JPH0859261A - Production of worked silica glass product - Google Patents

Production of worked silica glass product

Info

Publication number
JPH0859261A
JPH0859261A JP21317994A JP21317994A JPH0859261A JP H0859261 A JPH0859261 A JP H0859261A JP 21317994 A JP21317994 A JP 21317994A JP 21317994 A JP21317994 A JP 21317994A JP H0859261 A JPH0859261 A JP H0859261A
Authority
JP
Japan
Prior art keywords
silica glass
heated
powder
silica
tube
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
Application number
JP21317994A
Other languages
Japanese (ja)
Other versions
JP3327364B2 (en
Inventor
Tsukasa Sakaguchi
司 坂口
Shigeru Yamagata
茂 山形
Noboru Suzuki
昇 鈴木
Masanori Suzuki
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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Measuring Temperature Or Quantity Of Heat (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Devices For Use In Laboratory Experiments (AREA)

Abstract

PURPOSE: To provide a method for producing a worked silica glass product capable of readily and optionally preparing a perforated worked silica glass product ranging from a small to a large calibers. CONSTITUTION: This method for producing a worked silica glass product is to insert one or plural inner tubes 2, extending a circular or a polygonal cross- sectional shape in the axial direction and made of silica glass into a hollow outer silica glass tube 1 extending an optional cross-sectional shape in the axial direction, prepare a material to be heated, then fill silica powder in at least a part of a gap between the outer tube 1 and the inner tubes 2 in the material to be heated, subsequently thermally melt the material to be heated in the axial direction while controlling the pressure in at least a part between the outer tube 1 and the inner tubes 2 of the material to be heated according to a ring-shaped zone heating method and integrate the outer tube 1 with the inner tubes 2. Thereby, a perforated tube containing one or plural small holes present in the rod is obtained.

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 silica glass processed product having a predetermined size by using silica glass as a raw material, for example, an insulating tube for thermocouples and various sensors. The present invention relates to an invention of a silica glass processed product used as a protection tube, a crater of a glass burner, a bubbler tube, a physics and chemistry equipment member, a heat treatment jig material also serving as a gas pipe, a semiconductor heat treatment jig member, 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 heat treatment apparatus for wafers. All of these require high-purity, high-dimensional accuracy, low-cost manufacturing methods with no quality variations. The burner for processing these jigs or the burner for producing synthetic quartz by the oxyhydrogen flame hydrolysis method is also formed of silica glass, but such a burner blows gas into a large-diameter outer tube. Although a plurality of inner pipes forming the mouth are inserted, it is difficult to weld the inner pipe to the outer pipe airtightly and accurately through the 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 temperature, gas concentration, etc. in a high temperature atmosphere, a multi-hole silica glass rod having a large number of axial holes bored in the axial direction is provided in order to improve insulation and heat resistance. Although 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 contamination of impurities are provided. Need a rod.

【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 manufacture a multi-hole silica glass tube for such an application, a method of preparing several tubes and then welding and integrating them has been adopted. Therefore, the cost was high.

【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 various other members for semiconductor heat treatment jigs, and for bubbling a raw material liquid when manufacturing soot-like synthetic silica glass from a high-purity liquid raw material. In the bubbling vaporizer used, a large diameter outer tube with many inner tubes inserted and a bubbler tube with many small holes perforated by machining a silica glass bar have been developed. However, in such a bubbler tube, the small hole must be formed by welding or machining, and these methods inevitably have the following problems.

