WO2018131499A1 - 中空状多孔質石英ガラス母材の製造方法 - Google Patents
中空状多孔質石英ガラス母材の製造方法 Download PDFInfo
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- WO2018131499A1 WO2018131499A1 PCT/JP2017/047180 JP2017047180W WO2018131499A1 WO 2018131499 A1 WO2018131499 A1 WO 2018131499A1 JP 2017047180 W JP2017047180 W JP 2017047180W WO 2018131499 A1 WO2018131499 A1 WO 2018131499A1
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- quartz glass
- target
- base material
- hollow porous
- glass base
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/108—Forming porous, sintered or foamed beads
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01486—Means for supporting, rotating or translating the preforms being formed, e.g. lathes
- C03B37/01493—Deposition substrates, e.g. targets, mandrels, start rods or tubes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B15/00—Drawing glass upwardly from the melt
- C03B15/14—Drawing tubes, cylinders, or rods from the melt
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1484—Means for supporting, rotating or translating the article being formed
- C03B19/1492—Deposition substrates, e.g. targets
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
Definitions
- the present invention relates to a method of producing a hollow porous quartz glass base material and a method of producing a synthetic quartz glass cylinder.
- Synthetic quartz glass is widely used in the optical, semiconductor, and chemical industries, and in particular, as a lens material for projection and exposure systems in microlithography, and as a material for semiconductor manufacturing jigs and optical fibers.
- a hollow synthetic quartz glass cylinder In the production of a hollow synthetic quartz glass cylinder, it is general to produce a hollow porous quartz glass base material (soot body) and sinter it to be transparent.
- the OVD (outside vapor deposition) method is known for the production of soot, and fine SiO 2 particles are deposited by flame hydrolysis or thermal decomposition of a silicon-containing material on the outer surface of a target rotating around a long axis. Manufacture a soot body.
- the hollow porous quartz glass base material requires an operation of extracting the target before sintering, and the operation of extracting the target is performed by rotating the target and the hollow soot body relative to each other or moving in the long axis direction. This operation is extremely difficult when the soot body and the target are stuck. Furthermore, even if it can be extracted by applying a large force, a flaw is generated on the inner surface of the soot body at that time, and the created flaw remains as a local defect in the sintered quartz cylinder and becomes a defective part.
- the hollow quartz cylinder forms an inner diameter by passing a cylindrical or cylindrical mandrel of ceramic, quartz glass, carbon or the like into a hollow part of a soot body and sintering it in that state. By sintering through the mandrel, the soot body can be in close contact with the mandrel to obtain an inner surface shape conforming to the shape of the mandrel.
- the hollow quartz cylinder produced in this manner is machined into various shapes according to the application and processed into a desired shape.
- Patent Document 1 describes a method of facilitating the extraction operation by extracting the target in the direction of a larger outer diameter by making the target shape into a cone shape.
- Patent Document 2 is a gas condition in which the average density of the SiO 2 soot body is 0.3 to 0.5 g / cm 3 and the initial condition is reduced by 15% or more than the H 2 amount in the steady condition, and the source gas is steady. The method of making it easy by setting it as the gas condition of 30% or more of the condition is described. However, in this method, when the average bulk density is low, a large change of equipment is required, which is not preferable.
- Patent Document 3 deposits a first layer having a bulk density of 0.2 g / cm 3 or less adjacent to the target material, and a second layer having a density higher than that of the first layer by 0.03 g / cm 3 or more.
- the method of making it easy to withdraw by forming the layer and removing the first layer during or after withdrawing is described, and the smooth inner surface of the soot body is obtained.
- a low density layer of 0.2 g / cm 3 or less is formed in the first layer, the centrifugal force applied to the soot body when the weight is large to perform deposition while rotating the target in the long axis direction.
- the first layer (a low density layer of 0.2 g / cm 3 or less) collapses during deposition and growth, and the soot moves in the longitudinal direction on the target, and the soot body There is a concern that problems such as failure to follow the rotation of the lens may occur and it can not be manufactured.
- the method described in Patent Document 4 is a method of producing a hollow porous quartz glass base material, and in the deposition step, the bulk density is 0.45 g / cm 3 or more.
