CN110903034A - Preparation method of quartz glass cladding material for optical fiber and continuous melting furnace device - Google Patents
Preparation method of quartz glass cladding material for optical fiber and continuous melting furnace device Download PDFInfo
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- CN110903034A CN110903034A CN201911234456.3A CN201911234456A CN110903034A CN 110903034 A CN110903034 A CN 110903034A CN 201911234456 A CN201911234456 A CN 201911234456A CN 110903034 A CN110903034 A CN 110903034A
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- cladding material
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- glass cladding
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- continuous melting
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002844 melting Methods 0.000 title claims abstract description 33
- 230000008018 melting Effects 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000005253 cladding Methods 0.000 title claims abstract description 25
- 239000013307 optical fiber Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000006004 Quartz sand Substances 0.000 claims abstract description 16
- 239000010453 quartz Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 150000002500 ions Chemical class 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229910000421 cerium(III) oxide Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000013461 design Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052721 tungsten Inorganic materials 0.000 abstract description 6
- 239000010937 tungsten Substances 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000010309 melting process Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 2
- 229910000420 cerium oxide Inorganic materials 0.000 abstract 1
- 238000009826 distribution Methods 0.000 abstract 1
- 239000007791 liquid phase Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 abstract 1
- 238000009827 uniform distribution Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 239000011162 core material Substances 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Classifications
-
- 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
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
-
- 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
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/029—Furnaces therefor
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
The invention relates to a preparation method of quartz glass cladding material for optical fiber and a continuous melting furnace device, which uses high-purity quartz Sand (SiO) with the grain diameter of 0.1-0.25mm2) Adding 0.03-1wt% of aluminum oxide (Al) into the mixture by liquid phase doping method2O3) And cerium oxide (Ce)2O3) Uniformly stirring precursor solution containing doped ions and high-purity quartz sand, calcining for 2-4 h at 1100 ℃ in an oxidizing atmosphere, and screening and mixing to obtain doped SiO2Powder; will be doped with SiO2And putting the powder into a continuous melting furnace, and melting and drawing the doped quartz glass cladding material by adopting a continuous melting process. The invention improves the structure of the continuous melting furnace, increases the size of the tungsten crucible of the hearth, increases the number of heating electrodes, optimizes the distribution, is beneficial to increasing the quartz melt, has longer residence time in the furnace, and is beneficial to uniform distribution of doped ions, discharge of air bubbles and air lines and the like. The method adoptsThe doped quartz glass cladding material prepared by the two-step process has the characteristics of uniform doping, high doping concentration, accurate and controllable inner and outer diameter sizes of the quartz glass cladding material, high apparent quality and the like.
Description
Technical Field
The invention relates to a preparation method of a quartz glass material for optical fibers, belonging to the technical field of quartz glass material production.
Background
In recent years, doped silica fibers have been developed in a crossing manner based on the urgent need of high-power fiber lasers in the fields of Inertial Confinement Fusion (ICF), heavy industrial laser processing, military, medical treatment, and the like. At present, the doped quartz fiber laser is widely applied to high-end processing industries such as automobile manufacturing, laser processing and the like.
Compared with the traditional cladding quartz fiber (the fiber core is less than or equal to 20 mu m), the fiber core size of the large mode field doped quartz fiber is increased (40-100 mu m), so that the light beam quality (laser brightness) is poor. Currently, increasing the quality of the light beam by increasing the refractive index of the cladding quartz material has become a mainstream approach. Therefore, the doped quartz cladding material becomes a key core material for realizing high power and high brightness of the large mode field optical fiber, and the unprecedented importance of foreign research institutions, such as the Germany Jena university, the Heraeus company, the American NKT company and the like is brought. In 2014, Jena university prepared Al-doped silica glass as a cladding material of ytterbium-doped large mode field optical fiber, and realized refractive index matching with NA as low as 0.03, but doping uniformity still needs to be further improved. Various fiber laser companies in China have huge demands on high-power, high-brightness and large-mode-field quartz fibers, but almost no supply channel exists.
The invention provides a preparation method and a device of a quartz glass cladding material for an optical fiber, which can prepare the quartz glass cladding material matched with a large-mode-field doped quartz optical fiber.
Disclosure of Invention
The invention aims to provide a preparation method of a silica glass cladding material for an optical fiber, which is used for preparing a doped silica glass cladding material for the optical fiber.
The invention also aims to provide a continuous melting furnace for realizing the method.