【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 silica glass processed product is manufactured from agglomerated silica glass by cutting, laser processing or the like. However, in this method, since the silica glass is a brittle material, Not only cracks and breaks due to shearing by cutting tend to occur, but also contamination from cutting jigs and the like occurs. Furthermore, the cutting process has a limit on the drill length, and in particular, a long multi-hole silica glass cannot be produced. In addition, in the case of multi-hole silica glass, not only multi-hole silica glass having a fine hole size cannot be produced, but also multi-hole silica glass having various sizes 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 eliminate such drawbacks, a processing method by a hot molding method or a hot press molding has been proposed. That is, there is also a method of filling silica powder in a mold made of carbon or the like, or putting a lump, and producing a silica glass processed product of a predetermined shape by heat molding or heat pressure molding, but with such a molding method Dimension control cannot be performed accurately. In the case of processed multi-hole silica glass, various dimensions,
Not only is it impossible to continuously form shaped multi-hole silica glass, but 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。
In view of the above technical problems, the present invention provides 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 a method for producing a processed silica glass product, in particular, in the case of a multi-hole silica glass processed product, the inner surface of the hole is not roughened, has no scratches, etc., and can be continuously produced. To provide. It is another object of the present invention to provide a method for producing a processed silica glass product, which maintains high purity like raw materials without 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 extend axially from a long-hole multi-hole silica glass, a plate having a thickness of several mm to a rod having a length of 10 m and a fiber having a length of several 10 m. It is an object of the present invention to provide a method for producing a silica glass processed product, which can arbitrarily generate an arbitrary profile shape if it has an existing shape.

【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 product capable of easily and arbitrarily producing a processed product of a multi-hole silica glass having a small diameter to a large diameter. Another object of the present invention is, for example, an insulating tube for a thermocouple, a protective tube for various sensors, a crater of a glass burner, a bubbler tube, a physics and chemistry equipment member, a heat treatment jig material also serving as a gas pipe, a semiconductor heat treatment jig member. An object of the present invention is 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(以下多穴チューブという)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製内管を一
または複数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、次いで該被加熱体の外管と内管との間
の少なくとも一部の圧力を制御しつつ、該被加熱体を先
端側よりリングゾーン状の帯域加熱方法にて軸方向に沿
って加熱溶融させて外管と内管との間を一体化させる事
を第1の特徴とするものである。
The invention according to claim 1 is applied to a silica glass processed product (hereinafter referred to as a multi-hole tube) in which one or a plurality of small holes are present in a rod. Where, in the hollow silica glass outer tube with an arbitrary cross-sectional shape extending in the axial direction, one or more silica glass inner tubes with a circular or polygonal cross-sectional shape extending in the axial direction are inserted into a tubular shape. After creating the object to be heated, at least a part of the gap between the outer tube and the inner tube in the object to be heated is filled with silica powder, and then at least one portion between the outer tube and the inner tube of the object to be heated is filled. First, the outer tube and the inner tube are integrated by heating and melting the body to be heated along the axial direction from the tip side by a ring zone zone heating method while controlling the pressure of the part. It is a feature of.

【0012】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る事を第2の特徴とする。
In this case, in order to manufacture a multi-hole tube, the silica powder is filled into the portion of the body to be heated, which is to be filled with silica glass, uniformly in the gap between the outer tube and the inner tube. The second feature is that the outer tube and the inner tube are integrated without a gap by the zone heating.

【0013】この場合、管路若しくは通路を形成するた
めの内管内を開放正圧下に、即ち具体的には少なくとも
一端が開放状態で常圧ないしは加圧下に維持し、一方シ
リカ粉が充填される外管と内管との間は減圧下に維持し
た状態で加熱溶融させて一体化させるのがよい。これを
第3の特徴とする。
In this case, the inside of the inner pipe for forming the pipe or the passage is maintained under an open positive pressure, that is, at least one end is kept in an open state under normal pressure or under pressure, while silica powder is filled. The outer tube and the inner tube are preferably melted by heating while being kept under reduced pressure to be integrated. This is the third feature.

