JP6058693B2 - 合成石英ガラスを製造する方法及び光ファイバーのクラッド材としての石英ガラス - Google Patents
合成石英ガラスを製造する方法及び光ファイバーのクラッド材としての石英ガラス Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000013307 optical fiber Substances 0.000 title claims description 12
- 239000000463 material Substances 0.000 title claims description 11
- 238000005253 cladding Methods 0.000 title claims description 8
- 239000004071 soot Substances 0.000 claims description 67
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 53
- 229910052799 carbon Inorganic materials 0.000 claims description 53
- 238000000034 method Methods 0.000 claims description 38
- 239000000460 chlorine Substances 0.000 claims description 37
- 238000001035 drying Methods 0.000 claims description 36
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 30
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 30
- 229910052801 chlorine Inorganic materials 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 29
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 28
- 229910052760 oxygen Inorganic materials 0.000 claims description 24
- 239000001301 oxygen Substances 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 21
- 230000008021 deposition Effects 0.000 claims description 19
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 12
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 229910052736 halogen Inorganic materials 0.000 description 8
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- 229910052739 hydrogen Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
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- 230000005540 biological transmission Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
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- 150000003961 organosilicon compounds Chemical class 0.000 description 3
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- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
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- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
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- 150000002430 hydrocarbons Chemical class 0.000 description 2
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- 238000011144 upstream manufacturing Methods 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
- 206010021143 Hypoxia Diseases 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
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- 150000001721 carbon Chemical group 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
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- 229930195733 hydrocarbon Natural products 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000001393 microlithography Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
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- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
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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]
-
- 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]
- C03B37/01406—Deposition reactors therefor
-
- 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]
- C03B37/01413—Reactant delivery systems
-
- 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
- C03C13/00—Fibre or filament compositions
- C03C13/008—Polycrystalline optical fibres
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
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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
- C03B2201/80—Non-oxide glasses or glass-type compositions
- C03B2201/84—Halide glasses other than fluoride glasses, i.e. Cl, Br or I glasses, e.g. AgCl-AgBr "glass"
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
-
- 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
- C03C2213/00—Glass fibres or filaments
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- General Life Sciences & Earth Sciences (AREA)
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Description
(a)炭素含有ケイ素化合物を含む供給原料を酸素と反応帯において反応させて、SiO2粒子を得る工程と、
(b)SiO2粒子を堆積面に堆積させて、炭素と水酸基とを含む多孔質SiO2スート体を形成する工程と、
(c)多孔質SiO2スート体を乾燥させる工程と、
(d)スート体をガラス化温度まで加熱することによってガラス化して、合成石英ガラスを形成する工程と
を含む方法に関するものである。
H2O + C → CO + H2 (1)
2OH + C → CO2 + H2 (2)
OH + CO → CO2 + 1/2H2 (3)
