JP6532269B2 - Method of manufacturing synthetic quartz glass - Google Patents
Method of manufacturing synthetic quartz glass Download PDFInfo
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- JP6532269B2 JP6532269B2 JP2015083458A JP2015083458A JP6532269B2 JP 6532269 B2 JP6532269 B2 JP 6532269B2 JP 2015083458 A JP2015083458 A JP 2015083458A JP 2015083458 A JP2015083458 A JP 2015083458A JP 6532269 B2 JP6532269 B2 JP 6532269B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 189
- 238000004519 manufacturing process Methods 0.000 title claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 50
- 239000000463 material Substances 0.000 claims description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 238000003466 welding Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 description 18
- 239000011734 sodium Substances 0.000 description 17
- 239000012535 impurity Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- 238000000465 moulding Methods 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 230000002093 peripheral effect Effects 0.000 description 6
- 230000002950 deficient Effects 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000137 annealing Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000005350 fused silica glass Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000004050 Pentaglottis sempervirens Species 0.000 description 1
- 235000004522 Pentaglottis sempervirens Nutrition 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000005305 interferometry Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Description
本発明は、合成石英ガラスの製造方法に関し、特にレンズ母材等の光学用途に適した合成石英ガラスの製造方法に関する。 The present invention relates to a method of producing synthetic quartz glass, and more particularly to a method of producing synthetic quartz glass suitable for optical applications such as lens base materials.
半導体集積回路の製造のための露光装置には、光リソグラフィー技術が用いられている。近年、半導体集積回路の微細化、高集積化に伴い、露光用の光源の短波長化が進んでいる。現在、最先端の露光装置にはArFエキシマレーザー(波長193.4nm)が光源として用いられ、その光学部材には、高均質性、高透過性、及び高いレーザー耐性等を充たすことが要求されている。 An optical lithography technique is used for an exposure apparatus for manufacturing a semiconductor integrated circuit. In recent years, with the miniaturization and high integration of semiconductor integrated circuits, shortening of the wavelength of a light source for exposure has progressed. At present, ArF excimer laser (wavelength 193.4 nm) is used as a light source for the most advanced exposure apparatus, and the optical member is required to satisfy high homogeneity, high transparency, high laser resistance, etc. .
これらの高い要求を充たす光学部材として、高純度の合成石英ガラスが用いられる。この合成石英ガラスは、より高度に改良された工程で製造が行われるため、製造コストを抑えることが重要となる。すなわち歩留まりよく製造することが望まれる。 High purity synthetic quartz glass is used as an optical member satisfying these high requirements. Since this synthetic quartz glass is manufactured in a more highly improved process, it is important to reduce the manufacturing cost. That is, it is desirable to manufacture with high yield.
しかしながら、合成石英ガラスは、近年要求される品質が特に高度化しているため、合成石英ガラス自体が高価でありながら、歩留まりが悪い製法となってしまっている。具体的には、製造工程で汚染などにより外表面近傍の部分が品質の悪いものとなってしまうため、この部分を切り落として、あるいは、研削除去して製品としている。この除去する部分を見越して、製造設計され、母材重量を大きくして製造投入することとなり、歩留まりが悪いものとなってしまう。 However, since synthetic quartz glass has recently been required to have a particularly high quality, synthetic quartz glass itself is expensive, but it has become a manufacturing method with a low yield. Specifically, since a portion near the outer surface becomes poor in quality due to contamination or the like in the manufacturing process, this portion is cut off or ground and removed to make a product. It is manufactured and designed in anticipation of the portion to be removed, and the weight of the base material is increased to introduce the manufacturing, resulting in a poor yield.
特許文献１に記載された石英ガラスの熱アニール方法は前項に記載した製法の典型的な例であり、Na（ナトリウム）汚染を防ぐために、目的とするレンズ部材に対し、外径＋30mm以上、厚み＋30mm以上となるように、原料である合成石英ガラスインゴットを成型して熱処理を行うとしている。
The thermal annealing method for quartz glass described in
本発明は、上記した従来技術の問題点に鑑みてなされたもので、歩留まりよく合成石英ガラスを製造することが出来る合成石英ガラスの製造方法を提供することを目的とする。 The present invention has been made in view of the problems of the prior art described above, and it is an object of the present invention to provide a method for producing synthetic quartz glass capable of producing synthetic quartz glass with high yield.
上記課題を解決するために、本発明の合成石英ガラスの製造方法は、合成石英ガラス母材を、上下面及び側面を有する成型体に成型する成型工程と、前記成型体の前記上下面及び側面にダミー石英ガラスを溶着してダミー部を形成し、ダミー付中間体を作製する中間体作製工程と、前記ダミー付中間体を熱処理する熱処理工程と、前記ダミー付中間体の前記ダミー部を除去し、合成石英ガラスとするダミー部除去工程と、を含む製造方法である。 In order to solve the above-mentioned subject, the manufacturing method of synthetic quartz glass of the present invention comprises: a molding step of molding a synthetic quartz glass base material into a molding having upper and lower surfaces and side surfaces; The dummy quartz glass is welded to form a dummy portion, and an intermediate production step of producing an intermediate with dummy, a heat treatment step of heat treating the intermediate with dummy, and the dummy portion of the intermediate with dummy are removed And a dummy portion removing step of forming synthetic quartz glass.
前記ダミー石英ガラスとしては、ダミー用の合成石英ガラス又はダミー用の天然石英ガラスのいずれも適用できる。 As the dummy quartz glass, either synthetic quartz glass for dummy or natural quartz glass for dummy can be applied.