- JP-A-8-208242 JP, 2004-18364 A Japanese Patent Application Laid-Open No. 61-205632 JP, 2016-3162, A
- the present invention has been made in view of the problems of the prior art described above, and it is easy to extract the target even if the hollow porous quartz glass base material (soot body) is increased in weight and high in bulk density. It is an object of the present invention to provide a method for producing a hollow porous quartz glass base material and a method for producing a synthetic quartz glass cylinder capable of producing a large-weight soot body by holding and stably extracting a target.
- the method for producing a hollow porous quartz glass base material of the present invention is a cylindrical or cylindrical heat resistant substrate, and the surface roughness of the outer surface on which SiO 2 particles are deposited is Preparing a heat resistant substrate having a maximum height Rz of less than 9 ⁇ m and an arithmetic mean roughness Ra of less than 1 ⁇ m, rotating the heat resistant substrate to deposit SiO 2 particles on the outer surface of the heat resistant substrate And forming the glass fine particle deposited body, and extracting the heat resistant substrate from the glass fine particle deposited body to produce a hollow porous quartz glass base material.
- the heat resistant substrate is also referred to as a target.
- the surface roughness Ra and Rz are calculated based on JIS B 0601: 2001.
- Rz of the heat resistant substrate is 6.0 ⁇ m or less and Ra is 0.6 ⁇ m or less, more preferably, Rz is 4.0 ⁇ m or less and Ra is 0.4 ⁇ m or less.
- Rz is 2.0 ⁇ m or less More preferably, Ra is 0.2 ⁇ m or less.
- the heat-resistant substrate of the present invention is a heat-resistant substrate used in the method for producing a hollow porous quartz glass base material of the present invention, wherein the surface roughness of the outer surface on which SiO 2 particles are deposited has a maximum height Rz. Is less than 9 ⁇ m and the arithmetic mean roughness Ra is less than 1 ⁇ m.
- the method for producing a synthetic quartz glass cylinder of the present invention is characterized by using a hollow porous quartz glass substrate obtained by the method for producing a hollow porous quartz glass substrate of the present invention.
- the hollow porous quartz glass base material of the present invention is a hollow porous quartz glass base material obtained by the method for producing a hollow porous quartz glass base material of the present invention.
- the synthetic quartz glass cylinder of the present invention is a synthetic quartz glass cylinder obtained by the method of producing a synthetic quartz glass cylinder of the present invention.
- the present invention even if the hollow porous quartz glass base material (soot body) is increased in weight and increased in bulk density, it is possible to stably extract the target while maintaining ease of target extraction.
- a significant effect of providing a method of producing a hollow porous quartz glass base material capable of producing a weight soot body and a method of producing a synthetic quartz glass cylinder is exhibited.
- the present invention has an effect that the easiness of target extraction can be performed without lot-to-lot variation and, at the same time, the cleaning operation for removing the silica fine particles attached to the target extracted from the soot body becomes easy.
- the present inventors have found that in the production of a high-density heavy-weight soot body by the OVD method, the soot body of the lot for which extraction of the target was difficult and the target extracted from the soot body, and the lot for which the extraction was easy.
- the soot body and the target extracted from the soot body in detail, it was found that the larger the amount of silica fine particles attached to the target was, the more difficult the target was to extract. Then, after removing the silica particle which had adhered, it observed visually, but the big difference was not confirmed.
- a cylindrical or cylindrical heat-resistant substrate is rotated to deposit SiO 2 particles on the outer surface of the heat-resistant substrate to deposit glass particles.
- the heat-resistant substrate is removed from the glass particle deposition body to produce a hollow porous quartz glass base material, the surface of the outer surface on which SiO 2 particles are deposited as the heat-resistant substrate
- the target material used has a roughness Rz of less than 9 ⁇ m and an Ra of less than 1 ⁇ m.
- the surface roughness condition is at least applied to the target surface in contact with the glass particle deposit, that is, the outer surface of the portion on which the SiO 2 particles are deposited, and the surface roughness on the entire outer peripheral surface of the target material It is more preferable that the condition
- the surface roughness of the outer surface of the heat resistant substrate on which the SiO 2 particles are deposited is Rz of 9 ⁇ m or more, the irregularities on the outer surface of the heat resistant substrate easily catch on the inner surface of the soot body, and Ra is 1 ⁇ m.
- part of the inner surface of the soot body collapses and the generated soot powder adheres to the target surface, and another soot powder adheres to the adhered soot powder, whereby the soot powder is generated on the inner surface of the soot body and the target surface There is a problem of sticking between them.
