JPH0426522A - Production of synthetic quartz glass tube - Google Patents
Production of synthetic quartz glass tubeInfo
- Publication number
- JPH0426522A JPH0426522A JP13032790A JP13032790A JPH0426522A JP H0426522 A JPH0426522 A JP H0426522A JP 13032790 A JP13032790 A JP 13032790A JP 13032790 A JP13032790 A JP 13032790A JP H0426522 A JPH0426522 A JP H0426522A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- synthetic quartz
- manufacturing
- glass tube
- glass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/04—Re-forming tubes or rods
- C03B23/047—Re-forming tubes or rods by drawing
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/04—Re-forming tubes or rods
- C03B23/07—Re-forming tubes or rods by blowing, e.g. for making electric bulbs
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は合成石英ガラス管の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for manufacturing synthetic quartz glass tubes.
〔従来の技術１
現在、半導体製造工程においては天然の水晶を原料とす
る溶融石英ガラスがプロセスチューブ、ボート等に一般
的に用いられている。[Prior Art 1] Currently, in semiconductor manufacturing processes, fused silica glass made from natural quartz is generally used for process tubes, boats, etc.
一方、近年の半導体の高集積化の進展には著しいものが
あり、これにともない、半導体製造工程中で使用される
材質中からの不純物が半導体の歩留り低下の大きな原因
となることが明らかにされている。プロセスチューブ等
の石英部材においても従来使用されてきた溶融石英ガラ
スは、原料及び製造プロセスに由来するナトリウム、鉄
などの不純物が多いことから、これを高集積度の半導体
の製造プロセス、例えば拡散工程、酸化工程、ＣＶＤ工
程等で使用すると溶融石英ガラスチューブに含まれる不
純物がシリコンウェハー上に拡散浸透し歩留り低下をき
たすと言われており、高純度な石英ガラスチューブの開
発が強（望まれていた。On the other hand, in recent years, there has been remarkable progress in the integration of semiconductors, and along with this, it has become clear that impurities in the materials used in the semiconductor manufacturing process are a major cause of lower semiconductor yields. ing. Fused silica glass, which has traditionally been used in quartz components such as process tubes, contains many impurities such as sodium and iron derived from raw materials and manufacturing processes, so it is used in the manufacturing process of highly integrated semiconductors, such as diffusion process. It is said that when fused silica glass tubes are used in processes such as oxidation, CVD, etc., impurities contained in fused silica glass tubes diffuse into silicon wafers and reduce yields. Ta.
これに対し、合成石英ガラスチューブの製造方法として
、従来の溶融石英チューブと同様な方法、すなわち、高
純度な合成石英ガラス素材を黒鉛製容器中で高温度で溶
融した後、下部に設けたノズルより管状に成型加工する
方法があるが、この方法では一旦、摂氏２０００度以上
の高温度で溶融するために黒鉛容器中の不純物が合成石
英ガラス中に拡散浸透しガラス中の不純物を増加させて
しまうので高集積化された半導体製造用プロセスチュー
ブに用いる石英ガラス管としては純度の面から不十分で
あった。On the other hand, synthetic quartz glass tubes are manufactured using the same method as conventional fused silica tubes, that is, high-purity synthetic quartz glass material is melted at high temperature in a graphite container, and then a nozzle is installed at the bottom. There is a method of molding it into a more tubular shape, but in this method, impurities in the graphite container diffuse into the synthetic quartz glass and increase the impurities in the glass because it is melted at a high temperature of over 2,000 degrees Celsius. Therefore, from the viewpoint of purity, it was insufficient as a quartz glass tube for use in process tubes for highly integrated semiconductor manufacturing.
［発明の解決しようとする課題〕
本発明の目的は、従来使用されていた溶融石英ガラスの
有していた前述の欠点を解消しようとするものである。[Problems to be Solved by the Invention] An object of the present invention is to eliminate the above-mentioned drawbacks of conventionally used fused silica glass.