従来の製造方法では、不良部となる石英ガラスの外周部および上下部分を研削除去して合成石英ガラス製品を製造していたが、本発明の製造方法では、ダミー石英ガラスを合成石英ガラス母材の成型体の上下面及び側面に溶着した後に熱処理を行うことで、複屈折値の大きい不良部や、不純物濃度が大きいことによる不良部を、このダミー部が受け持ち、熱処理の工程の後にこのダミー部分を除去することで、合成石英ガラス製品を研削除去することなく、歩留まりよく製造することができる。 In the conventional manufacturing method, synthetic quartz glass products are manufactured by grinding and removing the outer peripheral part and upper and lower parts of the quartz glass which becomes a defective part, but in the manufacturing method of the present invention, dummy quartz glass is used as a synthetic quartz glass base material The heat treatment is performed after welding to the upper and lower surfaces and the side surfaces of the molded body, so that the dummy portion receives a defective portion with a large birefringence value and a defective portion due to a large impurity concentration. By removing the portion, the synthetic quartz glass product can be manufactured with high yield without grinding and removal.
また使用したダミー石英ガラスは、合成石英ガラス母材の成型体が同サイズであれば、複数回使用することができ、ダミー石英ガラスを作製する工程を省略することが可能であり、効率的である。 Further, the dummy quartz glass used can be used multiple times if the molded body of the synthetic quartz glass base material has the same size, and it is possible to omit the process of producing the dummy quartz glass, which is efficient. is there.
また、本発明の合成石英ガラスの製造方法では、アニール処理による品質調整時においても生じる、複屈折・屈折率均質性不良部である合成石英ガラス外表面近傍をダミー部が受け持つことができ、同様にこのダミー部を取り外して又は研削して除去することで不良部のない合成石英ガラスを歩留まりよく作製することができる。 Further, in the method of manufacturing synthetic quartz glass according to the present invention, the dummy portion can take charge of the vicinity of the outer surface of the synthetic quartz glass which is a birefringence / refractive index homogeneity defect portion which occurs also at the time of quality adjustment by annealing. By removing or grinding and removing this dummy portion, it is possible to produce a synthetic quartz glass free from defective portions with high yield.
前記熱処理工程の後、前記ダミー付中間体に対して水素処理を行う水素処理工程と、をさらに含むことが可能である。 After the heat treatment step, the dummy intermediate may be further subjected to a hydrogen treatment step of hydrogen treatment.
このときにおいても、本発明の合成石英ガラスの製造方法であれば、水素処理を施した場合、水素濃度が高くなってしまうことで生じる上下面近傍、外周側面近傍の品質不良部をダミー部が受け持つことができ、これも同様にダミー部を取り外し、あるいは研削除去することで不良部のない合成石英ガラスを歩留まりよく作製することができる。
水素濃度に関しては水素濃度の分布勾配が大きくできてしまうとその部分の屈折率が変化してしまい、屈折率均質性を悪化させてしまうことが知られている。本件のダミー部分を設けることにより、この合成石英ガラス製品部分の屈折率均質性の悪化を防ぐことができる。
Also in this case, according to the method for producing synthetic quartz glass of the present invention, when hydrogen treatment is performed, the dummy portion is a poor quality portion near the upper and lower surfaces and near the outer peripheral side surface caused by the hydrogen concentration becoming high. Similarly, the synthetic quartz glass having no defective portion can be manufactured with high yield by removing the dummy portion or grinding and removing it.
With regard to the hydrogen concentration, it is known that if the distribution gradient of the hydrogen concentration can be made large, the refractive index of the portion changes and the refractive index homogeneity is deteriorated. By providing the dummy portion of the present invention, it is possible to prevent the deterioration of the refractive index homogeneity of the synthetic quartz glass product portion.
前記上下面及び側面に溶着される前記ダミー石英ガラスの厚みが少なくとも１０ｍｍ以上であるのが好ましい。また、前記ダミー石英ガラスの厚みは、熱処理工程が長くなる点から、３０ｍｍ以下程度が好ましい。 The thickness of the dummy quartz glass welded to the upper and lower surfaces and the side surfaces is preferably at least 10 mm or more. The thickness of the dummy quartz glass is preferably about 30 mm or less from the viewpoint of lengthening the heat treatment process.
本発明に係る合成石英ガラスの製造方法によれば、歩留まりよく合成石英ガラスを製造することが出来る合成石英ガラスの製造方法を提供することができるという著大な効果を奏する。 The method for producing synthetic quartz glass according to the present invention has a remarkable effect of being able to provide a method for producing synthetic quartz glass capable of producing synthetic quartz glass with high yield.
本発明に係る合成石英ガラスの製造方法を図１に基づいて説明する。 A method of producing synthetic quartz glass according to the present invention will be described based on FIG.
まず、合成石英ガラスの前駆体となる合成石英ガラス母材１０を準備する（図１（ａ））。合成石英ガラス母材１０は、従来公知の合成石英ガラス母材と同様に製造することができる。 First, a synthetic quartz glass base material 10 to be a precursor of synthetic quartz glass is prepared (FIG. 1 (a)). The synthetic quartz glass base material 10 can be manufactured similarly to the conventionally known synthetic quartz glass base material.
より具体的には、例えば、四塩化珪素などを原料とした気相反応法によって合成石英ガラス母材を製造することができる。これは上記原料を水素・酸素火炎中に導入し、生成したシリカ微粒子を耐熱性ターゲット上に堆積させて多孔質体（スート）を製造することにより合成石英ガラス母材を製造する方法である。 More specifically, for example, a synthetic quartz glass base material can be manufactured by a vapor phase reaction method using silicon tetrachloride or the like as a raw material. This is a method of producing a synthetic quartz glass base material by introducing the above-mentioned raw material into a hydrogen / oxygen flame and depositing the produced silica fine particles on a heat resistant target to produce a porous body (soot).
