Fluorosilicate red fluorescent powder and preparation method thereof

A red phosphor, fluorosilicate technology, applied in chemical instruments and methods, luminescent materials, electrical components, etc., can solve the problems of high equipment requirements, harsh preparation conditions, high energy consumption, and achieve stable physical and chemical properties, luminous Stable performance and uniform particle size distribution

Pending Publication Date: 2021-12-10
烟台布莱特光电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of phosphor needs to be doped with rare earth, and the raw material requirements are relatively special. It usually needs to be prepared under high temperature and high pressure, and the preparation conditions are harsh.
Not only high energy consumption, but also low yield, so its production cost is high and the price is very expensive
Other current methods of preparing phosphors, such as hydrothermal method, microwave method, high-temperature solid-phase method, etc., are still complicated in production process, and the requirements for equipment are still high
In addition, since the absorption peak of the light conversion material of the blue LED is required to be located at 420-470nm, there are very few fluorescent materials that meet this requirement and the absorption intensity is low
The research of this kind of phosphor materials is relatively difficult, and there are not many varieties of phosphors that can be excited by blue light and emit visible light.

Method used

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  • Fluorosilicate red fluorescent powder and preparation method thereof
  • Fluorosilicate red fluorescent powder and preparation method thereof
  • Fluorosilicate red fluorescent powder and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The chemical formula of fluorosilicate red phosphor is Ca 0.6 SiO 2 f 2 :0.4Mn 2+ , prepared by the following steps:

[0025] (1) According to the chemical formula Ca 0.6 SiO 2 f 2 :0.4Mn 2+ The stoichiometric ratio of raw materials was weighed and mixed with calcium fluoride, potassium fluoride, silicon dioxide, oxalic acid, and manganese dioxide, stirred in ethanol, filtered, dried at 100°C, and sieved;

[0026] (2) adding 0.3% of the raw material weight of ammonium fluoride and ammonium chloride for grinding, grinding, mixing and sieving to obtain a mixture, wherein the weight ratio of ammonium fluoride and ammonium chloride is 4:1;

[0027] (3) The mixture obtained in step (2) is packed into a crucible, and heated in a high-temperature furnace under H 2 and N 2 Sintering in reducing atmosphere and 850°C for 5 hours, cooling to obtain manganese-doped fluorosilicate red phosphor Ca 0.6 SiO 2 f 2 :0.4Mn 2+ .

Embodiment 2

[0029] The chemical formula of fluorosilicate red phosphor is Ca 0.83 SiO 2 f 2 :0.17Mn 2+ , prepared by the following steps:

[0030] (1) According to the chemical formula Ca 0.83 SiO 2 f 2 :0.17Mn 2+ The stoichiometric ratio of raw materials was weighed and mixed with calcium fluoride, potassium fluoride, silicon dioxide, oxalic acid, and manganese dioxide, stirred in ethanol, filtered, dried at 100°C, and sieved;

[0031] (2) adding 0.4% of the weight of the raw material to ammonium fluoride and ammonium chloride for grinding, grinding, mixing and sieving to obtain a mixture, wherein the weight ratio of ammonium fluoride and ammonium chloride is 6:1;

[0032] (3) The mixture obtained in step (2) is packed into a crucible, and heated in a high-temperature furnace under H 2 and N 2 Sintering under reducing atmosphere and 950°C for 4 hours, cooling to obtain manganese-doped fluorosilicate red phosphor Ca 0.83 SiO 2 f 2 :0.17Mn 2+ .

Embodiment 3

[0034] The chemical formula of fluorosilicate red phosphor is Ca 0.44 SiO 2 f 2 :0.56Mn 2+ , prepared by the following steps:

[0035] (1) According to the chemical formula Ca 0.44 SiO 2 f 2 :0.56Mn 2+ The stoichiometric ratio of raw materials was weighed and mixed with calcium fluoride, potassium fluoride, silicon dioxide, oxalic acid, and manganese dioxide, stirred in ethanol, filtered, dried at 100°C, and sieved;

[0036] (2) adding 0.2% of the weight of the raw material to ammonium fluoride and ammonium chloride for grinding, grinding, mixing and sieving to obtain a mixture, wherein the weight ratio of ammonium fluoride and ammonium chloride is 8.4:1;

[0037] (3) The mixture obtained in step (2) is packed into a crucible, and heated in a high-temperature furnace under H 2 and N 2 Sintering under reducing atmosphere and 1000°C for 6 hours, cooling to obtain manganese-doped fluorosilicate red phosphor Ca 0.44 SiO 2 f 2 :0.56Mn 2+ .

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Abstract

The invention discloses fluorosilicate red fluorescent powder. The chemical formula of the fluorosilicate red fluorescent powder is Ca<1-x>SiO2F2:xMn2+, wherein the value range of x is 0.17 to 0.56. The invention also discloses a preparation method of the fluorescent powder. The preparation method comprises the following steps: (1) weighing raw materials according to the stoichiometric ratio of the chemical formula; (2) mixing the raw materials, adding a fluxing agent, performing grinding, uniformly performing grinding, and performing sieving to obtain a mixture; (3) putting the mixture obtained in the step (2) into a crucible, performing sintering for 4-6 hours in a high-temperature furnace in a reducing atmosphere at the sintering temperature of 800-1,000 DEG C, and performing cooling to obtain the fluorosilicate red fluorescent powder, wherein the raw material is a mixture of calcium fluoride, potassium fluoride, silicon dioxide, oxalic acid and manganese dioxide; the addition amount of the fluxing agent is 0.2-0.4% of the total weight of the raw materials, the fluxing agent is a mixture of ammonium fluoride and ammonium chloride, and the weight ratio of ammonium fluoride to ammonium chloride is (3.5-8.4): 1. According to the invention, the fluorosilicate red fluorescent powder with good dispersibility, uniform particle size distribution and high luminescence performance can be prepared, and the application requirements of fluorescent powder in LED packaging can be met.

Description

technical field [0001] The invention relates to the field of LED luminescent materials, in particular to a fluorosilicate red fluorescent powder and a preparation method thereof. Background technique [0002] A light-emitting diode (Light-Emitting Diode, referred to as LED) is a semiconductor electronic component that converts electrical energy into light energy. This kind of electronic component appeared as early as 1962. In the early days, it could only emit low-level red light, and later developed other versions of monochromatic light. Today, the light that can be emitted has covered visible light, infrared rays, and ultraviolet rays, and the breadth has also been increased to The higher level is called "fourth generation light source". Due to its advantages of energy saving, environmental protection, safety, and long life, it has been widely used in various aspects of industry and life, including indication, display, decoration, backlight, general lighting and other fie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61H01L33/50
CPCC09K11/617H01L33/504
Inventor 师琼周小平豆帆颜俊雄朱洪维王乖强姜涛涛曹永辉刘海燕
Owner 烟台布莱特光电材料有限公司
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