JP2005126261A - Method for manufacturing multilayer quartz glass tube and multilayer quartz glass rod - Google Patents
Method for manufacturing multilayer quartz glass tube and multilayer quartz glass rod Download PDFInfo
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- JP2005126261A JP2005126261A JP2003361922A JP2003361922A JP2005126261A JP 2005126261 A JP2005126261 A JP 2005126261A JP 2003361922 A JP2003361922 A JP 2003361922A JP 2003361922 A JP2003361922 A JP 2003361922A JP 2005126261 A JP2005126261 A JP 2005126261A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 544
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 230
- 239000000843 powder Substances 0.000 claims abstract description 51
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 50
- 238000012545 processing Methods 0.000 claims description 13
- 239000011521 glass Substances 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 abstract description 11
- 238000003466 welding Methods 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 308
- 235000012239 silicon dioxide Nutrition 0.000 description 10
- 230000004888 barrier function Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000005553 drilling Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000002788 crimping Methods 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 150000003377 silicon compounds Chemical class 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
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Classifications
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- 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
- C03B23/049—Re-forming tubes or rods by pressing
- C03B23/0496—Re-forming tubes or rods by pressing for expanding in a radial way, e.g. by forcing a mandrel through a tube or rod
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B23/00—Re-forming shaped glass
- C03B23/20—Uniting glass pieces by fusing without substantial reshaping
- C03B23/207—Uniting glass rods, glass tubes, or hollow glassware
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
本発明は、１層又は２層以上の中間層を有する多層石英ガラス管及び多層石英ガラス棒の製造方法に関する。 The present invention relates to a multilayer quartz glass tube having one or two or more intermediate layers and a method for producing a multilayer quartz glass rod.
半導体の製造工程では、高温雰囲気下において半導体ウエーハ表面に酸化膜、絶縁膜あるいは単結晶膜等を生成させるために、酸化、拡散、気相成長等の熱処理がなされており、その装置内の炉芯管、ボート、搬送治具等には純度が高くかつ化学的に安定な石英ガラス素材(管材、棒材、板材)が使用されている。特に、これらの用途には高温領域で変形せず、耐熱性を有する天然石英ガラスが主として使用されてきた。 In the semiconductor manufacturing process, heat treatments such as oxidation, diffusion, and vapor phase growth are performed in order to generate an oxide film, an insulating film, or a single crystal film on the surface of the semiconductor wafer in a high temperature atmosphere. Quartz glass materials (tube materials, rod materials, plate materials) with high purity and chemical stability are used for core tubes, boats, conveyance jigs, and the like. In particular, natural quartz glass that does not deform at high temperatures and has heat resistance has been mainly used for these applications.
近年、半導体チップの高集積化及び微細化に伴って、石英ガラス製治具等からウエーハへの汚染防止と歩留まり向上の観点から、天然石英ガラスに代えて、純度的に優れた合成石英ガラスが石英ガラス製治具の素材として使用されるようになってきた。しかしながら、合成石英ガラスは、電気溶融法や酸水素火炎溶融法によって製造された天然石英ガラスに比べると耐熱性が悪く、高温熱処理時に変形しやすいといった問題を抱えている。 In recent years, with the high integration and miniaturization of semiconductor chips, synthetic quartz glass excellent in purity is used in place of natural quartz glass from the viewpoint of preventing contamination of wafers from quartz glass jigs and the like and improving yield. It has come to be used as a material for quartz glass jigs. However, synthetic quartz glass has a problem that it has poor heat resistance compared to natural quartz glass produced by an electric melting method or an oxyhydrogen flame melting method, and is easily deformed during high-temperature heat treatment.
上記の耐熱性の問題を解決する手段として、耐熱性が優れた天然石英ガラスと組み合わせて二層構造にする、あるいは耐熱性を向上させるためにドーピングした合成石英ガラスと組み合わせて二層構造にすることにより、合成石英ガラスの耐熱性を向上させる方法が提案されている。 As a means to solve the above heat resistance problem, it is combined with natural quartz glass having excellent heat resistance to form a two-layer structure, or combined with synthetic quartz glass doped to improve heat resistance to form a two-layer structure. Thus, a method for improving the heat resistance of synthetic quartz glass has been proposed.
ところが炉芯管の場合、使用前に表面の汚れを除去するために必ずＨＦ洗浄を実施するが、上記のような二層構造の石英ガラスを使用すると天然石英ガラス層やドーピング元素がＨＦ溶液中に溶出し、ＨＦ溶液のクリーン度を損なうおそれがある。 However, in the case of a furnace core tube, HF cleaning is always performed in order to remove dirt on the surface before use. However, when quartz glass having the two-layer structure as described above is used, the natural quartz glass layer and the doping element are contained in the HF solution. The HF solution may lose its cleanness.
特許文献１には、この問題を回避する手段として、天然石英ガラス層やドーピング元素含有層を更に合成石英ガラス層で封じ込めてなる複合構造を有する石英ガラス管が提案されている。
そして、複合構造を有する石英ガラス管の製造方法として、合成石英ガラス管表面に、予め核形成元素を核としてクリストバライト等の結晶層を形成しておき、(1)シラン（ＳｉＨ４）の酸化反応が生じている雰囲気中に投入し、二酸化珪素（ＳｉＯ２）を結晶層の表面に堆積させる方法、及び、(2)結晶層表面に珪素化合物（シラノール）を塗布し、更に熱分解を行い、溶媒を揮発させると共に脱水し、二酸化珪素を堆積させる方法、が紹介されている。 As a method for producing a quartz glass tube having a composite structure, a crystal layer such as cristobalite is formed in advance on the surface of a synthetic quartz glass tube using a nucleating element as a nucleus, and (1) oxidation reaction of silane (SiH 4 ) And in a method of depositing silicon dioxide (SiO 2 ) on the surface of the crystal layer, and (2) applying a silicon compound (silanol) to the surface of the crystal layer, and further performing thermal decomposition, A method of volatilizing and dehydrating the solvent and depositing silicon dioxide is introduced.
これらの方法は、確かに結晶層表面に二酸化珪素のバリア層を堆積させ、ＨＦ溶液の汚染を防止するが、化学反応を利用していることからそのバリア層は堆積させるのに非常に時間がかかるとともに、形成されたバリア層は非常に薄いものである。したがって、ＨＦ洗浄を数回繰り返すと、バリア層がＨＦ溶液中に溶出し、バリア層が消失し結晶層がＨＦ溶液中に溶出するおそれがある。また、珪素化合物（シラノール）を使用する方法においては、塗布時に溶媒を使用するため、バリア層の純度が低下するおそれがある。 These methods certainly deposit a silicon dioxide barrier layer on the crystal layer surface to prevent contamination of the HF solution, but because of the chemical reaction, the barrier layer is very time consuming to deposit. In addition, the formed barrier layer is very thin. Therefore, when HF cleaning is repeated several times, the barrier layer may be eluted in the HF solution, the barrier layer may disappear, and the crystal layer may be eluted in the HF solution. Moreover, in the method using a silicon compound (silanol), since a solvent is used at the time of application | coating, there exists a possibility that the purity of a barrier layer may fall.
特許文献２には、外径の異なる２種類の石英ガラス管素管を組み合わせて二重構造の石英ガラス管を成形し、この二重構造石英ガラス管の隙間に核生成剤とシリカ粉末の混合物を充填し、それを上部から真空引きしつつ円筒型電気溶融炉で加熱し延伸して、３層構造石英ガラス管を製造する方法が記載されている。
In
この方法は、予め、特定の形状を有する石英ガラス管素管を２種類用意する必要がある。そして、その素管は、偏肉率や曲がりの精度等の寸法精度が求められ、この特定の寸法精度が良くなければ、最終生成物である３層構造石英ガラス管の形状は不適正となる。 In this method, it is necessary to prepare two types of quartz glass tube tubes having a specific shape in advance. Then, the base tube is required to have a dimensional accuracy such as an uneven thickness ratio and a bending accuracy. If this specific dimensional accuracy is not good, the shape of the three-layer structured quartz glass tube which is the final product is inappropriate. .