本発明は、前述の課題を解決すべくなされたものであり
、合成石英ガラスブロックから管を製造する方法におい
て、（１）該ブロックを厚内の円筒状ガラスに加工する
第１の工程と、（２）加熱下で該円筒状ガラス内部にガ
ス圧をかけ非接触で膨張させながら長さ方向に延伸して
薄肉・大口径化する第２の工程とを含むことを特徴とす
る合成石英ガラス管の製造方法を提供するものである。The present invention has been made to solve the above-mentioned problems, and provides a method for manufacturing a tube from a synthetic quartz glass block, including (1) a first step of processing the block into a thick cylindrical glass; (2) a second step of applying gas pressure to the inside of the cylindrical glass under heating and expanding it in a non-contact manner while stretching it in the length direction to make it thinner and larger in diameter; A method for manufacturing a tube is provided.
以下、本発明の詳細について説明する。The details of the present invention will be explained below.
まず、石英ガラスブロックから肉厚円筒状ガラスに加工
する工程について説明する。この加工工程では二つの方
法を採用することができる。その第一は機械加工による
方法である。はとんどの合成石英ガラスは円柱状に製造
されることから本発明の肉厚円筒状ガラスに加工するに
は、通常の機械加工の方が効率的な場合があり、例えば
、加工前の外径、長さが加工後のそれに近い場合、中く
り抜きした中の円柱状ガラスの有効利用が図られている
場合などである。First, the process of processing a quartz glass block into thick cylindrical glass will be explained. Two methods can be adopted in this processing step. The first method is by machining. Since most synthetic quartz glass is manufactured in a cylindrical shape, normal machining may be more efficient in processing the thick cylindrical glass of the present invention. This is the case when the diameter and length are close to those after processing, or when the hollowed-out cylindrical glass is being used effectively.
この場合は、コアドリルを用いて通常の中くり抜き、外
周研削加工し所定の寸法の肉厚円筒状ガラスに加工する
。In this case, a core drill is used to hollow out the glass and grind the outer periphery to produce a thick cylindrical glass of predetermined dimensions.
次にもう一つの方法である成型加工により肉厚円筒状ガ
ラスを作製する方法について説明する。図１は、本発明
の石英ガラスブロックから肉厚円筒状ガラスに加工する
工程（第１の工程）で用いる黒鉛製型枠の断面を示す。Next, another method of manufacturing thick cylindrical glass by molding will be explained. FIG. 1 shows a cross section of a graphite mold used in the step (first step) of processing a quartz glass block into thick cylindrical glass according to the present invention.
１１は成型加工前の合成石英ガラス、１２は黒鉛製型枠
、１３は円筒状加工用（穴明は用）黒鉛ロッド、１４は
プレス加工用黒鉛製おもり、１５は加熱炉をそれぞれ示
す。Reference numeral 11 indicates a synthetic quartz glass before forming, 12 a graphite mold, 13 a graphite rod for cylindrical processing (for drilling), 14 a graphite weight for pressing, and 15 a heating furnace.
この方法では、まず型枠は高純度化された黒鉛（例えば
東洋カーボン社製Ａ−２５０Ｋ）を材質として用い、さ
らに、被加ニガラスが直接型枠に接触して反応、融着し
ないように、高純度炭化珪素などの離型材（例えば、イ
ビデン社製ベータランダム）を型枠と被加ニガラスとの
接触面に塗布したものを用いる。このような型枠内に、
石英ガラス例えば石英ガラスブロックを装着し、電気炉
内に設置した後変形に必要な温度に昇温しで肉厚円筒状
に成型加工する。この加工方法としてはあらかじめ型枠
上部に所定の内径に近いオス型のロッド（型枠と同等の
材質、処理をしたもの）を設置し、おもりなどの一定荷
重下で変形させたり、あるいは別置きの加圧装置により
一定荷重あるいは一定速度で変形することができる。こ
の時の成型加工温度は、１６００〜１８００℃の範囲で
あることが好ましい、 １６００℃未満では成型加工に
時間を要することとガラス表面から失透しやす（なるこ
とから好ましくなく、又、１８００℃を超えると粘度が
低下して離型材が石英ガラスへ拡散しやすくなり石英ガ
ラスが直接黒鉛と接触し反応、融着が起こり型枠中の不
純物のガラスへの拡散浸透を促進しガラス中の不純物が
増加することと冷却時に成型加工したガラスにクラック
が入りやすくなることから好ましくない。In this method, first, highly purified graphite (for example, A-250K manufactured by Toyo Carbon Co., Ltd.) is used as the material for the formwork, and further, in order to prevent the glass to be added to the formwork from directly contacting the formwork and reacting and fusing, A mold release material such as high-purity silicon carbide (for example, Beta Random manufactured by Ibiden) is applied to the contact surface between the mold and the glass to be added. In such a formwork,