かかる合成石英ガラス母材１０を、上面１４ａ、側面１４ｂ、下面１４ｃを有する成型体１２に成型する（成型工程、図１（ｂ））。成型体１２に成型するにあたっては、合成石英ガラス母材１０を例えば溶融成型することで成型体１２が得ることができる。 The synthetic quartz glass base material 10 is molded into a molded body 12 having an upper surface 14a, a side surface 14b, and a lower surface 14c (a molding process, FIG. 1 (b)). In forming into the forming body 12, the forming body 12 can be obtained by, for example, melt-molding the synthetic quartz glass base material 10.
次に、かかる成型体１２の前記上下面１４ａ，１４ｃ及び側面１４ｂにダミー石英ガラス１８ａ，１８ｂ，１８ｃを溶着してダミー部１６を形成し、ダミー付中間体２０を作製する（中間体作製工程、図１（ｃ））。ダミー石英ガラス１８ａ，１８ｂ，１８ｃは、図示例では、それぞれ上面ダミー石英ガラス１８ａ，側面ダミー石英ガラス１８ｂ，下面ダミー石英ガラス１８ｃとから形成される。ダミー石英ガラス１８ａ，１８ｂ，１８ｃは、図示例では、それぞれ上面ダミー石英ガラス１８ａ，側面ダミー石英ガラス１８ｂ，下面ダミー石英ガラス１８ｃの厚さとしては、少なくとも１０ｍｍ以上であることが好ましく、３０ｍｍ以下程度が好ましい。このようにして、ダミー部１６が周囲に一体化されたダミー付中間体２０が作製される。 Next, the dummy quartz glass 18a, 18b, 18c is welded to the upper and lower surfaces 14a, 14c and the side surface 14b of the molded body 12 to form the dummy portion 16, and the dummy intermediate 20 is manufactured (intermediate manufacturing process , FIG. 1 (c)). The dummy quartz glasses 18a, 18b, and 18c are respectively formed of an upper surface dummy quartz glass 18a, a side surface dummy quartz glass 18b, and a lower surface dummy quartz glass 18c in the illustrated example. The thickness of the dummy quartz glass 18a, 18b, 18c is preferably at least 10 mm or more, about 30 mm or less in the illustrated example, as the thickness of the upper surface dummy quartz glass 18a, the side surface dummy quartz glass 18b, and the lower surface dummy quartz glass 18c. Is preferred. In this manner, a dummy-provided intermediate 20 in which the dummy portion 16 is integrated around is produced.
そして、得られたダミー付中間体２０に対して、熱処理を行う（熱処理工程、図１（ｄ））。熱処理としては、９００℃〜１３００℃の温度範囲で３０分〜８００時間の熱処理を行うことが好ましい。２０時間〜２００時間の熱処理を行うことがより好ましい。また、ダミー付中間体２０に対して、前記熱処理工程の後、水素処理を行うようにしてもよい（水素処理工程）。この水素処理工程としては、ダミー付中間体２０に対して、水素ガス含有雰囲気中で、３００℃〜７００℃の温度で熱処理を施し、水素分子を含有させるのが好ましい。 And heat processing is performed with respect to the obtained intermediate 20 with a dummy (heat processing process, FIG.1 (d)). As heat treatment, it is preferable to perform heat treatment for 30 minutes to 800 hours in a temperature range of 900 ° C. to 1300 ° C. It is more preferable to perform heat treatment for 20 hours to 200 hours. Further, hydrogen treatment may be performed on the dummy intermediate 20 after the heat treatment step (hydrogen treatment step). In the hydrogen treatment step, the dummy intermediate 20 is preferably heat-treated at a temperature of 300 ° C. to 700 ° C. in a hydrogen gas-containing atmosphere to contain hydrogen molecules.
次に、前記ダミー付中間体２０の前記ダミー部１６を除去する（ダミー部除去工程、図１（ｅ））。前記ダミー部１６を除去する方法としては、前記ダミー部１６を取り外して除去する方法でもよいし、あるいは前記ダミー部１６を研削で除去するようにしてもよい。 Next, the dummy part 16 of the dummy intermediate 20 is removed (dummy part removing step, FIG. 1 (e)). As a method of removing the dummy portion 16, the method of removing and removing the dummy portion 16 may be used, or the dummy portion 16 may be removed by grinding.
このようにして、ダミー部１６が除去された製品としての合成石英ガラス２２が得られる（図１（ｆ））。 Thus, the synthetic quartz glass 22 as a product from which the dummy part 16 is removed is obtained (FIG. 1 (f)).
以下に実施例をあげて本発明をさらに具体的に説明するが、これらの実施例は例示的に示されるもので限定的に解釈されるべきでないことはいうまでもない。 EXAMPLES The present invention will be more specifically described below with reference to examples, but it is needless to say that these examples are exemplarily shown and should not be construed as limiting.
（実施例１）
外径160mm以上の合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径310mm厚み85mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。また外径380mm内径320mm高さ80mmの合成石英ガラス製のリングを作製し、側面ダミー石英ガラスとした。さらに外径380mm厚み10mmの合成石英ガラス製の板を2枚作製し、それぞれ上面ダミー石英ガラス及び下面ダミー石英ガラスとした。
Example 1
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm or more, melt molding was performed using carbon as a mold, and a molded body of synthetic quartz glass having an outer diameter of 310 mm and a thickness of 85 mm was formed. . Further, a ring made of synthetic quartz glass having an outer diameter of 380 mm and an inner diameter of 320 mm and a height of 80 mm was produced and used as side dummy quartz glass. Furthermore, two plates made of synthetic quartz glass having an outer diameter of 380 mm and a thickness of 10 mm were produced, and used as upper surface dummy quartz glass and lower surface dummy quartz glass, respectively.
