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a k 2 sif 6 :mn 4+ Preparation method of nano phosphor powder

A nano-fluorescent powder and matrix technology, applied in chemical instruments and methods, luminescent materials, etc., can solve problems such as failure to meet application requirements, environmental and personnel damage, etc., and achieve increased luminous intensity, increased nucleation rate, and improved absorption rate Effect

Active Publication Date: 2022-04-12
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

While the commercially available K 2 SiF 6 :Mn 4+ The single particle size of powder is usually >30μm, which cannot meet the application requirements
And the prior art prepares K 2 SiF 6 :Mn 4+ Phosphor powder usually must use a large amount of highly toxic hydrofluoric acid as a solvent, causing huge damage to the environment and personnel

Method used

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  • a k <sub>2</sub> sif <sub>6</sub> :mn <sup>4+</sup> Preparation method of nano phosphor powder
  • a k <sub>2</sub> sif <sub>6</sub> :mn <sup>4+</sup> Preparation method of nano phosphor powder
  • a k <sub>2</sub> sif <sub>6</sub> :mn <sup>4+</sup> Preparation method of nano phosphor powder

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preparation example Construction

[0029] a kind of K 2 SiF 6 :Mn 4+ The preparation method of nanometer phosphor body, comprises the following steps:

[0030] (1) Weigh tetraethyl orthosilicate and surfactant and dissolve in commercially pure ethanol, and after fully stirring, A liquid is obtained. Among them, the molar concentration of tetraethyl orthosilicate dissolved in ethanol is 0.042mmol / ml~0.256mmol / ml, and the mass concentration of surfactant dissolved in ethanol should not be greater than 0.003g / ml.

[0031] It should be noted that the added surfactant can make K 2 SiF 6 :Mn 4+ Changes in the morphology of powder particles will also affect the uniformity, dispersion and particle size of the particles. It should be understood that the addition of surfactant is not necessary. However, surfactants can be added, depending on the properties of different surfactants, for K 2 SiF 6 : Mn 4+ The morphology, uniformity, dispersion and particle size of powder particles will have different effects.

[0...

Embodiment 1

[0047] Weigh 1.55g of tetraethyl orthosilicate and 0.1g of polyvinylpyrrolidone, dissolve them in 30ml of absolute ethanol, put them in a water bath at 0°C, and the obtained solution is called solution A. Weigh 2.16g of KF and dissolve it in 15ml of pure acetic acid, put it in a water bath at 0°C, and call it solution B. Using a syringe that can control the titration rate, drop solution A into solution B that is stirred at 600 r / min at a rate of 2 ml / min. After the solution is completely dripped, continue to stir and age for 10 minutes. The obtained precipitate was washed three times with ethanol. Put the obtained precipitate into a freeze-drying box for 12 hours to obtain nano-K 2 SiF 6 powder.

[0048] After the hydrofluoric acid (49wt%) of 10ml is mixed with the sulfuric acid (49wt%) of 5ml, add the K of 0.17g 2 MnF 6 , stirred for 10 minutes to fully dissolve it. Weigh the K of the small particle size obtained by the above steps 2 SiF 6 1.5g of powder was added in...

Embodiment 2

[0050] Weigh 1.6 g of tetraethyl orthosilicate and 0.1 g of polyethylene glycol, dissolve in 30 ml of absolute ethanol, and place in a water bath at 30° C. The resulting solution is called solution A. Weigh 1.5g of KF and dissolve it in 15ml of pure acetic acid in a 30°C water bath, called solution B. Using a syringe that can control the titration rate, drop solution A into solution B that is stirred at 600 r / min at a rate of 2 ml / min. After the solution is completely dripped, continue to stir and age for 30 minutes. The obtained precipitate was washed three times with ethanol. Put the obtained precipitate into a freeze-drying box for 12 hours to obtain nano-K 2 SiF 6 powder.

[0051] After the hydrofluoric acid (49wt%) of 10ml is mixed with the sulfuric acid (50wt%) of 5ml, add the K of 0.17g 2 MnF 6 , stirred for 10 minutes to fully dissolve it. Weigh the K of the small particle size obtained by the above steps 2 SiF 6 1.5g of powder was added into the solution, and...

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Abstract

The invention discloses a K 2 SiF 6 :Mn 4+ The preparation method of nano fluorescent powder belongs to the technical field of LED fluorescent powder, and comprises the following steps: dissolving tetraethyl orthosilicate in ethanol to obtain A solution; dissolving KF in acetic acid to obtain B solution; adding B solution dropwise to In solution A, aging for a period of time after full stirring. K was obtained after washing and drying 2 SiF 6 matrix. Then K 2 MnF 6 Dissolved in the mixed solution of hydrofluoric acid and sulfuric acid, the prepared K 2 SiF 6 Put the matrix into it, stir it well for a period of time, and get K after cleaning and drying 2 SiF 6 :Mn 4+ Nano phosphor powder. The K obtained by the preparation method of the present invention 2 SiF 6 :Mn 4+ The particle size is 50nm~500nm, the experimental steps are simple, the experimental equipment is simple, the output is high, and the use of less toxic and harmful substances is used. The obtained phosphor can be effectively excited by visible light in the range of 300nm~500nm, and has a sharp emission peak at 600~650nm. , which can be used for phosphor-conversion Mini-LED or Micro-LED device packaging.

Description

technical field [0001] The invention belongs to the technical field of LED phosphor powder and relates to a K 2 SiF 6 :Mn 4+ The preparation method of the nano fluorescent powder. Background technique [0002] The way to obtain white light directly by coating yellow phosphor powder on the blue light chip is currently the most widely used white light LED realization method. However, due to the lack of red components in the spectrum, the color temperature is high (>6000K) and the color rendering index is poor (<75). Therefore, red phosphor powder is usually added to the LED to improve its luminous performance. K 2 SiF 6 :Mn 4+ It is the most widely used red phosphor with excellent performance. Its absorption spectrum has two broad peaks at 350nm and 450nm, covering the entire blue light region, which can well match blue light chips; its emission spectrum is between 600nm and 650nm There are multiple sharp emission peaks between them, the intensity is high and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/61
CPCC09K11/616
Inventor 邵起越王易围姚乐琪邢俊杰董岩蒋建清
Owner SOUTHEAST UNIV
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