JP4700619B2 - レーザー活性石英ガラスの生産方法および使用 - Google Patents
レーザー活性石英ガラスの生産方法および使用 Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical class O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 76
- 239000008187 granular material Substances 0.000 claims description 61
- 238000000034 method Methods 0.000 claims description 60
- 239000002245 particle Substances 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 28
- 239000002019 doping agent Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 11
- 230000003179 granulation Effects 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- -1 transition metal cation Chemical class 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 239000000835 fiber Substances 0.000 description 17
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000011162 core material Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 239000007858 starting material Substances 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007970 homogeneous dispersion Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 206010040925 Skin striae Diseases 0.000 description 1
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 238000005550 wet granulation Methods 0.000 description 1
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- C03B19/063—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction by hot-pressing powders
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- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
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- C03B19/1005—Forming solid beads
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- C03B19/1005—Forming solid beads
- C03B19/106—Forming solid beads by chemical vapour deposition; by liquid phase reaction
- C03B19/1065—Forming solid beads by chemical vapour deposition; by liquid phase reaction by liquid phase reactions, e.g. by means of a gel phase
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- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C03C3/00—Glass compositions
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- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
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- C03C2201/00—Glass compositions
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- C03C2201/00—Glass compositions
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- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
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- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
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- C03C2203/00—Production processes
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Description
a)少なくとも40重量%の固形分を有し、SiO2ナノパウダーおよびドーパントを含み、液体中に希土類金属および遷移金属の陽イオンを含む分散物を供給する工程、
b)35重量%未満の含水量および少なくとも0.95g/cm3の密度を有する球状多孔性粒状粒子であるドープされたSiO2粒状体が形成されるまで、水分を除去しながら分散物を運動させることによる造粒工程、
c)SiO2粒状体を少なくとも温度1000℃に加熱することにより乾燥させ精製して、10ppm未満のOH含量を有するドープされた多孔性SiO2小粒を形成する工程、および
d)ドープされたSiO2小粒を還元雰囲気中で焼結または溶融させて、ドープされた石英ガラスの素材を形成する工程。
aa)負の圧力を加え、維持しながら、少なくとも1600℃の溶融温度へSiO2小粒を加熱する工程;
bb)少なくとも30分間の溶融期間の間、溶融温度と5〜15バールの範囲の超過圧力下に保持して、石英ガラス素材を形成する工程;
cc)石英ガラス素材を冷却する工程。
直径6mmのロッドを、0.7mol% Yb2O3および5.0mol% Al2O3をドープしたレーザー活性石英ガラスから作成する。
YbCl3×6H2O:87g
AlCl3×6H2O:387g。
直径10mm、長さ1mのロッドを1300ppm Nb2O3および0.5mol% Al2O3をドープしたレーザー活性石英ガラスから作成する。
Claims (15)
- レーザー活性石英ガラスのコンポーネント用の素材を生産するための、次の工程からなる方法であって:
a)少なくとも40重量%の固形分を有し、SiO2ナノパウダーおよびドーパントを含み、液体中に希土類金属および遷移金属の陽イオンを含む分散物を供給する工程、
b)35重量%未満の含水量および少なくとも0.95g/cm3の密度を有する球状多孔性粒状体粒子であるドープされたSiO2粒状体が形成されるまで、水分を除去しながら分散物を運動させることによる造粒工程、
c)SiO2粒状体を少なくとも温度1000℃に加熱することにより乾燥させ精製して、10ppm未満のOH含量を有するドープされた多孔性SiO2小粒を形成する工程、および
d)ドープされたSiO2小粒を還元雰囲気中で焼結または溶融させて、ドープされた石英ガラスの素材を形成する方法であって、次の工程からなるガス圧焼結工程を含むコンポーンネント用の素材を生産する方法において、
aa)負の圧力を加えおよび維持しながら、少なくとも1600℃の溶融温度へSiO2小粒を加熱する工程;
bb)少なくとも30分間の溶融期間の間、溶融温度と5〜15バールの範囲の超過圧力下に保持して、石英ガラス素材を形成する工程;
cc)超過圧力を維持しながら石英ガラス素材を冷却する工程;
からなることを特徴とする方法。 - 少なくとも50重量%の最初の固形分を分散物中に設定することを特徴とする請求項1に記載の方法。
- 工程b)によって得られるSiO2粒状体が、40m2/g〜70m2/gの範囲のBET表面積を有することを特徴とする請求項1または2に記載の方法。
- 工程b)によって得られるSiO2粒状体が少なくとも50m2/gのBET表面積を有することを特徴とする請求項3に記載の方法。
- 球状多孔性粒状体粒子が500μm未満の粒子サイズを有することを特徴とする請求項1〜4のいずれか1項に記載の方法。
- SiO2粒状体を、塩素を含む雰囲気下で乾燥および精製することを特徴とする請求項1〜5のいずれか1項に記載の方法。
- SiO2粒状体を少なくとも1050℃の温度で乾燥および精製することを特徴とする請求項1〜6のいずれか1項に記載の方法。
