JP3327364B2 - Method for producing silica glass processed product - Google Patents

Method for producing silica glass processed product

Info

Publication number
JP3327364B2
JP3327364B2 JP21317994A JP21317994A JP3327364B2 JP 3327364 B2 JP3327364 B2 JP 3327364B2 JP 21317994 A JP21317994 A JP 21317994A JP 21317994 A JP21317994 A JP 21317994A JP 3327364 B2 JP3327364 B2 JP 3327364B2
Authority
JP
Japan
Prior art keywords
powder
silica glass
heated
tube
silica
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.)
Expired - Fee Related
Application number
JP21317994A
Other languages
Japanese (ja)
Other versions
JPH0859261A (en
Inventor
司 坂口
茂 山形
昇 鈴木
正則 鈴木
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.)
Shin Etsu Quartz Products Co Ltd
Original Assignee
Shin Etsu Quartz Products Co Ltd
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 Shin Etsu Quartz Products Co Ltd filed Critical Shin Etsu Quartz Products Co Ltd
Priority to JP21317994A priority Critical patent/JP3327364B2/en
Publication of JPH0859261A publication Critical patent/JPH0859261A/en
Application granted granted Critical
Publication of JP3327364B2 publication Critical patent/JP3327364B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B23/00Re-forming shaped glass
    • C03B23/20Uniting glass pieces by fusing without substantial reshaping
    • C03B23/207Uniting glass rods, glass tubes, or hollow glassware
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/09Other methods of shaping glass by fusing powdered glass in a shaping mould

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は、シリカガラスを原材と
し所定寸法のシリカガラス加工品を容易かつ安価に製造
することができる発明に関するものであり、例えば熱電
対用絶縁管,各種センサー用保護管,ガラスバーナーの
火口,バブラー管,理化学機器部材,ガス配管を兼ねた
熱処理用治具材,半導体熱処理治具用部材等として利用
されるシリカガラス加工品の発明に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an invention capable of easily and inexpensively manufacturing a processed silica glass product having a predetermined size from silica glass as a raw material. The present invention relates to an invention of a processed silica glass product used as a protective tube, a crater of a glass burner, a bubbler tube, a member for physical and chemical equipment, a heat treatment jig material also serving as a gas pipe, a member for a semiconductor heat treatment jig, and the like.

【0002】[0002]

【従来の技術】従来よりウエーハの熱処理装置内に組込
まれる半導体治具として化学的安定性が高く、耐熱性を
有するシリカガラス製治具を用いており、この種の治具
に用いる材料に対していずれも高純度で高寸法精度とと
もに、ローコストで品質のバラツキのない製造方法が要
求される。そして、これらの治具を加工するためのバー
ナ若しくは酸水素炎加水分解法にて合成石英を製造する
ためのバーナもシリカガラスで形成されているが、かか
るバーナは太径の外管内にガス吹き出し口を構成する複
数の内管が挿設する構成をなすが、間隔保持部材を介し
て前記内管を気密的且つ精度よく外管に溶接するのは中
々困難である。
2. Description of the Related Art Conventionally, a silica glass jig having high chemical stability and heat resistance has been used as a semiconductor jig incorporated in a wafer heat treatment apparatus. All of them require a high-purity, high-dimensional accuracy, low-cost, and quality-free manufacturing method. Burners for processing these jigs or burners for producing synthetic quartz by oxyhydrogen flame hydrolysis are also formed of silica glass, but such burners blow gas into a large-diameter outer tube. Although a configuration is made in which a plurality of inner tubes constituting the mouth are inserted, it is difficult to hermetically and accurately weld the inner tube to the outer tube via a spacing member.

【0003】一方近年高温雰囲気下で温度やガス濃度等
を検知するセンサにおいては、絶縁性と耐熱性の向上を
図るために軸方向に多数の軸穴が穿孔された多穴シリカ
ガラスロッド内に前記センサを挿設したセンサ装置が開
発されているが、かかるセンサ用多穴シリカガラスロッ
ドにおいては、センサよりの検出信号のノイズ防止の為
に不純物の混入のない高純度で且つ高寸法精度のロッド
が必要である。
On the other hand, in recent years, in a sensor for detecting a temperature, a gas concentration, and the like in a high-temperature atmosphere, a multi-hole silica glass rod having a large number of axial holes formed in an axial direction in order to improve insulation and heat resistance. A sensor device in which the sensor is inserted has been developed. In such a multi-hole silica glass rod for a sensor, in order to prevent noise of a detection signal from the sensor, high purity and high dimensional accuracy without impurities are mixed. A rod is required.

【0004】従来この様な用途の多穴シリカガラスチュ
ーブを作るためには、数本のチューブを準備した後これ
を溶接して一体化する方法を採用していた。従ってコス
トは大きなものとなっていた。
Conventionally, in order to produce a multi-hole silica glass tube for such an application, a method of preparing several tubes and then welding them to integrate them has been adopted. Therefore, the cost was large.

【0005】又シリコンウエーハその他の半導体熱処理
治具用各種部材を洗浄する際に用いられるバブリング洗
浄装置や、すす状合成シリカガラスを高純度液体原料か
ら製造する際に、原料液体をバブリングする為に使用さ
れるバブリング気化装置においては、太径の外管内に多
数の内管を挿設したものや、シリカガラスのむく棒を機
械加工にて多数の小孔を穿孔したバブラ管が開発されて
いるが、かかるバブラ管も前記小孔を溶接若しくは機械
加工で形成せねばならず、これらの方法についても次の
様な問題が生じるのを避けられない。
A bubbling cleaning device used for cleaning silicon wafers and other members for semiconductor heat treatment jigs, and a method for bubbling a raw material liquid when producing soot-like synthetic silica glass from a high-purity liquid raw material. Among the used bubbling vaporizers, a large number of inner tubes are inserted into a large-diameter outer tube, and a bubbler tube in which a number of small holes are perforated by machining a solid bar of silica glass has been developed. However, in such a bubbler tube, the small holes must be formed by welding or machining, and the following problems cannot be avoided in these methods.

【0006】[0006]

【発明が解決しようとする課題】即ち機械加工による方
法では、塊状シリカガラスから切削、レーザー加工等に
よりシリカガラス加工品を製造しているが、かかる方法
ではシリカガラスが脆性材料であるために前記切削によ
る剪断加工による亀裂、破壊等が生じやすいのみなら
ず、切削治具等からの汚染が起こる。更に切削加工では
ドリル長さに限界を有し、特に長尺の多穴シリカガラス
を作ることができない。又多穴シリカガラスの場合、微
細穴寸法の多穴シリカガラスを作ることができないのみ
ならず、各種寸法、形状の多穴シリカガラスを連続的に
作ることができない。
That is, in the method by machining, a processed silica glass product is manufactured from bulk silica glass by cutting, laser processing, or the like. However, in this method, silica glass is a brittle material, so Not only are cracks and breakage easily caused by shearing due to cutting, but also contamination from cutting jigs and the like occurs. Furthermore, the cutting process has a limitation on the drill length, and in particular, a long multi-hole silica glass cannot be produced. In the case of a multi-hole silica glass, not only cannot a multi-hole silica glass having a fine hole size be produced, but also a multi-hole silica glass having various dimensions and shapes cannot be continuously produced.