- the target releasability can be easily stabilized.
- the method of preparing the heat-resistant substrate satisfying the above-mentioned surface roughness is not particularly limited, but it is preferable to carry out mechanical polishing using a diamond abrasive cloth or the like.
- the heat-resistant substrate used as a target may have a surface roughness which may be rough due to oxidative consumption or thermal deterioration of the target material during the production of the hollow porous quartz glass base material, so that the hollow porous quartz is continuously formed.
- a glass base material confirm the surface roughness of the target material before use, and if the surface roughness becomes rough, polish the target material each time and manage to meet the condition of the surface roughness. Is preferred.
- Rz of the heat resistant substrate is 6.0 ⁇ m or less and Ra is 0.6 ⁇ m or less, more preferably, Rz is 4.0 ⁇ m or less and Ra is 0.4 ⁇ m or less.
- Rz is 2.0 ⁇ m or less More preferably, Ra is 0.2 ⁇ m or less.
- the material of the heat resistant substrate is not particularly limited as long as it is heat resistant, but ceramics, carbon, metal materials, etc., typified by Al 2 O 3 , SiC, Si 3 N 4 and the like are preferable.
- FIG. 1 is a schematic explanatory view showing an example of a method for producing a hollow porous quartz glass base material of the present invention
- FIG. 2 is a schematic explanatory view showing extraction of a target from a glass particle deposition body.
- reference numeral 10 is a manufacturing apparatus for manufacturing a hollow porous quartz glass base material, and a target holding and rotating mechanism 20 for rotating and holding the target 14 and controlling the rotation speed, and a plurality of glass particle synthesizing burners 16a.
- a burner group movement control device 18 for controlling the movement of reciprocating (swing) and vertical movement of the burner group 16 and the burner group 16 for glass particulates synthesis arranged at a predetermined interval.
- the target 14 used has a surface roughness Rz of less than 9 ⁇ m and less than Ra of 1 ⁇ m on the outer surface on which the glass particles are deposited.
- a target material in which the surface roughness of the entire outer peripheral surface satisfies the above condition is used as the target 14.
- a cylindrical (rod) target material is used as the target 14
- a cylindrical target material may be used.
- FIG. 1 shows an example of the deposition of SiO 2 particles by hydrolysis by the flame of the glass particle synthesis burner 16a supplied with the glass raw material (SiCl 4 ), but the target is fine SiO 2 particles by pyrolysis. To form a glass particulate deposit.
- the target can be easily extracted even in the production of a hollow porous quartz glass base material having a large weight and a high bulk density, which has conventionally been difficult to extract the target.
- the target can be stably extracted, and a heavy-weight soot body can be manufactured.
- a hollow porous quartz glass base material having a large weight of 150 to 350 kg or a hollow porous quartz glass base material having a high bulk density of 0.5 to 0.8 g / cm 3 in average bulk density Can be easily obtained.
- the hollow porous quartz glass base material is preferably a large weight hollow porous quartz glass base material, preferably 150 to 350 kg, and more preferably 200 to 300 kg.
- the hollow porous quartz glass base material is preferably a high bulk density hollow porous quartz glass base material, and the average bulk density is 0.5 to 0.8 g / cm 3. Preferably, it is 0.6 to 0.7 g / cm 3 .
- the target can be easily extracted without lot-to-lot variation, and at the same time, the cleaning operation for removing the silica particles attached to the target extracted from the glass particle deposit can be facilitated.
- the method for producing a synthetic quartz glass cylinder of the present invention uses the hollow porous quartz glass base material obtained by the method of the present invention.
- the synthetic quartz glass cylinder may be produced by vitrifying the hollow porous quartz glass base material by a known method using the hollow porous quartz glass base material to produce the synthetic quartz glass cylinder, although there is no particular limitation. It is preferred to be transparent to obtain a synthetic quartz glass cylinder.
- Example 1 Twelve hollow porous quartz glass substrates were produced by the OVD method using the hollow porous quartz glass substrate manufacturing apparatus shown in FIG.
- For the target use a SiC cylinder polished with # 240 diamond abrasive cloth attached to a belt sander and finished to a maximum surface roughness of Rz 6.0 6.0 ⁇ m and Ra 0.6 0.6 ⁇ m throughout the outer peripheral surface, 12 The experiment was conducted in this series.