The invention prepares the doped quartz glass cladding material for the optical fiber, and the preparation method is realized by the following steps:
(1) the design formula is as follows: high-purity quartz Sand (SiO) with particle size of 0.1-0.25mm2) As raw material, 0.03-1wt% of Al2O3And Ce2O3;
(2) Accurately weighing Al according to the molar ratio2O3、Ce2O3Dissolving the precursor solution in 10% hydrochloric acid to obtain a precursor solution containing doped ions, and uniformly stirring the precursor solution and high-purity quartz sand;
(3) calcining for 2-4 h at 1100 ℃ in an oxidizing atmosphere, and screening the mixed material to obtain doped SiO2Powder;
(4) sieving and selecting doped SiO with proper granularity2And putting the powder into a continuous melting furnace, melting for more than or equal to 10 hours at the temperature of more than or equal to 2200 ℃, and melting and drawing the doped quartz glass cladding material.
A continuous melting furnace for realizing the method mainly comprises a molybdenum mandrel, a feeding pipe, a small furnace cover, a large furnace cover, a copper electrode, a tungsten crucible, a heat preservation layer, a forming opening, a furnace mouth mask and the like. The copper electrodes are 8 groups and 16 electrodes, so that the temperature rise rate of the continuous melting furnace is high, and the transverse temperature field in the furnace is uniform. The diameter of the tungsten crucible is 560mm, and the volume of the hearth of the continuous melting furnace is increased. The heat preservation layer is composed of zirconia sand, quartz sand and a graphite blanket, and the heat preservation effect of the continuous melting furnace body is improved.
During the melting process, the melting of the quartz sand particles, the removal of bubbles, and the diffusion of the components are all viscosity dependent. The high-purity quartz sand has high melting point, reduces the melting point of the quartz sand along with the addition of dopants, promotes the melting of the quartz sand, further improves the temperature, reduces the viscosity of quartz melt, is favorable for discharging bubbles and reducing the apparent defects of quartz glass, is favorable for the diffusion of doping ions, and is more uniformly distributed.
The structure of the continuous melting furnace has important influence on the quality of the quartz product. The number of the heating copper electrodes is increased to 8 groups of 16, the arrangement is more reasonable, the temperature rise rate of the continuous melting furnace is high, and the transverse temperature field in the furnace is more uniform. The size of the continuous melting furnace is increased, the quartz melt in the crucible is increased, and the quartz melt has longer residence time in the furnace, so that the melt level is relatively stable, doped ions have sufficient time to diffuse and disperse uniformly, impurities, bubbles and the like are discharged favorably, the uniform doping of quartz glass is ensured, and apparent defects are reduced.
The method adopts a two-step process to prepare the doped quartz glass cladding material, and has the characteristics of uniform doping, high doping concentration, accurate and controllable inner and outer diameter sizes of the quartz glass cladding material, high apparent quality and the like.
Drawings
Fig. 1 is a continuous melting furnace of the present invention, in which: 1 molybdenum mandrel, 2 feed pipes, 3 small furnace covers, 4 large furnace covers, 5 copper electrodes, 6 tungsten crucibles, 7 heat preservation layers, 8 forming ports and 9 furnace mask.
Detailed Description
The present invention will be further described with reference to specific examples, but the embodiments of the present invention are not limited thereto.
A continuous melting furnace is shown in figure 1, and mainly comprises a molybdenum mandrel 1, a charging tube 2, a small furnace cover 3, a large furnace cover 4, a copper electrode 5, a tungsten crucible 6, a heat-insulating layer 7, a forming opening 8 and a furnace opening cover 9. And 5 copper electrodes have 8 groups of 16 electrodes, so that the temperature rise rate of the continuous melting furnace is high, and the transverse temperature field in the furnace is uniform. The diameter of the 6 tungsten crucible is 560mm, and the volume of the hearth of the continuous melting furnace is increased. 7 the heat preservation layer is composed of zirconia sand, quartz sand and graphite blankets, thus improving the heat preservation effect of the continuous melting furnace body.
The preparation method of the silica glass cladding material for the optical fiber comprises the following implementation steps:
(1) the design formula is as follows: high-purity quartz Sand (SiO) with particle size of 0.1-0.25mm2) As raw material, 0.8wt% of Al is doped2O3And Ce2O3;
(2) Accurately weighing Al and Ce according to the molar ratio of 2, dissolving in 10% hydrochloric acid to obtain a precursor solution containing doped ions, and uniformly stirring with high-purity quartz sand;
(3) calcining for 2 h at 1100 ℃ in an oxidizing atmosphere, screening and mixing the materials to obtain doped SiO2Powder;
(4) sieving and selecting doped SiO with proper granularity2Powder is put into a continuous melting furnace, and the temperature in the furnace is controlledThe temperature is 2200 ℃, the smelting time is 11h, and the doped quartz glass cladding material is melted and drawn.
