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Preparation method of rare earth ion doped tungsten oxygen fluoride silicate up-converted luminescent glass

A technology of fluorooxytungsten silicate and luminescent glass is applied in the field of preparing rare earth ion-doped fluorooxytungsten silicate up-conversion luminescent glass, and achieves the effects of simple preparation method, low cost of raw materials and simple equipment

Inactive Publication Date: 2012-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-temperature melting annealing method is widely used because of simple equipment, simple reaction parameters and easy control of the reaction process. However, other methods are usually used to prepare up-conversion luminescent glasses, which require complex reaction processes to obtain

Method used

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  • Preparation method of rare earth ion doped tungsten oxygen fluoride silicate up-converted luminescent glass
  • Preparation method of rare earth ion doped tungsten oxygen fluoride silicate up-converted luminescent glass

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1) Put silicon dioxide, aluminum oxide, tungsten oxide, calcium fluoride, titanium dioxide, ytterbium oxide and erbium oxide in a molar ratio of 50: 15: 10: 20: 5: 5: 0.5 into the mortar, mix well and pour in the crucible;

[0016] 2) Put the above-mentioned crucible containing batch materials into a high-temperature furnace, and o C / min heating rate to 1550 o C, heat preservation for 2 h to melt;

[0017] 3) Pour the molten liquid in step 2) on 300 o The copper plate of C is cooled to room temperature, and then at 620 o C annealed for 2 h to obtain rare earth ion-doped oxytungstofluoride up-conversion luminescent glass.

[0018] Figure 1 Curve a is the upconversion emission spectrum of the oxyfluoride tungsten silicate glass prepared in this example at an excitation wavelength of 980 nm. It can be seen from the figure that corresponding to Er 3+ ion: 4 S 3 / 2 → 4 I 15 / 2 and 4 f 9 / 2 → 4 I 15 / 2 Green (~546 nm) and red (~665 nm) upconversion emission with st...

Embodiment 2

[0021] 1) Put silicon dioxide, aluminum oxide, tungsten oxide, calcium fluoride, titanium dioxide, ytterbium oxide and erbium oxide in a molar ratio of 50: 15: 10: 20: 5: 5: 1.0 into the mortar, mix well and pour in the crucible;

[0022] 2) Put the above-mentioned crucible containing the batch material into the high temperature furnace, o C / min heating rate to 1550 o C, heat preservation for 2 h to melt;

[0023] 3) Pour the molten liquid in step 2) on 300 o C on the copper plate cooled to room temperature, and then at 640 o C annealed for 3 h to obtain rare earth ion-doped oxytungstofluoride up-conversion luminescent glass.

[0024] The up-conversion emission spectrum of the product is as figure 1 As shown in curve b, it can be seen from the figure that the prepared oxyfluorotungstic silicate glass obtained strong green (~546 nm) and red (~665 nm) upconversion emission at the excitation wavelength of 980 nm.

Embodiment 3

[0026] 1) Put silicon dioxide, aluminum oxide, tungsten oxide, calcium fluoride, titanium dioxide, ytterbium oxide and erbium oxide in a molar ratio of 50: 15: 10: 20: 5: 5: 1.5 into the mortar, mix well and pour in the crucible;

[0027] 2) Put the above-mentioned crucible containing batch materials into a high-temperature furnace, o C / min heating rate to 1550 o C, heat preservation for 2 h to melt;

[0028] 3) Pour the molten liquid in step 2) on 300 o C on the copper plate cooled to room temperature, and then at 650 o C annealed for 4 h to obtain rare earth ion-doped oxytungstofluoride up-conversion luminescent glass.

[0029] The upconversion emission spectrum of the product is shown in Figure 1, curve c. It can be seen from the figure that the prepared oxyfluorotungstic silicate glass obtained strong green light (~546 nm) and red light (~665 nm) at the excitation wavelength of 980 nm. nm) up-conversion emission, and the luminous intensity is stronger than that of ...

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Abstract

The invention discloses a preparation method of rare earth ion doped tungsten oxygen fluoride silicate up-converted luminescent glass. The preparation method comprises the steps of: firstly, uniformly mixing silicon dioxide, germanium dioxide, aluminum oxide, tungsten oxide, calcium fluoride, titanium dioxide and rare earth oxide in a mortar; and then preparing the Er<3+>-Yb<3+> rare earth ions doped tungsten oxygen fluoride silicate up-converted luminescent glass by adopting a high-temperature melting annealing method. The method disclosed by the invention is simple in preparation method, low in raw material cost and simple in required device without a special device; and the overall preparation process is carried out in air atmosphere. According to the invention, tungsten oxide is introduced into an oxygen fluoride silicate glass substrate for the first time, and the further solution of the problems that the oxygen fluoride silicate glass is poor in chemical stability and mechanical strength after tungsten oxide is introduced is facilitated, so that the glass product has the advantages of low phonon energy of fluoride and good crystallization stability of oxide, thereby obtaining strong up-converted red and green light output visible to naked eyes.

Description

technical field [0001] The invention relates to a preparation method of oxyfluoride tungstosilicate glass, in particular to the preparation of rare earth ion-doped oxyfluoride tungstosilicate up-conversion luminescent glass. Background technique [0002] Tungsten oxide is an important VI B-VI A group indirect bandgap compound semiconductor material. There are usually five crystal forms: monoclinic (e-phase), triclinic (d-phase), monoclinic (g-phase), orthorhombic (b-phase), tetragonal (a-phase), tetragonal phase has high structural stability, and it has Excellent optical and electrical properties have broad application prospects in optical devices, light modulation devices, solar energy conversion, temperature and humidity sensors and other fields. Compared with borate glass and phosphate glass, tungsten oxide glass has better physical and chemical properties. doped WO 3 After that, due to W 6+ The ions have a large electronegativity and can acquire free oxygen and [WO ...

Claims

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Application Information

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IPC IPC(8): C03C4/12C03C3/253C03C3/112C03C3/062
Inventor 赵高凌揭光涛何云龙黄晟辰韩高荣
Owner ZHEJIANG UNIV
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