Oleylamine oleic acid modified tetravalent manganese doped fluoride red-light-emitting material and preparation method thereof

A technology of oleylamine oleic acid and tetravalent manganese, which is applied in the field of fluorescent materials, can solve the problems of slow response speed of devices, long fluorescence life, poor stability, etc. Effect

Pending Publication Date: 2021-11-02
CHINA JILIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, due to the Mn 4+ The red light emission of doped all-inorganic fluoride material is 2Eg→4Ag transition, which has the characteristics of double prohibition of

Method used

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  • Oleylamine oleic acid modified tetravalent manganese doped fluoride red-light-emitting material and preparation method thereof
  • Oleylamine oleic acid modified tetravalent manganese doped fluoride red-light-emitting material and preparation method thereof
  • Oleylamine oleic acid modified tetravalent manganese doped fluoride red-light-emitting material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (a) Prepare K by precipitation method 2 MnF 6

[0031] 0.2g KMnO 4 and 4.5g KHF 2 Dissolve in 15 mL HF (48%), stir it for 60 min, then add 0.5 mL hydrogen peroxide dropwise to precipitate a yellow powder K 2 MnF 6 , the precipitate K 2 MnF 6 Filter and clean with acetone and then dry in a vacuum oven for 5 hours;

[0032] (b) Preparation of [N(CH 3 ) 4 ] 2 TiF 6 :Mn 4+ (OA,OC)

[0033] According to the stoichiometric ratio of 1:2, weigh 1.63g of fluorotitanic acid and 1.86g of tetramethylammonium fluoride into a polytetrafluoroethylene beaker, and place the beaker on a magnetic stirring instrument at a speed of 500 rpm. Stir for 30 minutes. Then add oleylamine oleic acid (1mL+0.5mL) according to the stoichiometric ratio of 2:1 and continue to stir for 30 minutes, then dry 0.12g K 2 MnF 6 Dissolved in 10ml HF (48%). The dissolved K 2 MnF6 Slowly add dropwise to the beaker containing fluorotitanic acid and tetramethylammonium fluoride, and continue to st...

Embodiment 2

[0041] (a) Prepare K by precipitation method 2 MnF 6

[0042] 0.2g KMnO 4 and 4.5g KHF 2 Dissolve in 15 mL HF (48%), stir it for 60 min, then add 0.5 mL hydrogen peroxide dropwise to precipitate a yellow powder K 2 MnF 6 , the precipitate K 2 MnF 6 Filter and clean with acetone and then dry in a vacuum oven for 5 hours;

[0043] (b) Preparation of [N(CH 3 ) 4 ] 2 ZrF 6 :Mn 4+ (OA,OC)

[0044] According to the stoichiometric ratio of 1:2, weigh 2.54g of fluorozirconic acid and 1.86g of tetramethylammonium fluoride into a polytetrafluoroethylene beaker, and place the beaker on a magnetic stirring instrument at a speed of 500 rpm. Stir for 30 minutes. Then add oleylamine oleic acid (1mL+0.5mL) according to the stoichiometric ratio of 2:1 and continue to stir for 30 minutes, then dry 0.12g K 2 MnF 6 Dissolved in 10ml HF (48%). The dissolved K 2 MnF 6 Slowly add dropwise to the beaker containing fluozirconic acid and tetramethylammonium fluoride, and continue to ...

Embodiment 3

[0047] (a) Prepare K by precipitation method 2 MnF 6

[0048] 0.2g KMnO 4 and 4.5g KHF 2 Dissolve in 15 mL HF (48%), stir it for 60 min, then add 0.5 mL hydrogen peroxide dropwise to precipitate a yellow powder K 2 MnF 6 , the precipitate K 2 MnF 6 Filter and clean with acetone and then dry in a vacuum oven for 5 hours;

[0049] (b) Preparation of [N(CH 3 ) 4 ] 2 SiF 6 :Mn 4+ (OA,OC)

[0050] According to the stoichiometric ratio of 1:2, weigh 1.91 g of fluorosilicic acid and 1.86 g of tetramethylammonium fluoride in a polytetrafluoroethylene beaker, and place the beaker on a magnetic stirring instrument at a speed of 500 rpm for vigorous stirring 30 minutes. Then add oleylamine oleic acid (1mL+0.5mL) according to the stoichiometric ratio of 2:1 and continue to stir for 30 minutes, then dry 0.12g K 2 MnF 6 Dissolved in 10ml HF (48%). The dissolved K 2 MnF 6 Slowly add dropwise to the beaker containing fluosilicic acid and tetramethylammonium fluoride, and co...

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Abstract

The invention discloses an oleylamine oleic acid modified tetravalent manganese doped fluoride red-light-emitting material and a preparation method thereof. The material takes organic amine metal fluoride as a matrix, tetravalent manganese ions Mn < 4 + > as an activating agent and oleic acid oleylamine as a ligand, the chemical composition is A2B1-xF6: xMn < 4 + > (OA, OC), the value of x is 0.1%-5%, A is rigid symmetric-asymmetric structure organic fluoride salt, and B is Ti < 4 + >, Si < 4 + >, Zr < 4 + >, Ge < 4 + > and Sn < 4 + >; through excitation of a blue light lamp, the fluorescent powder emits bright red light, the luminous intensity is high, and the fluorescent powder has good stability and moisture resistance. The preparation method adopted in the invention is simple, the obtained product is stable in quality, the red light missing part of the commercial cold white light LED can be supplemented, the color rendering index of the commercial cold white light LED can be improved, the moisture resistance of the fluorescent material is greatly improved and the packaging difficulty is reduced through combination with ligands such as oleic acid oleylamine, and the method is suitable for large-scale production.

Description

technical field [0001] The invention relates to a red fluorescent luminescent material and its preparation method and application, in particular to a luminescent material coated with oleylamine oleic acid with excellent moisture-proof performance, which belongs to the technical field of fluorescent materials. Background technique [0002] Since the 1990s, white LED lighting technology has been widely used in people's daily life after the blue LED based on gallium nitride (GaN) was invented. White LED has high brightness, good stability and low power consumption. , is considered a green lighting technology. White light LEDs are usually formed by two methods. The first is to use "blue light technology" to cooperate with phosphors to form white light; the second is to mix multiple monochromatic lights. Both approaches have successfully produced white light devices. At present, large-scale commercial white LEDs are cool white LEDs based on blue chips exciting yellow phosphor Y...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/67C09K11/61
CPCC09K11/02C09K11/674C09K11/617Y02B20/00
Inventor 徐天侔蔡培庆万明杰许学森刘祖刚
Owner CHINA JILIANG UNIV
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