さらに、特許文献２には、一旦２層構造ロッドを作製し、熱間ドリル圧入法とよばれる方法で２層構造石英ガラス管を作製する方法が提案されている。しかしながら、この方法は、内層ロッドと外層シリンダーを加熱溶着させ２層構造ロッドを作製する工程と、２層ロッドを炭素ドリルで開孔する工程の２工程を必要とするものであるので、非効率であるだけでなく、一旦２層構造ロッドを作製する際に内層の偏芯が生じ、これが次工程の開孔精度に影響し、最終的に得られる２層構造管の寸法精度を悪化させる。
Furthermore,
本発明の目的は、１層又は２層以上の中間層を有する多層石英ガラス管及び多層石英ガラス棒を寸法精度よく製造することができる方法を提供することにある。 An object of the present invention is to provide a method capable of producing a multilayer quartz glass tube having a single layer or two or more intermediate layers and a multilayer quartz glass rod with high dimensional accuracy.
本発明にかかる、１層又は２層以上の中間層を有する多層石英ガラス管及び多層石英ガラス棒の製造方法は、次の(1)から(11)までのいずれかである。以下、それぞれ、本発明(1)〜本発明(11)という。本発明(1)〜本発明(11)を総称して、本発明ということがある。 The method for producing a multilayer quartz glass tube having a single layer or two or more intermediate layers and a multilayer quartz glass rod according to the present invention is any of the following (1) to (11). Hereinafter, the present invention (1) to the present invention (11), respectively. The present invention (1) to the present invention (11) may be collectively referred to as the present invention.
(1) 最外層素材として石英ガラス素管を、中間層素材として石英ガラス素管又はシリカ粉末を、そして最内層素材として石英ガラス棒を、それぞれ用いて棒状の多層石英ガラス素材を形成し、多層石英ガラス素材の片端部の端面の軸中心部にプラグを、片端部の外周にダイスを、それぞれ設置し、多層石英ガラス素材をダイス及びプラグに対して相対的な軸中心の回転を与えつつ、多層石英ガラス素材の片端から順次加熱軟化させて軸方向に沿って移動させて、その加熱軟化部分をプラグとダイスによって形成される空間部に圧入して送り込むことにより、多層石英ガラス素材の加熱軟化部分の最内層素材を穿孔するとともに多層石英ガラス素材を圧着させることを特徴とする、１層又は２層以上の中間層を有する多層石英ガラス管の製造方法。 (1) A rod-shaped multilayer quartz glass material is formed using a quartz glass tube as the outermost layer material, a quartz glass tube or silica powder as the intermediate layer material, and a quartz glass rod as the innermost layer material. While installing a plug in the axial center part of the end face of one end of the quartz glass material and a die on the outer periphery of the one end part, while giving the rotation of the axis center relative to the die and the plug, Heating and softening the multilayer quartz glass material by sequentially heating and softening from one end of the multilayer silica glass material and moving it along the axial direction, and press-fitting the heat-softened part into the space formed by the plug and the die. A method for producing a multilayer quartz glass tube having one or two or more intermediate layers, wherein the innermost layer material of a portion is perforated and the multilayer quartz glass material is pressure-bonded .
(2) 最外層素材及び最内層素材として石英ガラス素管を、そして中間層素材として石英ガラス素管又はシリカ粉末を、それぞれ用いて管状の多層石英ガラス素材を形成し、多層石英ガラス素材の片端部の端面の軸中心部にプラグを、片端部の外周にダイスを、それぞれ設置し、多層石英ガラス素材をダイス及びプラグに対して相対的な軸中心の回転を与えつつ、多層石英ガラス素材の片端から順次加熱軟化させて軸方向に沿って移動させて、その加熱軟化部分をプラグとダイスによって形成される空間部に圧入して送り込むことにより、多層石英ガラス素材の加熱軟化部分を圧着させることを特徴とする、１層又は２層以上の中間層を有する多層石英ガラス管の製造方法。 (2) A tubular multilayer quartz glass material is formed using a quartz glass element tube as the outermost layer material and innermost layer material, and a quartz glass element tube or silica powder as the intermediate layer material, respectively. A plug is installed at the axial center of the end face of the part, a die is installed at the outer periphery of one end part, and the multilayer quartz glass material is rotated relative to the die and the plug while rotating the axis center relative to the die and the plug. Heating and softening sequentially from one end, moving along the axial direction, press-fitting the heat-softening part into the space formed by the plug and die, and crimping the heat-softening part of the multilayer quartz glass material A method for producing a multilayer quartz glass tube having one or two or more intermediate layers.
(3) 多層石英ガラス素材の中間層として１本又は同軸上に重なった複数本の石英ガラス素管を用いて多層石英ガラス素材を形成することを特徴とする、上記(1)又は(2)の石英ガラス管の製造方法。 (3) The multilayer silica glass material is formed by using one or a plurality of quartz glass base tubes overlapping on the same axis as an intermediate layer of the multilayer quartz glass material, (1) or (2) Manufacturing method of quartz glass tube.
(4) 多層石英ガラス素材の中間層としてシリカ粉末を用いて多層石英ガラス素材を形成することを特徴とする、上記(1)又は(2)の石英ガラス管の製造方法。 (4) The method for producing a quartz glass tube according to (1) or (2), wherein the multilayer quartz glass material is formed using silica powder as an intermediate layer of the multilayer quartz glass material.
(5) 多層石英ガラス素材の中間層として１本又は同軸上に重なった複数本の石英ガラス素管とシリカ粉末を用いて多層石英ガラス素材を形成することを特徴とする、上記(1)又は(2)の石英ガラス管の製造方法。 (5) The multilayer quartz glass material is formed by using one or a plurality of quartz glass elementary tubes that are coaxially overlapped and silica powder as an intermediate layer of the multilayer quartz glass material, (2) A method for producing a quartz glass tube.
(6) 多層石英ガラス素材の加熱軟化部分をプラグとダイスによって形成される空間部に圧入して送り込む際に、多層石英ガラス素材及び／又は一体化加工後の多層石英ガラス管の内部を大気圧未満に減圧することを特徴とする、上記(1)〜(5)のいずれかの石英ガラス管の製造方法。 (6) When the heat-softened portion of the multilayer quartz glass material is press-fitted into the space formed by the plug and the die, the atmospheric pressure is applied to the interior of the multilayer quartz glass material and / or the integrated multilayer quartz glass tube. The method for producing a quartz glass tube according to any one of the above (1) to (5), wherein the pressure is reduced to below.
(7) 最外層素材として石英ガラス素管を、中間層素材として石英ガラス素管又はシリカ粉末を、そして最内層素材として石英ガラス素管又は石英ガラス棒を、それぞれ用いて管状又は棒状の多層石英ガラス素材を形成し、多層石英ガラス素材の片端部の外周にダイスを設置し、多層石英ガラス素材をダイスに対して相対的な軸中心の回転を与えつつ、多層石英ガラス素材の片端から順次加熱軟化させて軸方向に沿って移動させて、その加熱軟化部分をダイス内に圧入して送り込むことにより、多層石英ガラス素材の加熱軟化部分を圧着させることを特徴とする、１層又は２層以上の中間層を有する多層石英ガラス棒の製造方法。 (7) Quartz glass tube as the outermost layer material, quartz glass tube or silica powder as the intermediate layer material, and quartz glass tube or quartz glass rod as the innermost layer material, tubular or rod-shaped multilayer quartz A glass material is formed, a die is placed on the outer periphery of one end of the multilayer quartz glass material, and the multilayer quartz glass material is heated sequentially from one end of the multilayer quartz glass material while giving rotation of the axis center relative to the die. One layer or two or more layers characterized in that the heat softened portion of the multilayer quartz glass material is pressure-bonded by being softened and moved along the axial direction, and the heat softened portion is press-fitted into a die and fed. A method for producing a multilayer quartz glass rod having an intermediate layer.
