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Red phosphor powder without rare earth and preparation method of red phosphor powder

A technology of red phosphor and rare earth, applied in the field of rare earth-free red phosphor and its preparation, can solve the problems of toxicity, low output, unstable physical properties, etc., achieve good monochromaticity, low cost, and reduce production cost Effect

Active Publication Date: 2019-10-25
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

mn 4+ Doped fluoride red phosphors have become a new research direction due to their narrow-band emission of red light, being excited by ultraviolet and blue light, and cheap raw materials. HF, physical properties are also unstable

Method used

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  • Red phosphor powder without rare earth and preparation method of red phosphor powder
  • Red phosphor powder without rare earth and preparation method of red phosphor powder
  • Red phosphor powder without rare earth and preparation method of red phosphor powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0030] A preparation method of rare earth-free red phosphor, comprising the following steps:

[0031] (1) Weigh Li according to the stoichiometric ratio 2 CO 3 , GeO 2 , MnCO 3 Raw material powder 2g (each raw material mass ratio is Li 2 CO 3 :GeO 2 :MnCO 3 =0.3001:1.6994:0.0005), namely Li 2 CO 3 :( GeO 2 +MnCO 3 )=1:4, (GeO 2 :MnCO 3 )=3.999:0.001; then weigh 0.02g of NH 4 Cl, accounting for 1% of the mass of the raw material oxide powder.

[0032] (2) Put the above-mentioned raw materials in an agate mortar and grind them for 20 minutes, and mix them evenly. Then the mixture was loaded into an alumina crucible, placed in a muffle furnace, and calcined at 900° C. for 6 h to perform a solid-state reaction. After the product is cooled to room temperature, grind it evenly to obtain Li 2 Ge 4 o 9 :0.001Mn 4+ red phosphor.

[0033] (3) Use a fluorescence spectrometer (HITACHI F-7000) to test the spectral properties of the phosphor, and obtain the excitation-em...

Embodiment example 2

[0036] (1) Weigh Li according to the stoichiometric ratio 2 CO 3 , GeO 2 , MnCO 3 Raw material powder 2g (each raw material mass ratio is Li 2 CO 3 :GeO 2 :MnCO 3 =0.3001:1.6990:0.0009), then weigh 0.02g of NH 4 Cl.

[0037] (2) After grinding the above raw materials in an agate mortar for 20 minutes, mix them evenly, then load the mixture into an alumina crucible, put it in a muffle furnace, and calcinate it at 900°C for 6 hours, and wait for the product to cool After reaching room temperature, grind evenly to obtain Li 2 Ge 4 o 9 :0.002Mn 4+ red phosphor.

[0038] (3) Use a fluorescence spectrometer (HITACHI F-7000) to test the spectral properties of the phosphor. The results show that the phosphor emits red light with an emission peak wavelength at 671nm under excitation at 325nm. The emission spectrum of the phosphor is as follows: figure 1 shown.

[0039] (4) Use X-ray diffraction (Ultima IV-185) to study the crystal structure. Cu-Kα is used as the target fo...

Embodiment example 3

[0041] (1) Weigh Li according to the stoichiometric ratio 2 CO 3 , GeO 2 , MnCO 3 Raw material powder 2g (each raw material mass ratio is Li 2 CO 3 :GeO 2 :MnCO 3 =0.3001:1.6985:0.0014) and then weigh 0.02g of NH 4 Cl.

[0042] (2) Put the above-mentioned raw materials in an agate mortar and grind them for 20 minutes, and mix them evenly. Then the mixture was loaded into an alumina crucible, placed in a muffle furnace, and calcined at 900° C. for 6 h. After the product is cooled to room temperature, grind it evenly to obtain Li 2 Ge 4 o 9 :0.003Mn 4+ red phosphor.

[0043] (3) Use a fluorescence spectrometer (HITACHI F-7000) to test the spectral properties of the phosphor. The results show that the phosphor emits red light with an emission peak wavelength at 671nm under excitation at 325nm. The emission spectrum of the phosphor is as follows: figure 1 shown.

[0044] (4) Use X-ray diffraction (Ultima IV-185) to study the crystal structure. Cu-Kα is used as the t...

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Abstract

The invention relates to red phosphor powder without rare earth and a preparation method of the red phosphor powder. A general formula of the red phosphor powder is Li2Ge4O9:xMn<4+>, wherein the valueof the x in the formula is 0.001-0.008, and the red phosphor powder is prepared from the preparation raw materials including the following oxide components by stoichiometric ratio: Li2CO3 to (GeO2+MnCO3)=1 to 4, and (GeO2 to MnCO3)=(3.999 to 3.992) to (0.001 to 0.008); and the red phosphor powder is prepared by a solid phase reaction of the raw material components. Compared with the prior art, the red phosphor powder has the characteristics of wide-band excitation and narrow-band emission, ultraviolet chips and blue light chips can be effectively matched, and the characteristics of good light-emitting position of red light and good monochromaticity are further achieved; the preparation raw materials does not contain the rare earth, the red phosphor powder can be prepared by a solid phasereaction synthesis method under air atmosphere conditions, and the preparation method has the advantages of simple operation and low production cost; and the red phosphor powder and the preparation method can be widely applied to the fields such as white light LED, high quality LED illumination and display.

Description

technical field [0001] The invention relates to the technical field of phosphor preparation, in particular to a rare earth-free red phosphor and a preparation method thereof. Background technique [0002] White light LED has significant advantages such as low power consumption, high efficiency, green environmental protection, energy saving, long life, small size, fast response, and good color rendering. Therefore, it is known as the 21st century green lighting source and has broad market prospects and huge potential. socioeconomic benefits. [0003] Generally speaking, there are three paths for LEDs to achieve white light emission: the first is to mix and use three colors of LED light; the second is to use ultraviolet LED lights to excite three phosphors of red, green and blue, and mix the light of these three phosphors into white light ; The third is the use of blue LEDs and corresponding blue-light-excited yellow phosphors. At present, the third way to achieve white ligh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/66H01L33/50
CPCC09K11/661H01L33/502Y02B20/00
Inventor 房永征曹艳蓉侯京山丁建刘玉峰赵国营
Owner SHANGHAI INST OF TECH