【0007】かかる欠点を解消する為に、加熱成形法或
いは加熱加圧成形による加工方法も提案されている。即
ち、カーボン等で作成された鋳型内にシリカ粉を充填
し、あるいは塊状体をいれ、加熱成形若しくは加熱加圧
成形により所定形状のシリカガラス加工品を製造する方
法もあるが、かかる成形方法では寸法制御が正確に行な
えない。又多穴シリカガラス加工品の場合、各種寸法、
形状の多穴シリカガラスを連続的に作ることができない
のみならず、炉からの汚染が起こる等の問題が生じる。
[0007] In order to solve such a drawback, a processing method by heat molding or heat and pressure molding has been proposed. That is, there is a method of filling a silica powder in a mold made of carbon or the like, or putting a lump, and manufacturing a silica glass processed product of a predetermined shape by heat molding or heat and pressure molding. Dimension control cannot be performed accurately. In the case of multi-hole silica glass products, various dimensions,
Not only cannot the shape of the multi-hole silica glass be continuously produced, but also problems such as contamination from the furnace occur.

【0008】本発明はかかる技術的課題に鑑み、シリカ
粉体原料からシリカガラス加工品を作成するにあたり、
欠け、亀裂がなく高寸法精度のシリカガラス加工品の製
造方法を提供することを目的とする。本発明の他の目的
は、製造したシリカガラス加工品表面、特に多穴シリカ
ガラス加工品の場合穴内表面に荒れ、傷等がなく、更に
は連続的に製造可能なシリカガラス加工品の製造方法を
提供することにある。本発明の他の目的は、製造過程に
おいて不純物の汚染が生じる事なく、原材料と同様に高
純度の維持を図ったシリカガラス加工品の製造方法を提
供することにある。
[0008] In view of the above technical problems, the present invention provides a method for producing a processed silica glass product from a silica powder raw material.
An object of the present invention is to provide a method for producing a processed silica glass product having high dimensional accuracy without chipping or cracking. Another object of the present invention is to provide a method for producing a processed silica glass product which can be continuously produced without roughening, flaws, etc. on the surface of the manufactured silica glass processed product, particularly in the case of a multi-hole silica glass processed product. Is to provide. Another object of the present invention is to provide a method for producing a processed silica glass article which maintains high purity similarly to the raw material without causing contamination of impurities in the production process.

【0009】本発明の他の目的は、長尺寸法の多穴シリ
カガラス、厚さ数mmの板状体から、長さ10mのロッ
ド、又数10m長のファイバーのように、軸方向に延在
する形状であれば任意のプロフィル形状を任意に生成し
得るシリカガラス加工品の製造方法を提供することにあ
る。
Another object of the present invention is to provide a multi-hole silica glass having a long dimension, a plate having a thickness of several mm, and extending in the axial direction such as a rod having a length of 10 m or a fiber having a length of several tens m. It is an object of the present invention to provide a method for producing a processed silica glass article that can arbitrarily generate an arbitrary profile shape as long as the shape exists.

【0010】本発明の他の目的は、小口径から大口径の
多穴シリカガラス加工品を容易に且つ任意に作成可能な
シリカガラス加工品の製造方法を提供することを目的と
する。本発明の他の目的は、例えば熱電対用絶縁管,各
種センサー用保護管,ガラスバーナーの火口,バブラー
管,理化学機器部材,ガス配管を兼ねた熱処理用治具
材,半導体熱処理治具用部材等として適用されるシリカ
ガラス加工品を容易かつ安価に製造することができる製
造方法を提供する事にある。
Another object of the present invention is to provide a method for producing a processed silica glass article which can easily and arbitrarily produce a multi-hole silica glass processed article having a small diameter to a large diameter. Another object of the present invention is to provide, for example, a thermocouple insulating tube, a protective tube for various sensors, a crater of a glass burner, a bubbler tube, a physicochemical device member, a heat treatment jig material also serving as a gas pipe, and a member for a semiconductor heat treatment jig. It is an object of the present invention to provide a manufacturing method capable of easily and inexpensively manufacturing a processed silica glass product applied as the above.

【0011】[0011]

【課題を解決する為の手段】請求項1記載の発明は、ロ
ッド内に一又は複数の小孔を存在させているシリカガラ
ス加工品に適用されるもので、その特徴とするところ
は、任意の断面形状が軸方向に延在する中空シリカガラ
ス外管内に、円または多角形の断面形状が軸方向に延在
するシリカガラス内管を一または複数本挿入して管状被
加熱体を作成した後、この被加熱体内の外管と内管との
間隙先端より、粒径を50〜500ミクロンに調整した
合成シリカ粉からなる非晶質シリカ粉を主成分とする粉
状体を充填しその後に水晶粉その他の結晶質シリカ粉を
主成分とする粉状体を充填して、前記シリカ粉を充填し
た被加熱体の外管と内管の間を減圧下にかつ内管内を正
圧開放した状態で、前記被加熱体を先端側より帯域加熱
にて軸方向に沿って加熱溶融させて延伸一体化してなる
事を特徴とするものである。
Means for Solving the Problems The invention described in claim 1 is applied to a processed silica glass product having one or more small holes in a rod. A tubular heated object was prepared by inserting one or more silica glass inner tubes having a circular or polygonal cross-sectional shape extending in the axial direction into a hollow silica glass outer tube having a cross-sectional shape extending in the axial direction. Thereafter, the particle size was adjusted to 50 to 500 microns from the tip of the gap between the outer tube and the inner tube in the object to be heated .
Filled with a powder mainly composed of amorphous silica powder composed of synthetic silica powder, and then filled with a powder composed mainly of quartz powder or other crystalline silica powder, and filled with the silica powder. Reduce the pressure between the outer and inner pipes of the
In a state where the pressure is released, the object to be heated is heated and melted along the axial direction by zone heating from the front end side and stretched and integrated.

【0012】請求項2記載の発明は、ロッド内に複数の
小孔を存在させているシリカガラス加工品(以下多穴チ
ューブという)に適用されるもので、任意の断面形状が
軸方向に延在する中空シリカガラス外管内に、円または
多角形の断面形状が軸方向に延在するシリカガラス内管
を複数本挿入して管状被加熱体を作成した後、この被加
熱体内の外管と内管との間隙の少なくとも一部にシリカ
粉を充填して、前記シリカ粉を充填した被加熱体の外管
と内管の間を減圧下にかつ内管内を正圧開放した状態
、該被加熱体を先端側より帯域加熱にて軸方向に沿っ
て加熱溶融させて一体化して、ロッド内に複数の小孔を
存在させてなる多穴チューブを製造する事を特徴とす
る。この場合多穴チューブを製造する為に、この被加熱
体内の外管と内管との間隙の均一にシリカガラスが充填
されるべき部位にシリカ粉を充填させることにより、該
シリカ粉が前記帯域加熱により外管と内管の間が間隙な
く一体化させてもよく、好ましくは 前記被加熱体の内
管と外管の間隙先端より、粒径を50〜500ミクロン
に調整した合成シリカ粉からなる非晶質シリカ粉を主成
分とする粉状体を充填しその後に水晶粉その他の結晶質
シリカ粉を主成分とする粉状体を充填してなるのがよ
い。
[0012] The invention according to claim 2 is applied to a processed silica glass product having a plurality of small holes in a rod (hereinafter referred to as a multi-hole tube), and an arbitrary cross-sectional shape extends in the axial direction. After inserting a plurality of silica glass inner tubes having a circular or polygonal cross-sectional shape extending in the axial direction into the existing hollow silica glass outer tube to form a tubular body to be heated, the outer tube in the body to be heated is formed. At least a portion of the gap between the inner tube and the inner tube is filled with silica powder, and the outer tube of the body to be heated filled with the silica powder is filled.
With a reduced pressure between the inner tube and the inner tube and a positive pressure open inside the inner tube
Then, the object to be heated is heated and melted along the axial direction by zone heating from the distal end side and integrated to produce a multi-hole tube having a plurality of small holes in the rod. . In this case, in order to manufacture a multi-hole tube, a portion of the gap between the outer tube and the inner tube in the body to be heated, which is to be uniformly filled with silica glass, is filled with silica powder. The outer tube and the inner tube may be integrated by heating without a gap. Preferably, the particle size is 50 to 500 microns from the tip of the gap between the inner tube and the outer tube of the object to be heated.
It is preferable to fill a powder containing amorphous silica powder as a main component composed of a synthetic silica powder adjusted to a powder, and then to fill a powder containing quartz powder or other crystalline silica powder as a main component. .

