Mn<4+> doped fluoride red light fluorescent powder for high color rendering and warm white light LED (Light Emitting Diode) and preparation method of Mn<4+> doped fluoride red light fluorescent powder

A technology of red fluorescent powder and warm white light, which is applied in chemical instruments and methods, luminescent materials, sustainable buildings, etc., and can solve unfavorable large-scale industrial production, low phosphor yield and light efficiency, and difficult control of the preparation process, etc. problems, to achieve the effects of easy industrial production, low equipment requirements, and mild reaction conditions

Inactive Publication Date: 2017-05-10
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, the synthesis of this type of fluoride phosphor is often obtained by dissolving the raw materials in high-concentration hydrofluoric acid, and volatilizing and co-crystallizing to obtain the target product. During the synthesis process, a large amount of toxic gas HF will be generated, the preparation process is difficult to control, and it is not suitable for industrialization. Production
And use a certain low concentration of hydrofluoric acid as a solvent to synthesize the target product through hydrothermal reaction at high temperature (120-180°C). Compared with the previous synthesis method, the amount of hydrofluoric acid used in this method is reduced, but The yield and luminous efficiency of phosphors are low, which is still not conducive to industrial mass production

Method used

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  • Mn&lt;4+&gt; doped fluoride red light fluorescent powder for high color rendering and warm white light LED (Light Emitting Diode) and preparation method of Mn&lt;4+&gt; doped fluoride red light fluorescent powder
  • Mn&lt;4+&gt; doped fluoride red light fluorescent powder for high color rendering and warm white light LED (Light Emitting Diode) and preparation method of Mn&lt;4+&gt; doped fluoride red light fluorescent powder
  • Mn&lt;4+&gt; doped fluoride red light fluorescent powder for high color rendering and warm white light LED (Light Emitting Diode) and preparation method of Mn&lt;4+&gt; doped fluoride red light fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Rb 2 ZrF 6 :xMn 4+ (1.25%≤x≤20%) Preparation of Fluoride Phosphor Powder

[0036] 0.0077g K 2 MnF 6 Powder dissolved in 1.2ml H 2 O, stirred for 5 minutes (stirring speed is 1000r / min), to obtain a yellow solution; then 0.92g RbF powder and 0.383ml H 2 ZrF 6 Aqueous solution (concentration is 45wt%) joins in the yellow solution, continues stirring rapidly at room temperature for 60 minutes (stirring speed is 1000r / min), then centrifuges wash with water 3 times (centrifugal speed is 2000r / min), bakes at 80 ℃ again Dry for 6 hours to obtain the red phosphor material Rb 2 ZrF 6 :1.25%Mn 4+ , namely sample 1.

[0037] By changing the K in the raw material 2 MnF 6 The mass of different Mn 4+ Table 1 shows the specific ratio of raw materials and the properties of the prepared phosphors for samples 2 to 5 with doping amounts.

[0038] Table 1Rb 2 ZrF 6 :xMn 4+ Raw material ratio and relative luminous intensity of red phosphor

[0039]

[0040]

[0041] ...

Embodiment 2

[0047] Rb 2 TiF 6 :xMn 4+ (1.25%≤x≤20%) Preparation of Fluoride Phosphor Powder

[0048] 0.0077g K 2 MnF 6 Powder dissolved in 1.5ml H 2 O, stirred for 5 minutes (stirring speed is 1000r / min), to obtain a yellow solution; then 1.306g RbF powder and 0.245ml H 2 TiF 6 Aqueous solution (concentration: 50wt%) was added to the yellow solution, continued stirring at room temperature for 60 minutes (stirring speed was 1000r / min), then centrifugally washed with water for 3 times (centrifugal speed was 2000r / min), and then dried at 80°C 6h, get the red phosphor material Rb 2 TiF 6 :1.25%Mn 4+ , namely sample 6.

[0049] By changing the K in the raw material 2 MnF 6 The mass of different Mn 4+ Table 2 shows the specific ratio of raw materials and the properties of prepared phosphors for samples 7-10 with doping amount.

[0050] Table 2Rb 2 TiF 6 :xMn 4+ Raw material ratio and relative luminous intensity of red phosphor

[0051]

[0052] It can be seen from Table 2 t...

Embodiment 3

[0057] Rb 2 TiF 6 :10%Mn 4+ Encapsulated LED

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Abstract

The invention discloses Mn<4+> doped fluoride red light fluorescent powder for a high color rendering and warm white light LED (Light Emitting Diode) and a preparation method of the Mn<4+> doped fluoride red light fluorescent powder. The chemical composition of a fluorescent powder material is Rb2AF6:xMn<4+>, wherein A is Zr or Ti, x is the mol percentage coefficient of Mn<4+> doped ions relative to the A, and the x is greater than or equal to 1.25 percent and smaller than or equal to 20 percent. The fluorescent powder material has the effects of broadband absorption and narrowband emission, and can be used for packaging a high-quality LED. The preparation method comprises the following steps: at room temperature, adding K2MnF6 powder into water, and stirring until the power is completely dissolved; then adding RbF powder and H2AF6 aqueous solution, continuously stirring until the substances are dissolved, centrifuging, washing and drying to obtain an orange-yellow sediment, namely the Mn<4+> doped fluoride red light fluorescent powder for the high color rendering and warm white light LED. The preparation method disclosed by the invention has the advantages of simplicity and convenience in operation, greenness, environment friendliness, mild reaction conditions, high efficiency, quickness and suitability for industrial large-scale production.

Description

technical field [0001] The invention relates to the technical field of white light LED phosphor preparation, in particular to a Mn 4+ Doped high color rendering LED fluoride red fluorescent material and preparation method thereof. Background technique [0002] White light diodes (WLEDs) are widely used in transportation, medical equipment, military, display screens and daily life due to their energy saving, environmental protection and long service life. At present, commercial white LEDs are mainly realized by the combination of blue GaN chips (440-480nm) and YAG:Ce. This synthesis method is relatively simple and mature, but due to the lack of red components, the color temperature is high (CCT>4500K), and the color rendering index is relatively high. Lower (Ra﹤80). In order to further improve LED light efficiency, it is often necessary to add some red phosphors, such as MASiN 3 :Eu 2+ (M=Ca, Sr) and the like. Rare earth elements have rich electronic energy level tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/67
CPCC09K11/675Y02B20/00
Inventor 宋恩海王玲燕张勤远叶柿
Owner SOUTH CHINA UNIV OF TECH
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