【0014】この場合、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とともに、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。
In this case, after the powdery material containing amorphous silica powder as a main component is filled 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 mainly added. It is preferable that the powdery material as a component is filled and the particle diameter of the crystalline silica is preferably in the range of 10 to 1000 μm, and the content ratio of fine particles 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 amorphous silica powder is uniformly filled in the portion where the silica glass is uniformly filled and zone melting is performed, such amorphous silica powder has no so-called melting point and gradually softens from around 1600 ° C. Since it melts, a deposition gas or the like from the silica powder is caught 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 crystal powder is 1730
Since it has a melting point at ℃, it can be melted all at once by heating it to 1730 ℃ or more, and it is possible to suppress the generation of bubbles in the molten glass as much as possible, but crystalline silica powder such as crystal powder is α type at 573 ℃. To a β-type transition point, the tube is rapidly expanded by the transition from α-type to β-type of the crystal powder inside the tubular heated object before the viscosity of the tubular heated object decreases at the start of heating. 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。
Therefore, according to the present invention, since the powdery body containing the amorphous silica powder having no transition point as a main component is present on the tip side which is first zone-heated, the transition from α type to β type is caused. While preventing the breakage of the existing tube, the viscosity of the hollow tube decreases due to the preheating of the heat zone above it, and the crystalline silica powder in that part undergoes a rapid expansion due to the transition from α type to β type. However, crystalline silica powder such as crystal powder is filled only in the area where the breakage of the tube can be prevented. Incidentally, the filling width of the amorphous silica powder needs to be larger than the heat zone (uniform heating width) of the zone heating means, but if it is too large, the substantial bubble-free area decreases and the productivity becomes low. In order to reduce, it is preferably less than 20% of the total filling amount of 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 crystalline silica powder selected from natural quartz powder, synthetic quartz powder and synthetic cristobalite powder and has a particle size of 10 to 1000 μm, preferably 20 to 500 μm, more preferably 50 to 50 μm. Within the range of 200 μm, the content ratio of fine particles of less than 10 μm is 0.1 w
It must be t% or less. Kashidashi, the particle size is 1
If it is less than 0 μm, even if a vacuum is applied, a pressure loss occurs, so that it is not possible to apply a vacuum to the inside of the filling area, and even if the zone melts, it becomes difficult for the bubbles to escape, and the fused silica glass contains a large amount of bubbles. In addition, the heat insulating effect makes it difficult to uniformly heat and melt the central portion of the tubular object. If the particle size is 1000 μm or more, it will not be possible to eliminate the generation of bubbles due to the fact that the particles do not become uniform during melting, and similarly, even if quartz powder is used, the voids between the particles are wide.

【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。
Further, the silica powder is charged by first filling the lower end of the powder filling area of the tubular heated object with the amorphous silica powder and then with the mixed powder of the amorphous silica powder and the crystalline silica powder. Finally, it is preferable to fill the crystalline silica powder.

【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 producing a high-purity rod, it may not be possible to use the natural crystalline silica powder as described above. In such a case, it is preferable that the high-purity synthetic amorphous silica powder is heat-treated in advance in a hydrogen-containing atmosphere or a helium-containing atmosphere and then filled. As a result, even if a residual gas consisting of hydrogen or helium is present during the zone melting, these are occluded / doped in the molten glass during the melting, and it is possible to prevent the generation of bubbles, and a high-purity amorphous material like synthetic silica glass. Even if the silica powder is used, a substantially glass-free silica glass rod can be manufactured.

【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。
Further, as the above-mentioned silica powder, silica powder prepared by previously mixing metal or metal element compound powder may be used. In this case, it is preferable that the reduced pressure atmosphere in the powder-filled area during heating and melting is set to a vacuum of 1 KPa or less so that gas entrapment and expansion 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。
The multi-hole bar silica rod of the present invention is
It is applied as an insulating tube for thermocouples, a protective tube for sensors, a sealing member, a glass burner crater, a bubbler tube, a member for physics and chemistry equipment, and a member for semiconductor heat treatment jigs.

【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。
EXAMPLES Examples of the present invention will now be illustratively described in detail. However, unless otherwise specified, the materials, shapes, analysis values, etc. of the components described in this embodiment are not intended to limit the scope of the present invention thereto but are merely illustrative examples. .