【0013】[0013]

【0014】更に、前記被加熱体の外管と内管との間の
間隙先端より、非晶質シリカ粉を主成分とする粉状体を
充填後に水晶粉その他の結晶質シリカ粉を主成分とする
粉状体を充填する場合、好ましくは結晶質シリカの粒径
が10〜1000μmの範囲、かつ10μm未満の微粒
子含有比率が0.1wt%以下であるのがよい。
Further, after filling a powdery material containing amorphous silica powder as a main component from the tip of the gap between the outer tube and the inner tube of the object to be heated, quartz powder or other crystalline silica powder is added as a main component. When the powdery material is filled, it is preferable that the particle size of the crystalline silica is in the range of 10 to 1000 μm and the content ratio of fine particles having a particle size of less than 10 μm is 0.1 wt% or less.

【0015】このようにシリカ粉を特定した理由は次の
通りである。前記均一にシリカガラスを充填させる部位
に非晶質シリカ粉を充填して帯域溶融を行うと、このよ
うな非晶質シリカ粉はいわゆるメルティングポイントと
いうものがなく、1600℃前後より徐々に軟化溶融し
ていくものであるために、シリカ粉よりの析出ガス等が
巻き込まれ気泡が残存したシリカガラス体が形成されて
しまうことになる。
The reason for specifying the silica powder in this way is as follows. When the zone where the silica glass is uniformly filled is filled with amorphous silica powder and zone melting is performed, such an amorphous silica powder has no so-called melting point and gradually softens from around 1600 ° C. Because of melting, a deposition gas or the like from the silica powder is entrained, and a silica glass body in which bubbles remain is formed.

【0016】一方水晶粉等の結晶質シリカ粉は1730
℃にメルティングポイントを有する為に1730℃以上
に加熱する事により一気に溶融し、溶融ガラス内の気泡
発生を極力抑える事が出来るが、水晶粉等の結晶質シリ
カ粉は、573℃にα型からβ型への転移点を有するた
めに、加熱開始時に管状被加熱体の粘度が低下する前に
該管状被加熱体内部の水晶粉のα型からβ型への転移に
よる急激な膨張により管状被加熱体の破壊が生じてしま
う。
On the other hand, crystalline silica powder such as quartz powder is 1730
Since it has a melting point at ℃, it can be melted at once by heating to 1730 ℃ or more, and the generation of bubbles in the molten glass can be suppressed as much as possible. However, crystalline silica powder such as quartz powder has α-type at 573 ℃. To have a transition point from the β-type to the tubular-heated body at the start of heating before the viscosity of the tubular-heated body is reduced. The object to be heated is destroyed.

【0017】そこで本発明は、最初に帯域加熱される先
端側に、転移点のない非晶質シリカ粉を主成分とする粉
状体を存在させるために、α型からβ型への転移が存在
管の破壊を阻止させつつ、その上方域の既にヒートゾー
ンの予熱により中空管の粘度が低下し、その部分の結晶
質シリカ粉がα型からβ型への転移による急激な膨張が
生じても管の破壊を阻止し得る区域にのみ水晶粉等の結
晶質シリカ粉を充填している。尚、前記非晶質シリカ粉
の充填幅は、帯域加熱手段のヒートゾーン(均熱幅)よ
り大である事が必要であるが、余りに大きいと実質的な
無気泡域が少なくなり生産性が低下するために、好まし
くは粉状体の全充填量の20%未満がよい。
Accordingly, the present invention provides a method for converting α-type to β-type by providing a powdery material mainly composed of amorphous silica powder having no transition point on the tip side where the zone is heated first. While preventing the existing tube from breaking, the viscosity of the hollow tube decreases due to the preheating of the heat zone already in the upper region, and the crystalline silica powder in that portion undergoes rapid expansion due to the transition from α-type to β-type. The crystalline silica powder such as quartz powder is filled only in the area where the tube can be prevented from being broken. It is necessary that the filling width of the amorphous silica powder is larger than the heat zone (soaking width) of the zone heating means. However, if it is too large, a substantial bubble-free area is reduced, and productivity is reduced. In order to reduce the content, the content is preferably less than 20% of the total filling amount of the powder.

【0018】尚前記結晶質シリカ粉は、天然水晶粉、合
成水晶粉、合成クリストバライト粉のいずれかの結晶質
シリカであり、粒径が10〜1000μm、好ましくは
20〜500μm、より好ましくは50〜200μmの
範囲で、かつ10μm未満の微粒子含有比率が0.1w
t%以下である事が必要がある。けだし、前記粒径が1
0μm未満では、例え真空引きしても圧損が生ずるため
充填域内部まで真空にする事が出来ず、又帯域溶融でも
気泡がぬけにくくなってしまい、溶融したシリカガラス
中に気泡が多量に含まれてしまい、且つ断熱効果により
管状被加熱体中心部の均一な加熱溶融が困難になる。粒
径が1000μm以上では、溶融時均一にならなかった
り、同様に例え水晶粉を用いても粉体間の空隙が広いこ
とにより気泡の発生を解消出来ない。
The crystalline silica powder is any one of a natural quartz powder, a synthetic quartz powder and a synthetic cristobalite powder, and has a particle diameter of 10 to 1000 μm, preferably 20 to 500 μm, more preferably 50 to 500 μm. The content ratio of fine particles in the range of 200 μm and less than 10 μm is 0.1 w
It must be less than t%. The particle size is 1
If the thickness is less than 0 μm, even if a vacuum is applied, a pressure loss occurs, so that the inside of the filling region cannot be evacuated, and even if the zone is melted, bubbles are difficult to be removed, and a large amount of bubbles are contained in the fused silica glass. In addition, the heat insulation effect makes it difficult to uniformly heat and melt the central portion of the tubular object to be heated. If the particle diameter is 1000 μm or more, uniformity cannot be achieved during melting, and similarly, even if quartz powder is used, the generation of bubbles cannot be eliminated due to wide voids between the powders.

【0019】又シリカ粉の充填は管状被加熱体の粉体充
填域下端には先ず非晶質シリカ粉を充填し、次いで非晶
質シリカ粉と結晶質シリカ粉との混合粉を充填した後
に、最後に前記結晶質シリカ粉を充填するのがよい。
The silica powder is filled by filling the lower end of the powder-filled area of the tubular body with amorphous silica powder first, and then filling a mixed powder of amorphous silica powder and crystalline silica powder. Finally, the crystalline silica powder is preferably filled.