A quartz glass block, for example, a quartz glass block, is attached, placed in an electric furnace, heated to a temperature necessary for deformation, and formed into a thick cylindrical shape. As for this processing method, a male rod (made of the same material and treated as the formwork) with an inner diameter close to the specified one is installed in advance at the top of the formwork, and it is deformed under a constant load such as a weight, or it is placed separately. It can be deformed under a constant load or at a constant speed using a pressurizing device. The molding temperature at this time is preferably in the range of 1600 to 1800°C. If it is less than 1600°C, the molding process takes time and devitrification is likely to occur from the glass surface, so it is not preferable. If the viscosity is exceeded, the viscosity decreases and the mold release agent easily diffuses into the quartz glass, and the quartz glass directly contacts the graphite, causing a reaction and fusion, which promotes the diffusion of impurities in the mold into the glass, causing impurities in the glass. This is undesirable because it increases the temperature and makes it easier for cracks to form in the molded glass during cooling.
このように成型加工した肉厚円筒状ガラスは、形状や表
面状態を整える必要がある場合には、若干の表面仕上げ
を施した後次工程に供する。The thick cylindrical glass thus formed is subjected to a slight surface finish if it is necessary to adjust its shape and surface condition before being subjected to the next process.
次にもう一つの工程である加熱下で円筒状ガラスの内部
にガス圧をかけ膨張させながら長さ方向に延伸して薄肉
・大口径化する工程について説明する１図２は、本発明
の加熱下で円筒状ガラスの内部にガス圧をかけ膨張させ
ながら長さ方向に延伸して薄肉・大口径化する工程（第
２の工程）の一実施例の断面図である。Next, we will explain another process, which is the process of applying gas pressure to the inside of the cylindrical glass under heating to expand it while stretching it in the length direction to make it thinner and have a larger diameter. FIG. 3 is a cross-sectional view of an embodiment of the step (second step) of applying gas pressure to the inside of the cylindrical glass to expand it and stretch it in the length direction to make the glass thinner and have a larger diameter.
２１は加工前の肉厚円筒状石英ガラス、２２は加熱炉、
２３はガラス旋盤、２４は膨張後のガラス、２５は膨張
用ガス調圧供給装置、２６は高周波発生装！を示してい
る。加熱炉２２は内部に設けられた検出手段（例えばタ
ングステンーレニューム熱電対方式、放射温度計方式）
でコントロールされ、内側に若干のテーバを持たせた片
側内径１００＋＋＋ｍ 、他の片側内径１０４ｍｍ、外
径１５０ａ＋ｉ、長さ １９０ｍｍの緻密質高純度黒鉛
製発熱体（例えば、東洋カーボン社製ＡＸ−２１１０Ｋ
）が設置されている。これの加熱方法としては一般的な
高周波誘導加熱、抵抗加熱方式などがとられるが１局部
加熱の容易な高周波誘導加熱法が炉をコンパクトにでき
設計上有利である。21 is thick cylindrical quartz glass before processing, 22 is a heating furnace,
23 is a glass lathe, 24 is glass after expansion, 25 is an expansion gas pressure adjustment supply device, and 26 is a high frequency generator! It shows. The heating furnace 22 has an internal detection means (for example, a tungsten-renium thermocouple system, a radiation thermometer system).
A dense high-purity graphite heating element (for example, AX-2110K manufactured by Toyo Carbon Co., Ltd.
