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Preparation method of fluorine-containing low refractive index yb3+ doped quartz glass

A quartz glass, low refractive index technology, applied in the field of rare earth doped quartz glass, to achieve the effect of high uniformity

Active Publication Date: 2016-06-08
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reported fluorine-doped quartz glass with low refractive index is limited to quartz cladding materials, and there is no report on the co-doping of fluorine and rare earth ions with low refractive index quartz glass.

Method used

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  • Preparation method of fluorine-containing low refractive index yb3+ doped quartz glass
  • Preparation method of fluorine-containing low refractive index yb3+ doped quartz glass
  • Preparation method of fluorine-containing low refractive index yb3+ doped quartz glass

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Experimental program
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Effect test

Embodiment 1

[0039] The basic composition of the glass is 0.2Yb 2 o 3 -1.5Al 2 o 3 -98.3 SiO 2 (mol%), F was introduced with F / Si=5wt% when preparing the sol. Under room temperature and magnetic stirring, according to Si(OCH 3 ) 4 :CH 3 OH:H 2 The molar ratio of O=1:4:2, using ammonia water as a catalyst, prepares a transparent sol liquid. Then according to the designed glass formula, add AlCl 3 ·6H 2 O and YbCl 3 ·6H 2 O and NH 4 F, Stir at room temperature for 1 hour to form a doped sol, and let it stand in a closed container until it gels; place the gel in a tube furnace at 600°C in an oxygen atmosphere for 12 hours to remove residual carbon and hydroxyl groups, Obtain silicon oxide powder; use ball milling equipment to ball mill the silicon oxide powder, and use a 150-mesh polytetrafluoro sieve to screen the powder with a particle size below 100 microns; place the sieved powder in a vacuum of 10 -3 Melt at 1650°C for 8 hours in a Pa high temperature furnace. The refracti...

Embodiment 2

[0041] The basic composition of the glass is 0.1Yb 2 o 3 -1Al 2 o 3 -98.9SiO2 2 (mol%), F was introduced with F / Si=5wt% when preparing the sol. Under room temperature and magnetic stirring, according to Si(OC 2 h 5 ) 4 :C 2 h 5 OH:H 2 The molar ratio of O=1:4:2, using hydrochloric acid as a catalyst, prepares a transparent sol liquid. Then according to the designed glass formula, add AlCl 3 ·6H 2 O and YbCl 3 ·6H 2 O and (NH 4 ) 2 SiF 6 , stirred at room temperature for 10 hours to form a doped sol, which was left to stand in a closed container until gelation; the gel was placed in a tube furnace and kept at 1000°C for 8 hours to remove residual carbon and hydroxyl groups, and obtained Silica powder; use ball milling equipment to carry out ball milling to the described silica powder, and use a 150-mesh polytetrafluoro sieve to screen out the powder with a particle size below 100 microns; place the sieved powder in a vacuum of 10 -3 Melt at 1750°C for 3 hours ...

Embodiment 3

[0043] The basic composition of the glass is 0.1Yb 2 o 3 -1Al 2 o 3 -98.9SiO2 2 (mol%), F was introduced with F / Si=10wt% when preparing the sol. Under room temperature and magnetic stirring, according to Si(OC 2 h 5 ) 4 :C 2 h 5 OH:H 2 The molar ratio of O=1:20:10, using hydrochloric acid as a catalyst, prepares a transparent sol liquid. Then according to the designed glass formula, add AlCl 3 ·6H 2 O and YbCl 3 ·6H 2 O and NH 4 F, Stir at room temperature for 2 hours to form a doped sol, and let it stand in a closed container until it gels; place the gel in a tube furnace under an oxygen atmosphere and 1000°C for 8 hours to remove residual carbon and hydroxyl groups, Obtain silicon oxide powder; use ball milling equipment to ball mill the silicon oxide powder, and use a 150-mesh polytetrafluoro sieve to screen the powder with a particle size below 100 microns; place the sieved powder in a vacuum of 10 -3 Melt at 1750°C for 3 hours in a Pa high temperature furn...

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Abstract

The invention relates to a preparation method for fluorine-containing low-refractivity Yb<3+>-doped quartz glass. The method comprises the steps: starting from a solution, preparing evenly doped silicon oxide powder by using a sol-gel method; and carrying out decarbonization and dehydroxylation treatment on the powder, and finally sintering into glass. By applying the method, F<-> can be effectively introduced, and the rare earth-doped quartz glass with high uniformity, low hydroxyl content and the refractivity almost identical to that of the pure quartz glass can be obtained. The method can be applied to preparation of a high-brightness large-mode-field quartz optical fiber mandril.

Description

technical field [0001] The invention relates to rare earth doped quartz glass, especially a kind of fluorine-containing low refractive index Yb 3+ Preparation method of doped quartz glass. Background technique [0002] Rare earth doped quartz glass and optical fiber have been used in optical fiber communication, industrial processing and laser medical treatment and other fields. In order to meet the needs of industrial processing applications, it is necessary to increase the output power of lasers. Large-mode-field fibers have attracted extensive attention because they can solve the nonlinear effects and laser damage faced by high-power fiber lasers. Many research institutions at home and abroad, such as the German Jena Photonic Technology Institute in conjunction with Heraeus and the Danish PhotonicCrystalFiber company, Tsinghua University, Shanghai Institute of Optics and Fine Mechanics, etc. are committed to the research of ytterbium-doped large-mode-field fibers. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C3/06
Inventor 许文彬于春雷胡丽丽陈丹平冯素雅王世凯王孟周秦岭
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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