【0020】尚、高純度のロッドを製造する場合、前記
の様に天然の結晶質シリカ粉を用いる事が出来ない場合
がある。この様な場合は、前記高純度合成非晶質シリカ
粉をあらかじめ水素含有雰囲気若しくはヘリウム含有雰
囲気にて加熱処理を行なった後に充填するのがよい。こ
の結果、前記帯域溶融時に水素やヘリウムからなる残留
ガスが存在しても溶融時にこれらが溶融ガラス中に吸蔵
/ドープされ、気泡の発生を阻止でき、合成シリカガラ
スのように高純度非晶質シリカ粉を用いても実質的に無
気泡なシリカガラスロッドが製造できる。
When a high-purity rod is manufactured, natural crystalline silica powder may not be used as described above. In such a case, the high-purity synthetic amorphous silica powder is preferably filled after a heat treatment in a hydrogen-containing atmosphere or a helium-containing atmosphere in advance. As a result, even if residual gases consisting of hydrogen and helium are present during the zone melting, they are occluded / doped in the molten glass at the time of melting, and the generation of bubbles can be prevented. Even if silica powder is used, a substantially glass-free silica glass rod can be produced.

【0021】又、前記シリカ粉にはあらかじめ金属若し
くは金属元素化合物粉が混合してなるシリカ粉を用いて
もよい。この場合加熱溶融時の粉状充填域の減圧雰囲気
は1KPa以下の真空にすることにより気体の巻き込み
も膨張も防ぐことが出来、好ましい。
The silica powder may be a silica powder obtained by mixing a metal or metal element compound powder in advance. In this case, it is preferable that the depressurized atmosphere in the powdery filling region at the time of heating and melting is set to a vacuum of 1 KPa or less so that entrainment and expansion of gas can be prevented.

【0022】尚、本発明の多穴むく棒シリカロッドは、
熱電対用絶縁管,センサー用保護管,封止部材,ガラス
バーナー火口,バブラー管,理化学機器用部材及び半導
体熱処理治具用部材として適用される。
Incidentally, the multi-hole silica rod of the present invention comprises:
It is applied as a thermocouple insulating tube, a sensor protection tube, a sealing member, a glass burner crater, a bubbler tube, a member for physical and chemical equipment, and a member for a semiconductor heat treatment jig.

【0023】[0023]

【実施例】以下、本発明の実施例を例示的に詳しく説明
する。但しこの実施例に記載されている構成部品の、材
質、形状、分析値などは特に特定的な記載がない限り
は、この発明の範囲をそれのみに限定する趣旨ではなく
単なる説明例に過ぎない。
DESCRIPTION OF THE PREFERRED EMBODIMENTS The embodiments of the present invention will be illustratively described in detail below. However, the materials, shapes, analytical values, and the like of the components described in this embodiment are not intended to limit the scope of the present invention thereto, but are merely illustrative examples, unless otherwise specified. .

【0024】先ず、多穴むく棒状の熱電対用ダブルボア
管の製造手順を図1乃至図3に従って説明する。 (1)シリカガラス製の外管、略管状体(以下内管とい
う)等の用意 図2に示すように直径40mm、肉厚1.5mm、長さ
1.2mのシリカガラス製外管1および、内部に挿入す
る為の直径15mm、肉厚1.5mm、長さ1mのシリ
カガラス製内管2を2本を作成した。又、直径40m
m、中央に直径15mmの穴3aを対称に2つ開けた加
工寸法精度±0.1mmの円板状のシリカガラス板(底
板3)と、同様な外径で中央にガス抜き穴5aを開けた
シリカガラス板(ガス抜き用蓋板5)、及び直径を37
mmとし、中央に直径15mmの穴6bを対称に2つ開
けるとともに、上下両側にガス抜き穴6aを設けたシリ
カガラス板(中板6)を各1枚ずつ用意した。
First, the procedure for manufacturing a multi-hole, rod-shaped double bore tube for a thermocouple will be described with reference to FIGS. (1) Preparation of silica glass outer tube, substantially tubular body (hereinafter referred to as inner tube), etc. As shown in FIG. 2, silica glass outer tube 1 having a diameter of 40 mm, a wall thickness of 1.5 mm, and a length of 1.2 m, and Two inner tubes 2 made of silica glass having a diameter of 15 mm, a thickness of 1.5 mm, and a length of 1 m for insertion into the inside were prepared. Also, diameter 40m
m, a disk-shaped silica glass plate (bottom plate 3) with a processing dimension accuracy of ± 0.1 mm in which two holes 3a each having a diameter of 15 mm are formed symmetrically in the center, and a gas vent hole 5a in the center with the same outer diameter. Silica glass plate (cover plate 5 for degassing) and a diameter of 37
mm, and two 15 mm-diameter holes 6b were formed symmetrically at the center, and one silica glass plate (middle plate 6) provided with degassing holes 6a on both the upper and lower sides was prepared.

【0025】(2)前記外管及び内管の加工 図1(A)に示すように、内部に挿入する夫々の内管2
の一端2aを封止し、次に、該内管2の他端の開口端2
b側を底板3の穴3aに嵌着した後、該開口端2bを開
放した状態で、底板3に溶着する。
(2) Processing of the outer pipe and the inner pipe As shown in FIG. 1 (A), each inner pipe 2 inserted inside
One end 2a of the inner tube 2 and then open the other end 2a of the inner tube 2.
After the b side is fitted into the hole 3a of the bottom plate 3, it is welded to the bottom plate 3 with the opening end 2b opened.

【0026】次に図1(B)に示すように、中板6を内
管2封止端側の閉塞端近くに取り付けた後、図1(C)
に示すように、該中板6取り付け側より外管1に挿入
し、その終端側に位置する底板3周囲と外管1端部とを
気密的に溶接固着する。最後に、図1(D)に示すよう
に、外管1の上端にガス抜き用蓋板5を気密的に溶接固
着する。(以下これらを被加熱体10という)この結
果、外管1内の内管2端部2aは封止されており、又内
管2の他端2b側は外管1の底板3上に開口しているた
めに、蓋板5のガス抜き穴5aより減圧処理した場合で
も内管2は正圧下を維持できる。
Next, as shown in FIG. 1 (B), after the intermediate plate 6 is attached near the closed end on the inner tube 2 sealing end side, FIG.
As shown in (1), the inner plate 6 is inserted into the outer tube 1 from the mounting side, and the periphery of the bottom plate 3 located at the end side and the end of the outer tube 1 are hermetically welded and fixed. Finally, as shown in FIG. 1 (D), a gas vent cover plate 5 is hermetically welded and fixed to the upper end of the outer tube 1. As a result, the end 2a of the inner tube 2 in the outer tube 1 is sealed, and the other end 2b side of the inner tube 2 is opened on the bottom plate 3 of the outer tube 1. Therefore, even when the pressure is reduced through the gas vent hole 5a of the cover plate 5, the inner pipe 2 can maintain the positive pressure.

