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Green synthesis method of tetravalent manganese ion activated fluoride red luminescent material

A technology of red luminescence and green synthesis, which is applied in the direction of luminescent materials, chemical instruments and methods, semiconductor devices, etc., can solve the problems of unfavorable mass industrial production, insufficient synthesis conditions, long synthesis cycle, etc., and achieve the convenience of mass industry The effect of chemical preparation, large-scale production and fast synthesis speed

Pending Publication Date: 2022-04-22
INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Existing preparation of Mn 4+ Common methods to activate fluoride red luminescent materials include coprecipitation method, etching method, cation exchange method, hydrothermal method and microwave irradiation method, etc., but these methods will use a large amount of hydrofluoric acid in the synthesis process, so it is inevitable Lead to environmental pollution and safety problems, and have high requirements for equipment, which is not conducive to mass industrial production
Some researchers also reported the synthesis of Mn without using hydrofluoric acid. 4+ Activate the fluoride red powder material (Chem.Mater.2016,28(5),1495-1502), but its synthesis conditions are not mild enough (180°C, vacuum drying, etc.), the yield is low (hydrothermal method) and the synthesis cycle is long, which is not conducive to large-scale production

Method used

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  • Green synthesis method of tetravalent manganese ion activated fluoride red luminescent material
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  • Green synthesis method of tetravalent manganese ion activated fluoride red luminescent material

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Embodiment 1

[0029] At room temperature, weigh potassium hexafluoromanganate (K 2 MnF 6 )0.0148g, completely dissolved in fluosilicic acid (H 2SiF 6 , 30wt%) solution to obtain solution 1, the molar concentration of potassium hexafluoromanganate in solution 1 is 0.025mol / L, take potassium fluoride (KF) 0.3486g and dissolve in deionized water completely to obtain solution 2, in solution 2 The molar concentration of potassium fluoride is 0.6mol / L, solution 1 and solution 2 are mixed and stirred for 5 minutes to obtain solution 3, the mol ratio of potassium fluoride and potassium hexafluoromanganate in solution 3 is 100.17:1, solution 3 The precipitate was obtained by centrifugation, washed 3 times with ethanol, and then dried at 75°C for 2 hours to obtain the final product red luminescent material K 2 Si 0.99 mn 0.01 f 6 .

[0030] Detect the obtained red luminescent material, such as figure 1 , Figure 5 and Figure 6 shown. Such as figure 1 As shown, the prepared sample is a pu...

Embodiment 2

[0032] At room temperature, weigh potassium hexafluoromanganate (K 2 MnF 6 )0.0445g, completely dissolved in fluosilicic acid (H 2 SiF 6 , 30wt%) solution to obtain solution 1, the molar concentration of potassium hexafluoromanganate in solution 1 is 0.076mol / L, and potassium hydrogen fluoride (KHF 2 ) 2.3430g is completely dissolved in deionized water to obtain solution 2, the molar concentration of potassium bifluoride in solution 2 is 3mol / L, solution 1 and solution 2 are mixed and stirred for 10 minutes to obtain solution 3, potassium bifluoride and six The molar ratio of potassium fluoromanganate is 166.58:1. The solution in the above steps is centrifuged to obtain a precipitate, washed 3 times with ethanol, and then dried at 75°C for 2 hours to obtain the final product red luminescent material K 2 Si 0.97 mn 0.03 f 6 .

Embodiment 3

[0034] At room temperature, weigh potassium hexafluoromanganate (K 2 MnF 6 )0.0148g, completely dissolved in fluorotitanic acid (H 2 TiF 6 , 50wt%) solution to obtain solution 1, the molar concentration of potassium hexafluoromanganate in solution 1 is 0.051mol / L, and potassium bifluoride (KHF 2 ) 0.9372g, be completely dissolved in deionized water to obtain solution 2, the molar concentration of potassium bifluoride in solution 2 is 1.2mol / L, solution 1 and solution 2 are mixed and stirred for 10 minutes to obtain solution 3, potassium bifluoride in solution 3 The molar ratio to potassium hexafluoromanganate is 200.35:1. Centrifuge the solution in the above steps to obtain a precipitate, wash with ethanol three times, and then dry at 75°C for 2 hours to obtain the final product red luminescent material K 2 Ti 0.99 mn 0.01 f 6 .

[0035] Detect the obtained red luminescent material, such as figure 2 As shown, the prepared samples were pure phase.

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Abstract

The invention discloses a green synthesis method of a tetravalent manganese ion activated fluoride red luminescent material. The synthesis method comprises the following steps: adding potassium hexafluoromanganate into a fluosilicic acid solution or a fluotitanic acid solution until the potassium hexafluoromanganate is completely dissolved to obtain a solution 1, adding potassium fluoride, potassium bifluoride or barium chloride into water until the potassium fluoride, potassium bifluoride or barium chloride is completely dissolved to obtain a solution 2, the molar concentration of the potassium fluoride, potassium bifluoride or barium chloride in the solution 2 is 0.25-3.00 mol / L, and stirring to obtain a solution 3; mixing and stirring the solution 1 and the solution 2 to obtain a solution 3, centrifuging the solution 3 to obtain a precipitate, and washing and drying the precipitate to obtain a final product, namely the tetravalent manganese ion activated fluoride red luminescent material. The synthesis method provided by the invention has the advantages of greenness, environmental protection (no hydrofluoric acid), mild conditions (normal temperature, normal pressure and aqueous solution reaction), high synthesis speed (several minutes) and the like, and is convenient for large-scale industrial preparation.

Description

technical field [0001] The invention belongs to the technical field of inorganic luminescent materials, and in particular relates to a green synthesis method of fluoride red luminescent materials activated by tetravalent manganese ions. Background technique [0002] Compared with traditional incandescent lamps and halogen lamps, white LEDs have better color saturation and reproducibility in terms of color vision. The current commercial white LEDs are composed of blue LED chips and Y 3 al 5 o 12 : Ce 3+ Assembled with (YAG:Ce) yellow phosphor powder, because YAG:Ce-based white light LED emits cool white light, its color rendering index is low (CRI<80) and color temperature is high (CCT=4000-8000K), so limit its further application. The low CRI is caused by the lack of red light in the yellow phosphor. This problem has also attracted extensive attention from researchers. In recent years, many researchers have improved the color rendering index of white LEDs by inventing...

Claims

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Application Information

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IPC IPC(8): C09K11/61C09K11/67H01L33/50
CPCC09K11/617C09K11/675H01L33/502
Inventor 周建邦霍见生朱用洋林利添丁建红倪海勇
Owner INST OF RESOURCES UTILIZATION & RARE EARTH DEV GUANGDONG ACAD OF SCI
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