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Fluoride phosphor powder coating method based on atomic layer deposition technology

An atomic layer deposition, fluoride technology, applied in chemical instruments and methods, luminescent materials, electrical components, etc., can solve the problems of low coating efficiency, long coating time, high energy consumption, etc., to improve the coating efficiency , The effect of improving water stability and reducing consumption

Inactive Publication Date: 2019-10-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If coating is carried out at such a high temperature, the structure of the phosphor powder will be damaged to a certain extent, and due to the high reaction temperature and long coating time, the coating efficiency of this method is not high, the energy consumption is large, and the cost is high. Conducive to practical industrial production applications

Method used

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  • Fluoride phosphor powder coating method based on atomic layer deposition technology
  • Fluoride phosphor powder coating method based on atomic layer deposition technology
  • Fluoride phosphor powder coating method based on atomic layer deposition technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Select purchased washed and dried red fluoride phosphor ZYPF631Mn 4+ :K 2 GeF 6 , the uncoated sample is recorded as 0#, and another 1.5g aluminum oxide film coated on its surface for 30 cycles is recorded as 1#.

[0053] Put this 1.5g phosphor into the ALD deposition chamber, and then connect the phosphor deposition chamber to the equipment.

[0054] Introduce high-purity nitrogen to drive away the air in the system (deposition chamber and various channels).

[0055] Set the deposition parameters, turn on the high-purity nitrogen carrier gas of the atomic layer deposition equipment, the carrier gas flow rate is 150mL / min, the deposition temperature is 80°C, the precursor TMA reaction time is 30s, the purification time is 60s, and the precursor ozone reaction time is 30s , the purification time is 60s.

[0056] When the temperature of the deposition chamber reaches the preset deposition temperature, the reaction is started; the precursor and the phosphor are fully c...

Embodiment 2

[0059] 1.5 g of purchased washed and dried red fluoride phosphor ZYPF631 coated with aluminum oxide film for 20 cycles was recorded as 2#.

[0060] Put this 1.5g phosphor into the ALD deposition chamber, and then connect the phosphor deposition chamber to the equipment.

[0061] Introduce high-purity nitrogen to drive away the air in the system.

[0062] Set the deposition parameters, turn on the high-purity nitrogen carrier gas in the equipment, the carrier gas flow rate is 150mL / min, the deposition temperature is 80°C, the precursor TMA reaction time is 30s, the purification time is 80s, the precursor ozone reaction time is 30s, the purification The time is 80s.

[0063] When the temperature of the deposition chamber reaches the preset deposition temperature, the reaction is started; the precursor and the phosphor are fully contacted and reacted.

[0064] The deposition ends after 20 cycles, and the coated sample 2# is obtained.

Embodiment 3

[0066] 1.5 g of purchased washed and dried red fluoride phosphor ZYPF631 coated with 50-cycle aluminum oxide film on its surface is recorded as 3#.

[0067] Put this 1.5g phosphor into the ALD deposition chamber, and then connect the phosphor deposition chamber to the equipment.

[0068] Introduce high-purity nitrogen to drive away the air in the system.

[0069] Set the deposition parameters, turn on the high-purity nitrogen carrier gas in the equipment, the carrier gas flow rate is 150mL / min, the deposition temperature is 70°C, the precursor TMA reaction time is 10s, the purification time is 45s, the precursor ozone reaction time is 15s, the purification The time is 45s.

[0070] When the temperature of the deposition chamber reaches the preset deposition temperature, the reaction is started; the precursor and the phosphor are fully contacted and reacted.

[0071] The deposition ends after 50 cycles, and the coated sample 3# is obtained.

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Abstract

The invention relates to a fluoride phosphor powder coating method based on an atomic layer deposition technology, and relates to material surface treatment. The method comprises the following steps:1) carrying out pre-treatment on fluoride phosphor powder and placing the treated fluoride phosphor powder into a deposition chamber; 2) adjusting the temperature of the deposition chamber; 3) introducing trimethyl aluminum into the deposition chamber with nitrogen as a carrier gas, and purging the mixture; 4) stopping loading of trimethyl aluminum, introducing nitrogen gas into that deposition chamber, and purging the mixture; 5) stopping introduction of nitrogen gas, introducing ozone into the deposition chamber, and purging the mixture; 6) stopping introduction of ozone, introducing nitrogen gas into the deposition chamber, and purging the mixture; 7) repeating the steps 3) to 6); and 8) stopping introducing of nitrogen gas and naturally cooling the deposition chamber to obtain the coated fluoride phosphor powder. The reactant purging time is adjusted according to the repetition times so that the total reaction time does not exceed 2h, the temperature of the atomic layer depositioncoating operation is 50-90 DEG C and the time does not exceed 2h, and the coating adopts trimethyl aluminum and ozone as precursors.

Description

technical field [0001] The invention relates to material surface treatment, in particular to a fluoride fluorescent powder coating method based on atomic layer deposition technology. Background technique [0002] Due to the advantages of high efficiency, energy saving, and strong structure, LEDs are widely used in the fields of lighting and display. Based on LED technology, the easiest way to obtain white light is to use yellow YAG:Ce 3+ The phosphor is matched with the blue InGaN chip. However, due to the lack of red in the spectrum of this type of LED, its color rendering index is low and its color temperature is high. Therefore, in order to achieve high-quality lighting and display, it is crucial to explore red phosphors with high luminous efficiency, high color purity and good stability. [0003] Among many red phosphors, Eu 2+ doped with nitride and Mn 4+ Doped fluorides have been extensively studied and applied due to their excellent optical properties. But Mn 4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/66
CPCC09K11/025C09K11/665H01L33/502
Inventor 解荣军赵豫洁李烨周天亮
Owner XIAMEN UNIV
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