【0027】(3)前記被加熱体10の熱歪除去処理 前記のように形成した被加熱体10をヒータにて105
0゜Cで10hrs加熱処理を行ない、熱歪除去処理を
行った後、10wt%フッ化水素水溶液に前記被加熱体
を10min浸し洗浄およびマイクロクラックの除去を
行なった後、清浄な雰囲気で乾燥を行なった。
(3) Thermal distortion removal treatment of the object to be heated 10 The object to be heated 10 formed as described above is subjected to 105 heating by a heater.
After performing a heat treatment at 0 ° C. for 10 hrs to remove the heat distortion, the object to be heated is immersed in a 10 wt% aqueous solution of hydrogen fluoride for 10 minutes to wash and remove microcracks, and then dried in a clean atmosphere. Done.

【0028】(4)主原料シリカ粉の作成及び加熱純化
処理 シリカ粉の種類は天然水晶、合成水晶、合成クリストバ
ライト、合成シリカガラスのいずれか1種類以上用い、
塩素ガスや塩化水素ガス等の含有雰囲気で加熱純化処理
を行うが、非晶質シリカ粉を用いる場合は、水素含有雰
囲気若しくはヘリウム含有雰囲気にて加熱純化処理を行
なうのがよい。又シリカ粉の粒径は、10〜1000μ
mが好ましい。これ以下では、溶融したシリカガラス体
3中に気泡が多量に含まれてしまう。これ以上では、溶
融時均一にならなかったり、同様に気泡がぬけにくくな
ってしまう。
(4) Preparation of Main Raw Material Silica Powder and Purification by Heating The type of silica powder is at least one of natural quartz, synthetic quartz, synthetic cristobalite, and synthetic silica glass.
The heat purification treatment is performed in an atmosphere containing chlorine gas, hydrogen chloride gas, or the like. When amorphous silica powder is used, the heat purification treatment is preferably performed in a hydrogen-containing atmosphere or a helium-containing atmosphere. The particle size of the silica powder is 10 to 1000 μm.
m is preferred. Below this, a large amount of bubbles are contained in the fused silica glass body 3. Above this, it is not uniform at the time of melting or it is difficult to remove air bubbles.

【0029】そこで本実施例では主原料の結晶質シリカ
粉として、天然水晶粉体を粒径50〜500μmの範囲
かつ10μm未満の粉を0,1wt%以下に調整した。
又必要に応じて耐熱性等を増すために、金属元素化合物
粉等を前記純化処理後に混合してもよいが、その場合製
造後のシリカガラスロッドの特定ドープ元素の濃度が
0.1〜5wt%になるようにドープ用粉体と主原料シ
リカ粉の混合比を設定するのがよい。
Therefore, in the present embodiment, as a crystalline silica powder as a main raw material, a natural quartz powder was adjusted to a powder having a particle size in the range of 50 to 500 μm and less than 10 μm to 0.1 wt% or less.
If necessary, in order to increase heat resistance and the like, a metal element compound powder or the like may be mixed after the purification treatment. In this case, the concentration of the specific doping element in the manufactured silica glass rod is 0.1 to 5 wt. %, The mixing ratio of the powder for doping and the silica powder of the main raw material is preferably set.

【0030】(5)合成シリカガラス粉の調整 ゾルゲル法で製造した合成シリカガラス粉を粒径50〜
500μmに調整した。
(5) Preparation of Synthetic Silica Glass Powder The synthetic silica glass powder produced by the sol-gel method has a particle diameter of 50 to 50%.
It was adjusted to 500 μm.

【0031】(6)被加熱体内へのシリカガラス粉体の
投入充填 主原料シリカ粉に結晶質シリカを用いる場合は、非加熱
体の下端端部分には合成シリカガラス粉7aを入れ、次
いで徐々に水晶粉等の結晶粉の比率を大きくした粉を入
れていく。下端のシリカガラス粉7aの充填長さは、溶
融に使用するヒータ8の均熱長より大きくしなければな
らない。この理由は、先端部分にシリカガラス粉7aを
入れないで、いきなり水晶粉7bを入れて、上記ヒータ
8にて昇温すると、水晶のα型β型の転移温度にて急膨
張し、外管1を破壊させてしまうからである。尚、主原
料粉としてすべてを非晶質シリカガラスとする場合は、
先端部分からすべて同一種類のシリカガラス粉7を順次
充填すれば良い。
(6) Filling and Filling of Silica Glass Powder into Body to be Heated When crystalline silica is used as the main raw material silica powder, synthetic silica glass powder 7a is put into the lower end portion of the non-heated body and then gradually. The powder with an increased ratio of crystal powder such as crystal powder is added to the mixture. The filling length of the silica glass powder 7a at the lower end must be longer than the soaking length of the heater 8 used for melting. The reason for this is that the quartz glass powder 7b is suddenly put in without the silica glass powder 7a in the tip portion, and when the temperature is increased by the heater 8, the crystal suddenly expands at the α-type β-type transition temperature of the crystal. 1 will be destroyed. In addition, when using amorphous silica glass as the main raw material powder,
The same type of silica glass powder 7 may be sequentially filled from the tip.

【0032】従って本実施例においては、図3(A)及
び(B)に示すように、前記蓋板5のガス抜き穴5aよ
り中板6の切欠き6aを介して先ず50gの合成シリカ
ガラス粉7aを投入し、次に天然水晶:合成シリカガラ
ス=1:2(重量比)の混合粉体7a1を50gを投入
し、更に天然水晶:合成シリカガラス=1:1の混合粉
体7a2の50gを投入し、更に天然水晶:合成シリカ
ガラス=2:1の混合粉体7a3を50gを投入した。
最後に、天然水晶粉7bを500gを充填した。この結
果合成シリカガラス粉体層7aが6cm、混合粉体7a
1、混合粉体7a2、混合粉体7a3の層が夫々6cmと
なり、これらの層の累計がヒータ8の均熱長(5cm)
より大にする事が出来た。
Therefore, in the present embodiment, as shown in FIGS. 3A and 3B, first, 50 g of synthetic silica glass is passed through the gas vent hole 5a of the cover plate 5 through the notch 6a of the middle plate 6. powder 7a was charged, then natural crystal: synthetic silica glass = 1: 2 mixture powder 7a 1 (weight ratio) was charged with 50 g, further natural crystal: synthetic silica glass = 1: 1 mixed powder 7a 2 of 50g was charged, further natural crystal: synthetic silica glass = 2: the powder mixture 7a 3 of 1 was charged 50g.
Finally, 500 g of natural crystal powder 7b was filled. As a result, the synthetic silica glass powder layer 7a was 6 cm, and the mixed powder 7a
1 , the layer of the mixed powder 7a 2 and the layer of the mixed powder 7a 3 each become 6 cm, and the total of these layers is the soaking length (5 cm) of the heater 8.
I was able to make it bigger.

【0033】(7)ヒータ8を使った溶融透明ガラス化 次に図4に示すように、前記蓋板5のガス抜き穴5a
(筒部)より内管2と外管1の間のシリカ粉体の充填さ
れた区域内を10Torr以下に真空引きした後、前記
内管2と外管1とからなる被加熱体10をゆっくりヒー
タ8の上部より該ヒータ8内に挿入しつつ、そのヒータ
8内への送り速度と該ヒータ8により溶融されたシリカ
ガラスの引き速度を制御して帯域溶融と線引きを行っ
て、透明棒状のダブルホア管9を得る。
(7) Melting and Transparent Vitrification Using Heater 8 Next, as shown in FIG.
After evacuating the area filled with the silica powder between the inner tube 2 and the outer tube 1 from the (cylindrical portion) to 10 Torr or less, the heating target 10 including the inner tube 2 and the outer tube 1 is slowly moved. While being inserted into the heater 8 from above the heater 8, the zone melting and the drawing are performed by controlling the feeding speed into the heater 8 and the drawing speed of the silica glass melted by the heater 8, thereby forming a transparent rod-shaped. Obtain a double bore tube 9.