) is installed. Common heating methods such as high-frequency induction heating and resistance heating are used for this purpose, but the high-frequency induction heating method, which allows easy local heating, is advantageous in terms of design because it allows the furnace to be made compact.
この工程では、まず、肉厚円筒状ガラスの一方を閉じ更
に延伸用の石英棒を溶接し、もう片方には膨張させるガ
ス供給のために開けられた石英管をガラス旋盤上で溶接
する。In this process, first, one side of the thick cylindrical glass is closed and a quartz rod for stretching is welded to it, and a quartz tube opened to supply gas for expansion is welded to the other side on a glass lathe.
次に、中央に３ ＫＨｚの高周波誘導加熱炉を、更に、
炉の左右に各々独立に左右に駆動可能で任意の速度に設
定可能な非加工物を回転可能で固定する移動台を備えた
ガラス旋盤にセットし、膨張用ガスの回転可能な供給管
を接続する。膨張用ガスは圧力制御装置でガラス円筒内
部の圧力を一定圧に保つようにする。この膨張用ガスと
しては取扱い、安全性の面から窒素ガスが好ましい。肉
厚円筒状ガラスの薄肉・大口径化は該円筒ガラスを回転
させながら所定の温度まで昇温後、所定圧力を円筒内部
に加え加熱部ガラスの膨張を確認した後、肉厚円筒ガラ
スの供給と延伸を所定の速度で開始する。肉厚のコント
ロールは供給側と延伸側の速度比から、又、外径は黒鉛
発熱体出口側に設置した高純度黒鉛製治具で決定する。Next, a 3 KHz high frequency induction heating furnace was installed in the center, and
It is set in a glass lathe equipped with a movable table that rotatably fixes the unprocessed workpiece, which can be driven left and right independently on the left and right sides of the furnace and can be set at any speed, and connected to a rotatable supply pipe for expansion gas. do. The inflation gas is kept at a constant pressure inside the glass cylinder using a pressure control device. Nitrogen gas is preferred as this inflation gas from the viewpoint of handling and safety. To make thick cylindrical glass thinner and larger in diameter, the cylindrical glass is heated to a predetermined temperature while being rotated, a predetermined pressure is applied to the inside of the cylinder, and after checking the expansion of the heated glass, the thick cylindrical glass is supplied. and starts stretching at a predetermined speed. The wall thickness is controlled by the speed ratio between the supply side and the drawing side, and the outer diameter is determined by a high-purity graphite jig installed on the outlet side of the graphite heating element.
この時の成型加工温度は１７００〜１９００℃の範囲が
好ましい。１７００℃未満では、膨張に時間と大きな圧
力を要すること、又、１９００℃を超え高温になると被
加ニガラスの粘度が低下して膨張したガラスが黒鉛質発
熱体に接触し反応、融着が起こりやすくなることや外径
の制御が難しくなるので好ましくない。The molding temperature at this time is preferably in the range of 1700 to 1900°C. If the temperature is less than 1,700°C, it will take time and a lot of pressure to expand, and if the temperature exceeds 1,900°C, the viscosity of the glass to be added will decrease and the expanded glass will come into contact with the graphite heating element, causing a reaction and fusion. This is not preferable because it becomes easy to use and it becomes difficult to control the outer diameter.
又、膨俵圧力は、０．０１〜２．０気圧の範囲が好まし
い、 ０．０１気圧未満では膨張に時間を要し実際的で
ないので好ましくなく、２，０気圧を超えると膨張した
ガラスが黒鉛質発熱体内面に強く接触し表面形状が管状
に保たれないため好ましくない、さらに、肉厚円筒状ガ
ラスの肉厚Ｌ１と薄肉・大口径化したガラスの肉厚Ｌ２
の比Ｌ１／Ｌ、は２〜２０の範囲が好ましい。この比が
２未満では、膨張・延伸後の全長を、加工前の厚肉円筒
状ガラスの全長に対して大きくしないことから装置の能
力下限で運転することになり運転効率が悪（経済上好ま
しくなく、又、この比が２０を超えると膨張・延伸後の
肉厚Ｌ２をかなり薄くすることから肉厚や外径の制御が
難しくなり好ましくない。In addition, the expansion bale pressure is preferably in the range of 0.01 to 2.0 atm. If it is less than 0.01 atm, it takes time to expand and is not practical, so it is not preferable, and if it exceeds 2.0 atm, the expanded glass will deteriorate. This is undesirable because it strongly contacts the inner surface of the graphite heating element and the surface shape cannot be maintained in a tubular shape.Furthermore, the thickness L1 of the thick cylindrical glass and the thickness L2 of the thin and large diameter glass are undesirable.
