Pending JPH09165214A (en) 1995-12-19 1995-12-19 Production of synthetic quartz powder

Country Status (1)

Country Link
JP (1) JPH09165214A (en)

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JP2009222309A (en) * 2008-03-17 2009-10-01 Akami Seisakusho:Kk Heat treatment method and heat treatment device
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EP1088789A2 (en) * 1999-09-28 2001-04-04 Heraeus Quarzglas GmbH & Co. KG Porous silica granule, its method of production and its use in a method for producing quartz glass
EP1088789A3 (en) * 1999-09-28 2002-03-27 Heraeus Quarzglas GmbH & Co. KG Porous silica granule, its method of production and its use in a method for producing quartz glass
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CN103153887A (en) * 2010-10-28 2013-06-12 赫罗伊斯石英玻璃股份有限两合公司 Method for producing synthetic quartz glass granules
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US10676388B2 (en) 2015-12-18 2020-06-09 Heraeus Quarzglas Gmbh & Co. Kg Glass fibers and pre-forms made of homogeneous quartz glass
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US11053152B2 (en) 2015-12-18 2021-07-06 Heraeus Quarzglas Gmbh & Co. Kg Spray granulation of silicon dioxide in the preparation of quartz glass
US11236002B2 (en) 2015-12-18 2022-02-01 Heraeus Quarzglas Gmbh & Co. Kg Preparation of an opaque quartz glass body
US11299417B2 (en) 2015-12-18 2022-04-12 Heraeus Quarzglas Gmbh & Co. Kg Preparation of a quartz glass body in a melting crucible of refractory metal
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