【0034】このとき外管1内部に挿入された内管2の
内圧は大気若しくは正圧開放されている為に、減圧下の
粉状体充填域に比較し大きく、内管2の穴は溶融により
閉じることがない。又正圧開放されている為に内管2の
内圧は加熱によっても無用に増大する事なく、精度よい
寸法精度が維持されながら加熱溶融されることとなる。
尚、このボア管9の直径は、被加熱体10の直径の1/
2以下にするのが好ましく、本実施例においては、被加
熱体10のヒータ8内への送り速度およびガラス化した
ダブルホア管9の引き速度を調整することにより、外径
φ10mm、内径φ3mmの多数の熱電対用ダブルボア
管を作成した。
At this time, since the internal pressure of the inner tube 2 inserted into the outer tube 1 is open to the atmosphere or positive pressure, it is larger than that of the powder-filled area under reduced pressure. Never closes. Further, since the positive pressure is released, the internal pressure of the inner tube 2 does not needlessly increase by heating, and is heated and melted while maintaining accurate dimensional accuracy.
The diameter of the bore tube 9 is 1 / the diameter of the object to be heated 10.
In this embodiment, it is preferable to adjust the feed speed of the heated object 10 into the heater 8 and the pulling speed of the vitrified double bore tube 9 so that the outer diameter φ is 10 mm and the inner diameter φ 3 mm. Thermocouple double bore tube was made.

【0035】(8)物性評価 前記の様に製造したダブルボア管9の気泡の発生は10
0cm3に存在する泡の総面積は0.88mm2であっ
た。(ただし、測定法はDIN58927(1970)
に従う。)これは半導体治具に用いる本出願人の商品:
Heralux−Eと同レベルであり、実質的にほとん
ど気泡が発生していないといえる。次に前記のように製
造したダブルボア管9夫々の寸法精度は外径φ10m
m、内径φ3mmにおいて、外径半径方向円周振れ公差
±0.1(mm) 外径半径方向全周振れ公差 ±0.2(mm)、内口径
半径方向円周振れ公差±0.03(mm)、内口径半径
方向全周振れ公差±0.06(mm)といずれも精度よ
い加工が可能となる。又表面状態はいずれも擦り傷なく
非常に滑らかであった。
(8) Evaluation of physical properties The generation of air bubbles in the double bore tube 9 manufactured as described above is 10
The total area of the foam present at 0 cm 3 was 0.88 mm 2 . (However, the measuring method is DIN58927 (1970)
Obey. This is the applicant's product used for semiconductor jigs:
It is at the same level as Heralux-E, and it can be said that substantially no bubbles are generated. Next, the dimensional accuracy of each of the double-bore pipes 9 manufactured as described above has an outer diameter of 10 m.
m, inner diameter φ 3 mm, outer diameter radial direction circumferential runout tolerance ± 0.1 (mm) outer diameter radial direction whole circumferential runout tolerance ± 0.2 (mm), inner bore radial direction circumferential runout tolerance ± 0.03 ( mm) and the inner diameter radial direction full-circumference runout tolerance ± 0.06 (mm). The surface condition was very smooth without any scratches.

【0036】不純物分析は、表1に溶融前の天然水晶粉
と溶融透明ガラス化後の不純物濃度を示す。
In the impurity analysis, Table 1 shows the natural quartz powder before melting and the impurity concentration after vitrification.

【0037】[0037]

【表1】 [Table 1]

【0038】本表より原料粉の高純度がガラス化後も良
好に保存されていることが理解される。尚、Li、M
g、TiはICP質量分析法により、またNa、K、C
a、Cr、Fe、Ni、Cuは黒鉛炉加熱原子吸光分析
法により測定を行なった。
From this table, it is understood that the high purity of the raw material powder is well preserved even after vitrification. Note that Li, M
g and Ti were determined by ICP mass spectrometry, and Na, K, C
a, Cr, Fe, Ni, and Cu were measured by graphite furnace heating atomic absorption spectrometry.

【0039】(実施例2)実施例1と同様にダブルボア
管を作成した。 (1)シリカガラス製の外管1、内管2等の用意 図5に示すように、前記実施例同様に直径40mm、肉
厚1.5mmの内管2と外管1を夫々作成するが、本実
施例の場合は外管1より内管2の方を長くする。又、図
5に示すように底板3は前記実施例と同様であるが、中
板6は設けずに中央に直径15mmの穴5bを対称に2
つ開けるとともに、下側にガス抜き穴5aを開けたガス
抜き用蓋板5各1枚ずつ用意した。
(Example 2) A double bore tube was prepared in the same manner as in Example 1. (1) Preparation of Outer Tube 1, Inner Tube 2, etc. Made of Silica Glass As shown in FIG. 5, an inner tube 2 and an outer tube 1 each having a diameter of 40 mm and a wall thickness of 1.5 mm are prepared as in the previous embodiment. In the case of this embodiment, the length of the inner tube 2 is made longer than that of the outer tube 1. Also, as shown in FIG. 5, the bottom plate 3 is the same as that of the above-mentioned embodiment, but the center plate 6 is not provided, and a hole 5b having a diameter of 15 mm is
And a gas vent cover plate 5 having a gas vent hole 5a at the bottom was prepared.

【0040】(2)シリカガラス被加熱体10の加工 図6(A)に示すように、内管2の他端の開口端2b側
を底板3の穴に嵌着した後、該開口端2bを開放した状
態で、底板3に溶着する。次に図6(B)に示すよう
に、蓋板5を外管1長さと対応する内管2に固着させた
後、該蓋板5取り付け側より外管1に挿入し、その終端
側に位置する底板3周囲と外管1端部とを気密的に溶接
固着する。最後に、図6(C)に示すように、内管2を
外管1上に突設させた状態で蓋板5を気密的に溶接固着
する。この結果内管2は蓋板5より外管1上に突設され
ており、又内管2の他端2b側は外管1の底板3上に開
口しているために、蓋板5のガス抜き穴5aより減圧処
理しても内管2は正圧下を維持できる。前記加工後、前
記実施例と同様に、シリカガラス被加熱体10の熱歪除
去処理を行う。
(2) Processing of Heated Body 10 of Silica Glass As shown in FIG. 6A, the other end of the inner tube 2 at the open end 2b side is fitted into the hole of the bottom plate 3 and then the open end 2b Is welded to the bottom plate 3 in a state where is opened. Next, as shown in FIG. 6B, after the cover plate 5 is fixed to the inner tube 2 corresponding to the length of the outer tube 1, the cover plate 5 is inserted into the outer tube 1 from the side where the cover plate 5 is attached, and The periphery of the located bottom plate 3 and the end of the outer tube 1 are hermetically welded and fixed. Finally, as shown in FIG. 6 (C), the lid plate 5 is hermetically welded and fixed in a state where the inner pipe 2 is projected from the outer pipe 1. As a result, the inner tube 2 protrudes above the outer tube 1 from the cover plate 5, and the other end 2 b side of the inner tube 2 opens on the bottom plate 3 of the outer tube 1. Even if the pressure is reduced through the gas vent hole 5a, the inner tube 2 can maintain a positive pressure. After the processing, similarly to the above-described embodiment, the heat distortion removal treatment of the silica glass heated object 10 is performed.

