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Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature

A technology of oxynitride silicate and luminescent materials, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of high cost, long time consumption, high temperature, etc., achieve short sintering time, good crystallinity, and low reaction sintering temperature Effect

Inactive Publication Date: 2015-04-08
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the technical problems of high temperature, time-consuming and high cost in the method for preparing oxynitride silicate luminescent materials in the prior art, and to provide a method for preparing oxynitride silicate luminescent materials under normal pressure and low temperature. method

Method used

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  • Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature
  • Method for preparing nitrogen oxygen silicate luminescent material in normal pressure and at low temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Y 4(1-x) Si 2 N 2 o 7 :xCe 3+ (x=0.005) Preparation:

[0056] (1) put Y 2 o 3 With a certain concentration of dilute HNO 3 Heat until dissolved, add deionized water to dilute, and prepare Y(NO 3 ) 3 Solution; Weigh 0.0022gCe(NO 3 ) 3 ·6H 2 O was added to 7.96mLY(NO 3 ) 3 In the solution, add deionized water until the volume of the solution is 10mL. After stirring for 15min, add 1.6811g of citric acid monohydrate to the above solution; after stirring for 15min, add 0.4167g of TEOS dissolved in 10mL of absolute ethanol to the above mixed solution; stir After 30 minutes, add 2 g of PEG with a molecular weight of 10,000, and stir at 400 rpm for 2 hours at room temperature to make the above solution into a sol;

[0057] (2) Transfer the sol to a dish, heat and evaporate to dryness in a water bath at 60°C to obtain a gel; pre-burn the gel in a muffle furnace at 500°C for 2 hours; simply grind the obtained product and transfer it to In a corundum crucible, sinte...

Embodiment 2

[0060] to combine figure 1 and figure 2 Illustrative Example 2

[0061] Y 4(1-x) Si 2 N 2 o 7 :xCe 3+ (x=0.01) Preparation:

[0062] (1) put Y 2 o 3 With a certain concentration of dilute HNO 3 Heat until dissolved, add deionized water to dilute, and prepare Y(NO 3 ) 3 Solution; Weigh 0.0043gCe(NO 3 ) 3 ·6H 2 O was added to 7.92mLY(NO 3 ) 3 In the solution, add deionized water until the volume of the solution is 10mL. After stirring for 15min, add 1.6811g of citric acid monohydrate to the above solution; after stirring for 15min, add 0.4167g of TEOS dissolved in 10mL of absolute ethanol to the above mixed solution; stir After 30 minutes, add 2.4 g of PEG with a molecular weight of 10,000, and stir at 400 rpm for 2 hours at room temperature to make the above solution into a sol;

[0063] (2) Transfer the sol to a dish, heat and evaporate to dryness in a water bath at 70°C to obtain a gel; pre-fire the gel in a muffle furnace at 500°C for 3 hours; simply grind ...

Embodiment 3

[0068] Y 4(1-x) Si 2 N 2 o 7 :xCe 3+ (x=0.05) Preparation:

[0069] (1) put Y 2 o 3 With a certain concentration of dilute HNO 3 Heat until dissolved, add deionized water to dilute, and prepare Y(NO 3 ) 3Solution; Weigh 0.0217gCe(NO 3 ) 3 ·6H 2 O was added to 7.6mLY(NO 3 ) 3 In the solution, add deionized water until the volume of the solution is 10mL. After stirring for 30min, add 1.6811g of citric acid monohydrate to the above solution; after stirring for 15min, add 0.4167g of TEOS dissolved in 10mL of absolute ethanol to the above mixed solution; stir After 30 minutes, add 2 g of PEG with a molecular weight of 20,000, and stir at 500 rpm for 2 hours at room temperature to make the above solution into a sol;

[0070] (2) Transfer the sol to a dish, heat and evaporate to dryness in a water bath at 80°C to obtain a gel; pre-burn the gel in a muffle furnace at 500°C for 4 hours; simply grind the obtained product and transfer it to In a corundum crucible, sinter a...

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Abstract

The invention discloses a method for preparing a nitrogen oxygen silicate luminescent material in a normal pressure and at a low temperature, and belongs to the technical field of luminescent materials. The problems that in the prior art, a method for preparing the nitrogen oxygen silicate luminescent material requires a high temperature, the spent time is long, and the cost is high are solved. The method comprises the steps as follows: metal nitrate is taken as a metal ion source, and tetraethoxysilane is taken as a silicon source; a coordination agent and a cross-linking agent are added; sol is firstly prepared with a sol-gel method; then the obtained sol is heated and dried at the temperature of 60 DEG C-90 DEG C, presintered for 1-6 hours at the temperature of 400 DEG C-600 DEG C, and then sintered for 3-5 hours at the temperature of 700 DEG C-800 DEG C, so that a precursor is obtained; and finally, the obtained precursor is placed in a container, ammonia gas is led into the container, and the temperature is raised to 1150 DEG C-1200 DEG C; and the precursor is calcined for 4-12 hours in normal pressure, and cooling is performed, so that the nitrogen oxygen silicate luminescent material is obtained. According to the method, the operation steps are simple, the reaction sintering temperature is lower, the sintering time is short, and the cost is low.

Description

technical field [0001] The invention relates to a method for preparing an oxynitride silicate luminescent material under normal pressure and low temperature, and belongs to the technical field of luminescent materials. Background technique [0002] Nitride phosphor has unique excitation spectrum (excitation range covers ultraviolet, near ultraviolet, blue light and even green light) and excellent luminescence characteristics (emission of blue, green, yellow, red light, small thermal quenching, high luminous efficiency) , The material itself has the advantages of non-toxicity and good stability, and is widely used in white light LEDs. [0003] In the prior art, nitrides and nitrogen oxides are mostly formed by sintering oxide or nitride raw materials in a high-temperature, high-pressure nitrogen or ammonia atmosphere by using a high-temperature solid-state method (the effect of the nitrogen or ammonia atmosphere is to ensure that the nitrides The raw material is not oxidized...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/79
Inventor 林君耿冬苓
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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