(8) 多層石英ガラス素材の中間層として１本又は同軸上に重なった複数本の石英ガラス素管を用いて多層石英ガラス素材を形成することを特徴とする、上記(7)の石英ガラス棒の製造方法。 (8) The quartz glass rod according to (7), wherein a multilayer quartz glass material is formed by using one or a plurality of quartz glass tubes that are coaxially overlapped as an intermediate layer of the multilayer quartz glass material. Manufacturing method.
(9) 多層石英ガラス素材の中間層としてシリカ粉末を用いて多層石英ガラス素材を形成することを特徴とする、上記(7)の石英ガラス棒の製造方法。 (9) The method for producing a quartz glass rod according to (7), wherein the multilayer quartz glass material is formed using silica powder as an intermediate layer of the multilayer quartz glass material.
(10) 多層石英ガラス素材の中間層として１本又は同軸上に重なった複数本の石英ガラス素管とシリカ粉末を用いて多層石英ガラス素材を形成することを特徴とする、上記(7)の石英ガラス棒の製造方法。 (10) The multilayer quartz glass material according to (7), wherein the multilayer quartz glass material is formed by using one or a plurality of quartz glass base tubes that are coaxially overlapped and silica powder as an intermediate layer of the multilayer quartz glass material. Manufacturing method of quartz glass rod.
(11) 多層石英ガラス素材の加熱軟化部分をダイス内に圧入して送り込む際に多層石英ガラス素材の内部を大気圧未満に減圧することを特徴とする、上記(6)〜(10)のいずれかの石英ガラス棒の製造方法。 (11) Any of the above (6) to (10), characterized in that the inside of the multilayer quartz glass material is decompressed to less than atmospheric pressure when the heat-softened portion of the multilayer quartz glass material is pressed into the die and fed. A method for manufacturing such quartz glass rods.
本発明によれば、種々の寸法の多層石英ガラス管及び多層石英ガラス棒を寸法精度よく、製造することができる。また、中間層のガラス層を形成させる素材として石英ガラス管でもシリカ粉末(水晶粉)でも使用可能である。さらに、中間層のガラス層の素材として使用される石英ガラス管やシリカ粉末の種類を増やすことによって、より多層構造の石英ガラス管の製造も可能である。 According to the present invention, multilayer quartz glass tubes and multilayer quartz glass rods of various dimensions can be manufactured with high dimensional accuracy. Further, a quartz glass tube or silica powder (quartz powder) can be used as a material for forming an intermediate glass layer. Furthermore, it is possible to manufacture a quartz glass tube having a multilayer structure by increasing the types of silica glass tubes and silica powders used as the material for the glass layer of the intermediate layer.
本発明に係る、１層又は２層以上の中間層を有する多層石英ガラス管の製造方法は、まず、素材として、最内層に石英ガラス棒又は石英ガラス素管を用い、かつその他の層に石英ガラス素管を用いて、あるいはさらにシリカ粉末を組み合わせて用いて、棒状又は管状の多層石英ガラス素材を形成する。 According to the present invention, a method for producing a multilayer quartz glass tube having one or two or more intermediate layers first uses a quartz glass rod or quartz glass tube as the innermost layer, and quartz for the other layers. A rod-like or tubular multilayer quartz glass material is formed using a glass tube or a combination of silica powder.
そして、多層石英ガラス素材の片端部の端面の軸中心部にプラグを、片端部の外周にダイスを、それぞれ設置し、多層石英ガラス素材をダイス及びプラグに対して相対的な軸中心の回転を与えつつ、多層石英ガラス素材の片端から順次加熱軟化させて軸方向に沿って移動させて、その加熱軟化部分をプラグとダイスによって形成される空間部に圧入して送り込むことにより、多層石英ガラス素材の加熱軟化部分の最内層素材を穿孔するとともに多層石英ガラス素材を圧着させるものである。なお、この穿孔・圧着の際に、拡径若しくは縮径することや同一径のままとすることもできるので、様々な外径と内径を有する多層石英ガラス管を製造することができる。 A plug is installed at the axial center of one end of the multilayer quartz glass material, a die is installed at the outer periphery of the one end, and the multilayer quartz glass material is rotated about its axis relative to the die and the plug. The multilayer quartz glass material is heated and softened sequentially from one end of the multilayer quartz glass material while being fed and moved along the axial direction, and the heat-softened portion is press-fitted into the space formed by the plug and the die to feed it. The innermost layer material of the heat-softened portion is perforated and the multilayer quartz glass material is pressure-bonded. In addition, since the diameter can be expanded or reduced during the drilling / compression, or the same diameter can be maintained, multilayer quartz glass tubes having various outer diameters and inner diameters can be manufactured.
多層石英ガラス素材の最内層素材として石英ガラス棒に代えて石英ガラス素管を用いる場合は、多層石英ガラス素材の加熱軟化部分の最内層素材を穿孔する必要はないが、多層石英ガラス素材の加熱軟化部分を圧着する際に、様々な内径を有する多層石英ガラス管を得るためにプラグが用いられる。このように、拡径若しくは縮径することや同一径のままとすることもできるので、様々な外径と内径を有する多層石英ガラス管を製造することができる。 When a quartz glass tube is used instead of the quartz glass rod as the innermost layer material of the multilayer quartz glass material, it is not necessary to perforate the innermost layer material of the heat softened portion of the multilayer quartz glass material, but the heating of the multilayer quartz glass material is not necessary. When crimping the softened part, a plug is used to obtain a multilayer quartz glass tube having various inner diameters. In this way, the diameter can be expanded or reduced, or the diameter can be kept the same, so that multilayer quartz glass tubes having various outer diameters and inner diameters can be manufactured.
また、本発明に係る、１層又は２層以上の中間層を有する多層石英ガラス棒の製造方法は、まず、素材として、最内層に石英ガラス素管又は石英ガラス棒を用い、かつその他の層に石英ガラス素管を用いて、あるいはさらにシリカ粉末を組み合わせて用いて、多層石英ガラス素材を形成する。 In the method for producing a multilayer quartz glass rod having one or more intermediate layers according to the present invention, first, as a material, a quartz glass base tube or quartz glass rod is used as the innermost layer, and the other layers A multilayer quartz glass material is formed using a quartz glass tube or a combination of silica powder.
そして、多層石英ガラス素材の片端部の外周にダイスを設置し、多層石英ガラス素材をダイスに対して相対的な軸中心の回転を与えつつ、多層石英ガラス素材の片端から順次加熱軟化させて軸方向に沿って移動させて、その加熱軟化部分をダイス内に圧入して送り込むことにより、多層石英ガラス素材の加熱軟化部分を圧着させるものである。この場合も、この圧着の際に、拡径若しくは縮径することや同一径のままとすることもできるので、様々な外径を有する多層石英ガラス棒を製造することができる。 Then, a die is installed on the outer periphery of one end of the multilayer quartz glass material, and the multilayer quartz glass material is heated and softened sequentially from one end of the multilayer quartz glass material while giving rotation of the axis center relative to the die. The heat softened portion of the multilayer quartz glass material is pressure-bonded by moving along the direction and press-fitting the heat softened portion into a die. Also in this case, the diameter can be increased or reduced during the pressure bonding, or the diameter can be kept the same, so that multilayer quartz glass rods having various outer diameters can be manufactured.
