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High-temperature-resistant and high-humidity-resistant fluoride red fluorescent powder and preparation method thereof

A technology of red light phosphor and fluoride, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low quantum efficiency, thermal quenching, poor high temperature and high humidity resistance, etc., achieve high internal quantum efficiency, promote Good effect of crystal growth and high temperature and humidity resistance

Active Publication Date: 2017-03-08
HEBEI LIFU CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the purposes of the present invention is to provide a high-temperature and high-humidity resistant fluoride red phosphor to solve the problems of low internal quantum efficiency, thermal quenching, and poor high-temperature and high-humidity resistance of existing red phosphors

Method used

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  • High-temperature-resistant and high-humidity-resistant fluoride red fluorescent powder and preparation method thereof
  • High-temperature-resistant and high-humidity-resistant fluoride red fluorescent powder and preparation method thereof
  • High-temperature-resistant and high-humidity-resistant fluoride red fluorescent powder and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0035] Preparation of powder: add the oxide of M to 20-60wt% hydrofluoric acid solution, after all the solids are dissolved, continue to add KF and AF to the above solution 2 , KMnO 4 and K 2 MF 6 Substrate, dropwise add 20-40wt% hydrogen peroxide solution to the solution, stop the dropwise addition after the solution changes color, the whole process is carried out under stirring at 100-1000r / min, after stopping the dropwise addition of the hydrogen peroxide solution, put The reactant is dried at 0-200°C for 0-72 hours, and after drying, the filter cake is taken out, ground and broken through a 100-mesh sieve to obtain K m A n m 1-x f 6 :xMn 4+ solid product.

[0036] Coating of powder: according to the ratio of potassium silicate: hydroxymethylcellulose sodium aqueous solution (CMC-Na): polyethylene glycol aqueous solution (PEG) = 1g: 10 ~ 20mL: 5 ~ 30mL, the mass fraction is respectively measured as 1-5% CMC-Na, 2-10% PEG mass fraction, and stirring at room temperatu...

Embodiment 1

[0038] Example 1: K 1.8 Cu 0.1 Si 0.95 f 6 : 0.05Mn 4+ Phosphor powder preparation.

[0039] 10gSiO 2 Add it to 100mL 40wt% hydrofluoric acid solution, place the polytetrafluoroethylene beaker in a 25°C water bath, after all the solids are dissolved, continue to add 1.8g KF, 2g CuF 2 , 14gKMnO 4 and 10g K 2 SiF 6 , dropwise add 30% hydrogen peroxide solution in the solution, stop dripping after the solution turns golden yellow, the whole process is carried out under stirring at 100r / min, after stopping the dropwise addition of hydrogen peroxide solution, put the reactant in After standing at 25°C for 2 hours, filter the resulting precipitate, wash it with ethanol three times, put the filter cake in a vacuum drying oven, and dry it at 70°C for 1 hour. After drying, take out the filter cake, grind and crush it through a 100-mesh sieve That is, yellow K 1.8 Cu 0.1 Si 0.95 f 6 : 0.05Mn 4+ Phosphor.

[0040] Observed under a microscope, the obtained fluorescent powde...

Embodiment 2

[0041] Example 2: K 1.8 Cu 0.1 Si 0.95 f 6 : 0.05Mn 4+ Encapsulation of phosphor powder.

[0042] Measure 10mL of CMC-Na with a mass fraction of 1%, and 10mL of 5% PEG, and stir at room temperature to fully swell, add 1g of potassium silicate to the above mixed solution, and stir for 30min to form a mixed sol. Weigh 2g of the fluorescent powder prepared in Example 1 and add it to the above sol, stir at room temperature for 30min, disperse with ultrasonic waves with a frequency of 20KHz, supplemented by stirring at the same time, the stirring rate is 110r / min, stir for 1h, and pump it Filtration, washing with ethanol during the suction filtration, after the suction filtration, place the filter cake in a vacuum drying oven, and vacuum dry at 70°C for 2 hours to obtain a fluoride red phosphor with a core-shell structure.

[0043] The coated phosphor is a kind of yellowish crystal, and the fluffy substance coated on the surface can be seen under the scanning electron microsco...

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Abstract

The invention provides a high-temperature-resistant and high-humidity-resistant fluoride red fluorescent powder and a preparation method thereof. The fluorescent powder has a general chemical formula of KmAnM1-xF6: xMn<4+>. In the general chemical formula, A is one or two selected from the group consisting of Cu, Ba and Zn; M is at least one selected from the group consisting of Ti, Si and Ge; m + 2n are equal to 2; n is no less than 0.05 and no more than 0.2; m is no less than 1.6 and no more than 1.9; x is more than 0 and less than 0.2; and the surface of the fluorescent powder is coated with a mixture of potassium silicate, carboxymethyl cellulose sodium and polyethylene glycol. The fluorescent powder provided by the invention can be effectively excited by light with the excitation wavelength being in a range of 300 to 500 nm, so red light with a peak wavelength of 610 to 650 nm and a half-peak breadth of only 2 to 9 nm is generated, and high color purity is obtained. The preparation method provided by the invention has simple flow, can prepare target products at low temperature and under normal pressure, and facilitates to large-scale industrial production; and a special coating technology is adopted in the invention, and a coating reagent is utilized to change the surface state of fluorescent powder particles, so the problem of agglomeration of solid particles can be effectively solved, and a fluorescent powder product with good dispersion properties and high-temperature-resistant and high-humidity-resistant performances can be obtained.

Description

technical field [0001] The invention relates to a red light phosphor and a preparation method thereof, in particular to a high temperature and high humidity resistant fluoride red light phosphor and a preparation method thereof. Background technique [0002] In 1996, white LEDs combined with blue LEDs and YAG phosphors appeared, known as the fourth-generation lighting sources that will surpass incandescent lamps, fluorescent lamps and xenon lamps (HID lamps). Because of its advantages of energy saving, environmental protection, safety, and long life, it has been widely used in various aspects of production and life, including indication, display, decoration, backlight, general lighting and other fields. In 1997, Nichia first reported Y 3 al 5 o 12 : Ce 3+ (YAG:Ce) yellow fluorescent material is combined with a blue light InGaN chip, but because the red band of its spectrum is weak, the color reproduction of white light is poor, and the color rendering index is low. Anot...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/61C09K11/66
CPCC09K11/025C09K11/616C09K11/665
Inventor 杨志平李璇璇田兰强赵金鑫
Owner HEBEI LIFU CHEM TECH
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