Claims (4)
1. A method for preparing quartz glass cladding material for optical fiber and a continuous melting furnace device sequentially comprise the following steps:
(1) the design formula is as follows: high-purity quartz Sand (SiO) with particle size of 0.1-0.25mm2) As raw material, 0.03-1wt% of Al2O3And Ce2O3;
(2) Accurately weighing Al according to the molar ratio2O3、Ce2O3Dissolving the precursor solution in 10% hydrochloric acid to obtain a precursor solution containing doped ions, and uniformly stirring the precursor solution and high-purity quartz sand;
(3) calcining for 2-4 h at 1100 ℃ in an oxidizing atmosphere, and screening the mixed material to obtain doped SiO2Powder;
(4) sieving and selecting doped SiO with proper granularity2And putting the powder into a continuous melting furnace, melting for more than or equal to 10 hours at the temperature of more than or equal to 2200 ℃, and melting and drawing the doped quartz cladding material.
2. The method for producing a silica glass cladding material for optical fiber according to claim 1, wherein: the used basic raw material is high-purity quartz Sand (SiO) with the grain diameter of 0.1-0.25mm2) Al with a doping amount of 0.03-1wt%2O3And Ce2O3The molar ratio of Al to Ce is 1.5-3.5.
3. The method for producing a silica glass cladding material for optical fiber according to claim 1, wherein: calcining the uniformly stirred high-purity quartz sand for 2-4 h at 1100 ℃ in an oxidizing atmosphere.
4. The method for producing a silica glass cladding material for optical fiber according to claim 1, wherein: the temperature in the continuous melting furnace is more than or equal to 2200 ℃, and the melting time is more than or equal to 10 h.
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CN101000390A (en) * | 2006-01-12 | 2007-07-18 | 上海大学 | High-property anti-radiation quartz optical fibre and manufacturing process of combined method |
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CN101234844A (en) * | 2008-02-27 | 2008-08-06 | 徐胜利 | Method for producing heavy caliber quartz glass pipe for IC industry by continuous melting process |
CN101328014A (en) * | 2008-07-28 | 2008-12-24 | 湖北菲利华石英玻璃股份有限公司 | Manufacturing method of doping quartz glass fibre |
CN102875007A (en) * | 2012-09-19 | 2013-01-16 | 江苏太平洋石英股份有限公司 | Continuous melting furnace for producing quartz glass bar and manufacture technology |
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US20130294737A1 (en) * | 2011-01-19 | 2013-11-07 | Fiber Optics Research Center Of The Russian Academy Of Sciences (Forc Ras) | Multicore optical fiber (variants) |
CN203360262U (en) * | 2013-06-28 | 2013-12-25 | 江苏丰源光伏科技有限公司 | Continuous melting furnace for producing elliptical quartz tubes |
CN103880278A (en) * | 2014-02-25 | 2014-06-25 | 连云港市弘扬石英制品有限公司 | Preparation method of optical fiber covering quartz capillary perform and continuous melting furnace equipment |
CN105439426A (en) * | 2015-12-04 | 2016-03-30 | 太仓市建兴石英玻璃厂 | Making method for doping type quartz glass tube |
CN106746637A (en) * | 2017-02-20 | 2017-05-31 | 单祥发 | A kind of production method of low oxyhydroxide and rear-earth-doped quartz ampoule |
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2019
- 2019-12-05 CN CN201911234456.3A patent/CN110903034A/en active Pending
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101000390A (en) * | 2006-01-12 | 2007-07-18 | 上海大学 | High-property anti-radiation quartz optical fibre and manufacturing process of combined method |
CN200992517Y (en) * | 2007-01-19 | 2007-12-19 | 王绪东 | Continuous melting furnace for drawing colored quartz glass pipe |
CN101234844A (en) * | 2008-02-27 | 2008-08-06 | 徐胜利 | Method for producing heavy caliber quartz glass pipe for IC industry by continuous melting process |
CN101328014A (en) * | 2008-07-28 | 2008-12-24 | 湖北菲利华石英玻璃股份有限公司 | Manufacturing method of doping quartz glass fibre |
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CN203360262U (en) * | 2013-06-28 | 2013-12-25 | 江苏丰源光伏科技有限公司 | Continuous melting furnace for producing elliptical quartz tubes |
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