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Preparation method of K2SiF6: Mn < 4 + > nano fluorescent 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 good dispersion Effect

Active Publication Date: 2021-09-07
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Preparation method of K2SiF6: Mn &lt; 4 + &gt; nano fluorescent powder
  • Preparation method of K2SiF6: Mn &lt; 4 + &gt; nano fluorescent powder
  • Preparation method of K2SiF6: Mn &lt; 4 + &gt; nano fluorescent powder

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preparation example Construction

[0029] a 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.

[0032] The...

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 preparation method of K2SiF6: Mn < 4 + > nano fluorescent powder, which belongs to the technical field of LED fluorescent powder, and comprises the following steps of: dissolving tetraethyl orthosilicate in ethanol to obtain a solution A; dissolving KF in acetic acid to obtain a solution B; dropwise adding the solution B into the solution A, fully stirring, and aging for a period of time; cleaning and drying to obtain a K2SiF6 matrix; and then dissolving K2MnF6 in a mixed solution of hydrofluoric acid and sulfuric acid, putting the prepared the K2SiF6 matrix into the mixed solution, fully stirring for a period of time, and cleaning and drying to obtain the K2SiF6: Mn < 4 + > nano fluorescent powder. The particle size of the K2SiF6: Mn < 4 + > obtained by the preparation method is 50 nm-500 nm. The experimental steps are simple and convenient, experimental equipment is simple, the yield is high, and few toxic and harmful substances are used. The obtained fluorescent powder can be effectively excited by visible light within the range of 300 nm-500 nm, has a sharp emission peak at 600-650 nm, and can be used for packaging fluorescence conversion type Mini-LED or Micro-LED devices.

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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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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