再びカーボンを型として、側面ダミー石英ガラスである合成石英ガラス製のリングの内側に合成石英ガラス成型体を配置し、その上下に上面ダミー石英ガラス及び下面ダミー石英ガラスの合成石英ガラス製の板を1枚ずつ配置して、溶融成型を行い、側面ダミー石英ガラスのリング、上面ダミー石英ガラス及び下面ダミー石英ガラスの板、成型体が一体となった外径380mm厚み100mmの合成石英ガラスのダミー付中間体を作製した。 Again using the carbon as a mold, the molded synthetic quartz glass is placed inside the ring made of synthetic quartz glass which is a side surface dummy quartz glass, and a plate made of synthetic quartz glass of upper surface dummy quartz glass and lower surface dummy quartz glass Arranged one by one and melt-molded, ring of dummy quartz glass on the side, plate of dummy quartz glass on upper side and dummy quartz glass on lower side, dummy of synthetic quartz glass of outer diameter 380 mm and thickness 100 mm integrated with molding. An intermediate was made.
この一体となったダミー付中間体を熱処理炉（大気炉）内の炉材上に設置し、室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後ヒーターによる加熱を停止し、放冷した。さらにこの熱処理後にこのダミー付中間体を加圧加熱炉内に設置して、室温から4時間かけて500℃まで昇温し、500℃で800時間維持した後、加熱を停止して放冷した。この加圧加熱炉での熱処理時は、雰囲気を水素、圧力を１気圧とした。 This integrated dummy intermediate is placed on a furnace material in a heat treatment furnace (atmospheric furnace), heated from room temperature to 1200 ° C. over 10 hours, maintained at 1200 ° C. for 50 hours, and then taken over 100 hours The temperature was lowered to 1000 ° C., after which heating by the heater was stopped and allowed to cool. After this heat treatment, this dummy intermediate was placed in a pressure heating furnace, heated from room temperature to 500 ° C. over 4 hours, maintained at 500 ° C. for 800 hours, then stopped heating and allowed to cool . At the time of heat treatment in this pressure heating furnace, the atmosphere was hydrogen and the pressure was 1 atm.
この2つの熱処理工程の後、上・下に配置溶着した上面ダミー石英ガラス及び下面ダミー石英ガラスの板を切断し、側面ダミー石英ガラスのリングに内包溶着した合成石英ガラス部分をくり貫き、ダミー部を除去した。このようにして、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。この合成石英ガラスの製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定と、水素濃度の測定も行った。 After these two heat treatment steps, the upper and lower dummy quartz glass plates arranged and welded on the upper and lower sides are cut, and the synthetic quartz glass portion embedded and welded in the ring of the side dummy quartz glass is cut away. Was removed. Thus, a product of cylindrical synthetic quartz glass having an outer diameter of 320 mm and a thickness of 80 mm was obtained. The birefringence of the product of this synthetic quartz glass and the refractive index homogeneity were measured. Further, measurement of impurity concentration (Na) and measurement of hydrogen concentration were also performed.
複屈折は、光ヘテロダイン干渉法を用いて測定し、屈折率均質性は、フィゾー型光干渉計を用い、オイルオンプレート法により測定した。測定に使用した波長は６３３ｎｍであった。また不純物濃度（Na）測定は、ICPMS分析法を用い、水素濃度測定は、ラマン分光法を用いた。 Birefringence was measured using optical heterodyne interferometry, and refractive index homogeneity was measured using oil-on-plate method using a Fizeau-type optical interferometer. The wavelength used for the measurement was 633 nm. The impurity concentration (Na) was measured using ICPMS analysis, and the hydrogen concentration was measured using Raman spectroscopy.
不純物濃度(Na)の測定は、図２（ａ）に示した円柱状の合成石英ガラスにおいて、図２（ｂ）に示したように、円柱状の合成石英ガラスの外周表面から中心方向へ５ｍｍずつ内側に入った３か所で測定した。図２（ｂ）において、符号１が外周表面から５ｍｍ位置まで、符号２が５ｍｍ〜１０ｍｍ位置まで、符号３が１０ｍｍ〜１５ｍｍ位置まで、をそれぞれ示す。
The measurement of the impurity concentration (Na) is 5 mm in the center direction from the outer peripheral surface of the cylindrical synthetic quartz glass, as shown in FIG. 2 (b), in the cylindrical synthetic quartz glass shown in FIG. It measured in three places which went inside one by one. In FIG.2 (b), code |
測定の結果、複屈折値（複屈折位相差）の最大値は0.3nm/cm、屈折率均質性は0.8×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：4.0ppb、5mm〜10mm：2.0ppb、10mm〜15mm：0.5ppb、水素濃度については、最小で1.0×1017分子/cm3、最大で2.0×1017分子/cm3であった。原料14kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 The measurement results show that the maximum birefringence value (birefringence retardation) is 0.3 nm / cm, the refractive index homogeneity is 0.8 × 10 -6 , and the impurity concentration (Na) is 5 mm from the surface of the side surface: 4.0 ppb 5 mm to 10 mm: 2.0 ppb, 10 mm to 15 mm: 0.5 ppb, and the hydrogen concentration was a minimum of 1.0 × 10 17 molecules / cm 3 and a maximum of 2.0 × 10 17 molecules / cm 3 . Using 14 kg of raw material (weight of synthetic quartz glass base material), 14 kg of a product (finally obtained synthetic quartz glass) was obtained. The results are shown in Table 1.