The ratio L1/L is preferably in the range of 2 to 20. If this ratio is less than 2, the total length after expansion and stretching will not be larger than the total length of the thick cylindrical glass before processing, resulting in poor operating efficiency (economically unfavorable). Moreover, if this ratio exceeds 20, the wall thickness L2 after expansion and stretching becomes considerably thinner, making it difficult to control the wall thickness and outer diameter, which is not preferable.
又、高集積度半導体製造用プロセスチューブは前述のよ
うに金属不純物量が低い必要があるが、この金属不純物
の合計量がｌｐｐｍ以下の合成石英ガラスを本発明の方
法により加工して得られる合成石英ガラス管を素材とし
て使用することにより高集積度半導体製造用のプロセス
チューブを得ることができる。In addition, as mentioned above, process tubes for manufacturing highly integrated semiconductors must have a low amount of metal impurities, and synthetic quartz glass with a total amount of metal impurities of 1 ppm or less is processed by the method of the present invention. By using a quartz glass tube as a material, a process tube for manufacturing highly integrated semiconductors can be obtained.
さらに、プロセスチューブは高温の工程でも用いられる
事から本発明により加工する合成石英ガラスの耐熱性を
、ビームベンディング法で測定した徐冷点で表した場合
、１１５０℃以上の合成石英ガラスが好ましい。徐冷点
がこの温度未満の合成石英ガラスでは使用できる工程が
低温工程に限られ前述の目的である高集積度半導体製造
が不可能となる。Furthermore, since the process tube is also used in high-temperature processes, synthetic quartz glass that has a heat resistance of 1150° C. or higher when expressed in terms of annealing point measured by the beam bending method is preferable. Synthetic quartz glass having an annealing point below this temperature can only be used in low-temperature processes, making it impossible to manufacture highly integrated semiconductors as described above.
［作用Ｊ
本発明において、高純度な合成石英ガラスは、まず、冷
間での機械加工や離型材を塗布した黒鉛型枠内で肉厚円
筒状ガラスに成型加工されるが、冷間で機械加工した石
英ガラスは加工時に発生したマイクロクラックに金属な
どの不純物が進入するがこれはフッ酸洗浄などで除去可
能であること、又、加熱下型枠中での加工では高純度部
材を採用したことと加熱条件として比較的低温、短時間
で行なうことで部材中の不純物のガラスへの拡散浸透を
抑えられる。次に加熱下で円筒状ガラス内部にガス圧を
かけて薄肉・大口径化する工程ではガラスの外側面が加
熱時の膨張直後に短時間低温の黒鉛に接触する程度で、
円筒内部にはガス以外の物質は接触しない加工方法であ
ることから使用部材からガラスへの不純物の混入を抑止
できる。[Operation J] In the present invention, high-purity synthetic quartz glass is first cold-machined or molded into a thick cylindrical glass in a graphite mold coated with a mold release agent. Processed quartz glass has metal and other impurities that enter into microcracks that occur during processing, but these can be removed by cleaning with hydrofluoric acid, and high-purity materials are used when processing in heated formwork. In addition, by heating at a relatively low temperature and for a short time, impurities in the member can be prevented from diffusing into the glass. Next, in the process of applying gas pressure to the inside of the cylindrical glass under heating to make it thinner and larger in diameter, the outer surface of the glass only comes into contact with the low-temperature graphite for a short time immediately after expansion during heating.
Since this processing method does not allow any substances other than gas to come into contact with the inside of the cylinder, it is possible to prevent impurities from entering the glass from used parts.