【0041】(3)高純度合成シリカガラス粉の雰囲気
加熱処理 ゾルゲル法で製造した合成シリカガラス粉を粒径50〜
500μmに調整した。 タングステンメッシュヒータ
ー、ステンレススチールジャケットの雰囲気電気加熱炉
内にて、H2 ガス雰囲気にて800℃、3hrs加熱処
理を行なった。
(3) Atmospheric heat treatment of high-purity synthetic silica glass powder Synthetic silica glass powder produced by the sol-gel method has a particle diameter of 50 to 50%.
It was adjusted to 500 μm. Heat treatment was performed at 800 ° C. for 3 hours in a H 2 gas atmosphere in an atmosphere electric heating furnace having a tungsten mesh heater and a stainless steel jacket.

【0042】(4)被加熱体10内へのシリカガラス粉
体の投入充填 主原料粉として非晶質シリカガラスを用いているため
に、先端部分からすべて同一種類のシリカガラス粉2を
順次充填すれば良い。
(4) Injection and Filling of Silica Glass Powder into Heated Body 10 Since amorphous silica glass is used as the main raw material powder, the same kind of silica glass powder 2 is sequentially filled from the tip portion. Just do it.

【0043】(5)ヒータ8を使った溶融透明ガラス化 図7に示すように前記実施例と同様にフランジのガス抜
き穴5aより内管2と外管1の間のシリカ粉体の充填さ
れた区域内を10Torr以下に真空引きし、且つ内管
2内にそれ以上の圧力、例えば正圧に維持した状態で、
前記実施例と同様な方法で帯域溶融と線引きを行って、
透明棒状のダブルホア管9を得る。このとき内部に挿入
された内管2の内圧は、減圧下の粉状体充填域に比較し
大きく、内管2の穴は溶融により閉じることがなく所定
の寸法精度を維持できる。尚、充填されるシリカ粉およ
びシリカガラス被加熱体10等に高純度合成シリカを使
用したが、作成されたダブルボア管の物性は実施例1と
同様であり、不純物分析を行なった結果を表2に示す。
本表より原料粉の高純度がガラス化後も良好に保持され
ていることがわかる。
(5) Melting and Transparent Vitrification Using Heater 8 As shown in FIG. 7, the silica powder between the inner tube 2 and the outer tube 1 is filled through the gas vent hole 5a of the flange as in the previous embodiment. While the inside of the section was evacuated to 10 Torr or less, and maintained at a higher pressure in the inner tube 2, for example, a positive pressure,
By performing zone melting and drawing in the same manner as in the above embodiment,
A transparent rod-shaped double bore tube 9 is obtained. At this time, the internal pressure of the inner pipe 2 inserted therein is larger than that of the powdered material filling area under reduced pressure, and the hole of the inner pipe 2 can be maintained at a predetermined dimensional accuracy without being closed by melting. Although high-purity synthetic silica was used for the silica powder to be filled and the silica glass to be heated 10 and the like, the physical properties of the double-bore tube produced were the same as in Example 1, and the results of the impurity analysis are shown in Table 2. Shown in
From this table, it can be seen that the high purity of the raw material powder is maintained well after vitrification.

【0044】[0044]

【表2】 [Table 2]

【0045】かかる実施例によれば、例えば図8(A)
に示すような太径の多穴ロッド12の製作も可能であ
る。又内管2の配置断面形状は、(B)に示すように任
意に設定できる。更に前記内管2は開放正圧下に維持さ
れている為に、精度よく形状維持しながら帯域加熱が可
能であるために、例えば(C)に示すように、角型の多
穴ロッド13の製作も可能である。
According to this embodiment, for example, FIG.
It is also possible to manufacture a large-diameter multi-hole rod 12 as shown in FIG. The arrangement cross-sectional shape of the inner tube 2 can be set arbitrarily as shown in FIG. Further, since the inner tube 2 is maintained under an open positive pressure, it is possible to perform zone heating while maintaining the shape accurately. For example, as shown in FIG. Is also possible.

【0046】更に前記線引き速度を変化させることによ
り、テーパ状の多穴ロッドの製作も可能である。
Further, by changing the drawing speed, a tapered multi-hole rod can be manufactured.

【0047】[0047]

【発明の効果】以上記載のごとく本発明によれば、シリ
カガラス原材からシリカガラス加工品を作成するにあた
り、欠け、亀裂がなく高寸法精度のシリカガラス加工品
を得る事が出来る。又本発明によれば、製造したシリカ
ガラス加工品表面、特に多穴シリカガラス加工品の場合
穴内表面に荒れ、傷等がなく、更には連続的に製造可能
なシリカガラス加工品を得る事が出来る。本発明によれ
ば、製造過程において不純物の汚染が生じる事なく、原
料材と同様に高純度の維持を図ったシリカガラス加工品
を得る事が出来る。本発明によれば、長尺寸法の多穴シ
リカガラス、厚さ数mmの板状体から、長さ10mのロ
ッド、又数10m長のファイバーのように、軸方向に延
在する形状であれば任意のプロフィル形状を任意に生成
し得る。本発明によれば、小口径から大口径の多穴シリ
カガラス加工品を容易に且つ任意に作成出来る。本発明
によれば、例えば熱電対用絶縁管,各種センサー用保護
管,ガラスバーナーの火口,バブラー管,理化学機器部
材,ガス配管を兼ねた熱処理用治具材,半導体工業用部
材等として利用されるシリカガラス加工品を容易かつ安
価に得る事が出来る。
As described above, according to the present invention, when producing a processed silica glass product from a raw material of silica glass, it is possible to obtain a processed silica glass product having high dimensional accuracy without chipping or cracking. Further, according to the present invention, it is possible to obtain a processed silica glass product which can be continuously manufactured without roughening, scratches and the like on the surface of the manufactured silica glass processed product, particularly in the case of a multi-hole silica glass processed product. I can do it. According to the present invention, it is possible to obtain a processed silica glass product in which high purity is maintained in the same manner as the raw material without causing contamination of impurities in the manufacturing process. According to the present invention, a multi-hole silica glass having a long dimension, a plate having a thickness of several mm, a rod having a length of 10 m, or a fiber extending in the axial direction such as a fiber having a length of several tens of meters can be used. Any profile shape can be generated arbitrarily. According to the present invention, it is possible to easily and arbitrarily create a multi-hole silica glass product having a small diameter to a large diameter. According to the present invention, for example, it is used as a thermocouple insulating tube, a protective tube for various sensors, a crater of a glass burner, a bubbler tube, a physicochemical device member, a jig material for heat treatment which also serves as a gas pipe, a member for semiconductor industry, and the like. The processed silica glass product can be easily and inexpensively obtained.

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

【図1】(A)(B)(C)(D)は図2に示す材料よ
り被加熱体を製造する為の製造工程を示す。
FIGS. 1A, 1B, 1C, and 1D show manufacturing steps for manufacturing a body to be heated from the materials shown in FIGS.

【図2】本発明の実施例に係るシリカガラス被加熱体に
示す材料を示す。
FIG. 2 shows a material for a silica glass object to be heated according to an example of the present invention.

【図3】被加熱体内へのシリカガラス粉体の投入充填状
態を示す。
FIG. 3 shows a state in which silica glass powder is charged and filled into a body to be heated.