複屈折値は1.0nm/cm以下が好ましく、より好ましくは0.5nm/cm以下である。屈折率均質性は、5.0×10-6以下が好ましく、より好ましくは2.0×10-6以下、さらに好ましくは1.0×10-6以下である。不純物濃度（Na）は、10ppb以下が好ましく、より好ましくは5ppb以下、さらに好ましくは2ppb以下である。水素濃度Δ（最大-最小）は、3.0×1017分子/cm3以下が好ましく、より好ましくは2.0×1017分子/cm3以下、さらに好ましくは1.0×1017分子/cm3以下である。 The birefringence value is preferably 1.0 nm / cm or less, more preferably 0.5 nm / cm or less. The refractive index homogeneity is preferably 5.0 × 10 −6 or less, more preferably 2.0 × 10 −6 or less, and still more preferably 1.0 × 10 −6 or less. The impurity concentration (Na) is preferably 10 ppb or less, more preferably 5 ppb or less, and still more preferably 2 ppb or less. The hydrogen concentration Δ (maximum-minimum) is preferably 3.0 × 10 17 molecules / cm 3 or less, more preferably 2.0 × 10 17 molecules / cm 3 or less, and still more preferably 1.0 × 10 17 molecules / cm 3 or less.
（実施例２）
外径160mmの合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径310mm厚み85mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。また外径360mm内径320mm高さ80mmの合成石英ガラス製のリングを作製し、側面ダミー石英ガラスとした。さらに外径380mm高さ20mmの合成石英ガラス製板を2枚作製し、それぞれ上面ダミー石英ガラス及び下面ダミー石英ガラスとした。
(Example 2)
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm, and melt molding was performed using carbon as a mold to produce a molded body of synthetic quartz glass having upper and lower surfaces and side surfaces of a cylindrical shape having an outer diameter of 310 mm and a thickness of 85 mm. Further, a ring made of synthetic quartz glass having an outer diameter of 360 mm, an inner diameter of 320 mm and a height of 80 mm was produced and used as a side dummy quartz glass. Furthermore, two synthetic quartz glass plates having an outer diameter of 380 mm and a height of 20 mm were produced, and used as upper surface dummy quartz glass and lower surface dummy quartz glass, respectively.
再びカーボンを型として、側面ダミー石英ガラスである合成石英ガラス製のリングの内側に合成石英ガラス成型体を配置し、その上下に上面ダミー石英ガラス及び下面ダミー石英ガラスの合成石英ガラス製の板を1枚ずつ配置して、溶融成型を行い、側面ダミー石英ガラスのリング、上面ダミー石英ガラス及び下面ダミー石英ガラスの板、成型体が一体となった外径360mm厚み120mmの合成石英ガラスのダミー付中間体を作製した。 Again using the carbon as a mold, the molded synthetic quartz glass is placed inside the ring made of synthetic quartz glass which is a side surface dummy quartz glass, and a plate made of synthetic quartz glass of upper surface dummy quartz glass and lower surface dummy quartz glass Arranged one by one and melt-molded, ring of dummy quartz glass on the side, plate of dummy quartz glass on upper side and dummy quartz glass on lower side, dummy of synthetic quartz glass of outer diameter 360 mm and thickness 120 mm integrated with molding. An intermediate was made.
この一体となったダミー付中間体を熱処理炉（大気炉）内の炉材上に設置し、室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後、ヒーターの加熱を停止し、放冷した。さらにこの熱処理後に一体となったダミー付中間体を加圧加熱炉内に設置して、室温から4時間かけて500℃まで昇温し、500℃で1000時間維持した後、加熱を停止して放冷した。この加熱加圧炉での熱処理時は、雰囲気を水素、圧力を1気圧とした。 This integrated dummy intermediate is placed on a furnace material in a heat treatment furnace (atmospheric furnace), heated from room temperature to 1200 ° C. over 10 hours, maintained at 1200 ° C. for 50 hours, and then taken over 100 hours Then, the heating of the heater was stopped and allowed to cool. Further, the dummy-provided intermediate after heat treatment is placed in a pressure heating furnace, heated from room temperature to 500 ° C. over 4 hours, maintained at 500 ° C. for 1000 hours, and then stopped heating. It was allowed to cool. During the heat treatment in this heating and pressurizing furnace, the atmosphere is hydrogen and the pressure is 1 atm.
この2つの熱処理工程の後、上・下に配置溶着した上面ダミー石英ガラス及び下面ダミー石英ガラスの板を切断し、側面ダミー石英ガラスのリングに内包溶着した合成石英ガラス部分をくり貫き、ダミー部を除去した。このようにして、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。この合成石英ガラスの製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定と、水素濃度の測定も行った。 After these two heat treatment steps, the upper and lower dummy quartz glass plates arranged and welded on the upper and lower sides are cut, and the synthetic quartz glass portion embedded and welded in the ring of the side dummy quartz glass is cut away. Was removed. Thus, a product of cylindrical synthetic quartz glass having an outer diameter of 320 mm and a thickness of 80 mm was obtained. The birefringence of the product of this synthetic quartz glass and the refractive index homogeneity were measured. Further, measurement of impurity concentration (Na) and measurement of hydrogen concentration were also performed.
測定の結果、複屈折値（複屈折位相差）の最大値は、0.4nm/cm、屈折率均質性は、1.0×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：6.0ppb、5mm〜10mm：2.5ppb、10mm〜15mm：0.7ppb、水素濃度については、最小で1.0×1017分子/cm3、最大で2.5×1017分子/cm3であった。原料14kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 As a result of the measurement, the maximum value of the birefringence value (birefringence retardation) is 0.4 nm / cm, the refractive index homogeneity is 1.0 × 10 −6 , and the impurity concentration (Na) is within 5 mm from the side surface: 6.0 ppb, 5 mm to 10 mm: 2.5 ppb, 10 mm to 15 mm: 0.7 ppb, and the hydrogen concentration was a minimum of 1.0 × 10 17 molecules / cm 3 and a maximum of 2.5 × 10 17 molecules / cm 3 . Using 14 kg of raw material (weight of synthetic quartz glass base material), 14 kg of a product (finally obtained synthetic quartz glass) was obtained. The results are shown in Table 1.