SiO2スート体200は図1に概略的に示される装置によって作製される。一列に並んだ複数の火炎加水分解用バーナー140が酸化アルミニウムの支持管160に沿って配置され、スートを堆積するのに回転支持管160に沿って連結バーナー列の形で反転往復運動する。各バーナー火炎143は支持管160の全長未満しか移動しない。火炎加水分解用バーナー140は連結バーナーブロック141上に載置され、この連結バーナーブロック141は、長手軸161に対して定常的な位置にある2つの反転点の間を支持管160の長手軸161に平行して往復運動し、矢印142に示されるように長手軸に対して垂直方向に位置を変えることができる。バーナー140は石英ガラスで構成されており、互いの中心間距離は15cmである。
製造プロセスに起因して導入される水酸基を除去するために、スート管に対して脱水処理を行う。スート管は脱水炉へと垂直方向に投入され、900℃の予備加熱プロセス後にその温度で塩素含有雰囲気下において脱水する。処理期間は24時間である。
化学量論比[燃焼性ガス+OMCTS]/酸素V: 1
SiO2構築率(RSiO2)(相対単位): 100%
構築期間tbuild−up(相対単位): 100%
乾燥温度Tdrying(℃): 900
乾燥期間tdrying(h): 24
C含有量[C](重量ppm): <1
塩素含有量[Cl2](重量ppm): 1600
水酸基含有量[OH](重量ppm): <0.2
減衰係数k248(cm−1): 0.0019
Claims (9)
- 合成石英ガラスを製造する方法であって、
(a)炭素含有ケイ素化合物を含む供給原料を酸素と反応帯において反応させて、SiO2粒子を得る工程と、
(b)前記SiO2粒子を堆積面に堆積させて、炭素と水酸基とを含む多孔質SiO2スート体を形成する工程と、
(c)前記多孔質SiO2スート体を塩素含有雰囲気下において加熱することによって乾燥させる工程と、
(d)前記スート体をガラス化温度まで加熱することによってガラス化して、合成石英ガラスを形成する工程と
を含み、炭素含有量が1重量ppm〜50重量ppmの範囲内のスート体を作製すること及びガラス化後の前記合成石英ガラス中の塩素含有量が800重量ppm〜2500重量ppmの範囲内に調節されるように前記乾燥工程を行うことを特徴とする方法。 - 方法工程(a)による前記供給原料の反応中に、化学量論比を超える前記炭素含有ケイ素化合物が前記反応帯において与えられることで前記炭素含有量が得られることを特徴とする請求項1に記載の方法。
- 前記炭素含有ケイ素化合物の前記反応帯中の滞留時間を前記供給原料の完全燃焼に必要とされるよりも短く調節することで前記炭素含有量が得られることを特徴とする請求項1又は2に記載の方法。
- 前記滞留時間が、反応帯を短くすることによって、及び/又は該反応帯において前記供給原料の流速を高めることによって与えられることを特徴とする請求項3に記載の方法。
- 石英ガラスの密度(2.21g/cm3)に対して平均相対密度が20%〜35%の範囲内のスート体を作製することを特徴とする請求項1〜4のいずれか一項に記載の方法。
- 前記合成石英ガラス中の水酸基含有量が1重量ppm未満に調節されるように前記乾燥工程を行うことを特徴とする請求項1〜5のいずれか一項に記載の方法。
- 炭素含有量が2重量ppm〜25重量ppmの範囲内のスート体を作製することを特徴とする請求項1〜6のいずれか一項に記載の方法。
- 前記供給原料としてOMCTSを使用することを特徴とする請求項1〜7のいずれか一項に記載の方法。
- 光ファイバーのクラッド材としての合成石英ガラスであって、波長248nmでの減衰係数k248によって表される酸素欠陥センターの含有量が0.0035cm−1<k248<0.1cm−1であり、塩素含有量[Cl]が800重量ppm〜2500重量ppmの範囲内であり、水酸基含有量が0.5重量ppm未満であり、且つ[Cl]/k248比が100000<[Cl]/k248<550000であることを特徴する合成石英ガラス。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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DE102011121153.9 | 2011-12-15 | ||
DE102011121153A DE102011121153B3 (de) | 2011-12-15 | 2011-12-15 | Verfahren zur Herstellung von synthetischem Quarzglas sowie Quarzglas für den Einsatz als Mantelmaterial einer optischen Faser |
PCT/EP2012/075197 WO2013087678A1 (de) | 2011-12-15 | 2012-12-12 | Verfahren zur herstellung von synthetischem quarzglas sowie quarzglas für den einsatz als mantelmaterial einer optischen faser |
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JP2015505809A JP2015505809A (ja) | 2015-02-26 |
JP6058693B2 true JP6058693B2 (ja) | 2017-01-11 |
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US (1) | US9272942B2 (ja) |
EP (1) | EP2791070B8 (ja) |
JP (1) | JP6058693B2 (ja) |
KR (1) | KR101569797B1 (ja) |
CN (1) | CN103987670B (ja) |
DE (1) | DE102011121153B3 (ja) |
IN (1) | IN2014CN04288A (ja) |
WO (1) | WO2013087678A1 (ja) |
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Publication number | Priority date | Publication date | Assignee | Title |
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DE102011121190A1 (de) * | 2011-12-16 | 2013-06-20 | Heraeus Quarzglas Gmbh & Co. Kg | OMCTS-Verdampfungsverfahren |
EP2835360A1 (de) * | 2013-08-06 | 2015-02-11 | Heraeus Quarzglas GmbH & Co. KG | Verfahren zur Herstellung eines SiO2-Sootkörpers in Gegenwart von Kohlenstoffmonoxid |
JP2019502633A (ja) | 2015-12-18 | 2019-01-31 | ヘレウス クワルツグラス ゲーエムベーハー ウント コンパニー カーゲー | 均質な石英ガラス製のガラス繊維および母材 |
WO2017103160A1 (de) | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Herstellung von quarzglaskörpern aus siliziumdioxidgranulat |
TWI808933B (zh) | 2015-12-18 | 2023-07-21 | 德商何瑞斯廓格拉斯公司 | 石英玻璃體、二氧化矽顆粒、光導、施照體、及成型體及其製備方法 |
US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
KR20180095618A (ko) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 다중-챔버 가열로에서 실리카 유리체의 제조 |
KR20180095619A (ko) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 실리카 유리 제조 동안 규소 함량의 증가 |
KR20180095879A (ko) * | 2015-12-18 | 2018-08-28 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 상승된 온도에서 탄소-도핑된 실리카 과립을 처리하여 실리카 과립의 알칼리 토금속 함량의 감소 |
EP3390302B1 (de) | 2015-12-18 | 2023-09-20 | Heraeus Quarzglas GmbH & Co. KG | Herstellung eines quarzglaskörpers in einem schmelztiegel aus refraktärmetall |
EP3390290B1 (de) | 2015-12-18 | 2023-03-15 | Heraeus Quarzglas GmbH & Co. KG | Herstellung eines opaken quarzglaskörpers |
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IN2014CN04288A (ja) | 2015-09-04 |
CN103987670B (zh) | 2016-10-19 |
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