本発明に係る、１層又は２層以上の中間層を有する多層石英ガラス管又は多層石英ガラス棒の製造方法において、多層石英ガラス素材は、最外層に石英ガラス管、最内層に石英ガラス棒又は石英ガラス素管を用いることは固定されているが、中間層においては次の(1)〜(4)に記載したとおり、種々の組み合せがある。 In the method for producing a multilayer quartz glass tube or multilayer quartz glass rod having one or more intermediate layers according to the present invention, the multilayer quartz glass material is composed of a quartz glass tube as the outermost layer and a quartz glass rod as the innermost layer. Although the use of the quartz glass tube is fixed, there are various combinations in the intermediate layer as described in the following (1) to (4).
(1) ３層石英ガラス管を形成するための線状素材の組み合せ：下記(a)〜(d)の４通り
(a)最外層：石英ガラス素管、
中間層：石英ガラス素管、
最内層：石英ガラス棒
(b)最外層：石英ガラス素管、
中間層：石英ガラス素管、
最内層：石英ガラス素管
(c)最外層：石英ガラス素管、
中間層：シリカ粉末、
最内層：石英ガラス棒
(d)最外層：石英ガラス素管、
中間層：シリカ粉末、
最内層：石英ガラス素管
(2) ４層以上の石英ガラス管を形成するための線状素材の組合せ：下記(a)〜(d)の４通り
(a)最外層：石英ガラス素管、
中間層：複数本の石英ガラス素管、
最内層：石英ガラス棒
(b)最外層：石英ガラス素管、
中間層：複数本の石英ガラス素管、
最内層：石英ガラス素管
(c)最外層：石英ガラス素管、
中間層：１本以上の石英ガラス素管と１種類以上のシリカ粉末、
最内層：石英ガラス棒
(d)最外層：石英ガラス素管、
中間層：１本以上の石英ガラス素管と１種類以上のシリカ粉末、
最内層：石英ガラス素管
(3) ３層石英ガラス棒を形成するための線状素材の組合せ：下記(a)〜(d)の４通り
(a)最外層：石英ガラス素管、
中間層：石英ガラス素管、
最内層：石英ガラス棒
(b)最外層：石英ガラス素管、
中間層：石英ガラス素管、
最内層：石英ガラス素管
(c)最外層：石英ガラス素管、
中間層：シリカ粉末、
最内層：石英ガラス棒
(d)最外層：石英ガラス素管、
中間層：シリカ粉末、
最内層：石英ガラス素管
(4) ４層以上の石英ガラス棒を形成するための線状素材の組合せ：下記(a)〜(d)の４通り
(a)最外層：石英ガラス素管、
中間層：複数本の石英ガラス素管、
最内層：石英ガラス棒
(b)最外層：石英ガラス素管、
中間層：複数本の石英ガラス素管、
最内層：石英ガラス素管
(c)最外層：石英ガラス素管、
中間層：１本以上の石英ガラス素管と１種類以上のシリカ粉末、
最内層：石英ガラス棒
(d)最外層：石英ガラス素管、
中間層：１本以上の石英ガラス素管と１種類以上のシリカ粉末、
最内層：石英ガラス素管
以下に、図面を用いて、本発明を説明する。
(1) Combination of linear materials to form a three-layer quartz glass tube: 4 types (a) to (d) below
(a) Outermost layer: quartz glass tube,
Intermediate layer: Silica glass tube,
Innermost layer: quartz glass rod
(b) Outermost layer: quartz glass tube,
Intermediate layer: Silica glass tube,
Innermost layer: quartz glass tube
(c) Outermost layer: quartz glass tube,
Intermediate layer: silica powder,
Innermost layer: quartz glass rod
(d) Outermost layer: quartz glass tube,
Intermediate layer: silica powder,
Innermost layer: quartz glass tube
(2) Combinations of linear materials to form four or more layers of quartz glass tubes: 4 types (a) to (d) below
(a) Outermost layer: quartz glass tube,
Intermediate layer: Multiple quartz glass tubes,
Innermost layer: quartz glass rod
(b) Outermost layer: quartz glass tube,
Intermediate layer: Multiple quartz glass tubes,
Innermost layer: quartz glass tube
(c) Outermost layer: quartz glass tube,
Intermediate layer: one or more quartz glass tubes and one or more types of silica powder,
Innermost layer: quartz glass rod
(d) Outermost layer: quartz glass tube,
Intermediate layer: one or more quartz glass tubes and one or more types of silica powder,
Innermost layer: quartz glass tube
(3) Combination of linear materials to form a three-layer quartz glass rod: 4 types (a) to (d) below
(a) Outermost layer: quartz glass tube,
Intermediate layer: Silica glass tube,
Innermost layer: quartz glass rod
(b) Outermost layer: quartz glass tube,
Intermediate layer: Silica glass tube,
Innermost layer: quartz glass tube
(c) Outermost layer: quartz glass tube,
Intermediate layer: silica powder,
Innermost layer: quartz glass rod
(d) Outermost layer: quartz glass tube,
Intermediate layer: silica powder,
Innermost layer: quartz glass tube
(4) Combination of linear materials to form four or more layers of quartz glass rods: 4 types (a) to (d) below
(a) Outermost layer: quartz glass tube,
Intermediate layer: Multiple quartz glass tubes,
Innermost layer: quartz glass rod
(b) Outermost layer: quartz glass tube,
Intermediate layer: Multiple quartz glass tubes,
Innermost layer: quartz glass tube
(c) Outermost layer: quartz glass tube,
Intermediate layer: one or more quartz glass tubes and one or more types of silica powder,
Innermost layer: quartz glass rod
(d) Outermost layer: quartz glass tube,
Intermediate layer: one or more quartz glass tubes and one or more types of silica powder,
Innermost layer: quartz glass tube The present invention will be described below with reference to the drawings.
図１は、３層石英ガラス管の製造の態様を示したものである。 FIG. 1 shows an embodiment of manufacturing a three-layer quartz glass tube.
ここでは、３層石英ガラス素材は、最外層素材１及び中間層素材２として石英ガラス素管、そして最内層素材３として石英ガラス棒を、それぞれ、用いて形成されたものである。３層石英ガラス素材の片端と他端にはダミーシリンダー５がそれぞれ溶着によって取り付けられ、回転及び水平移動の可能な出側チャック１０及び入側チャック１１に、それぞれ把持される。
Here, the three-layer quartz glass material is formed using a quartz glass base tube as the
入側チャック１１と出側チャック１０の間にはヒーター１５が設置されている。３層石英ガラス素材は左から右の方向へ入側チャック１１とともに移動し、ヒーター１５によりその片端から順次加熱軟化されて軸方向に沿って移動し、その加熱軟化部分がプラグ２０とダイス２１によって形成される空間部に圧入して送り込まれる。なお、プラグはマンドレル２２によって保持されている。
A
３層石英ガラス素材の加熱軟化部分の最内層素材である石英ガラス棒は、プラグ２０により穿孔され、中間層素材である石英ガラス素管の内面と圧着され、また、最外層素材である石英ガラス素管は、ダイス２１により中間層素材である石英ガラス素管の外面と圧着されされ、３層全体が一体化された３層石英ガラス管が形成される。
The quartz glass rod, which is the innermost layer material of the heat-softened portion of the three-layer quartz glass material, is perforated by the
図２は、一体化された３層石英ガラス管が形成される工程を示す、プラグ及びダイス近傍の拡大模式図である。このように３層石英ガラス素材は順次加熱され、穿孔及び圧着の加工により、一体化された３層石英ガラス管３０が順次に形成され、３層石英ガラス素材の他端まで加工される。
FIG. 2 is an enlarged schematic view in the vicinity of a plug and a die, showing a process of forming an integrated three-layer quartz glass tube. In this way, the three-layer quartz glass material is sequentially heated, and the integrated three-layer
そして、入側チャックの移動速度と出側チャックの移動速度の比は、３層石英ガラス素材の断面積と、一体化加工により形成される３層石英ガラス管の断面積の比の逆数に設定される。また、入側チャックの回転速度と出側チャックの回転速度は、各断面での３層の厚みを一定比率に維持するため、速度差がない方が望ましい。 The ratio of the moving speed of the inlet chuck and the moving speed of the outlet chuck is set to the reciprocal of the ratio of the cross-sectional area of the three-layer quartz glass material and the cross-sectional area of the three-layer quartz glass tube formed by the integrated processing. Is done. Further, it is desirable that the rotational speed of the entrance side chuck and the rotational speed of the exit side chuck have no speed difference in order to maintain the thickness of the three layers in each cross section at a constant ratio.