（実施例３）
外径160mm以上の合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径310mm厚み85mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。また外径380mm内径320mm高さ80mmの合成石英ガラス製のリングを作製し、側面ダミー石英ガラスとした。さらに外径380mm厚み10mmの合成石英ガラス製の板を2枚作製し、それぞれ上面ダミー石英ガラス及び下面ダミー石英ガラスとした。
(Example 3)
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm or more, melt molding was performed using carbon as a mold, and a molded body of synthetic quartz glass having an outer diameter of 310 mm and a thickness of 85 mm was formed. . Further, a ring made of synthetic quartz glass having an outer diameter of 380 mm and an inner diameter of 320 mm and a height of 80 mm was produced and used as side dummy quartz glass. Furthermore, two plates made of synthetic quartz glass having an outer diameter of 380 mm and a thickness of 10 mm were produced, and used as upper surface dummy quartz glass and lower surface dummy quartz glass, respectively.
再びカーボンを型として、側面ダミー石英ガラスである合成石英ガラス製のリングの内側に合成石英ガラス成型体を配置し、その上下に上面ダミー石英ガラス及び下面ダミー石英ガラスの合成石英ガラス製の板を1枚ずつ配置して、溶融成型を行い、側面ダミー石英ガラスのリング、上面ダミー石英ガラス及び下面ダミー石英ガラスの板、成型体が一体となった外径380mm厚み100mmの合成石英ガラスのダミー付中間体を作製した。この一体となったダミー付中間体を熱処理炉（大気炉）内の炉材上に設置し、室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後ヒーターによる加熱を停止し、放冷した。 Again using the carbon as a mold, the molded synthetic quartz glass is placed inside the ring made of synthetic quartz glass which is a side surface dummy quartz glass, and a plate made of synthetic quartz glass of upper surface dummy quartz glass and lower surface dummy quartz glass Arranged one by one and melt-molded, ring of dummy quartz glass on the side, plate of dummy quartz glass on upper side and dummy quartz glass on lower side, dummy of synthetic quartz glass of outer diameter 380 mm and thickness 100 mm integrated with molding. An intermediate was made. This integrated dummy intermediate is placed on a furnace material in a heat treatment furnace (atmospheric furnace), heated from room temperature to 1200 ° C. over 10 hours, maintained at 1200 ° C. for 50 hours, and then taken over 100 hours The temperature was lowered to 1000 ° C., after which heating by the heater was stopped and allowed to cool.
この熱処理工程の後、上・下に配置溶着した上面ダミー石英ガラス及び下面ダミー石英ガラスの板を切断し、側面ダミー石英ガラスのリングに内包溶着した合成石英ガラス部分をくり貫き、ダミー部を除去した。このようにして、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。この合成石英ガラスの製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定を行った。 After this heat treatment step, the upper and lower dummy quartz glass plates arranged and welded on the upper and lower sides are cut, and the synthetic quartz glass portion embedded and welded in the ring of the side dummy quartz glass is cut away to remove the dummy portion. did. Thus, a product of cylindrical synthetic quartz glass having an outer diameter of 320 mm and a thickness of 80 mm was obtained. The birefringence of the product of this synthetic quartz glass and the refractive index homogeneity were measured. Furthermore, the impurity concentration (Na) was measured.
測定の結果、複屈折値（複屈折位相差）の最大値は、0.3nm/cm、屈折率均質性は、0.5×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：4.2ppb、5mm〜10mm：2.2ppb、10mm〜15mm：0.6ppbであった。原料14kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 As a result of the measurement, the maximum value of the birefringence value (birefringence retardation) is 0.3 nm / cm, the refractive index homogeneity is 0.5 × 10 −6 , and the impurity concentration (Na) is within 5 mm from the side surface: It was 4.2 ppb, 5 mm to 10 mm: 2.2 ppb, 10 mm to 15 mm: 0.6 ppb. Using 14 kg of raw material (weight of synthetic quartz glass base material), 14 kg of a product (finally obtained synthetic quartz glass) was obtained. The results are shown in Table 1.
（比較例１）
外径160mm以上の合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径320mm厚み80mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。この合成石英ガラスの成型体を熱処理炉（大気炉）内の炉材上に設置し、室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後ヒーターによる加熱を停止し、放冷した。さらにこの熱処理後にこの合成石英ガラスの成型体を加圧加熱炉内に設置して、室温から4時間かけて500℃まで昇温し、500℃で600時間維持した後、加熱を停止して放冷した。この加圧加熱炉での熱処理時は、雰囲気を水素、圧力を１気圧とした。このようにして、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。
(Comparative example 1)
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm or more, melt molding was performed using carbon as a mold, and a molded body of synthetic quartz glass having an outer diameter of 320 mm, a cylindrical shape of 80 mm thickness, upper and lower surfaces and side surfaces was produced. . The molded body of this synthetic quartz glass is placed on a furnace material in a heat treatment furnace (atmospheric furnace), heated to 1200 ° C. over 10 hours from room temperature, maintained at 1200 ° C. for 50 hours, then 1000 for 100 hours. The temperature was lowered to ° C, after which heating by the heater was stopped and allowed to cool. Further, after this heat treatment, the molded body of this synthetic quartz glass is placed in a pressure heating furnace, heated to 500 ° C. from room temperature over 4 hours and maintained at 500 ° C. for 600 hours. It was cold. At the time of heat treatment in this pressure heating furnace, the atmosphere was hydrogen and the pressure was 1 atm. Thus, a product of cylindrical synthetic quartz glass having an outer diameter of 320 mm and a thickness of 80 mm was obtained.
このようにして得られた合成石英ガラスの製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定と、水素濃度の測定も行った。 The birefringence and refractive index homogeneity of the product of synthetic quartz glass thus obtained were measured. Further, measurement of impurity concentration (Na) and measurement of hydrogen concentration were also performed.