【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 bar-shaped double-bore tube for a thermocouple will be described with reference to FIGS. (1) Preparation of outer tube made of silica glass, substantially tubular body (hereinafter referred to as inner tube), etc. As shown in FIG. 2, a 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 wall thickness of 1.5 mm, and a length of 1 m to be inserted thereinto were prepared. Also, diameter 40m
m, a disk-shaped silica glass plate (bottom plate 3) with a machining dimensional accuracy of ± 0.1 mm in which two holes 3a having a diameter of 15 mm are symmetrically formed in the center, and a gas vent hole 5a is formed in the center with the same outer diameter. Silica glass plate (gas vent cover plate 5) and diameter of 37
mm, and two holes 6b having a diameter of 15 mm were symmetrically formed in the center, and one silica glass plate (middle plate 6) provided with gas vent holes 6a on both 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 to be inserted inside
One end 2a of the inner tube 2 is sealed, and
After the side b is fitted into the hole 3a of the bottom plate 3, the bottom plate 3 is welded with the open end 2b open.

【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 sealing end side of the inner tube 2, FIG.
As shown in FIG. 3, the inner plate 6 is inserted into the outer tube 1 from the mounting side, and the periphery of the bottom plate 3 located on the terminal side thereof and the end of the outer tube 1 are hermetically welded and fixed. Finally, as shown in FIG. 1D, the gas vent cover plate 5 is airtightly welded and fixed to the upper end of the outer tube 1. As a result, the inner tube 2 end 2a 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, the inner tube 2 can be maintained under a positive pressure even when the pressure reduction process is performed through the gas vent hole 5a of the lid plate 5.

【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 strain removal treatment of the heated body 10 The heated body 10 formed as described above is heated by a heater 105.
Heat treatment is performed at 0 ° C for 10 hours to remove thermal strain, and then the object to be heated is immersed in a 10 wt% hydrogen fluoride aqueous solution for 10 minutes to wash and remove microcracks, and then dried in a clean atmosphere. I did.

【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 heat purification treatment The silica powder is selected from natural quartz, synthetic quartz, synthetic cristobalite and synthetic silica glass.
The heating purification treatment is performed in an atmosphere containing chlorine gas, hydrogen chloride gas, etc. When the amorphous silica powder is used, the heating purification treatment is preferably performed in a hydrogen containing atmosphere or a helium containing atmosphere. The particle size of silica powder is 10 to 1000μ.
m is preferred. Below this, a large amount of bubbles are contained in the fused silica glass body 3. If the amount is higher than this, it will not be uniform when melted, and likewise bubbles will be hard to escape.

【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 this embodiment, as the main raw material crystalline silica powder, natural quartz powder was adjusted to have 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, metal element compound powder and the like may be mixed after the purification treatment, in which case the concentration of the specific doping element of the silica glass rod after production is 0.1 to 5 wt. It is preferable to set the mixing ratio of the dope powder and the main raw material silica powder so as to be 100%.