この一体化加工の際、３層石英ガラス素材は水平方向の軸の周りに回転させながら、その加熱軟化部分をダイス２１及びプラグ２０によって形成される空間部に圧入して送り込ませる。これは３層石英ガラス素材の円周方向の加熱状態を均一にし、偏芯を抑制し寸法精度を向上させると共に、一体化加工される３層石英ガラス管の各界面での空孔の発生を抑制するためである。なお、回転速度が遅ければ均熱効果が不十分であり、速すぎるとダイスやプラグとの接触頻度が増し、それらの損耗が激しくなると共に、得られた３層石英ガラス管３０の表面性状も損なわれるので、回転速度は５〜２０ｒｐｍ程度が好ましい。
At the time of this integration processing, the three-layer quartz glass material is pressed around and fed into the space formed by the
ここまでは、最内層素材として石英ガラス棒を用いた３層石英ガラス素材により、３層石英ガラス管を製造する方法を説明してきたが、最内層素材として石英ガラス棒を用いる代わりに、石英ガラス素管を用いた３層石英ガラス素材でもよい。 Up to this point, a method of manufacturing a three-layer quartz glass tube with a three-layer quartz glass material using a quartz glass rod as the innermost layer material has been described, but instead of using a quartz glass rod as the innermost layer material, quartz glass is used. A three-layer quartz glass material using a raw tube may be used.
図３に、最内層素材３として石英ガラス素管を用いた３層石英ガラス素材から、３層石英ガラス管３０を製造する際のダイス及びプラグ近傍の断面模式図を示す。最内層素材３として石英ガラス素管を用いることにより、３層石英ガラス素材を成形用ダイス及びプラグに圧入する時の負荷を軽減することが可能である。また、形成される３層石英ガラス管３０の偏肉を低減することができ、したがって、３層石英ガラス管の寸法精度をより向上させることができる。
FIG. 3 shows a schematic cross-sectional view in the vicinity of a die and a plug when a three-layer
これまでは、中間層素材２として石英ガラス素管を用いた３層石英ガラス素材により、３層石英ガラス管３０を製造する方法を説明してきたが、中間層素材２として石英ガラス素管を用いる代わりに、シリカ粉末を用いた３層石英ガラス素材でもよい。
So far, the method of manufacturing the three-layer
図４に、中間層素材２としてシリカ粉末を用いた３層石英ガラス素材から、３層石英ガラス管３０を製造する際のダイス及びプラグ近傍の断面模式図を示す。ここで、最外層素材１が石英ガラス素管、最内層素材３が石英ガラス棒である。
FIG. 4 is a schematic cross-sectional view in the vicinity of a die and a plug when a three-layer
図５は、同じく中間層素材２としてシリカ粉末を用いた３層石英ガラス素材から３層石英ガラス管３０を製造する例であるが、ここでは、最外層素材１が石英ガラス素管、最内層素材３が石英ガラス素管である。
FIG. 5 shows an example in which a three-layer
ここまでは３層石英ガラス管を製造する方法を説明してきたが、石英ガラス素材を４層あるいはそれ以上の多層とすることにより、４層あるいはそれ以上の多層石英ガラス管を製造することができる。なお、中間層素材としてシリカ粉末を用いると、中間層に石英ガラスの特性向上元素等を比較的容易に添加することができる。 Up to this point, the method of manufacturing a three-layer quartz glass tube has been described. However, by forming a quartz glass material into four or more layers, a four-layer or more multilayer quartz glass tube can be manufactured. . In addition, when silica powder is used as the intermediate layer material, it is possible to relatively easily add an element for improving characteristics of quartz glass or the like to the intermediate layer.
図６に、最外層素材１として石英ガラス素管、第１中間層素材５２として石英ガラス素管、第２中間層素材６２としてシリカ粉末、そして最内層素材３として石英ガラス管からなる４層石英ガラス素材を用いて、４層石英ガラス管７０を製造する際のダイス及びプラグ近傍の断面模式図を示す。
FIG. 6 shows a quartz glass tube as the
なお、図１〜６では、圧着あるいは穿孔・圧着の一体化加工時に、多層石英ガラス素材の外径に対し、得られる多層石英ガラス管の外径が拡径される場合を示したが、本発明は拡径するだけでなく、一体化加工後の多層石英ガラス管の外径を逆に縮径させることも可能であり、また同一径とすることも可能である。 1 to 6 show a case where the outer diameter of the obtained multilayer quartz glass tube is expanded with respect to the outer diameter of the multilayer quartz glass material at the time of pressing or integrated processing of drilling and pressing. The invention not only expands the diameter, but also allows the outer diameter of the multilayer quartz glass tube after integrated processing to be reduced, and the diameter can be made the same.
このように、ダイスの内径とプラグの外径を選定し、入側チャックと出側チャックの、それぞれの走行速度を調整することにより、同じ寸法の多層石英ガラス素材から、種々の外径及び内径を有する多層石英ガラス管を製造することができる。 In this way, by selecting the inner diameter of the die and the outer diameter of the plug, and adjusting the respective traveling speeds of the inlet side chuck and the outlet side chuck, various outer diameters and inner diameters can be obtained from multilayer quartz glass materials having the same dimensions. A multilayer quartz glass tube having the following can be manufactured.
多層石英ガラス素材を構成する石英ガラス棒又は素管の材料としては、ＶＡＤ法などで製造される合成石英ガラスでも、水晶粉などを原料にし天然石英ガラスでもいずれでもよく、特には限定しない。また、同様に中間層形成用として使用されるシリカ粉末も、ゾルーゲル法などで人工的に製造される合成粉末でも、天然から得られる水晶粉でもいずれでも良く、特には限定しない。また、最終的に最外層、中間層、最内層の各層に用いられる石英ガラス材料の組み合わせも目的に応じ自在であり、中間層の形成においても石英ガラス素管又はシリカ粉末と目的に応じ自在に選択できる。 The material of the quartz glass rod or the raw tube constituting the multilayer quartz glass material may be either synthetic quartz glass manufactured by the VAD method or the like, or natural quartz glass using quartz powder as a raw material, and is not particularly limited. Similarly, the silica powder used for forming the intermediate layer may be either a synthetic powder artificially produced by a sol-gel method or the like, or a quartz powder obtained from nature, and is not particularly limited. In addition, the combination of quartz glass materials finally used for the outermost layer, the intermediate layer, and the innermost layer can be freely selected according to the purpose, and also in the formation of the intermediate layer, it can be freely selected depending on the purpose of the quartz glass tube or silica powder. You can choose.