黒鉛炉に高純度炭化珪素粉を塗布した内径７０ｗ５ｔｎ
、高さ２４０ｍｍの高純度黒鉛質の円筒状型枠を設置し
、該型枠内にフッ酸洗浄した外径６６５ｍ、高さ１８０
ｍｍの円柱状合成石英ガラス（ビームベンディング法で
測定した徐冷点１１５５℃）をおき、さらに、高純度炭
化珪素粉を塗布した外径３４ｍａｒの穴明は用の高純度
黒鉛質ロッドを備えた蓋をセット後、穴明は用黒鉛ロッ
ドの上に約２ｋｇのプレス用黒鉛質おもりをセットする
。Inner diameter 70w5tn coated with high purity silicon carbide powder in graphite furnace
A high-purity graphite cylindrical formwork with a height of 240mm was installed, and a hydrofluoric acid-washed cylindrical formwork with an outer diameter of 665m and a height of 180m was installed inside the formwork.
A cylindrical synthetic quartz glass (annealing point 1155°C measured by beam bending method) of 1.0 mm was placed, and a high-purity graphite rod with an outer diameter of 34 mm coated with high-purity silicon carbide powder was installed. After setting the lid, Anaki sets a graphite weight of about 2 kg for press on top of the graphite rod.
さらに、所定の操作で１７３０℃に昇温後３０分間保持
し冷却後取り出し寸法を測定したところ内径３４ｍｍ、
外径７０ｍｍ、高さ２０８ｍｍの円筒状石英ガラスを得
た。さらに、機械加工で内径３６）、外径６６１Ｉ１１
に内外周面を加工した後一部分を採取しフッ酸で分解後
フレームレス原子吸光法により代表的な微量不純物を円
筒化前と比較測定したところ次の表−２のような結果に
なり、加工前後での不純物の顕著な増加は認められなか
った。Furthermore, when the temperature was raised to 1730°C by a prescribed operation and held for 30 minutes, and the dimensions taken out after cooling were measured, the inner diameter was 34 mm.
A cylindrical quartz glass with an outer diameter of 70 mm and a height of 208 mm was obtained. In addition, by machining, the inner diameter is 36) and the outer diameter is 661I11.
After machining the inner and outer circumferential surfaces, a portion was taken and decomposed with hydrofluoric acid, and representative trace impurities were measured by flameless atomic absorption spectrometry in comparison with those before cylindricalization, and the results shown in Table 2 below were obtained. No significant increase in impurities before and after was observed.
さらに、加工した円筒状石英ガラス２木を溶接して内径
３６ｍｍ、外径６６ｍｍ、長さ４００ｍａ＋の円筒状ガ
ラスに加工した後、片側に外径３０ｍｍの石英棒を、も
う一方に外径３０ｍａ＋、内径２６ｍｍの石英管を溶接
し前述のガラス旋盤にセットし毎分２０回転で回転させ
ながら１８５０℃に９０分で昇温後円筒内部の圧力をを
０，０５気圧に保つように窒素ガスを供給した。３分後
に、膨張した事を確認後肉厚円筒状ガラスを毎分７ｍｅ
の速度で炉側に供給を開始し、同時に延伸側の台を炉に
離れる方向へ毎分１４ｍ５＋で延伸させ、約５０分間運
転した。取り外し後寸法を測定したところ、結果は表−
１に示すように肉厚分布、外径分布ともに管として充分
な精度であった。寸法の測定方法は長さは巻尺、外径は
ノギス、肉厚は超音波厚み計をそれぞれ用いた。又、外
径は周囲方向角度０度、９０度の２ケ所、肉厚は周囲方
向角度０度、９０度、１８０度、２７０度の４ケ所を測
定した。Furthermore, after welding two pieces of processed cylindrical quartz glass into a cylindrical glass with an inner diameter of 36 mm, an outer diameter of 66 mm, and a length of 400 ma+, a quartz rod with an outer diameter of 30 mm is placed on one side, and an outer diameter of 30 mm+ on the other side. A quartz tube with an inner diameter of 26 mm was welded, set in the glass lathe mentioned above, heated to 1850°C in 90 minutes while rotating at 20 revolutions per minute, and nitrogen gas was supplied to maintain the pressure inside the cylinder at 0.05 atm. did. After 3 minutes, after confirming that it has expanded, the thick cylindrical glass is heated at 7me per minute.