- 多孔性粒状体の乾燥と精製を酸素が含まれる雰囲気下で行なうことを特徴とする請求項1〜7のいずれか1項に記載の方法。
- 工程c)によって得られる多孔性SiO2小粒が1重量ppm未満のOH含量を有することを特徴とする請求項1〜8のいずれか1項に記載の方法。
- 工程c)によって得られる多孔性SiO2小粒が20m2/g未満のBET表面積を有することを特徴とする請求項1〜9のいずれか1項に記載の方法。
- 工程d)に先立って、SiO2小粒の密度を熱により高めることを特徴とする請求項1〜10のいずれか1項に記載の方法。
- 石英ガラス素材を、少なくとも1120℃の温度で少なくとも40時間の保持期間焼鈍することを特徴とする請求項1〜11のいずれか1項に記載の方法。
- 工程d)によるSiO2小粒を鋳型の中で溶融することを特徴とする請求項1〜12のいずれか1項に記載の方法。
- 工程d)によるSiO2素材を3次元的に均質化することを特徴とする請求項1〜13のいずれか1項に記載の方法。
- 放射状に不均質な屈折率分布を有するバルク体を様々な屈折率のSiO2小粒から形成すること、およびバルク体を焼結または溶融してSiO2素材を得ることを特徴とする請求項1〜14のいずれか1項に記載の方法。
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DE10357580 | 2003-12-08 | ||
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DE102004006017.7 | 2004-02-06 | ||
DE102004006017A DE102004006017B4 (de) | 2003-12-08 | 2004-02-06 | Verfahren zur Herstellung von laseraktivem Quarzglas und Verwendung desselben |
PCT/EP2004/013544 WO2005054139A1 (de) | 2003-12-08 | 2004-11-30 | Verfahren zur herstellung von laseraktivem quarzglas und verwendung desselben |
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DE102007045097B4 (de) * | 2007-09-20 | 2012-11-29 | Heraeus Quarzglas Gmbh & Co. Kg | Verfahren zur Herstellung von co-dotiertem Quarzglas |
FR2939246B1 (fr) * | 2008-12-02 | 2010-12-24 | Draka Comteq France | Fibre optique amplificatrice et procede de fabrication |
DE102012012524B3 (de) | 2012-06-26 | 2013-07-18 | Heraeus Quarzglas Gmbh & Co. Kg | Verfahren zur Herstellung eines dotierten SiO2-Schlickers sowie Verwendung des SiO2-Schlickers |
DE102013204815A1 (de) | 2013-03-19 | 2014-09-25 | Heraeus Quarzglas Gmbh & Co. Kg | Fluorierung von dotiertem Quarzglas |
EP3000790B2 (de) * | 2014-09-29 | 2023-07-26 | Heraeus Quarzglas GmbH & Co. KG | Verfahren für die Herstellung von Bauteilen aus synthetischem Quarzglas aus SiO2-Granulat |
KR20180095616A (ko) * | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 용융 가열로에서 이슬점 조절을 이용한 실리카 유리체의 제조 |
JP7044454B2 (ja) | 2015-12-18 | 2022-03-30 | 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 | 石英ガラス調製時の中間体としての炭素ドープ二酸化ケイ素造粒体の調製 |
EP3390304B1 (de) | 2015-12-18 | 2023-09-13 | Heraeus Quarzglas GmbH & Co. KG | Sprühgranulieren von siliziumdioxid bei der herstellung von quarzglas |
KR20180094087A (ko) | 2015-12-18 | 2018-08-22 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 실리카 과립으로부터 실리카 유리 제품의 제조 |
TW201731782A (zh) | 2015-12-18 | 2017-09-16 | 何瑞斯廓格拉斯公司 | 在多腔式爐中製備石英玻璃體 |
JP6881777B2 (ja) * | 2015-12-18 | 2021-06-02 | 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 | 合成石英ガラス粒の調製 |
KR20180095622A (ko) | 2015-12-18 | 2018-08-27 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | 내화성 금속으로 제조된 용융 도가니에서 실리카 유리 제품의 제조 |
CN108779014A (zh) * | 2015-12-18 | 2018-11-09 | 贺利氏石英玻璃有限两合公司 | 于立式烧结坩埚中制备石英玻璃体 |
JP6881776B2 (ja) | 2015-12-18 | 2021-06-02 | 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 | 不透明石英ガラス体の調製 |
US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
EP3390306A2 (de) * | 2015-12-18 | 2018-10-24 | Heraeus Quarzglas GmbH & Co. KG | Herstellung eines quarzglaskörpers in einem hängenden sintertiegel |
US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
WO2017103112A1 (de) * | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Herstellung eines quarzglaskörpers in einem hängenden blechtiegel |
EP3263533B1 (de) | 2016-06-28 | 2019-05-08 | Heraeus Quarzglas GmbH & Co. KG | Seltenerdmetall-dotiertes quarzglas sowie verfahren für dessen herstellung |
EP3381870B1 (de) | 2017-03-30 | 2020-12-23 | Heraeus Quarzglas GmbH & Co. KG | Verfahren zur herstellung eines bauteils aus seltenerdmetalldotiertem quarzglas |
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JPH08507490A (ja) * | 1993-03-05 | 1996-08-13 | アルカテル・セル・アクチェンゲゼルシャフト | 約1300nmの波長範囲の光ファイバ増幅器用の光導波体 |
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JPS6428244A (en) * | 1987-07-22 | 1989-01-30 | Seiko Epson Corp | Neodymium doped quartz glass and production thereof |
DE19729505A1 (de) * | 1997-07-10 | 1999-01-14 | Heraeus Quarzglas | Verfahren zur Herstellung von Si0¶2¶-Granulat |
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JPH08507490A (ja) * | 1993-03-05 | 1996-08-13 | アルカテル・セル・アクチェンゲゼルシャフト | 約1300nmの波長範囲の光ファイバ増幅器用の光導波体 |
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