Red fluorescent powder with high luminous intensity, thermal stability and water resistance and preparation method thereof

A technology of red phosphor and thermal stability, which is applied in the direction of luminescent materials, chemical instruments and methods, electrical components, etc., and can solve the problems of inactivation, low thermal stability, and non-luminescence

Pending Publication Date: 2022-03-08
广西经正涂料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing Mn 4+ Doped fluoride red phosphors also have some disadvantages to overcome: (1) The luminous intensity is higher than that of yellow phosphors YAG:Ce 3+ The weight ratio of it to yellow light powder is as high as 2:1-3:1 during application; (2) The thermal stability is not high, and the luminous intensity is often caused by thermal quenching at the working temperature of white LEDs (about 150°C). extinguished and dropped to 70-80% of the original; (3) poor moisture resistance, in humid environment, Mn 4+ Easily hydrolyzed into opaque MnO 2 , and then rapidly deactivate without emitting light

Method used

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  • Red fluorescent powder with high luminous intensity, thermal stability and water resistance and preparation method thereof
  • Red fluorescent powder with high luminous intensity, thermal stability and water resistance and preparation method thereof
  • Red fluorescent powder with high luminous intensity, thermal stability and water resistance and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1. Preparation [K 2 SiF 6 :0.06Mn 4+ -SP], referred to as (KSF:0.06Mn 4+ -SP)

[0044] (1) Get 18.63mLHF solution (mass concentration 40%) (V HF / W K2SiF6 =0.9mL / g), 8.28gKF·2H 2 O(W KF / W K2SiF6 =0.4), 0.9482g (6mmol) KMnO 4 The powder is placed in a 200mL plastic beaker, stirred with a magnetic stirrer at normal temperature and pressure until the solid material is completely dissolved to obtain a purple solution; then 20.71g (94.0mmol) K 2 SiF 6 Powder is added in the above-mentioned solution (x=(KMnO 4 / (K 2 SiF 6 +KMnO 4 ), x=0.06), seal the mouth of the beaker with plastic wrap, stir and react at normal temperature and pressure for 40h to obtain the reactant mixture (i), and the reaction mixture (i) is filtered with absolute ethanol After washing, dry at 80°C for 3.5 hours to obtain KSF without surface modification: 0.06Mn 4+ (Sample No. (01));

[0045] (2) Add 80 mL of 20% hydrofluoric acid (mass percentage concentration) to the reaction...

Embodiment 2

[0054] Embodiment 2. preparation [K 2 SiF 6 :0.01Mn 4+ -SP], referred to as (KSF:0.01Mn 4+ -SP)

[0055] Get 20.72mLHF solution (mass concentration 40%) (V HF / W K2SiF6 =0.95mL / g), 10.90gKF·2H 2 O(W KF / W K2SiF6 =0.50), 0.1580g (1.0mmol) KMnO 4 The powder is placed in a 200mL plastic beaker, stirred with a magnetic stirrer at normal temperature and pressure until the solid material is completely dissolved to obtain a purple-red solution; then 21.72g (99.0mmol) K 2 SiF 6 Powder is added in the above-mentioned solution (x=(KMnO 4 / (K 2 SiF 6 +KMnO 4 ), x=0.01), seal the mouth of the beaker with plastic wrap, stir and react at normal temperature and pressure for 45h to obtain the reaction mixture (i);

[0056] Then add 80 mL of 20% hydrofluoric acid (mass percentage concentration) to the above-mentioned reaction mixture (i) under stirring and stir evenly, then slowly add 21.72 g of oxalic acid powder, continue stirring for 15 min after adding, and filter under reduc...

Embodiment 3

[0059] Embodiment 3. preparation [K 2 SiF 6 :0.02Mn 4+ -SP], referred to as (KSF:0.02Mn 4+ -SP)

[0060] Get 21.59mLHF solution (mass concentration 40%) (V HF / W K2SiF6 =1.00mL / g), 11.58gKF·2H 2 O(W KF / W K2SiF6 =0.60), 0.31611g (2.0mmol) KMnO 4 The powder is placed in a 200mL plastic beaker, stirred with a magnetic stirrer at normal temperature and pressure until the solid raw material is completely dissolved to obtain a purple-red solution; then 21.59g (98.0mmol) K 2 SiF 6 Powder is added in the above-mentioned solution (x=(KMnO 4 / (K 2 SiF 6 +KMnO 4 ), x=0.02), seal the mouth of the beaker with plastic wrap, stir and react at normal temperature and pressure for 50h to obtain the reaction mixture (i);

[0061] Then add 80mL of 20% hydrofluoric acid (mass percentage concentration) to the above-mentioned reaction mixture (i) under stirring and stir evenly, then slowly add 21.59g of oxalic acid powder, continue stirring for 20min after adding, and depressurize Fi...

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Abstract

The invention belongs to the field of preparation of fluorescent powder, and particularly relates to red fluorescent powder with high luminous intensity, thermal stability and water resistance and a preparation method of the red fluorescent powder, and the general formula of the combination ratio of the prepared red fluorescent powder is K2MF6: xMn < 4 + >-SP, wherein SP represents surface passivation, and M is Ti or Si; x is Mn < 4 + > doped mole fraction, and x is more than 0 and less than or equal to 0.12. According to the preparation method, materials are taken from industrial and commercial raw materials, the process is simple, preparation is carried out under the conditions of normal temperature and normal pressure, the preparation method is suitable for large-scale and industrial production, the luminous intensity of the prepared red fluorescent powder is 1.1 times that of an unpassivated control sample, the thermal stability of the red fluorescent powder is shown as follows: the integral luminous intensity at 180 DEG C is 1.70 times or above of the initial value at 30 DEG C, and the red fluorescent powder is suitable for industrial production. After being soaked in water for 6 hours, the light yellow light appearance is kept all the time, and the residual emitted light intensity is up to 88% or above.

Description

technical field [0001] The invention belongs to the field of fluorescent powder preparation, and in particular relates to a red fluorescent powder with high luminous intensity, thermal stability and water resistance and a preparation method thereof. Background technique [0002] Diodes (white LEDs) have the advantages of high luminous efficiency, energy saving, long life, low energy consumption, and environmental protection. Therefore, LEDs are regarded as a new generation of solid-state light-emitting devices. At present, the most mature and commercialized white LEDs are based on blue chip and yellow phosphor YAG:Ce 3+ Realized by the combination of yellow light phosphor YAG:Ce 3+ Absorption of the blue light emitted by the blue chip produces yellow fluorescence, which is combined with the chip's blue light to obtain white light. Because this kind of white light lacks red light components, it has disadvantages such as high color temperature and low color purity, so it is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/61C09K11/67H01L33/50
CPCC09K11/617C09K11/675C09K11/025H01L33/504
Inventor 黄映恒廖森黄毅钟雪李燕石云浩
Owner 广西经正涂料有限公司
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