測定の結果、複屈折値（複屈折位相差）の最大値は、1.2nm/cm、屈折率均質性は、1.7×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：25ppb、5mm〜10mm：11ppb、10mm〜15mm：3.0ppb、水素濃度については、最小で1.0×1017分子/cm3、最大で5.0×1017分子/cm3であった。原料14kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 As a result of the measurement, the maximum value of the birefringence value (birefringence retardation) is 1.2 nm / cm, the refractive index homogeneity is 1.7 × 10 −6 , and the impurity concentration (Na) is within 5 mm from the side surface: 25 ppb, 5 mm to 10 mm: 11 ppb, 10 mm to 15 mm: 3.0 ppb, and the hydrogen concentration was a minimum of 1.0 × 10 17 molecules / cm 3 and a maximum of 5.0 × 10 17 molecules / cm 3 . Using 14 kg of raw material (weight of synthetic quartz glass base material), 14 kg of a product (finally obtained synthetic quartz glass) was obtained. The results are shown in Table 1.
（比較例２）
外径160mm以上の合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径380mm厚み100mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。この合成石英ガラスの成型体を熱処理炉（大気炉）内の炉材上に設置し、室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後ヒーターによる加熱を停止し、放冷した。さらにこの熱処理後にこの合成石英ガラスの成型体を加圧加熱炉内に設置して、室温から4時間かけて500℃まで昇温し、500℃で800時間維持した後、加熱を停止して放冷した。この加圧加熱炉での熱処理時は、雰囲気を水素、圧力を１気圧とした。
(Comparative example 2)
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm or more, melt molding was performed using carbon as a mold, and a molded body of synthetic quartz glass having an outer diameter of 380 mm and a cylindrical shape with a thickness of 100 mm was produced. . The molded body of this synthetic quartz glass is placed on a furnace material in a heat treatment furnace (atmospheric furnace), heated to 1200 ° C. over 10 hours from room temperature, maintained at 1200 ° C. for 50 hours, then 1000 for 100 hours. The temperature was lowered to ° C, after which heating by the heater was stopped and allowed to cool. Further, after this heat treatment, the molded body of this synthetic quartz glass is placed in a pressure heating furnace, heated to 500 ° C. from room temperature over 4 hours and maintained at 500 ° C. for 800 hours. It was cold. At the time of heat treatment in this pressure heating furnace, the atmosphere was hydrogen and the pressure was 1 atm.
この2つの熱処理工程の後、上・下10mmを切断し、外周部30mmを研削して、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。この合成石英ガラス製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定と、水素濃度の測定も行った。 After these two heat treatment steps, the upper and lower 10 mm were cut, and the outer peripheral portion 30 mm was ground to obtain a cylindrical synthetic quartz glass product having an outer diameter of 320 mm and a thickness of 80 mm. The birefringence and refractive index homogeneity of this synthetic quartz glass product were measured. Further, measurement of impurity concentration (Na) and measurement of hydrogen concentration were also performed.
測定の結果、複屈折値（複屈折位相差）の最大値は、0.3nm/cm、屈折率均質性は、0.8×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：4.0ppb、5mm〜10mm：2.0ppb、10mm〜15mm：0.5ppb、水素濃度については、最小で1.0×1017分子/cm3、最大で2.0×1017分子/cm3、原料25kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 As a result of the measurement, the maximum value of the birefringence value (birefringence retardation) is 0.3 nm / cm, the refractive index homogeneity is 0.8 × 10 −6 , and the impurity concentration (Na) is within 5 mm from the side surface: 4.0 ppb, 5 mm to 10 mm: 2.0 ppb, 10 mm to 15 mm: 0.5 ppb, the minimum hydrogen concentration is 1.0 × 10 17 molecules / cm 3 , the maximum 2.0 × 10 17 molecules / cm 3 , the raw material 25 kg (synthetic quartz glass The weight of the base material was used to obtain 14 kg of a product (synthetic quartz glass finally obtained). The results are shown in Table 1.
（比較例３）
外径160mm以上の合成石英ガラス母材から必要重量を切り出して、カーボンを型として溶融成型を行い、外径320mm厚み80mmの円柱形状の上下面及び側面を有する合成石英ガラスの成型体を作製した。また外径380mm内径325mm高さ82mmの合成石英ガラス製のリングを作製し、側面ダミー石英ガラスとした。さらに外径380mm厚み10mmの合成石英ガラス製の板を2枚作製し、それぞれ上面ダミー石英ガラス及び下面ダミー石英ガラスとした。
(Comparative example 3)
A necessary weight was cut out of a synthetic quartz glass base material having an outer diameter of 160 mm or more, melt molding was performed using carbon as a mold, and a molded body of synthetic quartz glass having an outer diameter of 320 mm, a cylindrical shape of 80 mm thickness, upper and lower surfaces and side surfaces was produced. . Further, a ring made of synthetic quartz glass having an outer diameter of 380 mm, an inner diameter of 325 mm and a height of 82 mm was produced and used as side dummy quartz glass. Furthermore, two plates made of synthetic quartz glass having an outer diameter of 380 mm and a thickness of 10 mm were produced, and used as upper surface dummy quartz glass and lower surface dummy quartz glass, respectively.