【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 A synthetic silica glass powder produced by the sol-gel method has a particle size 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 the heated body When crystalline silica is used as the main raw material silica powder, synthetic silica glass powder 7a is put into the lower end of the non-heated body, and then gradually. Add powder with a high ratio of crystal powder such as crystal powder to. The filling length of the silica glass powder 7a at the lower end must be larger than the soaking length of the heater 8 used for melting. The reason for this is that when silica glass powder 7a is not put in the tip portion but crystal powder 7b is suddenly put in and the temperature is raised by the heater 8, it rapidly expands at the α-type β-type transition temperature of the crystal and the outer tube Because it destroys 1. If all of the main raw material powder is amorphous silica glass,
The silica glass powder 7 of the same type 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 this embodiment, as shown in FIGS. 3 (A) and 3 (B), 50 g of synthetic silica glass is first introduced from the gas vent hole 5a of the cover plate 5 through the notch 6a of the intermediate plate 6. Powder 7a is charged, then 50 g of mixed powder 7a 1 of natural crystal: synthetic silica glass = 1: 2 (weight ratio), and further mixed powder 7a of natural crystal: synthetic silica glass = 1: 1. 50 g of 2 was added, and further 50 g of mixed powder 7a 3 of natural crystal: synthetic silica glass = 2: 1 was added.
Finally, 500 g of natural crystal powder 7b was filled. As a result, the synthetic silica glass powder layer 7a is 6 cm, and the mixed powder 7a is
1 , the layers of the mixed powder 7a 2 and the mixed powder 7a 3 are 6 cm, respectively, and the cumulative 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) Melt transparent vitrification using heater 8 Next, as shown in FIG.
After the area inside the inner tube 2 and the outer tube 1 filled with silica powder is evacuated to 10 Torr or less from the (cylindrical portion), the heated body 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 feeding speed into the heater 8 and the drawing speed of the silica glass melted by the heater 8 are controlled to perform zone melting and wire drawing to form a transparent rod-shaped member. Obtain the double-hore 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 in the powdery material filling region under reduced pressure, and the hole of the inner tube 2 melts. Will never close. Further, since the positive pressure is released, the internal pressure of the inner tube 2 does not increase unnecessarily even by heating, and the heating and melting are performed while maintaining the accurate dimensional accuracy.
The diameter of the bore tube 9 is 1 / the diameter of the heated body 10.
It is preferable that the number is 2 or less. In the present embodiment, by adjusting the feed rate of the heated body 10 into the heater 8 and the pulling rate of the vitrified double-hore tube 9, a large number of outer diameter φ10 mm and inner diameter φ3 mm can be obtained. A double-bore tube for a thermocouple was prepared.

【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 double-bore tube 9 manufactured as described above has 10 bubbles.
The total area of bubbles present at 0 cm 3 was 0.88 mm 2 . (However, the measuring method is DIN 58927 (1970)
Follow This is the applicant's product for use in 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 3 mm, outer diameter radial runout tolerance ± 0.1 (mm) outer diameter radial full runout tolerance ± 0.2 (mm), inner diameter radial runout tolerance ± 0.03 ( mm) and the inner circumference radial direction runout tolerance of ± 0.06 (mm), which enables accurate machining. Further, the surface condition was very smooth without 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 crystal powder before melting and the impurity concentration after melting and transparent 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. Incidentally, Li, M
g and Ti are measured by ICP mass spectrometry, and Na, K and C
A, Cr, Fe, Ni, and Cu were measured by a 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 and Inner Tube 2 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 above embodiment. In the case of this embodiment, the inner tube 2 is made longer than the outer tube 1. Further, as shown in FIG. 5, the bottom plate 3 is the same as that of the above-mentioned embodiment, but the middle plate 6 is not provided and the hole 5b having a diameter of 15 mm is symmetrically formed in the center.
Along with the opening, one degassing lid plate 5 having a degassing hole 5a on the lower side 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 the silica glass heated body 10 As shown in FIG. 6 (A), after the opening end 2b side of the other end of the inner tube 2 is fitted in the hole of the bottom plate 3, the opening end 2b is formed. Is welded to the bottom plate 3 in the open state. Next, as shown in FIG. 6 (B), after fixing the cover plate 5 to the inner pipe 2 corresponding to the length of the outer pipe 1, the lid plate 5 is inserted into the outer pipe 1 from the mounting side, and the end plate is attached to the end side. The periphery of the positioned bottom plate 3 and the end of the outer tube 1 are air-tightly welded and fixed. Finally, as shown in FIG. 6 (C), the cover plate 5 is airtightly welded and fixed in a state in which the inner pipe 2 is projected on the outer pipe 1. As a result, the inner pipe 2 is projected above the outer pipe 1 from the lid plate 5, and the other end 2b side of the inner pipe 2 is opened on the bottom plate 3 of the outer pipe 1, so that the lid plate 5 Even if the pressure reduction process is performed through the gas vent hole 5a, the inner pipe 2 can be maintained under a positive pressure. After the processing, the thermal strain removal treatment of the silica glass heated body 10 is performed as in the above-described embodiment.