The feed to the furnace side was started at a speed of 1, and at the same time, the table on the stretching side was stretched at a rate of 14 m5+ per minute in the direction away from the furnace, and the operation was continued for about 50 minutes. When the dimensions were measured after removal, the results are shown in Table-
As shown in Figure 1, both the wall thickness distribution and the outer diameter distribution had sufficient accuracy as a pipe. The dimensions were measured using a tape measure for length, a caliper for outer diameter, and an ultrasonic thickness gauge for wall thickness. The outer diameter was measured at two locations at circumferential angles of 0 degrees and 90 degrees, and the wall thickness was measured at four locations at circumferential angles of 0 degrees, 90 degrees, 180 degrees, and 270 degrees.
表−１
さらに、薄肉・大口径化したガラスの一部を採取し代表
的な不純物についてフッ酸で分解後フレームレス原子吸
光法で分析した。測定結果を表−２に示すように加工前
後での不純物増加は認められなかった。Table 1 Furthermore, a portion of the thin-walled, large-diameter glass was sampled, and representative impurities were decomposed with hydrofluoric acid and analyzed using flameless atomic absorption spectrometry. As shown in Table 2, no increase in impurities was observed before and after processing.
表−２
〔発明の効果Ｊ
本発明によれば、成形加工時に不純物の新たな混入がな
く合成石英ガラスの特性の一つである高純度性を保った
まま、ブロックから管を成形し、高純度の石英ガラス管
を得ることができる。Table 2 [Effect of the invention J According to the present invention, a tube can be molded from a block while maintaining high purity, which is one of the characteristics of synthetic quartz glass, without introducing new impurities during the molding process. You can get the purity quartz glass tube.
本発明による合成石英ガラス管は、高集積化された半導
体製造プロセス用チューブに特に優れて使用できる特徴
を有する。The synthetic quartz glass tube according to the present invention has characteristics that make it particularly suitable for use as a tube for highly integrated semiconductor manufacturing processes.
図１は、第１の工程の一実施例における黒鉛製型枠等の
断面図、また図２は第２の工程における装置の一実施例
の断面図である。
１１・・・・成形加工前の合成石英ガラスブロック１２
・・・・黒鉛製型枠
１３ ・円筒状加工用黒鉛製ロッド
１４・・・おもり
１５・−・・加熱炉
２１・・・加工前の肉厚円筒状石英ガラス２２・・・加
熱炉
２３・・・・旋盤
２４・・・・膨張後のガラス管
図FIG. 1 is a cross-sectional view of a graphite mold etc. in an example of the first step, and FIG. 2 is a cross-sectional view of an example of the apparatus in the second step. 11...Synthetic quartz glass block 12 before forming processing
Graphite formwork 13 Graphite rod for cylindrical processing 14 Weight 15 Heating furnace 21 Thick cylindrical quartz glass 22 before processing Heating furnace 23 ... Lathe 24 ... Glass tube diagram after expansion
Claims (1)
いて、（１）該ブロックを厚肉の 円筒状ガラスに加工する第１の工程と、 （２）加熱下で該円筒状ガラス内部にガス圧をかけて非
接触で膨張させながら長さ方向に延伸して薄肉・大口径
化する第２の工程とを含むことを特徴とする合成石英ガ
ラス管の製造方法。 ２、前記第１の工程が、１６００〜１８００℃の温度域
で高純度な離型材を塗布した高純度黒鉛製型枠内で成型
加工する工程であることを特徴とする請求項１記載の合
成石英ガラス管の製造方法。 ３、前記第２の工程が、冷間の機械加工であることを特
徴とする請求項１記載の合成石英ガラス管の製造方法。 ４、前記第２の工程が、高周波誘導加熱炉内に設置され
た黒鉛製発熱体内で行なわれることを特徴とする請求項
１記載の合成石英ガラス管の製造方法。 ５、前記第２の工程における加熱温度が１７００〜１９
００℃の範囲内であることを特徴とする請求項１記載の
合成石英ガラス管の製造方 法。 ６、前記第２の工程における加圧のためのガス圧が０．
０１〜２．０気圧の範囲内であることを特徴とする請求
項１記載の合成石英ガラス管の製造方法。 ７、加熱下で円筒状ガラス内部にガス圧をかけて非接触
で膨張させながら長さ方向に延伸して肉薄・大口径化す
る前記第２の工程において、円筒状ガラスの肉厚Ｌ＿１
と延伸された肉薄ガラスの肉厚Ｌ＿２との比Ｌ＿１／Ｌ
＿２が、２〜２０の範囲であることを特徴とする請求項
１記載の合成石英ガラス管の製造方法。 ８、前記合成石英ガラスブロックが、ハロゲン化珪素を
原料として製造された石英ガラスからなることを特徴と
する請求項１記載の合成石英ガラス管の製造方法。 ９、前記合成石英ガラス管に含まれる重金属の合計が、
１ｐｐｍ以下であることを特徴とする請求項１記載の合
成石英ガラス管の製造方 法。 １０、前記合成石英ガラス管の徐冷点（ｌｏｇη＝１３
．０である濃度）が１１５０℃以上であることを特徴と
