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Rare earth ion activated nano barium hexafluorosilicate strongly near ultraviolet emission fluorophor and preparation method

A technology of hexafluorosilicon barium and rare earth ions, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of cumbersome operation and achieve the effect of uniform particle distribution and simple spectral correction operation

Inactive Publication Date: 2015-04-29
DALIAN NATIONALITIES UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the mercury pollution of energy-saving lamps, they are being replaced by white LEDs, and during operation, it is necessary to use white paper to scatter the light of energy-saving lamps into the detection port, and the operation is cumbersome.

Method used

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  • Rare earth ion activated nano barium hexafluorosilicate strongly near ultraviolet emission fluorophor and preparation method
  • Rare earth ion activated nano barium hexafluorosilicate strongly near ultraviolet emission fluorophor and preparation method
  • Rare earth ion activated nano barium hexafluorosilicate strongly near ultraviolet emission fluorophor and preparation method

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Experimental program
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Embodiment 1

[0022] Take by weighing 1.023ml fluosilicic acid (analytically pure, content 32%), 0.271g Ba(CH 3 COO) 2 , 0.0022g EuCl 2 , add 8ml oleic acid and 19ml 1-octadecene into a 100ml three-neck flask, stir at a vacuum of 0.08Mpa for 10 minutes, then heat to raise the temperature to 160°C and keep for 20min. After completely dissolving, cool naturally to room temperature , to obtain the precursor. Add 10ml of 0.6M methanolic solution of ammonium bifluoride dropwise to the obtained precursor under stirring condition (weigh 0.257g NH 4 HF 2 dissolved in 10ml of anhydrous methanol). After the dropwise addition is completed, stir for 10 minutes under the protection of nitrogen, heat to raise the temperature to 70°C, and keep it for 2 hours. room temperature. Add 2ml of absolute ethanol to the solution obtained above, centrifuge at room temperature at 9000rpm for 10min, then wash three times with cyclohexane:ethanol=1:3 (v / v) mixed solution, and then dry at 80°C for 8 hours. The o...

Embodiment 2

[0024] Take by weighing 1.023ml fluosilicic acid (analytically pure, content 32%), 0.246g Ba(CH 3 COO) 2 , 0.0223g EuCl 2 , Add in the 100ml three-neck flask that 16ml oleic acid and 37ml 1-octadecene are housed. Stir for 10 minutes above a vacuum of 0.08Mpa, then heat to raise the temperature to 160°C and keep for 20 minutes. After completely dissolving, cool naturally to room temperature to obtain a precursor. Add 10ml of 0.6M methanolic ammonium bifluoride solution (weigh 0.514g NH 4 HF 2 dissolved in 10ml of anhydrous methanol). After the dropwise addition is completed, stir for 10 minutes under the protection of nitrogen, heat to raise the temperature to 90°C, and keep it for 2 hours. After no methanol is evaporated, then heat up rapidly to raise the temperature to 320°C and keep it for 0.5h, then cool down naturally. to room temperature. Add 5ml of absolute ethanol to the solution obtained above, centrifuge at room temperature at 9000rpm for 10min, then wash three ...

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Abstract

The invention relates to a rare earth ion activated nano barium hexafluorosilicate strongly near ultraviolet emission fluorophor and a preparation method. The chemical expression formula of the barium hexafluorosilicate fluorophor is Ba(1-x)SiF6:x Eu<2+>. The preparation method comprises the following steps: weighing a certain amount of fluosilicic acid, EuCl2 and Ba(CH3COO)2; firstly preparing a precursor in a mixed solution of oleic acid and 1-octadecene; then, adding a methanol solution of ammonium hydrogen fluoride; under nitrogen protection, raising the temperature and steaming methanol and then raising the temperature to 300-320 DEG C for high-temperature thermal decomposition; finally washing, drying and grinding to obtain the fluorophor. The preparation method provided by the invention is relatively complex, and the prepared barium hexafluorosilicate fluorophor has the advantages of ultraviolet-activated near ultraviolet emission, sharp peak shape, fixed peak position and strong luminescence and is an ideal fluorescent material which is applied to calibrating a fluorescence spectrophotometer and a near ultraviolet laser.

Description

technical field [0001] The invention relates to a luminescent material and a preparation method thereof. Background technique [0002] During the production, installation and commissioning of the fluorescence spectrometer, a standard sample with a fixed emission peak is required to calibrate the instrument. On the other hand, due to changes in various conditions and factors during the long-term use of the fluorescence spectrometer in use, the "drift phenomenon" of the detection results often occurs, and a standard sample with a fixed emission peak is also required to calibrate the instrument. [0003] At present, the spectral correction of the fluorescence spectrometer is divided into the wavelength correction of the excitation light path and the wavelength correction of the emission light path. The wavelength correction of the excitation light path is usually based on the narrow-band emission at 473.4nm in the characteristic scanning spectrum of the xenon lamp, and ±0.5nm ...

Claims

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Application Information

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IPC IPC(8): C09K11/61
Inventor 华瑞年张伟肇欣赵君
Owner DALIAN NATIONALITIES UNIVERSITY