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
- doped
- glass cladding
- melting furnace
- continuous melting
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
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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
- C03B37/02—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
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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| CN201911234456.3A CN110903034A (en) | 2019-12-05 | 2019-12-05 | Preparation method of quartz glass cladding material for optical fiber and continuous melting furnace device |
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Citations (11)
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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 |
| 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 |
|---|---|---|---|---|
| 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 |
| US20130294737A1 (en) * | 2011-01-19 | 2013-11-07 | Fiber Optics Research Center Of The Russian Academy Of Sciences (Forc Ras) | Multicore optical fiber (variants) |
| CN103319071A (en) * | 2012-03-20 | 2013-09-25 | 东海县圣达石英制品有限公司 | Quart continuous melting furnace |
| 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 |
| 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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