本発明では、多層石英ガラス素材を構成する各層の断面積比は、加工後の多層石英ガラス管の各層の断面積比と同じであるので、各層の厚さの比は多層石英ガラス素材の各層を構成する各石英ガラス材料あるいは充填されるシリカ粉末の断面積比で調整する必要がある。なお、同じ寸法の多層石英ガラス素材からであっても、ダイスとプラグの選定により種々の外径及び内径を有する多層石英ガラス管を製造することができる。 In the present invention, the cross-sectional area ratio of each layer constituting the multi-layer quartz glass material is the same as the cross-sectional area ratio of each layer of the multi-layer quartz glass tube after processing. It is necessary to adjust by the cross-sectional area ratio of each quartz glass material or silica powder to be filled. In addition, even if it is from the multilayer quartz glass raw material of the same dimension, the multilayer quartz glass tube which has various outer diameters and internal diameters by selection of a die | dye and a plug can be manufactured.
多層石英ガラス素材の各層に、石英ガラス棒あるいは石英ガラス素管が隣り合う形で用いられる場合の石英ガラス棒あるいは石英ガラス素管の隙間は０．５〜１０ｍｍとするのが好ましい。この隙間は小さいほど好ましいが、０．５ｍｍを下回ると、石英ガラス素管内に、石英ガラス棒あるいは石英ガラス素管を挿入する際、接触により傷が発生し、得られる多層石英ガラス管の各層の境界に傷が残る場合がある。１０ｍｍを超えると、得られる多層石英ガラス管の各層の境界に空孔が発生したり、内径が偏芯し寸法精度が損なわれる場合がある。 When a quartz glass rod or a quartz glass base tube is used adjacent to each layer of the multilayer quartz glass material, the gap between the quartz glass rod or the quartz glass base tube is preferably 0.5 to 10 mm. The gap is preferably as small as possible. However, if the gap is less than 0.5 mm, when a quartz glass rod or quartz glass element tube is inserted into the quartz glass element tube, scratches are caused by contact, and each layer of the resulting multilayer quartz glass tube Scratches may remain at the boundary. If it exceeds 10 mm, voids may be generated at the boundaries between the layers of the resulting multilayer quartz glass tube, or the inner diameter may be decentered and the dimensional accuracy may be impaired.
また、中間層素材としてシリカ粉末を使用する場合は、密に充填するのが好ましい。充填状態が良くないと、得られる多層石英ガラス管の各層の境界に空孔が残る場合があり、寸法精度に影響を及ぼす場合もあるからである。 Moreover, when using silica powder as an intermediate | middle layer raw material, it is preferable to pack densely. This is because if the filling state is not good, voids may remain at the boundary between the layers of the resulting multilayer quartz glass tube, which may affect the dimensional accuracy.
一体化加工時の多層石英ガラス素材の加熱温度は、軟化点がＯＨ基濃度やＣｌ濃度により大きく変化するので一概には決められない。多層石英ガラス素材の加熱は、ダイスの直前で最も高い温度になり、それよりやや低下したところでダイスに、あるいはさらにプラグに接して成形されるようにするのが好ましい。 The heating temperature of the multilayer quartz glass material at the time of integrated processing cannot be determined unconditionally because the softening point varies greatly depending on the OH group concentration and Cl concentration. It is preferable that the multilayer quartz glass material is heated at the highest temperature immediately before the dice, and is formed on the die or further in contact with the plug at a temperature slightly lower than that.
ヒーターの設定温度は２０００〜２７００℃程度となる。これらの温度域に適用できるダイスやプラグの材料は、酸化アルミナ系の酸化物、タングステン、モリブデン等の金属や黒鉛等に限られるが、高温域での強度並びに純度の面から黒鉛が最適である。なお、酸化防止のため不活性雰囲気中で一体化加工されるのが好ましい。 The set temperature of the heater is about 2000 to 2700 ° C. Dies and plug materials that can be used in these temperature ranges are limited to oxides of alumina oxide, metals such as tungsten and molybdenum, graphite, etc., but graphite is optimal in terms of strength and purity at high temperatures. . In order to prevent oxidation, it is preferable to perform integrated processing in an inert atmosphere.
さらに、多層石英ガラス管を製造する際に、多層石英ガラス素材の内部あるいは一体化加工後の多層石英ガラス管の内部を減圧すると、得られる多層石英ガラス管の寸法精度の向上を図ることができるし、各層の境界における気泡の発生を抑制することもできる。減圧することによって、気泡の原因となる気体が排除され、またダイスに入る前の多層石英ガラス素材の各層間の隙間やシリカ粉末との隙間が減少するからであると推定される。また、内径の寸法精度が向上するのは、得られる多層石英ガラス管の内面がプラグの径部に沿って開孔されるためと思われる。 Further, when the multilayer quartz glass tube is manufactured, if the inside of the multilayer quartz glass material or the interior of the multilayer quartz glass tube after integrated processing is decompressed, the dimensional accuracy of the resulting multilayer quartz glass tube can be improved. In addition, the generation of bubbles at the boundary between the layers can be suppressed. It is presumed that by reducing the pressure, the gas that causes bubbles is eliminated, and the gap between the layers of the multilayer quartz glass material and the gap with the silica powder before entering the die are reduced. Further, the reason why the dimensional accuracy of the inner diameter is improved is considered that the inner surface of the obtained multilayer quartz glass tube is opened along the diameter portion of the plug.
多層石英ガラス素材の内部あるいは一体化加工後の多層石英ガラス管の内部を減圧する方法を、図１を用いて説明する。多層石英ガラス素材から多層石英ガラス管を製造する際に、加工中の管の両端に外気の進入を遮断するホルダー４１を設置する。多層石英ガラス素材の側では、最外層の石英ガラス素管内を真空ポンプ４２によって用いて排気する。そして、一体化加工後の３層石英ガラス管の側では、プラグを保持するマンドレルを中空とし、マンドレルの側面に排気できる小孔４３を設け、このマンドレルを介して真空ポンプ４２を用いて排気する。
A method of decompressing the inside of the multilayer quartz glass material or the inside of the multilayer quartz glass tube after integrated processing will be described with reference to FIG. When manufacturing a multilayer quartz glass tube from a multilayer quartz glass material,
このような減圧処理は、多層石英ガラス素材側または一体化加工後の３層石英ガラス管側（プラグ側）のどちらか一方でもよいが、両側から減圧処理するのが好ましい。減圧処理はわずかでも有効であるが、過剰に減圧するとプラグとの接触が激しくなり、内表面に傷が発生する場合があるので、内部の圧力は100000Pa以下が好ましい。減圧による寸法精度の向上を図るためには、素材側で30000〜60000Pa、プラグ側で1000〜10000Paとするのが、特に好ましい。 Such a decompression treatment may be performed on either the multilayer quartz glass material side or the three-layer quartz glass tube side (plug side) after integrated processing, but it is preferable to perform the decompression treatment from both sides. The pressure reduction treatment is effective even slightly, but if the pressure is excessively reduced, contact with the plug becomes intense and scratches may occur on the inner surface, so the internal pressure is preferably 100000 Pa or less. In order to improve the dimensional accuracy by reducing the pressure, it is particularly preferable that the pressure is 30000 to 60000 Pa on the material side and 1000 to 10,000 Pa on the plug side.
