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Fluoride/oxyfluoride fluorescent glass ceramic, preparation method and application thereof

A technology of oxyfluoride and fluorescent glass, which is applied in glass manufacturing equipment, glass molding, manufacturing tools, etc., can solve the problems that the rare earth ion active luminescent center cannot be firm, it is difficult to meet the needs of practical applications, and the fluorescence emission intensity is reduced. Avoiding non-radiative transitions, high photoconversion efficiency and luminous performance, and short holding time

Inactive Publication Date: 2020-09-11
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the traditional preparation process, the rare earth ion active luminescent center of fluoride nanocrystalline composite fluorescent glass ceramics cannot firmly and effectively occupy the fluoride lattice sites, and is easy to form defects, resulting in a decrease in fluorescence emission intensity and a shortened fluorescence lifetime. , it is difficult to meet the practical application requirements

Method used

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  • Fluoride/oxyfluoride fluorescent glass ceramic, preparation method and application thereof
  • Fluoride/oxyfluoride fluorescent glass ceramic, preparation method and application thereof
  • Fluoride/oxyfluoride fluorescent glass ceramic, preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0023] La(NO 3 ) 3 ·6H 2 O and Eu(NO 3 ) 3 ·XH 2 O was accurately weighed at a molar ratio of (La:Eu=95:5), dissolved in deionized water at room temperature, placed in an oil bath at 65°C with magnetic stirring, and the stirring rate was set at 500rpm; excess NH 4 F dissolved in a small amount of deionized water, the NH 4 Solution F is slowly dripped into the above mixed solution, and a white precipitate can be observed, then add nitric acid or hydrochloric acid solution to adjust the pH value to 2-3, continue stirring and heating for 90 minutes; further perform hydrothermal treatment on the mixed solution, and mix the precipitated Move the solution into a 100ml hydrothermal kettle and react at 180°C for 18 hours. After the reaction, take out the hydrothermal kettle and cool it to room temperature naturally, pour off the supernatant, and wash the precipitate with deionized water and absolute ethanol respectively. , centrifuged three times, and the obtained white precipit...

Embodiment 2

[0026] Y(NO 3 ) 3 ·6H 2 O and Eu(NO 3 ) 3 ·XH 2 O was accurately weighed at a molar ratio of (Y:Eu=95:5), dissolved in deionized water at room temperature, placed in an oil bath at 65°C with magnetic stirring, and the stirring rate was set at 500rpm; excess NH 4 F dissolved in a small amount of deionized water, the NH 4 The F solution is slowly dropped into the above mixed solution, and a white precipitate can be observed, then a certain amount of nitric acid or hydrochloric acid solution is added to adjust the pH value to 2-3, and the stirring and heating are continued for 90 minutes; the mixed solution is further hydrothermally treated, and the The precipitated mixed solution was transferred to a 100ml hydrothermal kettle, and reacted at 180°C for 18 hours. After the reaction, the hydrothermal kettle was taken out and cooled to room temperature naturally, and the supernatant was poured out, and deionized water and absolute ethanol were used to The precipitate was washe...

Embodiment 3

[0029] The dried YF after centrifugation of embodiment 2 3 :Eu 3+ The nanocrystals are fully ground in a mortar, and then the powder is put into a muffle furnace and heated to 300°C, 400°C, 500°C, 600°C, 700°C, 800°C, and 900°C at a heating rate of 2°C / min. , after three hours of heat preservation, it was naturally cooled to room temperature to obtain YOF:Eu 3+ Nanocrystalline.

[0030] Using MCM-41 mesoporous silicon-based powder and YOF:Eu 3+ The luminous nano crystal powder is used as the starting material. Raw materials were mixed in different weight ratios (YOF:Eu 3+ Luminescent nanocrystalline powder: 1wt%, 2wt%, 3wt%, 4wt%, 5wt%) are uniformly ground and mixed, and then moved into a graphite mold with an inner diameter of 10mm. By spark plasma sintering, the mixed powder was sintered under a uniaxial pressure of 100 MPa for about 10 min according to specific sintering parameters. The detailed sintering parameters are as follows: After heating at 600 °C for 3 min, ...

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Abstract

The invention relates to a fluoride / oxyfluoride nanocrystalline composite fluorescent glass ceramic material, a preparation method and application thereof. The fluorescent glass ceramic is composed ofa mesoporous silicon-based material and fluoride / oxyfluoride fluorescent nanocrystals. According to the invention, the luminescent property of the fluoride / oxyfluoride nanocrystal is effectively retained, and meanwhile, the fluoride / oxyfluoride nanocrystalline composite fluorescent glass ceramic has the characteristics of simple preparation process, good thermal stability and long fluorescence lifetime, and has great application potential in the aspects of color displays, sensors, lasers, optical fiber amplifiers and the like.

Description

technical field [0001] The invention belongs to the field of fluorescent glass ceramic materials, in particular to a fluoride / oxyfluoride fluorescent glass ceramic and its preparation method and application. Background technique [0002] Fluorescent glass-ceramic is a new type of luminescent material, also known as glass-ceramics. It not only has an amorphous phase matrix, but also coexists with crystal phases. Compared with traditional glass materials, the composite material obtained by heat treatment not only has the characteristics of glass, such as high hardness, high mechanical strength, good chemical stability, and durability. It has excellent abrasiveness, stable dielectric constant, and has the advantages of high thermal conductivity of ceramic phase crystals and can be doped with luminescent ions. Therefore, it can be used not only as a structural material, but also as a functional material, and has gradually been widely used in fields such as energy, chemical indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C14/00C03C10/00C03C4/12C03B19/06
CPCC03B19/06C03C4/12C03C10/00C03C14/006C03C2214/20C03C2214/30
Inventor 王连军王建成黄平周蓓莹江莞
Owner DONGHUA UNIV
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