Fluorine-oxygen microcrystalline glass based on rare earth ion in-situ crystallization as well as preparation method and application of fluorine-oxygen microcrystalline glass

A rare earth ion, glass-ceramic technology, applied in glass manufacturing equipment, glass furnace equipment, manufacturing tools, etc., can solve the problems of optical scattering, high crystallinity, small luminous enhancement, etc., to achieve strong adaptability and applicability , Simple process, controllable effect of crystallization

Active Publication Date: 2020-12-01
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the valence and radius mismatch between different ions, the number of rare earth ions entering the crystal is often small, and most of the rare earth ions remain in the glass phase, and the luminescence enhancement is not large.
In addition, in these glass-ceramics, a large number of glass components participate in crystallization, and the degree of crystallization is high, resulting in severe optical scattering
As a result, the luminescence enhancement caused by the precipitation of fluoride crystals is not enough to offset the loss caused by crystal scattering, and it is difficult for glass ceramics to be practically applied in optical gain devices such as visible fiber lasers.

Method used

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  • Fluorine-oxygen microcrystalline glass based on rare earth ion in-situ crystallization as well as preparation method and application of fluorine-oxygen microcrystalline glass
  • Fluorine-oxygen microcrystalline glass based on rare earth ion in-situ crystallization as well as preparation method and application of fluorine-oxygen microcrystalline glass
  • Fluorine-oxygen microcrystalline glass based on rare earth ion in-situ crystallization as well as preparation method and application of fluorine-oxygen microcrystalline glass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Glass-ceramics adopts the following formula: including matrix glass components and YbF 3 , where YbF 3 Incorporated in the form of external doping, the molar percentage is 1.0% of the matrix glass component;

[0031] The molar percentages of each component of the matrix glass component are:

[0032] GeO 2 :70%

[0033] MnF 2 :15%

[0034] NaF: 15%

[0035] (2) Weigh 50 g of high-purity powdery raw materials according to the composition formula, and fully mix them uniformly in a ball mill jar.

[0036] (3) Pour the uniformly mixed material into a 100ml quartz crucible, add a lid, put it into a high-temperature electric furnace, slowly raise the temperature to 1350°C and keep it warm for 30min, then put it into a stirring rod, stir at a slow speed (10 rpm) for 30min, Keep warm for another 1 hour, cool down to 1250°C and discharge, and shape into block glass samples.

[0037] (4) Put the glass into a muffle furnace, raise the temperature to 520° C. for precise ...

Embodiment 2

[0041] (1) Glass-ceramics adopts the following formula: including matrix glass components, YbF 3 and TbF 3 , where YbF 3 and TbF 3 Incorporated in the form of external doping, the molar percentages are 1.0% and 0.5% of the matrix glass component;

[0042] The molar percentages of each component of the matrix glass component are:

[0043]B 2 o 3 :70%

[0044] MgF 2 :15%

[0045] CsF: 15%

[0046] (2) Weigh 50 g of high-purity powdery raw materials according to the composition formula, and fully mix them uniformly in a ball mill jar.

[0047] (3) Pour the uniformly mixed material into a 100ml quartz crucible, add a lid, put it into a high-temperature electric furnace, slowly raise the temperature to 950°C and keep it warm for 30min, then put it into a stirring rod, stir at a slow speed (10 rpm) for 30min, Then keep it warm for 1 hour, cool down to 900°C and discharge, and shape it into a rectangular glass sample.

[0048] (4) Put the glass into a muffle furnace, raise...

Embodiment 3

[0052] (1) Glass-ceramics adopts the following formula: including matrix glass components and TmF 3 , where TmF 3 Incorporated in the form of external doping, the molar percentage is 1.0% of the matrix glass component;

[0053] The molar percentages of each component of the matrix glass component are:

[0054] TeO 2 :60%

[0055] ZnF 2 :20%

[0056] NaF: 20%

[0057] (2) Weigh 50 g of high-purity powdery raw materials according to the composition formula, and fully mix them uniformly in a ball mill jar.

[0058] (3) Pour the uniformly mixed material into a 100ml corundum crucible, add a lid, put it into a high-temperature electric furnace, slowly raise the temperature to 750°C and keep it for 30 minutes, then put it into a stirring rod, and stir at a slow speed (10 rpm) for 30 minutes, Keep warm for another 1 hour, cool down to 700°C and discharge, and shape into a rectangular strip-shaped glass sample.

[0059] (4) Put the glass into a muffle furnace, raise the temper...

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PUM

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Abstract

The invention belongs to the technical field of photoelectric materials, and particularly discloses oxyfluoride microcrystalline glass based on rare earth ion in-situ crystallization as well as a preparation method and application of the oxyfluoride microcrystalline glass. The method specifically comprises the following steps: fully and uniformly mixing a matrix glass component and rare earth ionfluoride in a ball-milling tank, then melting and uniformly stirring, carrying out heat preservation, cooling to 50-100 DEG C, discharging, molding into blocky glass, heating to a glass transition temperature, carrying out heat treatment on the blocky glass, and separating out fluoride nanocrystals containing rare earth ions from the glass to prepare a transparent microcrystalline glass sample. The obtained glass has high luminous efficiency and high transmittance, and has a great application prospect in the aspect of preparation of high-efficiency optical gain materials.

Description

technical field [0001] The invention belongs to the technical field of optoelectronic materials, and in particular relates to an oxyfluoride glass-ceramic based on in-situ crystallization of rare earth ions and its preparation method and application. Background technique [0002] The current development of visible fiber lasers is relatively slow, mainly due to the contradiction between the luminous efficiency and thermodynamic stability of fiber glass materials. In the past few decades, most of the research on visible fiber lasers has been based on fluoride fiber materials. Although fluoride glass has high luminous efficiency, its thermodynamic stability is low and its resistance to laser damage threshold is low, which restricts the further improvement of laser power. However, some oxide glass materials have good stability, but their phonon energy is relatively high, resulting in low visible luminous efficiency. The emergence of oxyfluoride glass-ceramic perfectly solves t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16C03C4/12C03B5/16C03B32/02C03C13/04
CPCC03C10/16C03C4/12C03B5/16C03B32/02C03C13/04
Inventor 方再金李剑锋关柏鸥龙益郑书培
Owner JINAN UNIVERSITY
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