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A kind of preparation method of silicate yellow-green phosphor

A technology of yellow-green fluorescent powder and silicate, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of high cost, unsatisfactory, pollution, etc., and achieve the effect of low production cost and increased luminous intensity

Active Publication Date: 2018-07-03
JIANGSU BREE OPTRONICS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the phosphor powder prepared by this patent has low luminous efficiency and poor stability, which cannot meet the needs of practical applications.
[0004] At present, the methods commonly used to prepare phosphors are thermal carbon reduction, hydrogen reduction, or nitrogen-hydrogen mixed gas. The thermal carbon reduction method is often accompanied by carbon pollution to the powder, which seriously affects the luminescence of phosphors. Hydrogen or nitrogen-hydrogen mixed gas The reduction method implies the safety problems of flammable gas and high-pressure gas cylinders, and the cost is also relatively high, so it is necessary to develop a new and effective reduction preparation method for phosphor

Method used

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  • A kind of preparation method of silicate yellow-green phosphor
  • A kind of preparation method of silicate yellow-green phosphor
  • A kind of preparation method of silicate yellow-green phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Step (1): Weigh CaCO 3 100g, BaCO 3 79g, SrCO 3 76.8g, SiO 2 60.1g, Eu 2 o 3 14.07g is raw material;

[0055] Step (2) adding 10 g of LiCl flux to the raw materials described in step (1), and mixing uniformly to obtain a mixture;

[0056] Step (3): Take 30g of calcium hydride and put it into the bottom of the crucible, add a microporous ceramic plate above the calcium hydride, put the mixture described in step (2) on the microporous ceramic plate, Add a layer of SiO above the mixture 2 , B 2 o 3 and CaCO 3 A self-sealing layer mixture in which SiO 2 6g, B 2 o 3 9.8g and SrCO 3 45.8g; put the crucible directly into the air furnace, raise the temperature to 850°C at a heating rate of 5°C / min and keep it for 1h, then raise the temperature to 1200°C at a heating rate of 2°C / min, and put it under normal pressure at 1200°C Sintering at constant temperature for 10 hours; after the reaction, cool to room temperature to obtain crude phosphor;

[0057] Step (4): Th...

Embodiment 2

[0060] Step (1): Weigh BaCO 3 315.7g, SiO 2 60.1g, Eu 2 o 3 70.4g is the raw material;

[0061] Step (2) adding 15g of LiF flux to the raw materials described in step (1), and mixing uniformly to obtain a mixture;

[0062] Step (3): Take 12g calcium hydride and put it into the bottom of the crucible, add a microporous ceramic plate above the calcium hydride, put the mixture described in step (2) on the microporous ceramic plate, Add a layer of SiO above the mixture 2 , B 2 o 3 and CaCO 3 A self-sealing layer mixture in which SiO 2 6g, B 2 o 3 14g and CaCO 3 80g; Put the crucible directly into the air furnace, raise the temperature to 800°C at a heating rate of 5°C / min and hold for 5 hours, then raise the temperature to 1100°C at a heating rate of 2°C / min, and keep the temperature at 1100°C under normal pressure Sintering for 20 hours; after the reaction, cool to room temperature to obtain crude phosphor powder;

[0063] Step (4): The crude phosphor powder obtained...

Embodiment 3

[0066] Step (1): Weighing, BaCO 3 256g, CaCO 3 50g, SiO 2 60.1g, Eu 2 o 3 35.2g is raw material; Step (2) adds the NaCl fluxing agent of 21g in the raw material described in step (1), and mixes, obtains compound;

[0067] Step (3): Weigh 22g of calcium hydride and put it into the bottom of the crucible, add a microporous ceramic plate above the calcium hydride, put the mixture described in step (2) on the microporous ceramic plate, Add a layer of SiO above the mixture 2 , B 2 o 3 and CaCO 3 A self-sealing layer mixture in which SiO 2 12g, B 2 o 3 1.4g and CaCO 3 40.6g; Put the crucible directly into the air furnace, raise the temperature to 1000°C at a heating rate of 5°C / min and keep it for 0.5h, then raise the temperature to 1350°C at a heating rate of 2°C / min, and put it under normal pressure at 1350°C Sintering at a constant temperature for 0.5h; after the reaction, cool to room temperature to obtain crude phosphor;

[0068] Step (4): The crude phosphor powder...

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Abstract

The invention discloses a preparation method of yellow green silicate phosphor.The preparation method comprises the steps that calcium hydride is adopted as a reducing agent, placed at the bottom of a high-temperature-resisting container and covered with a microporous high-temperature-resisting plate; a mixture of raw materials and a fluxing agent is placed on the high-temperature-resisting plate, and a layer of a self-sealing layer material is placed on the high-temperature-resisting plate; calcinations is performed in an air atmosphere, and aftertreatment is performed to obtain the yellow green silicate phosphor.According to the preparation method, the mixed material of SiO2, B2O3 and ACO3 or AO (A is selected from at least one of Ca, Sr and Ba) of the different proportions is adopted as the self-sealing layer, the borosilicate glass self-sealing layer is formed at the high temperature, and the yellow green silicate phosphor is prepared under the inert-free gas protection condition for the first time.The preparation method is simple, convenient, high in production efficiency and low in cost; the luminous intensity of the prepared yellow green silicate phosphor is significantly improved compared with yellow green silicate phosphor prepared through a N2-H2 atmosphere reduction or carbon heating method and is 10%-20% higher than the luminous intensity of similar commercial phosphor.

Description

technical field [0001] The invention relates to the field of LED luminescent materials, in particular to a preparation method of silicate yellow-green fluorescent powder. Background technique [0002] White LED technology with high efficiency and low energy consumption is considered a major breakthrough in the field of lighting and display in the 21st century. There are three main methods to realize white light LED: one is the phosphor powder conversion method, that is, coating the phosphor powder on the LED chip, and the light emitted by the chip and the phosphor powder is combined to form white light; the other is the multi-chip method, using red, green, blue The LED chips of three colors use the principle of three primary colors to emit white light according to a certain ratio; the third is the integrated single-chip method (also called the multi-quantum well method), which uses multiple active layers in one chip to make the LED chip emit white light directly. . Fluores...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/59
CPCC09K11/7734
Inventor 何锦华谈高梁超符义兵刘冯新
Owner JIANGSU BREE OPTRONICS CO LTD