熱処理炉（大気炉）内の炉材上に、作製した下面ダミー石英ガラスの板を敷き、この上に円柱形状の合成石英ガラスの成型体を配置し、この合成石英ガラスの成型体が内包するように合成石英ガラス製の側面ダミー石英ガラスのリングを配置し、これらの上に作製した合成石英ガラスの上面ダミー石英ガラスの板を配置した。溶着はしていないが一体とした石英ガラス中間体を室温から10時間かけて1200℃まで昇温し、1200℃で50時間維持した後、100時間かけて1000℃まで降温し、その後ヒーターによる加熱を停止し、放冷した。さらにこの熱処理後にこの溶着はしていないが一体とした石英ガラス中間体を加圧加熱炉内に設置して、室温から4時間かけて500℃まで昇温し、500℃で600時間維持した後、加熱を停止して放冷した。この加圧加熱炉での熱処理時は、雰囲気を水素、圧力を１気圧とした。 A plate of the prepared lower surface dummy quartz glass is laid on a furnace material in a heat treatment furnace (atmospheric furnace), a cylindrical synthetic quartz glass molded body is disposed thereon, and the synthetic quartz glass molded body is contained As described above, the rings of the side dummy quartz glass made of synthetic quartz glass were disposed, and the plate of the upper surface dummy quartz glass of the synthetic quartz glass fabricated above was disposed. The fused quartz intermediate which is not welded but integrated is heated from room temperature to 1200 ° C. over 10 hours, maintained at 1200 ° C. for 50 hours, then cooled to 1000 ° C. over 100 hours, and then heated by a heater Stop and let it cool. After this heat treatment, the fused quartz intermediate body which has not been welded but is integrated is placed in a pressure heating furnace and heated from room temperature to 500 ° C. over 4 hours and maintained at 500 ° C. for 600 hours Stop heating and let it cool. At the time of heat treatment in this pressure heating furnace, the atmosphere was hydrogen and the pressure was 1 atm.
この2つの熱処理工程の後、溶着はしていないが一体とした石英ガラス中間体から側面ダミー石英ガラスのリング、上面ダミー石英ガラス及び下面ダミー石英ガラスの板を外し、外径320mm厚み80mmの円柱形状の合成石英ガラスの製品を得た。この合成石英ガラス製品の複屈折と、屈折率均質性を測定した。さらに不純物濃度(Na)の測定と、水素濃度の測定も行った。 After these two heat treatment steps, remove the ring of dummy quartz glass on the side surface, the upper surface dummy quartz glass and the lower surface dummy quartz glass from the integrated quartz glass intermediate which is not welded but integrated, and the column of outer diameter 320 mm and thickness 80 mm A product of synthetic quartz glass in shape was obtained. The birefringence and refractive index homogeneity of this synthetic quartz glass product were measured. Further, measurement of impurity concentration (Na) and measurement of hydrogen concentration were also performed.
測定の結果、複屈折値（複屈折位相差）の最大値は、0.6nm/cm、屈折率均質性は、1.7×10-6、不純物濃度（Na）は、側面の表面から5mm内部まで：12ppb、5mm〜10mm：6.0ppb、10mm〜15mm：2.0ppb、水素濃度については、最小で1.0×1017分子/cm3、最大で5.0×1017分子/cm3であった。原料14kg（合成石英ガラス母材の重量）を使用し、14kgの製品（最終的に得られた合成石英ガラス）を得た。結果を表１に示す。 As a result of the measurement, the maximum value of the birefringence value (birefringence retardation) is 0.6 nm / cm, the refractive index homogeneity is 1.7 × 10 −6 , and the impurity concentration (Na) is within 5 mm from the side surface: 12 ppb, 5 mm to 10 mm: 6.0 ppb, 10 mm to 15 mm: 2.0 ppb, the hydrogen concentration was a minimum of 1.0 × 10 17 molecules / cm 3 and a maximum of 5.0 × 10 17 molecules / cm 3 . Using 14 kg of raw material (weight of synthetic quartz glass base material), 14 kg of a product (finally obtained synthetic quartz glass) was obtained. The results are shown in Table 1.
上記結果からわかるように、実施例１〜３では、品質が良く且つ歩留りのよい合成石英ガラス製品が得られた。 As can be seen from the above results, in Examples 1 to 3, synthetic quartz glass products with good quality and good yield were obtained.
１：外周表面から５ｍｍ位置、２：５ｍｍ〜１０ｍｍ位置、３：１０ｍｍ〜１５ｍｍ位置、１０：合成石英ガラス母材、１２：成型体、１４ａ：上面、１４ｂ：側面、１４ｃ：下面、１６：ダミー部、１８ａ：上面ダミー石英ガラス、１８ｂ：側面ダミー石英ガラス、１８ｃ：下面ダミー石英ガラス、２０：ダミー付中間体、２２：合成石英ガラス。 1: 5 mm from the outer peripheral surface, 2: 5 to 10 mm, 3: 10 to 15 mm, 10: synthetic quartz glass base material, 12: molded body, 14a: upper surface, 14b: side surface, 14c: lower surface, 16: dummy Part, 18a: upper surface dummy quartz glass, 18b: side surface dummy quartz glass, 18c: lower surface dummy quartz glass, 20: intermediate with dummy, 22: synthetic quartz glass.
Claims (3)
前記成型体の前記上下面及び側面にダミー石英ガラスを溶着してダミー部を形成し、ダミー付中間体を作製する中間体作製工程と、
前記ダミー付中間体を熱処理する熱処理工程と、
前記ダミー付中間体の前記ダミー部を除去し、合成石英ガラスとするダミー部除去工程と、
を含み、
前記合成石英ガラスの屈折率均質性が１．０×１０ −６ 以下である、合成石英ガラスの製造方法。 Forming a synthetic quartz glass base material into a molded body having upper and lower surfaces and side surfaces;
An intermediate body producing step of producing a dummy portion by welding a dummy quartz glass to the upper and lower surfaces and side surfaces of the molded body to form a dummy portion;
A heat treatment step of heat treating the intermediate with dummy;
A dummy portion removing step of removing the dummy portion of the intermediate body with dummy to obtain synthetic quartz glass;
Only including,
The manufacturing method of synthetic quartz glass whose refractive index homogeneity of the said synthetic quartz glass is 1.0 * 10 < -6> or less .
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