する請求項１記載の合成石英ガラス管の製造方法。 １１、請求項１、８、９および１０のうちのいずれか１
項記載の方法により製造された合成石英ガラス管を使用
したことを特徴とする半導体製造用プロセスチューブ。[Claims] 1. A method for manufacturing a tube from a synthetic quartz glass block, comprising: (1) a first step of processing the block into a thick cylindrical glass; (2) processing the block into a thick cylindrical glass under heating; A method for producing a synthetic quartz glass tube, comprising a second step of applying gas pressure to the inside of the glass to expand it in a non-contact manner while stretching it in the length direction to make it thinner and larger in diameter. 2. The synthesis according to claim 1, wherein the first step is a step of molding in a high-purity graphite mold coated with a high-purity mold release material at a temperature range of 1600 to 1800°C. Method for manufacturing quartz glass tubes. 3. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the second step is cold machining. 4. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the second step is carried out in a graphite heating element installed in a high-frequency induction heating furnace. 5. The heating temperature in the second step is 1700 to 19
2. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the temperature is within a range of 00°C. 6. The gas pressure for pressurization in the second step is 0.
2. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the pressure is within a range of 0.01 to 2.0 atm. 7. In the second step of applying gas pressure to the inside of the cylindrical glass under heating and expanding it in a non-contact manner while stretching it in the length direction to make it thinner and larger in diameter, the thickness of the cylindrical glass is L_1.
The ratio of L_1/L to the thickness L_2 of the stretched thin glass
2. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein _2 is in the range of 2 to 20. 8. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the synthetic quartz glass block is made of quartz glass manufactured using silicon halide as a raw material. 9. The total amount of heavy metals contained in the synthetic quartz glass tube is
2. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the content is 1 ppm or less. 10. Annealing point of the synthetic quartz glass tube (log η = 13
．． 2. The method for manufacturing a synthetic quartz glass tube according to claim 1, wherein the concentration of the synthetic quartz glass tube is 1150° C. or higher. 11. Any one of claims 1, 8, 9 and 10.
A process tube for semiconductor manufacturing, characterized in that it uses a synthetic quartz glass tube manufactured by the method described in 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2130327A JP3039789B2 (en) | 1990-05-22 | 1990-05-22 | Manufacturing method of synthetic quartz glass tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2130327A JP3039789B2 (en) | 1990-05-22 | 1990-05-22 | Manufacturing method of synthetic quartz glass tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0426522A true JPH0426522A (en) | 1992-01-29 |
| JP3039789B2 JP3039789B2 (en) | 2000-05-08 |
Family
ID=15031704
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2130327A Expired - Fee Related JP3039789B2 (en) | 1990-05-22 | 1990-05-22 | Manufacturing method of synthetic quartz glass tube |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3039789B2 (en) |
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