Mn<4+>-doped alkali metal fluoro-phosphate red luminescent material and preparation method thereof

A technology of fluorophosphate and red luminescence, which is applied in the direction of luminescent materials, chemical instruments and methods, and can solve the problems of limited application prospects, expensive production raw materials, and harsh synthesis conditions

Active Publication Date: 2020-04-24

YUNNAN MINZU UNIV

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Problems solved by technology

However, these nitrogen oxides doped with rare earth ions have expensive raw mater...

Abstract

The invention relates to the field of inorganic functional materials, and discloses a Mn<4+>-doped alkali metal fluoro-phosphate red luminescent material and a preparation method thereof. The chemicalcomposition of the Mn<4+> doped alkali metal fluoro-phosphate red luminescent material is AP1-xF6:xMn<4+>, wherein x is the molar percentage coefficient of correspondingly doped Mn<4+> ions relativeto P<5+> ions, and x is greater than 0 and less than or equal to 0.10; and A is Cs, Rb or K. The provided red luminescent material is mainly used for emitting red light of about 633 nm under the excitation of blue light, and the light emitting efficiency is high. The preparation method of the Mn<4+>-doped alkali metal fluoro-phosphate red luminescent material is an ion exchange method, the synthesis process is simple, and the preparation method is suitable for large-scale industrial production.

Application Domain

Luminescent compositions

Technology Topic

Ion exchangeRed light +6

Image

Examples

Experimental program(6)

Example Embodiment

[0020] Example 1:

[0021] Weigh 11.14 g of cesium fluoride, add 10 ml (40%) hydrofluoric acid (HF) and 2.2 ml hexafluorophosphoric acid, and react for 30 minutes. Then 0.15 g of potassium hexafluoromanganate was added to this solution to continue the reaction for 60 minutes. The obtained solid precipitate was washed 5 times with acetic acid, and then the solid precipitate was dried in a vacuum drying oven for 24 hours. The pink powder obtained was the final product CsPF 6 :Mn 4+.

[0022] Attached figure 1 Shown is the XRD diffraction pattern of this luminescent material, and the standard card JCPDS 34-0506 (CsPF 6 ) Is basically the same, which shows that the structure of the sample we synthesized is similar to CsPF 6 Consistent.

[0023] Attached figure 2 Shown are the room temperature excitation spectrum (monitoring wavelength is 633 nm) and emission spectrum (excitation wavelength of 455 nm) of the sample. The sample has a strong broadband excitation in the blue light region. Under the excitation of 455 nm light, the sample showed a series of red light emission peaks, of which the strongest emission peak was at 633 nm. These red emission peaks correspond to Mn 4+ of 2 E g - 4 A 2g Energy level transition. The spectral CIE coordinate value is: x = 0.694, y = 0.306. The CIE value of our sample is close to the red light NTSC (National Television Standard Committee) standard value ( x = 0.67, y = 0.33).

[0024] image 3 For CsPF 6 : Mn 4+ The SEM photo of the sample shows that the sample has a smooth and uniform appearance, with a particle size of about 15 μm.

[0025] Attached Figure 4 To use our synthesized samples and commercial Y 3 Al 5 O 12 :Ce 3+ The luminescence spectrum of a white LED device coated on a blue LED chip under excitation of 20 mA current. In the figure, the blue emission peak at ~ 460 nm is attributed to the blue light emitted by the GaN chip, and the emission peak from 500 nm to 600 nm corresponds to the yellow phosphor Y 3 Al 5 O 12 :Ce 3+ The yellow light emission. A series of sharp red light peaks between 600nm and 650nm correspond to the red light emission of our sample, with the strongest emission peak at 633 nm. The color temperature of this white LED is 4102 K), and the color rendering index is 82.6.

Example Embodiment

[0026] Example 2:

[0027] Weigh 7.82 g of rubidium fluoride and add it to 10 ml (40 %) of hydrofluoric acid (HF) and 2.2 ml of hexafluorophosphoric acid to react for 60 minutes. Then 0.15 g of potassium hexafluoromanganate was added to this solution to continue the reaction for 60 minutes. The obtained solid precipitate was washed 4 times with acetic acid, and then the solid precipitate was dried in a vacuum drying oven for 24 hours, and the pink powder obtained was the final product RbPF 6 :Mn 4+.

[0028] Attached Figure 5 Shown is the XRD diffraction pattern of this luminescent material, and the standard card JCPDS 32-0936 (RbPF 6 ) Is basically the same, which shows that the structure of the sample we synthesized is similar to that of RbPF 6 Consistent.

[0029] Attached Image 6 Shown is the sample RbPF 6 :Mn 4+ Room temperature excitation spectrum (monitoring wavelength is 632 nm) and emission spectrum (excitation wavelength is 452 nm). The sample has a strong broadband excitation in the blue light region. Under 452 nm light excitation, the sample showed a series of red light emission peaks, of which the strongest emission peak was at 632 nm. These red emission peaks correspond to Mn 4+ of 2 E g - 4 A 2g Energy level transition. The spectral CIE coordinate value is: x = 0.692, y = 0.308. The CIE value of our sample is close to the red light NTSC (National Television Standard Committee) standard value ( x = 0.67, y = 0.33).

[0030] Figure 7 RbPF 6 : Mn 4+ The SEM photo of the sample shows that the sample has a smooth and uniform appearance and a particle size of about 10 μm.

Example Embodiment

[0031] Example 3:

[0032] Weigh 7.82 g of potassium fluoride and add it to 10 ml (40%) of hydrofluoric acid (HF) and 2.2 ml of hexafluorophosphoric acid to react for 60 minutes. Then 0.15 g of potassium hexafluoromanganate was added to this solution to continue the reaction for 120 minutes. The obtained solid precipitate was washed 5 times with acetic acid, and then the solid precipitate was dried in a vacuum drying oven for 24 hours. The pink powder obtained was the final product KPF 6 :Mn 4+.

[0033] Attached Picture 8 Shown is the XRD diffraction pattern of this luminescent material, and the standard card JCPDS 52-1826 (KPF 6 ) Is basically the same, which shows that the structure of the sample we synthesized is similar to that of KPF 6 Consistent.

[0034] Attached Picture 9 Shown are the room temperature excitation spectrum (monitoring wavelength is 630 nm) and emission spectrum (excitation wavelength of 464 nm) of the sample. The sample has a strong broadband excitation in the blue light region. Under 464 nm light excitation, the sample showed a series of red light emission peaks, of which the strongest emission peak was at 630 nm. These red emission peaks correspond to Mn 4+ of 2 E g - 4 A 2g Energy level transition. The spectral CIE coordinate value is: x = 0.693, y = 0.307. The CIE value of our sample is close to the red light NTSC (National Television Standard Committee) standard value ( x = 0.67, y = 0.33).

[0035] Picture 10 For KPF 6 : Mn 4+ The SEM photo of the sample shows that the sample has a smooth and uniform appearance and a particle size of about 20 μm.

PUM

Property	Measurement	Unit
Particle size	15.0	µm
Particle size	20.0	µm

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