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Method for preparing silicon-based oxynitride fluorescent powder

A technology of nitride phosphors and silicon-based oxygen, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of unmentioned multi-component systems and affect optical properties, and achieve reduced energy consumption, reduced degree of agglomeration, and reduced synthesis The effect of temperature

Inactive Publication Date: 2010-09-01
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these patents are only applicable to the manufacture of silicon nitride powder, film and ceramics, and do not mention the situation in the multi-component system, whether it affects the optical properties

Method used

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  • Method for preparing silicon-based oxynitride fluorescent powder
  • Method for preparing silicon-based oxynitride fluorescent powder
  • Method for preparing silicon-based oxynitride fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 1) According to the chemical formula Ca of the target product silicon-based oxynitride phosphor 0.95 Eu 0.05 Si 9 Al 3 ON 15 , Weigh 1.1886g CaCO 3 , 0.1100gEu 2 o 3 , 5.1758gAlF 3 ·3H 2 0, 3.1596g particle size is 400 mesh silicon powders as starting material, puts into 100mL agate ball mill jar jointly, adds 12mL ethanol as medium, ball mills more than 5 hours with the rotating speed of 500 rev / mins, makes various raw materials fully mix, Dry the collection at 80°C.

[0044] 2) Take 3g of the above-mentioned completely mixed raw material powder and put it into a corundum boat, put it into a corundum tube furnace, and perform a vacuum operation on the high temperature furnace so that the vacuum degree in the high temperature furnace is -0.1MPa, and then pass through the reduction The gas is NH with a purity of 99.99% 3 to slightly positive pressure, in flowing NH 3 In the atmosphere, the temperature was raised to 1000°C at a heating rate of 5°C / min, and then...

Embodiment 2

[0047]1) According to the chemical formula Sr of the target product silicon-based oxynitride phosphor 0.98 Eu 0.02 Si 2 o 2 N 2 , weighed 8.2959gSr(NO 3 ) 2 , 0.1408gEu 2 o 3 , 2.2464g of silicon powder with a particle size of 200 mesh as the starting material, put them together into a 100mL agate ball mill jar, add 15mL of ethanol as the medium, and ball mill at a speed of 485 rpm for 10 hours to fully mix the various raw materials. Collect dry.

[0048] 2) Take 3g of the obtained powder and put it into a corundum boat, put it into a corundum tube furnace, and vacuumize the high-temperature furnace so that the vacuum degree in the high-temperature furnace is -0.1MPa, and then feed the reducing gas, that is, the purity is 99.99% N 2 to slightly positive pressure, in flowing N 2 In the atmosphere, the temperature was raised to 1000°C at a heating rate of 5°C / min, and then the gas was adjusted to NH 3 , the flow rate is 0.5L / min, and then the temperature is raised to ...

Embodiment 3

[0051] 1) According to the chemical formula Y of the target product silicon-based oxynitride phosphor powder 3.8 Ce 0.2 Si 2 o 7 N 2 , weighed 2.1452gY 2 o 3 , 0.1721gCeO 2 , 0.150 2 gSiO 2 , 0.2106g of silicon powder with a particle size of 600 mesh as the starting material, put them together in a BN mortar, manually grind for 1 hour, and collect.

[0052] 2) Take 2g of the obtained powder and put it into a corundum boat, put it into a corundum tube furnace, and vacuumize the high-temperature furnace so that the vacuum degree in the high-temperature furnace is -0.1MPa, and then feed the reducing gas, that is, the purity is 99.99% N 2 to slightly positive pressure, in flowing N 2 In the atmosphere, the temperature was raised to 1000°C at a heating rate of 5°C / min, and then the N 2 The flow rate is 0.3L / min, and the flow rate is 50mL / min H 2 , then raise the temperature to 1350°C at a heating rate of 4°C / min, keep the temperature for 2 hours, and turn off the H 2 ,...

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Abstract

The invention discloses a method for preparing silicon-based oxynitride fluorescent powder, which comprises the following steps of: weighing corresponding raw materials and silica powder based on stoichiometric proportion of each element in the chemical formula of the silicon-based oxynitride fluorescent powder, after uniformly mixing the raw materials and the silica powder, raising the temperature to 800 to 1,000 DEG C under any one of the conditions of condition a to condition c, performing reduction reaction under the condition c or the condition d, and cooling the reaction product to roomtemperature to obtain the silicon-based oxynitride fluorescent powder, wherein the condition a is vacuum; the condition b is the atmosphere of inert gases; the condition c is the atmosphere of nitrogen-containing gases; and the condition d is the atmosphere of reductive gas. The silicon-based oxynitride fluorescent powder doped with various luminescent ions and prepared by the method has bright fluorescence under the excitation of ultraviolet ray, near ultraviolet or visible light. The method has the advantages of low preparation temperature of the product, high phase purity of the product, controllable particle size of the product, good luminous intensity of the product, low cost, simple process and the like, and is easy to enlarge industrialization.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and relates to a method for preparing silicon-based oxynitride fluorescent powder. Background technique [0002] Rare earth-doped oxynitride phosphors have the characteristics of wide excitation band, long emission wavelength, high luminous efficiency, good chemical stability, high thermal stability, and no environmental pollution, and have developed into promising luminescent materials. The structural unit of silicon-based oxynitride is Si-(O, N) tetrahedron, which forms a two-dimensional layered structure or a three-dimensional network structure. The ratio of oxygen and nitrogen can be changed within a certain range to maintain a stable structure, and the emission wavelength will change. Shifting with nitrogen content, with continuously tunable spectral properties, is a very important class of materials in science and industry. Its preparation generally adopts high-temperature so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/80C09K11/79
Inventor 徐鑫杨秀芳唐家业田锦森
Owner UNIV OF SCI & TECH OF CHINA
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