Rare earth-doped oxyfluoride germanate microcrystalline glass and preparation method thereof

A technology of oxygermanate fluoride and rare earth doping, applied to rare earth-doped oxygermanate fluoride glass-ceramics and its preparation, rare-earth-doped glass-ceramics containing fluoride nanocrystal up-conversion luminescent material and its preparation In this field, it can solve the problems that the research has not yet been reported, and achieve the effects of good luminous performance, high environmental protection and safety, and improved luminous intensity.

Inactive Publication Date: 2015-07-01
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the precipitation of alkaline earth metal fluoride sodium salt nanocrystalline phases in rare earth-doped oxygermanate glasses has not been reported yet.

Method used

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  • Rare earth-doped oxyfluoride germanate microcrystalline glass and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] By composition 39GeO 2 20BaF 2 10ZnO 10AlF 3 10Na 2 O·10NaF·0.2ErF 3 0.3TmF 3 0.5YbF 3 (mol%) Weigh the GeO required for a total mass of 10 grams 2 、BaF 2 , ZnO, AlF 3 、Na 2 CO 3 , NaF, ErF 3 , TmF 3 and YbF 3 The powder raw materials are mixed thoroughly and placed in a crucible with a cover and placed at 1450°C for 60 minutes to melt, and then the glass melt is quickly cast on a stainless steel template that has been preheated to 400°C. ℃ for 4 h, and naturally cooled down to room temperature to obtain glass containing rare earth ions, and the prepared glass was cut, ground and polished; Heat treatment at 50°C for 60 min, and naturally cool to room temperature to obtain NaBaAlF 6 Nanocrystalline rare earth doped glass-ceramics.

Embodiment 2

[0018] By composition 43.5GeO 2 25BaF 2 5ZnO 5AlF 3 1Na 2 O 20NaF 0.5ErF 3 (mol%) Weigh the GeO required for a total mass of 10 grams 2 、BaF 2 , ZnO, AlF 3 、Na 2 CO 3 , NaF and ErF 3 The powder raw materials are mixed thoroughly and put into a crucible with a cover and placed at 1350°C for 45 minutes to melt, and then the glass melt is quickly cast on a stainless steel template that has been preheated to 300°C. ℃ for 8 h, and naturally cooled to room temperature to obtain a glass containing rare earth ions, and the glass was cut, ground and polished; the glass was heat-treated at the second crystallization peak temperature 15min, naturally cooled to room temperature, that is containing NaBaAlF 6 Nanocrystalline rare earth doped glass-ceramics.

[0019] Er in this embodiment 2 3+ Doped fluorogermanate glass and containing NaBaAlF 6 The upconversion luminescence spectrum of nanocrystalline oxygermanate glass-ceramics such as figure 1 Shown; As can be seen from the ...

Embodiment 3

[0021] By composition 55GeO 2 ·10BaF 2 15ZnO 15AlF 3 5Na 2 O·5NaF·0.2ErF 3 0.8TbF 3 ·4YbF 3 (mol%) Weigh the GeO required for a total mass of 10 grams 2 、BaF 2 , ZnO, AlF 3 、Na 2 CO 3 , NaF, ErF 3 , TbF 3 and YbF 3 The powder raw materials are mixed thoroughly and placed in a crucible with a cover and melted at 1400°C for 30 minutes, then the molten glass is quickly cast onto a stainless steel template that has been preheated to 350°C, The crystal peak temperature was kept at 30°C for 5 h, and the temperature was naturally cooled to room temperature to obtain a glass containing rare earth ions, which was cut, ground and polished; heat treatment at 30°C for 30 min, and naturally cooled to room temperature to obtain NaBaAlF 6 Nanocrystalline rare earth doped glass-ceramics.

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Abstract

The invention discloses rare earth-doped oxyfluoride germanate microcrystalline glass and a preparation method thereof, and belongs to the technical field of luminescent materials. The microcrystalline glass comprises the following components in percentage by mole: 39-55% of GeO2, 5-15% of ZnO, 5-15% of AlF3, 10-25% of BaF2, 1-10% of Na2O, 1-20% of NaF and 0.5-5% of RF2 (R is rare earth elements). The preparation method comprises the following steps: firstly preparing oxyfluoride germanate glass by using a melt quenching method; and then, carrying out micro-crystallization on matrix glass by virtue of a thermal treatment process to obtain transparent oxyfluoride germanate microcrystalline glass, wherein the prepared oxyfluoride germanate microcrystalline glass has good transmission of light in a range from near-infrared rays to visible light, and the up-conversion luminescence of rare earth ions is remarkably enhanced. The prepared rare earth-doped oxyfluoride germanate microcrystalline glass containing NaBaAlF6 nano-crystals is simple in preparation method, high in environmental-friendly safety and relatively low in production cost.

Description

technical field [0001] The invention relates to a rare earth-doped oxygermanate fluoride glass-ceramic and a preparation method thereof, in particular to a rare-earth-doped fluoride-containing nanocrystal glass-ceramic up-conversion luminescent material and a preparation method thereof, belonging to the luminescent material technology field. Background technique [0002] Rare earth-doped frequency conversion luminescence technology has great potential application value in the fields of solid-state laser, data storage, general lighting, three-dimensional display, microscopic imaging, sensing technology, solar cells, anti-counterfeiting technology and military confrontation. Therefore, domestic and foreign Rare earth doped luminescent materials have been extensively studied. [0003] The research results show that after heat treatment of rare earth-doped matrix glass, after the crystal phase appears inside the glass, rare earth ions will be preferentially enriched in the prec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16
Inventor 胡曰博高源邱建备
Owner KUNMING UNIV OF SCI & TECH
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