A way to improve mn 4+ Method for Humidity Resistance of Doped Fluoride Red Phosphor Powder Material

A technology of red phosphor and fluoride, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of affecting the service life and instability of white LEDs, and achieve the effect of not easy to hydrolyze, improve moisture resistance, and simple and easy to implement.

Active Publication Date: 2020-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But Mn 4+ Fluoride-doped red phosphors are unstable in high humidity environments, which affects the service life of white LEDs

Method used

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  • A way to improve mn <sup>4+</sup> Method for Humidity Resistance of Doped Fluoride Red Phosphor Powder Material
  • A way to improve mn <sup>4+</sup> Method for Humidity Resistance of Doped Fluoride Red Phosphor Powder Material
  • A way to improve mn <sup>4+</sup> Method for Humidity Resistance of Doped Fluoride Red Phosphor Powder Material

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Experimental program
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preparation example Construction

[0043] (1)A 2 MnF 6 Preparation of fluoromanganate

[0044] press A 2 MnF 6 The stoichiometric ratio of fluoromanganate is to dissolve the fluoride of A or the hydrogen fluoride of A in a hydrofluoric acid solution with a mass concentration of 49%, and add KMnO 4 , after completely dissolving, cool to below 5°C, add hydrogen peroxide solution with a mass concentration of 30.00% drop by drop until the solution turns from purple to yellow, then stop immediately, let stand, precipitate, filter, and pass the obtained yellow precipitate through acetone Wash and dry at 80°C for 2h to obtain A 2 MnF 6 Fluoromanganate;

[0045] (2) Mn 4+ Preparation of Fluoride-doped Red Phosphor

[0046] According to the Mn 4+ For the stoichiometric ratio of doped fluoride red phosphor, take the compound containing M or T element (the oxide, acid or salt of M or T element) and dissolve it in a hydrofluoric acid solution with a mass concentration of 0-60%. rejoin A 2 MnF 6 Fluoromanganate,...

Embodiment 1

[0052] K 2 TiF 6 :Mn 4+ The preparation of fluoride red fluorescent powder specifically comprises the following steps:

[0053] press K 2 TiF 6 :Mn 4+ Stoichiometric ratio, weigh 0.490ml H 2 TiF 6 Dissolve in 5ml of distilled water, add 0.062g of potassium hexafluoromanganate and react for 10 minutes; then add 0.581g of potassium fluoride and continue to stir for 30 minutes; let stand, precipitate, filter to remove the supernatant, and wash the obtained precipitate with absolute ethanol 3 times , and finally dry it in a 70°C drying oven for 2 hours, and the obtained orange-yellow powder is the final product K 2 TiF 6 :Mn 4+ Fluoride red phosphor.

[0054] Prepared sample K 2 TiF 6 :Mn 4+ The XRD diffraction pattern of the red phosphor is as follows figure 1 shown by figure 1 It can be seen that the diffraction peak of the sample is consistent with the standard card JCPDS 08-0488 (K 2 TiF 6 ) are completely consistent, and no diffraction peaks of any heterogene...

Embodiment 2

[0058] K 2 TiF 6 :Mn 4+ The preparation of fluoride red fluorescent powder and the improvement of moisture resistance performance specifically include the following steps:

[0059] press K 2 TiF 6 :Mn 4+ Stoichiometric ratio, weigh 0.40g TiO 2 Dissolve in 5ml hydrofluoric acid solution (49 wt%), stir at room temperature for 60min until completely dissolved, add 0.124g potassium hexafluoromanganate, react for 10 minutes; then add 1.16g potassium fluoride and continue stirring for 30min; stand still, precipitate , filtered to remove the supernatant, the resulting precipitate was washed 3 times with absolute ethanol, and finally dried in an oven at 80°C for 4 hours, and the obtained orange-yellow powder was the final product K 2 TiF 6 :Mn 4+ Fluoride red phosphor.

[0060] K 2 TiF 6 :Mn 4+ Fluoride red fluorescent powder is placed in ethanol solution containing 20wt% hydrogen peroxide and stirred for 1h, and the K with improved moisture resistance is obtained through ...

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Abstract

The invention discloses a method for improving moisture-proof performance of a Mn<4+> fluoride-doped red phosphor material. The method comprises the following steps: placing Mn<4+> fluoride-doped red phosphor in hydrogen peroxide solution, adequately and uniformly stirring, stewing, and filtering to obtain a sediment, washing and drying the obtained sediment, to obtain the Mn<4+> fluoride-doped red phosphor with the improved moisture-proof performance. The chemical formula of the Mn<4+> fluoride-doped red phosphor is A2M1-(i)x( / i)F6:(i)x( / i)Mn<4+>, A3T1-(i)x( / i)F6:(i)x( / i)Mn<4+> or BM1-(i)x( / i)F6:(i)x( / i)Mn<4+>. The method is simple and easy to operate, green and environmental. The cost is cheap, and the modification conditions are moderate. The method is capable of effectively improving the moisture-proof performance of the Mn<4+> fluoride-doped red phosphor material, and remarkably improving the stability of the Mn<4+> fluoride-doped red phosphor material in the high-temperature and high-humidity environments.

Description

technical field [0001] The invention relates to the technical field of phosphor material preparation for LEDs, in particular to a Mn 4+ A method for doping fluoride red phosphor material with moisture resistance. Background technique [0002] Compared with traditional lighting sources such as incandescent lamps and fluorescent lamps, white LEDs have outstanding advantages such as low heat generation, low power consumption, fast response, no flicker, and long life, and are known as a new generation of solid-state lighting sources. Currently, mainstream commercial white LEDs are composed of blue InGaN chips and yellow phosphor Y 3 al 5 o 12 : Ce 3+ (YAG:Ce 3+ ) combined, the principle is phosphor YAG:Ce 3+ After absorbing part of the blue light (440-460nm) emitted by the chip, it emits yellow light (490-550nm), which is mixed with the unabsorbed blue light to form white light. Due to the yellow phosphor YAG:Ce 3+ The lack of red light components in the spectrum leads t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67C09K11/61C09K11/62
CPCC09K11/616C09K11/628C09K11/675
Inventor 宋恩海周亚运张勤远
Owner SOUTH CHINA UNIV OF TECH
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