３層石英ガラス管を製造するために、高純度のＳｉＣｌ4を酸水素火炎にて加水分解して生成したＳｉＯ2より得た合成石英ガラス又は天然石英ガラスから、３層石英ガラス素材に用いる石英ガラス棒及び石英ガラス素管を作製した。また、シリカ粉末を用意した。そして、図１に示す製造装置にて、一体化加工された３層石英ガラス管を製造した。ここで、最外層の石英ガラス素管には外径１４２ｍｍのものを用いた。ダイスは黒鉛製で口径１６０ｍｍと１２５ｍｍの２種類を用い、プラグは外径８５ｍｍと３０ｍｍの２種類を用いた。 Quartz used as a three-layer quartz glass material from synthetic quartz glass or natural quartz glass obtained from SiO 2 produced by hydrolyzing high-purity SiCl 4 with an oxyhydrogen flame to produce a three-layer quartz glass tube A glass rod and a quartz glass blank were produced. Moreover, silica powder was prepared. And the three-layer quartz glass tube processed integrally was manufactured with the manufacturing apparatus shown in FIG. Here, the outermost silica glass tube having an outer diameter of 142 mm was used. The die was made of graphite and used in two types having a diameter of 160 mm and 125 mm, and the plug was used in two types having an outer diameter of 85 mm and 30 mm.
最外層の石英ガラス素管の中に、中間層となる石英ガラス素管を挿入し、さらに最内層となる石英ガラス棒あるいは石英ガラス素管を挿入し、３層石英ガラス素材を準備した。そして、３層石英ガラス素材の片端部には、一体化加工後の３層石英ガラス管の内径より大きな内径を有する石英ガラス製ダミーシリンダー、他端部には一体化加工後の３層石英ガラス管の外径と同じ外径の石英ガラス製ダミーシリンダーを溶着した。 A quartz glass element tube serving as an intermediate layer was inserted into the outermost layer quartz glass element tube, and a quartz glass rod or quartz glass element tube serving as an innermost layer was further inserted to prepare a three-layer quartz glass material. A quartz glass dummy cylinder having an inner diameter larger than the inner diameter of the integrated three-layer quartz glass tube is provided at one end of the three-layer quartz glass material, and an integrated three-layer quartz glass is provided at the other end. A quartz glass dummy cylinder having the same outer diameter as that of the tube was welded.
また、中間層にシリカ粉末を用いる３層石英ガラス素材の場合は、最外層の石英ガラス素管の片端の口を閉じた上で、その石英ガラス素管を垂直方向に設置する。そして、その中に、最内層となる石英ガラス棒あるいは石英ガラス素管を同軸上になるように挿入し保持したのち、最外層と最内層の隙間に中間層素材としてのシリカ粉末を充填し、その後、開口側は真空引き可能な状態で栓をすることによって、３層石英ガラス素材を準備した。 このようにして準備された３層石英ガラス素材の構成及び寸法は、表１に示すとおりである。 Further, in the case of a three-layer quartz glass material using silica powder for the intermediate layer, the quartz glass element tube is installed in the vertical direction after closing one end of the outermost layer quartz glass element tube. And after inserting and holding the quartz glass rod or the quartz glass base tube that is the innermost layer so as to be coaxial, the silica powder as the intermediate layer material is filled in the gap between the outermost layer and the innermost layer, Thereafter, the opening side was plugged in a vacuumable state, thereby preparing a three-layer quartz glass material. The structure and dimensions of the three-layer quartz glass material prepared in this way are as shown in Table 1.
ヒーターの設定温度は２４００℃として、一体化加工により３層石英ガラス管を製造した。また、この際、石英ガラス管内を減圧した場合としない場合の両方を行ったが、減圧する場合は、３層石英ガラス素材側では内圧を50000Pa、プラグ側では1500Paとした。 A set temperature of the heater was 2400 ° C., and a three-layer quartz glass tube was manufactured by an integrated process. At this time, both the cases where the inside of the quartz glass tube was decompressed and the case where it was not decompressed were performed. However, when decompressing, the internal pressure was set to 50000 Pa on the three-layer quartz glass material side and 1500 Pa on the plug side.
得られた３層石英ガラス管について、長さ方向にてほぼ等間隔に１０ヶ所の位置で、円周を８等分した４方向にて外径を測定し、平均値をその位置の外径とした。同じ位置で超音波肉厚計を用い、円周方向の８ヶ所で肉厚を測定し平均値をその位置の肉厚とし、外径と肉厚からその位置の内径を計算により求めた。１０ヶ所の測定値から、その３層石英ガラス管の平均外径及び平均内径を、そして最大値と最小値との差から外径変動及び内径変動をそれぞれ求めた。また、目視にて観察し、各層の界面における空孔の有無についても検査を行った。 About the obtained three-layer quartz glass tube, the outer diameter was measured in four directions obtained by dividing the circumference into eight equal parts at approximately ten positions in the length direction, and the average value was determined as the outer diameter of the position. It was. Using an ultrasonic thickness meter at the same position, the thickness was measured at eight locations in the circumferential direction, the average value was taken as the thickness at that position, and the inner diameter at that position was calculated from the outer diameter and thickness. From the 10 measured values, the average outer diameter and average inner diameter of the three-layer quartz glass tube were obtained, and the outer diameter fluctuation and inner diameter fluctuation were obtained from the difference between the maximum value and the minimum value. Moreover, it observed visually and also examined about the presence or absence of the void | hole in the interface of each layer.
表１から明らかなように、３層石英ガラス素材に用いられる各層の素材がそれぞれ異なっても、種々の寸法の３層石英ガラスが、寸法精度よく製造されている。また、各層の界面に気泡のない石英ガラス管が得られていることがわかる。 As is apparent from Table 1, even if the materials of the respective layers used in the three-layer quartz glass material are different, three-layer quartz glass having various dimensions is manufactured with high dimensional accuracy. Moreover, it turns out that the quartz glass tube without a bubble is obtained in the interface of each layer.
４層又は５層の石英ガラス管を製造するために、高純度のＳｉＣｌ4を酸水素火炎にて加水分解して生成したＳｉＯ2より得た合成石英ガラス及び天然石英ガラスから、４層又は５層の石英ガラス素材に用いる石英ガラス棒及び石英ガラス素管を作製した。また、シリカ粉末を用意した。そして、図１に示す製造装置にて、一体化加工された４層又は５層の石英ガラス管を製造した。ここで、最外層の石英ガラス素管には外径１４２ｍｍのものを用いた。ダイスは黒鉛製で口径１６０ｍｍのものを用い、プラグは外径８５ｍｍのものを用いた。 From the synthetic quartz glass and natural quartz glass obtained from SiO 2 produced by hydrolyzing high-purity SiCl 4 in an oxyhydrogen flame to produce a 4-layer or 5-layer quartz glass tube, 4 or 5 A quartz glass rod and a quartz glass base tube used for the quartz glass material of the layer were prepared. Moreover, silica powder was prepared. And the 4-layer or 5-layer quartz glass tube by which the integrated process was carried out was manufactured with the manufacturing apparatus shown in FIG. Here, the outermost silica glass tube having an outer diameter of 142 mm was used. The die was made of graphite and had a diameter of 160 mm, and the plug had an outer diameter of 85 mm.
このようにして得られた石英ガラス素材から、４層又は５層の石英ガラス素材を作る方法は、基本的には、実施例１と同様である。 The method for producing a four-layer or five-layer quartz glass material from the quartz glass material thus obtained is basically the same as in Example 1.
すなわち、最外層の石英ガラス素管の中に、中間層となる石英ガラス素管を２個又は３個挿入し、さらに最内層となる石英ガラス棒あるいは石英ガラス素管を挿入し、４層又は５層の石英ガラス素材を準備した。 That is, in the outermost quartz glass tube, two or three quartz glass tubes serving as intermediate layers are inserted, and further, a quartz glass rod or quartz glass tube serving as the innermost layer is inserted, and four layers or Five layers of quartz glass material were prepared.