【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 size of 50 to 50.
It was adjusted to 500 μm. Atmosphere of tungsten mesh heater and stainless steel jacket In an electric heating furnace, heat treatment was performed at 800 ° C. for 3 hours in an H 2 gas atmosphere.

【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) Filling and filling of silica glass powder into the object to be heated 10 Since amorphous silica glass is used as the main raw material powder, silica glass powder 2 of the same type is sequentially filled from the tip. 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) Molten transparent vitrification using heater 8 As shown in FIG. 7, silica powder is filled between the inner tube 2 and the outer tube 1 through the gas vent hole 5a of the flange as in the above-mentioned embodiment. In a state in which the inside of the above area is evacuated to 10 Torr or less and the inner tube 2 is maintained at a higher pressure, for example, a positive pressure,
Zone melting and wire drawing were carried out in the same manner as in the above example,
A transparent rod-shaped double-hore tube 9 is obtained. At this time, the internal pressure of the inner tube 2 inserted inside is larger than that in the powdery material filling region under reduced pressure, and the hole of the inner tube 2 is not closed by melting, so that a predetermined dimensional accuracy can be maintained. Although high-purity synthetic silica was used for the silica powder to be filled, the silica glass heated body 10 and the like, the physical properties of the double bore tube produced were the same as in Example 1, and the results of impurity analysis are shown in Table 2. Shown in.
It can be seen from this table that the high purity of the raw material powder is maintained well even 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 such an embodiment, for example, FIG.
It is also possible to manufacture a multi-hole rod 12 having a large diameter as shown in FIG. The arrangement cross-sectional shape of the inner pipe 2 can be arbitrarily set as shown in (B). Furthermore, since the inner tube 2 is maintained under open positive pressure, it is possible to perform zone heating while maintaining the shape with high accuracy. For example, as shown in (C), fabrication of a square multi-hole rod 13 is made. 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, it is possible to manufacture a tapered multi-hole rod.

【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 a silica glass processed product is prepared from a silica glass raw material, it is possible to obtain a silica glass processed product with high dimensional accuracy without chipping or cracking. In addition, according to the present invention, it is possible to obtain a processed silica glass product, particularly a multi-hole silica glass processed product, which has no roughness or scratches on the inner surface of the hole and which can be continuously manufactured. I can. According to the present invention, it is possible to obtain a processed silica glass product in which high purity is maintained similarly to the raw material without causing contamination of impurities in the manufacturing process. According to the present invention, a long-length multi-hole silica glass, a plate having a thickness of several mm, a rod having a length of 10 m, or a fiber having a length of several tens of m may have a shape extending in the axial direction. For example, any profile shape can be generated arbitrarily. According to the present invention, a multi-hole silica glass processed product having a small diameter to a large diameter can be easily and arbitrarily prepared. INDUSTRIAL APPLICABILITY According to the present invention, for example, it is used as an insulating tube for thermocouples, a protective tube for various sensors, a crater of a glass burner, a bubbler tube, a member of physics and chemistry equipment, a jig material for heat treatment also serving as a gas pipe, a member for semiconductor industry, etc. It is possible to easily and inexpensively obtain processed silica glass products.

【図面の簡単な説明】[Brief description of 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。
1 (A), (B), (C) and (D) show manufacturing steps for manufacturing a heated body from the materials shown in FIG.

【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 materials shown in a silica glass heated object 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 of charging and filling silica glass powder into a heated body.

【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 melting 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 shown in a silica glass heated body 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。
6 (A), (B) and (C) show manufacturing steps for manufacturing a heated body from the material shown in FIG.

