An efficient and stable mn 4+ Doped fluoride light-emitting material and preparation method thereof

A technology of luminescent materials and fluorides, which is applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of insufficient high temperature and humidity resistance, and achieve the effects of high temperature stability and humidity resistance, short time, and easy process control

Active Publication Date: 2022-03-15
XIAMEN INST OF RARE EARTH MATERIALS
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  • Application Information

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Problems solved by technology

[0004] In order to solve the deficiencies of the prior art, the object of the present invention is to provide a highly efficient and stable Mn 4+ Doped fluoride luminescent material and preparation method thereof, to solve the shortcomings of insufficient high temperature and humidity resistance of fluoride luminescent material, and at the same time effectively improve the luminous efficiency of phosphor powder

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  • An efficient and stable mn <sup>4+</sup> Doped fluoride light-emitting material and preparation method thereof
  • An efficient and stable mn <sup>4+</sup> Doped fluoride light-emitting material and preparation method thereof
  • An efficient and stable mn <sup>4+</sup> Doped fluoride light-emitting material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Example 1: K 2 TiF 6 :Mn 4+ Phosphor powder preparation

[0040] 0.4000g K 2 MnF 6 Dissolve in 6mL hydrofluoric acid (49wt.%) solution, stir 5 minutes to obtain orange-yellow transparent solution, then 5.1850g K 2 TiF 6 Add the powder into the solution, continue stirring at room temperature for 30 minutes, stop stirring and filter with filter paper, then wash with acetone to remove any residual HF, and dry to obtain K 2 TiF 6 :Mn 4+ powder. The excitation and emission spectra, fluorescence quantum yield and absorption efficiency of the product were measured by a FLS980 (Edinburgh Instrument) fluorescence spectrometer.

Embodiment 2

[0041] Example 2: Modified K 2 TiF 6 :Mn 4+ Phosphor powder preparation

[0042] By adding K to 10 ml of 49% HF solution 2 TiF 6 Compound, until no longer dissolved (about 1.7000g, at room temperature), filter the undissolved K 2 TiF 6 , get K 2 TiF 6 Saturated solution in 49% HF solution. Then add this saturated solution to the K 2 TiF 6 :Mn 4+ In the phosphor container, keep stirring at room temperature for 30min. Then perform vacuum filtration; repeat the above stirring and soaking steps twice, and finally filter and wash with acetone several times to remove residual HF, and dry at 70°C for 2 hours to obtain phosphor. X-ray powder diffraction showed that the product was still in the hexagonal phase K 2 TiF 6 structure( figure 1 ); The excitation and emission spectra and the internal fluorescence quantum yield of the product were measured by a FLS980 type (Edinburgh Instrument) fluorescence spectrometer, figure 2 For its excitation and emission spectra, Tabl...

Embodiment 3

[0043] Example 3: Modified K 2 TiF 6 :Mn 4+ Phosphor powder preparation

[0044] By adding K to 10 ml of 49% HF solution 2 TiF 6 compound, the solution was heated to 70°C and stirred continuously until it was no longer dissolved (about 2.3000g), and the undissolved K was filtered 2 TiF 6 , get K 2 TiF 6 Saturated solution in 49% HF solution at 70 °C. Then add this saturated solution to the K 2 TiF 6 :Mn 4+ In the phosphor container, the temperature was slowly lowered at a cooling rate of 0.5 °C / min, and the stirring was continued until room temperature. Then perform vacuum filtration, wash with acetone several times to remove residual HF, and dry at 70°C for 2 hours to obtain phosphor. Table 1 shows the important physicochemical and optical performance parameters of the prepared phosphors, including Mn 4+ The doping concentration, the preparation raw material ratio and the fluorescence quantum yield and absorption efficiency of the sample.

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Abstract

The invention discloses a highly efficient and stable modified Mn 4+ Doped fluoride luminescent material and preparation method thereof, the preparation method can efficiently synthesize A in the temperature range of 0-120°C 2 MF 6 compound coated A 2 MF 6 :Mn 4+ Fluoride phosphors, avoid Mn 4+ It degrades directly in contact with the external environment, has high temperature stability and good moisture resistance, and further improves the luminous efficiency of the phosphor. The method has low preparation temperature, short time and easy process control, and is suitable for industrial large-scale preparation.

Description

technical field [0001] The invention relates to the technical field of rare earth luminescent materials and lighting displays, in particular to a highly efficient and stable Mn 4+ Doped fluoride luminescent material and its preparation method. Background technique [0002] As a new type of solid-state light source, white LED has the advantages of environmental protection, energy saving, high efficiency and fast response compared with traditional incandescent lamps and fluorescent lamps. The fourth generation of green light source after the light source. In the LED light source, the performance of the phosphor determines the technical indicators such as the luminous efficiency, color rendering index, color temperature and service life of the LED. Therefore, the phosphor plays a pivotal role in the white LED and has received widespread attention. At present, the most commonly used method is to combine the blue LED chip (luminous wavelength 440-480nm) with yellow phosphor (su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/02C09K11/67C09K11/61
CPCC09K11/02C09K11/616C09K11/675
Inventor 朱浩淼黄得财卢灿忠陈学元
Owner XIAMEN INST OF RARE EARTH MATERIALS
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