- the surface roughness of the target was measured using a surface roughness tester (small surface roughness measuring device: Surf Test SJ-210, manufactured by Mitutoyo Co., Ltd.) based on JIS B 0601: 2001. If the surface roughness becomes rough due to oxidative consumption or thermal deterioration of the target material while creating a hollow porous quartz glass base material in a row of 12 pieces, the target material is polished each time and managed to become the above surface roughness I went there.
- a surface roughness tester small surface roughness measuring device: Surf Test SJ-210, manufactured by Mitutoy
- a plurality of burners for introducing and burning oxygen gas and hydrogen gas are disposed perpendicular to the axial direction of the target by installing the burner swing and vertical movement device, and the plurality of burners are swung parallel to the axial direction of the target
- silica fine particles were deposited on the outer peripheral surface of the target to prepare a glass fine particle deposited body, thereby obtaining a glass fine particle deposited body with an outer diameter of 400 mm.
- the manufacturing conditions at that time are 1020 g / min of silicon tetrachloride, the distance between the burner and the target or soot body: 300 mm, and the swing speed: 300 mm / min.
- the target was extracted from the obtained glass particle deposition body, and a hollow porous quartz glass base material (soot body) was obtained.
- Figure 3 shows the time taken to extract the target. As shown in FIG. 3, the target extraction properties were all good, and the variation in the time required for the extraction operation was also small.
- the density of the obtained soot body was a soot body having a maximum density of about 0.8 g / cm 3 and a minimum density of about 0.5 g / cm 3 although the density varies depending on the site of the soot body.
- the density was calculated from the measured weight and the volume calculated from the outer diameter and length of the soot body.
- the obtained soot body was provided with a mandrel in the inner hole of the soot body to sinter-clear.
- the obtained soot body had no flaws or the like on its inner surface because extraction of the target was easy. By sintering and clarifying this soot body, it was possible to obtain a synthetic quartz glass cylinder in intimate contact with the mandrel, having a uniform inner diameter, and having no local defects on the inner surface.
- Example 2 The procedure was performed under the same conditions as in Example 1 except that the target material was changed, to obtain 12 hollow porous quartz glass base materials (soot bodies).
- a SiC cylinder that is polished with # 800 diamond abrasive cloth attached to a belt sander, and the surface roughness is finished to the maximum value Rz 2.0 2.0 ⁇ m and Ra 0.2 0.2 ⁇ m all over the outer peripheral surface 12
- the experiment was conducted in this series.
- the target material is polished and controlled so as to have the above surface roughness each time.
- Figure 3 shows the time taken to extract the target. As shown in FIG. 3, the ease of target extraction was higher than in Example 1, and the maximum value decreased and the variation decreased.
- Example 1 The procedure was performed under the same conditions as in Example 1 except that the target material was changed, to obtain 12 hollow porous quartz glass base materials (soot bodies).
- Figure 3 shows the time taken to extract the target. Although the extraction of the target was easy in some cases but difficult in many cases, the time required for the extraction varied greatly. The most difficult lot took 65 minutes.
- 10 manufacturing apparatus
- 12 glass particle deposition body
- 14 target
- 16 burner group for glass particle synthesis
- 16a burner for glass particle synthesis
- 18 swing and raising / lowering device for glass particle synthesis group
- 20 Target holding and rotating mechanism.