【図4】ヒータを使った溶融透明ガラス化工程を示す。FIG. 4 shows a molten transparent vitrification process using a heater.

【図5】本発明の第2実施例に係るシリカガラス被加熱
体に示す材料を示す。
FIG. 5 shows materials for a silica glass object to be heated according to a second embodiment of the present invention.

【図6】(A)(B)(C)は図2に示す材料より被加
熱体を製造する為の製造工程を示す。
FIGS. 6A, 6B, and 6C show a manufacturing process for manufacturing a body to be heated from the material shown in FIG. 2;

【図7】ヒータを使った透明ガラス化工程を示す。FIG. 7 shows a transparent vitrification process using a heater.

【図8】(A)は本発明により製造される太径の多穴ロ
ッドを示し、(B)はその断面形状の各種例を示す。
(C)は本発明により製造される角型の多穴ロッドであ
る。
FIG. 8A shows a large-diameter multi-hole rod manufactured according to the present invention, and FIG. 8B shows various examples of its cross-sectional shape.
(C) is a square multi-hole rod manufactured by the present invention.

【符号の説明】[Explanation of symbols]

1 外管 2 内管 3 底板 5 蓋板 6 中板 7 原料シリカ粉 7a 非晶質シリカ粉 7b 水晶粉 8 ヒータ 10 被加熱体 DESCRIPTION OF SYMBOLS 1 Outer tube 2 Inner tube 3 Bottom plate 5 Cover plate 6 Middle plate 7 Raw material silica powder 7a Amorphous silica powder 7b Quartz powder 8 Heater 10 Heated object

───────────────────────────────────────────────────── フロントページの続き (72)発明者 鈴木 正則 福島県郡山市田村町金屋字川久保88 信 越石英株式会社郡山工場内 (56)参考文献 特開 昭58−204830(JP,A) 特開 昭63−282134(JP,A) 特許3258175(JP,B2) (58)調査した分野(Int.Cl.7,DB名) C03B 20/00 H01L 21/22 501 G01K 1/00 ──────────────────────────────────────────────────続 き Continued on the front page (72) Inventor Masanori Suzuki 88 Kawakubo, Kanaya, Tamura-cho, Koriyama-shi, Fukushima Shin-Etsu Quartz Co., Ltd. Koriyama Plant (56) References JP-A-58-204830 (JP, A) 63-282134 (JP, A) Patent 3258175 (JP, B2) (58) Fields investigated (Int. Cl. 7 , DB name) C03B 20/00 H01L 21/22 501 G01K 1/00

Claims (3)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 任意の断面形状が軸方向に延在する中空
シリカガラス外管内に、円または多角形の断面形状が軸
方向に延在するシリカガラス内管を一または複数本挿入
して管状被加熱体を作成した後、この被加熱体内の外管
と内管との間隙先端より、粒径を50〜500ミクロン
に調整した合成シリカ粉からなる非晶質シリカ粉を主成
分とする粉状体を充填しその後に水晶粉その他の結晶質
シリカ粉を主成分とする粉状体を充填して、 前記シリカ粉を充填した被加熱体の外管と内管の間を減
圧下にかつ内管内を正圧開放した状態で、前記被加熱体
を先端側より帯域加熱にて軸方向に沿って加熱溶融させ
て延伸一体化してなる事を特徴とするシリカガラス加工
品の製造方法。
1. A tube formed by inserting one or more silica glass inner tubes having a circular or polygonal cross section extending in the axial direction into a hollow silica glass outer tube having an arbitrary cross section extending in the axial direction. After forming the object to be heated, a particle size of 50 to 500 microns is measured from the tip of the gap between the outer tube and the inner tube in the object to be heated.
Filled with a powder mainly composed of amorphous silica powder composed of synthetic silica powder adjusted to the above, and then filled with a powder composed mainly of quartz powder or other crystalline silica powder, the silica powder In a state where the space between the outer tube and the inner tube of the object to be heated is filled under reduced pressure and the inside of the inner tube is opened under a positive pressure , the object to be heated is heated and melted along the axial direction by zone heating from the distal end side. A process for producing a processed silica glass product, characterized by being stretched and integrated.
【請求項2】 任意の断面形状が軸方向に延在する中空
シリカガラス外管内に、円または多角形の断面形状が軸
方向に延在するシリカガラス内管を複数本挿入して管状
被加熱体を作成した後、この被加熱体内の外管と内管と
の間隙の少なくとも一部にシリカ粉を充填して、前記シ
リカ粉を充填した被加熱体の外管と内管の間を減圧下に
かつ内管内を正圧開放した状態で、該被加熱体を先端側
より帯域加熱にて軸方向に沿って加熱溶融させて一体化
して、ロッド内に複数の小孔を存在させてなる多穴チュ
ーブを製造する事を特徴とするシリカガラス加工品の製
造方法。
2. A tube to be heated by inserting a plurality of silica glass inner tubes having a circular or polygonal cross section extending in the axial direction into a hollow silica glass outer tube having an arbitrary cross section extending in the axial direction. After the body is made, at least a part of the gap between the outer tube and the inner tube in the heated body is filled with silica powder ,
Reduce the pressure between the outer and inner pipes of the heated object filled with lica powder.
In a state where the inside of the inner tube is opened to a positive pressure , the object to be heated is heated and melted along the axial direction by zone heating from the distal end side to be integrated, and a plurality of small holes are present in the rod. A method for producing a processed silica glass product, which comprises producing a tube.
【請求項3】 前記被加熱体の内管と外管の間隙先端よ
り、粒径を50〜500ミクロンに調整した合成シリカ
粉からなる非晶質シリカ粉を主成分とする粉状体を充填
しその後に水晶粉その他の結晶質シリカ粉を主成分とす
る粉状体を充填してなる事を特徴とする請求項2記載の
シリカガラス加工品の製造方法。
3. A synthetic silica particle having a particle size adjusted to 50 to 500 microns from a tip of a gap between an inner tube and an outer tube of the object to be heated.
Claim, characterized in that formed by filling a powdery body consisting mainly of quartz powder other crystalline silica powder of amorphous silica powder consisting of powdery subsequently filled with powdery bodies mainly 2 A method for producing a processed silica glass product according to the above.
JP21317994A 1994-08-15 1994-08-15 Method for producing silica glass processed product Expired - Fee Related JP3327364B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP21317994A JP3327364B2 (en) 1994-08-15 1994-08-15 Method for producing silica glass processed product

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP21317994A JP3327364B2 (en) 1994-08-15 1994-08-15 Method for producing silica glass processed product

Publications (2)

Publication Number Publication Date
JPH0859261A JPH0859261A (en) 1996-03-05
JP3327364B2 true JP3327364B2 (en) 2002-09-24

Family

ID=16634858

Family Applications (1)

Application Number Title Priority Date Filing Date
JP21317994A Expired - Fee Related JP3327364B2 (en) 1994-08-15 1994-08-15 Method for producing silica glass processed product

Country Status (1)

Country Link
JP (1) JP3327364B2 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6606116B2 (en) 2017-03-24 2019-11-13 古河電気工業株式会社 Optical fiber manufacturing method
WO2019150622A1 (en) * 2018-01-30 2019-08-08 株式会社フルヤ金属 Thermocouple structure and method for manufacturing same
JP7236284B2 (en) * 2019-02-12 2023-03-09 東京応化工業株式会社 Substrate heating device and substrate processing system

Also Published As

Publication number Publication date
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