Moisture-resistant fluoride red fluorescent powder and preparation method thereof

A red phosphor, fluoride technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of reduced luminous intensity, color shift, loss, etc., and achieve the effects of improving stability, simple process and strong universality

Pending Publication Date: 2021-01-22
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] It is worth noting that Mn 4+ Fluoride-doped red phosphors tend to absorb water and deliquesce in high humidity environments, resulting in reduced or even lost luminous performance, which seriously affects the luminous performance and service life of white LEDs
Therefore, researchers have improved the moisture resistance of phosphor powder by coating organic or inorganic waterproof layer materials. Currently, the following methods are mainly reported: (1) The hydrophilic groups of amphiphilic organic compounds are chemically bonded on the surface of phosphor powder, exposing The external hydrophobic groups resist the erosion of water (Angew.Chem.Int.Ed.2015,54(37),10862-6; ACS Appl.Mater.Interfaces 2017,9(8),7232-7240; ACS Appl .Mater.Interfaces 2018,10(1),880-889); However, the organic coating layer is usually not uniform and dense, and it is easy to age under the long-term irradiation of high-power ch

Method used

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  • Moisture-resistant fluoride red fluorescent powder and preparation method thereof
  • Moisture-resistant fluoride red fluorescent powder and preparation method thereof
  • Moisture-resistant fluoride red fluorescent powder and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] In this example, Mn 4+ The chemical formula of doped fluoride red phosphor material is K 2 Ti 0.93 f 6 :0.07Mn 4+ .

[0033] The above Mn 4+ Doped Fluoride Red Phosphor K 2 Ti 0.93 f 6 :0.07Mn 4+ The preparation method, the specific process is: 3.765g KF·2H 2 O, 0.173g K 2 MnF 6 Put in the same plastic container, add 20ml 49wt% HF solution, stir until completely dissolved, then add 1.979g (NH 4 ) 2 TiF 6 , continue to stir for 0.5h, stand still, precipitate, then centrifuge to remove the supernatant, the lower sediment is washed with absolute ethanol, then centrifuged, repeatedly washed and centrifuged twice; the obtained precipitate is dried in an oven at 80 ° C to obtain the product K 2 Ti 0.93 f 6 :0.07Mn 4+ (labeled KTFM-1).

[0034] One of the above Mn 4+ The coating method of doped fluoride red phosphor powder, by Mn 4+ The red fluorescent powder doped with fluoride is coated with the alkaline earth metal fluoride waterproof layer to obtain a m...

Embodiment 2

[0041] In this example, Mn 4+ The chemical formula of doped fluoride red phosphor material is K 2 Si 0.96 f 6 :0.04Mn 4+ (labeled KSFM-3).

[0042] A preparation method of moisture-resistant fluoride red phosphor: weigh 1.823g K 2 Si 0.96 f 6 :0.04Mn 4+ (KSFM-3) Phosphor powder is placed in a plastic container, add 2mol / L KHF 2 30ml aqueous solution, fully stirred for 20min, added dropwise 1mol / L Ca(NO 3 ) 2 6ml of aqueous solution, stirred for 0.5h, left to stand, and precipitated; centrifuged to remove the supernatant, the lower layer of sediment was washed with distilled water, then centrifuged, repeatedly washed and centrifuged twice, and the precipitate was dried in an oven at 80°C to obtain a moisture-resistant fluoride red Phosphor. The chemical formula of the moisture-resistant fluoride red phosphor can be expressed as K 2 Ti 0.96 f 6 :0.04Mn 4+ @CaF 2 (labeled KSFM-4).

[0043] Phosphor powder KSFM-3, KSFM-4 in embodiment 2 are carried out X-ray diffr...

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Abstract

The invention discloses moisture-resistant fluoride red fluorescent powder, which comprises Mn<4+>-doped fluoride red fluorescent powder and an alkaline earth metal fluoride waterproof layer, whereinthe alkaline earth metal fluoride waterproof layer coats the surface of the Mn<4+>-doped fluoride red fluorescent powder; and the alkaline earth metal fluoride waterproof layer is one or a mixture ofmore than one of CaF2, SrF2 and BaF2. The preparation method comprises the steps of puttingMn<4+>-doped fluoride red fluorescent powder into a potassium bifluoride aqueous solution, fully stirring, dropwise adding an aqueous solution of alkaline-earth metal salt, standing, filtering, washing the obtained precipitate, and drying to obtain the moisture-resistant fluoride red fluorescent powder. On the basis that the luminous efficiency is not obviously reduced, the stability of the Mn<4+>-doped fluoride red fluorescent powder in a high-humidity environment is remarkably improved.

Description

technical field [0001] The invention relates to the technical field of LED phosphor preparation, in particular to a moisture-resistant fluoride red phosphor and a preparation method thereof. [0002] technical background [0003] White LED has outstanding advantages such as high efficiency, energy saving, fast response, no flicker, and long life, and is known as a new generation of green solid-state lighting source. Currently, mainstream commercial white LEDs are made of InGaN blue chips and Y 3 al 5 o 12 : Ce 3+ (YAG:Ce 3+ ) yellow fluorescent powder combination. YAG:Ce 3+ After absorbing the blue light emitted by the chip, it emits yellow light, which mixes with the unabsorbed blue light to form white light. Since YAG:Ce 3+ The lack of red light components in the spectrum makes it difficult for the light and color performance of the device (such as color temperature, color rendering index, etc.) to meet the high-quality requirements of indoor and outdoor lighting an...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/67C09K11/61
CPCC09K11/025C09K11/675C09K11/617
Inventor 张瑞方志勇
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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