Abstract
Description
本発明方法において、Rzが9μm未満であり且つRaが1μm未満のターゲット材を用いることにより、ターゲット抜け性を容易な状態に安定化することが出来る。
図1に示した中空状多孔質石英ガラス母材の製造装置を用いて、OVD法により、12本の中空状多孔質石英ガラス母材を作製した。ターゲットには、ベルトサンダーに取り付けた#240ダイヤモンド研磨布紙で研磨し外周面全域において表面粗さが最大値Rz≦6.0μm且つRa≦0.6μmに仕上げたSiC製円筒を使用し、12本連続で実験を行った。ターゲットの表面粗さの測定は、表面粗さ計(小形表面粗さ測定機:サーフテストSJ-210、株式会社ミツトヨ製)を用い、JIS B 0601:2001に基づき行った。12本連続で中空状多孔質石英ガラス母材を作成する内にターゲット材の酸化消耗や熱的変質など表面粗さが粗くなる場合はその都度ターゲット材を研磨し上記表面粗さになるよう管理しながら行った。
得られたスート体はスート体の内孔に心棒を設置し、焼結透明化を行った。得られたスート体はターゲットの抜き出しが容易であったため内面にキズ等が無かった。このスート体を焼結透明化する事により、心棒に密着し均一な内径を持ち、かつ内面に局所的な欠陥を持たない、合成石英ガラスシリンダを得る事ができた。
ターゲット材を変更した以外は実施例1と同じ条件で行い、12本の中空状多孔質石英ガラス母材(スート体)を得た。ターゲットには、ベルトサンダーに取り付けた#800ダイヤモンド研磨布紙で研磨し、外周面全域において表面粗さが最大値Rz≦2.0μm且つRa≦0.2μmに仕上げたSiC製円筒を使用し12本連続で実験を行った。また、12本連続で作成する内にターゲット材の酸化消耗や熱的変質など表面粗さが粗くなる場合はその都度ターゲット材を研磨し上記表面粗さになるよう管理しながら行った。
ターゲット材を変更した以外は実施例1と同じ条件で行い、12本の中空状多孔質石英ガラス母材(スート体)を得た。ターゲットは、外周面の表面粗さの最大値がRz=9.8μm且つRa=1.8μmのターゲットを用いた。図3にターゲットの抜き出しに要した時間を示す。ターゲットの抜き出しは容易な場合もあったが困難な場合が多く、その抜き出しに要する時間には大きなバラツキが生じた。最も困難であったロットでは65分の時間を要した。
Claims (6)
- 円柱状又は円筒状の耐熱性基体であり、SiO2粒子を堆積させる外表面の表面粗さが、最大高さRzが9μm未満であり且つ算術平均粗さRaが1μm未満である耐熱性基体を準備する工程と、
該耐熱性基体を回転させ、該耐熱性基体の外表面にSiO2粒子を堆積させてガラス微粒子堆積体を形成する工程と、
該ガラス微粒子堆積体から該耐熱性基体を抜き取り、中空状多孔質石英ガラス母材を製造する工程と、
を含むことを特徴とする中空状多孔質石英ガラス母材の製造方法。 - 前記耐熱性基体のRzが6.0μm以下であり且つRaが0.6μm以下であることを特徴とする請求項1記載の中空状多孔質石英ガラス母材の製造方法。
- 請求項1又は2記載の方法に用いられる耐熱性基体であって、SiO2粒子を堆積させる外表面の表面粗さが、最大高さRzが9μm未満であり且つ算術平均粗さRaが1μm未満であることを特徴とする耐熱性基体。
- 請求項1又は2記載の方法により得られる中空状多孔質石英ガラス母材を用いることを特徴とする合成石英ガラスシリンダの製造方法。
- 請求項1又は2記載の方法により得られる、中空状多孔質石英ガラス母材。
- 請求項4記載の方法により得られる、合成石英ガラスシリンダ。
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EP17890911.5A EP3521250B1 (en) | 2017-01-11 | 2017-12-28 | Method for producing hollow porous quartz glass base material |
US16/477,461 US11401192B2 (en) | 2017-01-11 | 2017-12-28 | Method for producing hollow porous quartz glass base material |
CN201780080125.1A CN110139837B (zh) | 2017-01-11 | 2017-12-28 | 中空多孔石英玻璃基底材料的制造方法 |
KR1020197012291A KR102072822B1 (ko) | 2017-01-11 | 2017-12-28 | 중공형 다공질 석영유리 모재의 제조 방법 |
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- 2017-12-28 KR KR1020197012291A patent/KR102072822B1/ko active IP Right Grant
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US20200270162A1 (en) | 2020-08-27 |
EP3521250A4 (en) | 2020-05-13 |
US11401192B2 (en) | 2022-08-02 |
CN110139837B (zh) | 2021-11-16 |
KR20190051072A (ko) | 2019-05-14 |
EP3521250B1 (en) | 2024-03-27 |
JPWO2018131499A1 (ja) | 2019-07-11 |
CN110139837A (zh) | 2019-08-16 |
KR102072822B1 (ko) | 2020-02-03 |
JP6556384B2 (ja) | 2019-08-07 |
EP3521250A1 (en) | 2019-08-07 |
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