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Mn<4+> doping red fluorescent material for white light LED and preparation method of Mn<4+> doping red fluorescent material

A technology of red fluorescence and white light, applied in luminescent materials, chemical instruments and methods, sustainable buildings, etc., can solve the problems of difficult control of the preparation process, unsuitable for large-scale production, unsuitable for industrial production, etc., to achieve good fluorescent thermal stability, Easy to promote operation, low cost effect

Active Publication Date: 2016-04-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation method described in the patent is to dissolve the raw materials in high-concentration hydrofluoric acid, and then heat and volatilize the co-crystallization to obtain the target product. This method will produce a large amount of toxic gas HF, and the preparation process is difficult to control and is not suitable for industrial production.
Patent WO2009 / 119486 discloses another preparation method, which is to dissolve metal Si in potassium permanganate solution and react to obtain the product, but the preparation efficiency of this method is very low, and it is also not suitable for large-scale production

Method used

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  • Mn&lt;4+&gt; doping red fluorescent material for white light LED and preparation method of Mn&lt;4+&gt; doping red fluorescent material
  • Mn&lt;4+&gt; doping red fluorescent material for white light LED and preparation method of Mn&lt;4+&gt; doping red fluorescent material
  • Mn&lt;4+&gt; doping red fluorescent material for white light LED and preparation method of Mn&lt;4+&gt; doping red fluorescent material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] K 2 MnF 6Powder preparation:

[0028] At room temperature, 2.25g KMnO 4 Dissolve the powder in 150ml of 49wt% HF aqueous solution, stir evenly, add 45gKHF 2 The powder continued to stir for 40min, then cooled rapidly with ice water, and added 4ml of 49wt% H 2 o 2 Aqueous solution, when the color of the reactant solution changes from purple to brownish yellow, K 2 MnF 6 Suspension; let stand for 4h, centrifuge and wash (wash with acetone), and dry at 70°C for 6h to obtain K 2 MnF 6 Powder, spare.

Embodiment 2

[0030] Na 3 AlF 6 :0.5%Mn 4+ Preparation of fluorescent materials:

[0031] 0.00617gK 2 MnF 6 with 0.419gAlF 3 Dissolve in 10ml of hydrofluoric acid (49wt.%), stir for 10 minutes (stirring speed is 4000r / min), to obtain a transparent solution; then add 0.999g of NaOH powder to the transparent solution, continue stirring at room temperature for 30 minutes, and quickly cool to 4°C, centrifuge, wash with ethanol three times, and dry at 80°C for 7 hours to obtain Na 3 AlF 6 :0.5%Mn 4+ .

[0032] The sample glows bright red when excited by violet and blue light. The excitation spectrum of the sample consists of two broad bands at 357nm and 460nm, among which the strongest excitation band (460nm) perfectly matches the blue light emitted by the GaN blue chip, and the emission spectrum consists of six bands located at 606nm, 610nm, 620nm, 628nm, The sharp peaks at 632nm and 645nm are composed, and its color coordinates are located at: x=0.687, y=0.312, which belongs to pure ...

Embodiment 3

[0034] Na 3 AlF 6 :0.5%Mn 4+ Preparation of fluorescent materials:

[0035] 0.00617gK 2 MnF 6 with 0.419gAlF 3 Dissolved in 10ml of hydrofluoric acid (49wt.%), stirred for 10 minutes to obtain a transparent solution; then 2.649gNa 2 CO 3 Add the powder into the transparent solution, continue to stir at room temperature for 30 minutes (the stirring speed is 4000r / min), quickly cool to 4°C to obtain a light yellow precipitate, centrifuge, wash with acetone for 3 times, and dry at 80°C for 8h to obtain Na 3 AlF 6 :0.5%Mn 4+ .

[0036] The sample glows bright red when excited by violet and blue light. The excitation spectrum of the sample consists of two broad bands at 357nm and 460nm, among which the strongest excitation band (460nm) perfectly matches the blue light emitted by the GaN blue chip, and the emission spectrum consists of six bands located at 606nm, 610nm, 620nm, 628nm, The sharp peaks at 632nm and 645nm are composed, and its color coordinates are located a...

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Abstract

The invention belongs to the technical field of light-emitting materials and discloses a Mn<4+> doping red fluorescent material for a white light LED and a preparation method of the Mn<4+> doping red fluorescent material. The method comprises the following steps: 1, preparing K<2>MnF<6> powder; 2, adding the K<2>MnF<6> powder and aluminum source powder into an HF aqueous solution, and conducting stirring till the powder is dissolved completely; then adding sodium source powder, continuing stirring, cooling the mixture quickly, leaving the mixture standing still, and conducting centrifugation, washing and drying, so that the red fluorescent material is obtained. The chemical composition of the material is Na<3>AlF<6>: xMn<4+>, wherein x ranges from 0.5% to 30%. According to the Mn<4+> doping red fluorescent material and the preparation method thereof, raw materials are easy to obtain, and cost is low; the preparation method is simple, the temperature is low, the amount of used hydrofluoric acid is small, the condition is controllable, and the Mn<4+> doping red fluorescent material and the preparation method are suitable for industrialized mass production; meanwhile, the red fluorescent material has good fluorescence thermal stability.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a kind of Mn 4+ Doped red fluorescent material and preparation method thereof. Background technique [0002] Due to its unique advantages over traditional light sources, such as long life (>100,000 hours), environmental protection, high efficiency, and energy saving, white LEDs have been applied in the fields of automobiles, transportation, military affairs, and people's daily life. The realization of commercial white LED is mainly yellow phosphor Y 3 Al 5 o 12 : Ce 3+ (YAG) + Blu-ray chip combination type. Part of the blue light generated by the chip excites YAG to produce yellow light, while the remaining blue light of the chip is combined with the yellow light of the phosphor to obtain white light. This method is simple, easy to implement and has high luminous efficiency. However, the white light obtained in this way has a high color temperature (CCT>...

Claims

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Application Information

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IPC IPC(8): C09K11/64
CPCC09K11/57C09K11/645Y02B20/00
Inventor 张勤远宋恩海叶柿
Owner SOUTH CHINA UNIV OF TECH
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