【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 according to 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 1 Outer Tube 2 Inner Tube 3 Bottom Plate 5 Lid Plate 6 Middle Plate 7 Raw 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 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Masanori Suzuki 88 Kawakubo, Kanaya, Tamura-cho, Koriyama-shi, Fukushima Shin-Etsu Quartz Co., Ltd.

Claims (4)

【特許請求の範囲】[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
と内管との間隙の少なくとも一部にシリカ粉を充填し
て、該被加熱体の外管と内管の間の少なくとも一部の圧
力を制御しつつ、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 tubular shape in which one or more silica glass inner tubes having a circular or polygonal cross-sectional shape extending in the axial direction are inserted into a hollow silica glass outer tube having an arbitrary cross-sectional shape extending in the axial direction. After creating the object to be heated, at least a part of the gap between the outer tube and the inner tube in the object to be heated is filled with silica powder, and at least a part between the outer tube and the inner tube of the object to be heated is filled. A method for producing a processed silica glass product, characterized in that the body to be heated is melted and integrated along the axial direction by zone heating from the tip side while controlling the pressure.
【請求項2】 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制御し、または内管内を常圧又は
加圧下に制御した状態で、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請求項1記載のシリカガラス加工
品の製造方法。
2. The tip of the object to be heated is controlled under a reduced pressure between the outer tube and the inner tube of the object to be heated filled with the silica powder, or under normal pressure or under pressure inside the inner tube. The method for producing a silica glass processed product according to claim 1, wherein the process is performed by heating from the side along the axial direction by zone heating to melt and stretch and integrate.
【請求項3】 前記被加熱体の内管と外管の間隙先端よ
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
体を充填するとともに、結晶質シリカの粒径が10〜1
000μmの範囲、かつ10μm未満の微粒子含有比率
が0.1wt%以下であることを特徴とする請求項1記
載のシリカガラス加工品の製造方法。
3. A powdery material having an amorphous silica powder as a main component is filled from the tip of a gap between the inner tube and the outer tube of the object to be heated, and then quartz powder or other crystalline silica powder is used as a main component. And the crystalline silica has a particle size of 10 to 1
The method for producing a silica glass processed product according to claim 1, wherein the content ratio of fine particles in the range of 000 μm and less than 10 μm is 0.1 wt% or less.
【請求項4】 前記粉状充填域の減圧雰囲気が1KPa
以下の真空であることを特徴とする請求項1記載のシリ
カガラス加工品の製造方法。
4. The reduced pressure atmosphere in the powdery filling area is 1 KPa.
The method for producing a silica glass processed product according to claim 1, wherein the following vacuum is applied.
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 true JPH0859261A (en) 1996-03-05
JP3327364B2 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
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WO2019150622A1 (en) * 2018-01-30 2019-08-08 株式会社フルヤ金属 Thermocouple structure and method for manufacturing same
JP2020129648A (en) * 2019-02-12 2020-08-27 東京応化工業株式会社 Substrate heating device and substrate processing system

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018173774A1 (en) * 2017-03-24 2018-09-27 古河電気工業株式会社 Manufacturing method for optical fiber
JP2018162170A (en) * 2017-03-24 2018-10-18 古河電気工業株式会社 Method for manufacturing optical fiber
US11237322B2 (en) 2017-03-24 2022-02-01 Furukawa Electric Co., Ltd. Optical fiber manufacturing method using relative bulk densities
WO2019150622A1 (en) * 2018-01-30 2019-08-08 株式会社フルヤ金属 Thermocouple structure and method for manufacturing same
JPWO2019150622A1 (en) * 2018-01-30 2020-02-06 株式会社フルヤ金属 Thermocouple structure and method of manufacturing the same
TWI779089B (en) * 2018-01-30 2022-10-01 日商古屋金屬股份有限公司 Thermocouple construction and method of making the same
JP2020129648A (en) * 2019-02-12 2020-08-27 東京応化工業株式会社 Substrate heating device and substrate processing system

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