また、中間層にシリカ粉末を用いる４層又は５層の石英ガラス素材の場合は、最外層の石英ガラス素管の片端の口を閉じた上で、その石英ガラス素管を垂直方向に設置する。そして、その中に、中間層となる石英ガラス素管を１個又は２個挿入し、さらに最内層となる石英ガラス棒あるいは石英ガラス素管を同軸上になるように挿入し保持したのち、最外層ガラス素管と中間層ガラス素管の隙間、又は、最内層ガラス棒若しくは最内層ガラス素管と中間層ガラス素間の隙間、に中間層素材としてのシリカ粉末を１層又は２層充填し、その後、開口側は真空引き可能な状態で栓をすることによって、４層又は５層の石英ガラス素材を準備した。 Further, in the case of a four-layer or five-layer quartz glass material using silica powder for the intermediate layer, the quartz glass element tube is installed in the vertical direction after closing one end of the outermost layer quartz glass element tube. . Then, insert one or two quartz glass blanks as the intermediate layer, and insert and hold the quartz glass rod or quartz glass blank as the innermost layer on the same axis. One or two layers of silica powder as the intermediate layer material are filled in the gap between the outer layer glass element tube and the intermediate layer glass element tube, or the innermost layer glass rod or the gap between the innermost layer glass element tube and the intermediate layer glass element. Then, the quartz glass material of 4 layers or 5 layers was prepared by plugging the opening side in a vacuumable state.
そして、４層又は５層の石英ガラス素材の片端部には、一体化加工後の４層又は５層の石英ガラス管の内径より大きな内径を有する石英ガラス製ダミーシリンダー、他端部には一体化加工後の４層又は５層の石英ガラス管の外径と同じ外径の石英ガラス製ダミーシリンダーを溶着した。 A quartz glass dummy cylinder having an inner diameter larger than the inner diameter of the integrated four-layer or five-layer quartz glass tube is formed at one end of the four-layer or five-layer quartz glass material, and integrated at the other end. A dummy cylinder made of quartz glass having the same outer diameter as that of the four-layer or five-layer quartz glass tube after the chemical processing was welded.
このようにして準備された４層又は５層の石英ガラス素材の構成及び寸法は、表２に示すとおりである。 The composition and dimensions of the four-layer or five-layer quartz glass material prepared in this way are as shown in Table 2.
ヒーターの設定温度は２３５０℃として、一体化加工により、４層又は５層の石英ガラス管を製造した。また、この際、石英ガラス管内を減圧した場合としない場合の両方を行ったが、減圧する場合は、３層石英ガラス素材側では内圧を40000Pa、プラグ側では2000Paとした。 A set temperature of the heater was set to 2350 ° C., and a four-layer or five-layer quartz glass tube was manufactured by integrated processing. At this time, both the cases where the inside of the quartz glass tube was decompressed and the case where it was not decompressed were performed. However, when decompressing, the internal pressure was 40,000 Pa on the three-layer quartz glass material side and 2000 Pa on the plug side.
得られた４層又は５層の石英ガラス管について、長さ方向にてほぼ等間隔に１０ヶ所の位置で、円周を８等分した４方向にて外径を測定し、平均値をその位置の外径とした。同じ位置で超音波肉厚計を用い、円周方向の８ヶ所で肉厚を測定し平均値をその位置の肉厚とし、外径と肉厚からその位置の内径を計算により求めた。１０ヶ所の測定値から、その管の平均外径及び平均内径を、そして最大値と最小値との差から外径変動及び内径変動をそれぞれ求めた。また、目視にて観察し、各層の界面における空孔の有無についても検査を行った。 About the obtained 4-layer or 5-layer quartz glass tube, the outer diameter was measured in four directions obtained by dividing the circumference into eight equal parts at approximately equal positions in the length direction, and the average value was calculated. The outer diameter of the position was used. Using an ultrasonic thickness meter at the same position, the thickness was measured at eight locations in the circumferential direction, the average value was taken as the thickness at that position, and the inner diameter at that position was calculated from the outer diameter and thickness. The average outer diameter and average inner diameter of the tube were determined from the measured values at 10 locations, and the outer diameter fluctuation and inner diameter fluctuation were determined from the difference between the maximum value and the minimum value. Moreover, it observed visually and also examined about the presence or absence of the void | hole in the interface of each layer.
表２から明らかなように、４層又は５層の石英ガラス素材に用いられる各層の素材がそれぞれ異なっても、種々の寸法の４層又は５層の石英ガラスが、寸法精度よく製造されている。また、各層の界面に気泡のない石英ガラス管が得られていることがわかる。 As is apparent from Table 2, even if the materials of the layers used in the 4-layer or 5-layer quartz glass material are different from each other, the 4-layer or 5-layer quartz glass having various dimensions is manufactured with high dimensional accuracy. . Moreover, it turns out that the quartz glass tube without a bubble is obtained in the interface of each layer.
本発明によれば、１層又は２層以上の中間層を有する多層石英ガラス管及び多層石英ガラス棒を、種々の寸法について、量産性に適した方法で、且つ優れた寸法精度で製造することができる。 According to the present invention, a multilayer quartz glass tube and a multilayer quartz glass rod having one or two or more intermediate layers are manufactured with various dimensions in a method suitable for mass production and with excellent dimensional accuracy. Can do.
１ 最外層素材
２ 中間層素材
３ 最内層素材
５ ダミーシリンダー
１０ 出側チャック
１１ 入側チャック
１５ ヒーター
２０ プラグ
２１ ダイス
２２ マンドレル
３０ ３層石英ガラス管
４１ ホルダー
４２ 真空ポンプ
４３ 小孔
５２ 第１中間層素材
６２ 第２中間層素材
７０ ４層石英ガラス管
DESCRIPTION OF
Claims (11)
The quartz according to any one of claims 6 to 10, wherein the inside of the multilayer quartz glass material is depressurized to less than atmospheric pressure when the softened portion of the multilayer quartz glass material is pressed into the die and fed. A method of manufacturing a glass rod.
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| JP2003361922A JP4236037B2 (en) | 2003-10-22 | 2003-10-22 | Multilayer quartz glass tube and method for producing multilayer quartz glass rod |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271650A (en) * | 2015-11-03 | 2016-01-27 | 江苏亨通光电股份有限公司 | Device and method for preparing low hydroxyl quartz socket tube |
| CN110372186A (en) * | 2019-06-27 | 2019-10-25 | 武义超野五金制品有限公司 | Clamping device |
| CN115849710A (en) * | 2022-12-09 | 2023-03-28 | 湖南旗滨医药材料科技有限公司 | Gradient air hole glass rotary tube and preparation method thereof |
-
2003
- 2003-10-22 JP JP2003361922A patent/JP4236037B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271650A (en) * | 2015-11-03 | 2016-01-27 | 江苏亨通光电股份有限公司 | Device and method for preparing low hydroxyl quartz socket tube |
| CN105271650B (en) * | 2015-11-03 | 2017-11-28 | 江苏亨通光导新材料有限公司 | A kind of device and method for preparing low hydroxyl quartz socket tube |
| CN110372186A (en) * | 2019-06-27 | 2019-10-25 | 武义超野五金制品有限公司 | Clamping device |
| CN110372186B (en) * | 2019-06-27 | 2024-04-02 | 浙江伊水家居用品有限公司 | Clamping device |
| CN115849710A (en) * | 2022-12-09 | 2023-03-28 | 湖南旗滨医药材料科技有限公司 | Gradient air hole glass rotary tube and preparation method thereof |
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