Preparation method of Mn<4+> doped fluoride fluorescent powder material and method for surface modification of Mn<4+> doped fluoride fluorescent powder material

A fluoride and phosphor technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of unfavorable white LED application, instability, and large particle size.

Inactive Publication Date: 2015-11-11
BEIJING YUJI SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, manganese (Mn 4+ ) The particle size of the doped fluoride red phosphor is very large, which is not conducive to the application in white light LED
And many of these fluoride red phosphors are unstable in high-temperature, high-humidity environments

Method used

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  • Preparation method of Mn&lt;4+&gt; doped fluoride fluorescent powder material and method for surface modification of Mn&lt;4+&gt; doped fluoride fluorescent powder material
  • Preparation method of Mn&lt;4+&gt; doped fluoride fluorescent powder material and method for surface modification of Mn&lt;4+&gt; doped fluoride fluorescent powder material
  • Preparation method of Mn&lt;4+&gt; doped fluoride fluorescent powder material and method for surface modification of Mn&lt;4+&gt; doped fluoride fluorescent powder material

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preparation example Construction

[0039] In the preparation method of the present invention, by adjusting the molar ratio of the substances of each element, mainly the luminescence center Mn 4+ The doping concentration can increase the luminous intensity and internal and external quantum efficiency.

[0040] Due to these manganese (Mn 4+ ) doped fluoride red phosphors are sensitive to moisture and will degrade in a high temperature, high humidity environment, causing the brightness of these phosphor materials to decrease significantly over time. In order to prolong the light emission of the LED, the present invention coats the surface of the prepared fluoride red fluorescent powder particles with organic or inorganic materials, so that it has a protective function against moisture.

[0041] The present invention is to the prepared manganese (Mn 4+ ) doped fluoride red phosphor powder was coated with inorganic materials, and its surface was Al 2 o 3 Coating: the prepared A 2 MF 6 :Mn 4+ The crystal powde...

Embodiment 1

[0048] Preparation of K with small particle size and high brightness 2 SiF 6 :Mn 4+ Fluoride red phosphor

[0049] Weigh 30gKHF 2 , dissolved in 100ml of 40wt% hydrofluoric acid, added 1.5gKMnO 4 , after all dissolved, place the polytetrafluoroethylene beaker in an ice-salt water bath, cool to below 20°C, add 30wt% H2O dropwise after the temperature reaches the requirement 2 o 2 , stop dropping until the purple solution turns golden yellow. During the dropwise addition, a precipitate precipitates out of the solution, then filter, wash with acetone three times, put the filter cake in an oven at 100°C for 2 hours, and take out the dry filter cake after the drying is complete. Grind and crush to get golden yellow potassium hexafluoromanganate (K 2 MnF 6 ).

[0050] Weigh 10ml35wt%H 2 SiF 6 Add 60ml of 49wt% hydrofluoric acid, then add 0.6g of synthetic K 2 MnF 6 As the first solution, 4.9gKHF 2 Dissolve in 15ml of 49wt% hydrofluoric acid as the second solution. After...

Embodiment 2

[0053] Preparation of High Stability K by Atomic Layer Deposition Technology 2 SiF 6 :Mn 4+

[0054] Atomic layer deposition (ALD), also known as atomic layer deposition or atomic layer epitaxy, is a method that can coat substances layer by layer in the form of a single atomic film on the surface of a substrate.

[0055] K will be produced 2 SiF 6 :Mn 4+ The crystal powder is placed in the Φ5mm special sample cell, and then the sample cell is placed in the sample deposition chamber of the ALD deposition equipment, the window temperature is set to 185°C, the airflow speed and flow rate are controlled, and the aluminum oxide material is deposited for 48 hours. The deposition thickness is 20-30nm, the prepared sample number is KSFM-2.

[0056] The quantum efficiency was measured by Hitachi F-7000 fluorescence spectrometer, and the internal quantum efficiency was confirmed to be 75, the external quantum efficiency was 54%, and the chromaticity parameters (as shown in Table 1...

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Abstract

The invention relates to a preparation method of a Mn<4+> doped fluoride fluorescent powder material and a method for the surface modification of the Mn<4+> doped fluoride fluorescent powder material, and belongs to the field of preparation of LED fluorescent powder. The preparation method comprises the following steps: firstly, preparing A2MnF6; then, dropwise adding a second solution, obtained through dissolving fluoride or hydrofluoride of A into a hydrofluoric acid solution, into a first solution containing an HF solution, A2MnF6 and fluoride of a quadrivalent element M, and performing solid-liquid separation, so as to obtain a solid precipitation product generated after reaction. The fluorescent powder prepared by the method is small in particle size and excellent in luminous performance. The invention further provides a method for the surface modification of the Mn<4+> doped fluoride fluorescent powder particles. The surfaces of the prepared A2[MF6]:Mn<4+> fluoride red fluorescent powder particles are coated with an inorganic or organic functional material through a monoatomic deposition technology, a chemical precipitation reaction method and a surface chemical coating modification method, so that the stability of the prepared A2[MF6]:Mn<4+> fluoride red fluorescent powder particles in high-temperature and high-humidity environments is remarkably improved.

Description

technical field [0001] The present invention relates to a kind of manganese (Mn 4+ ) a method for preparing a doped fluoride phosphor material, and a method for modifying the surface of the prepared fluoride phosphor particles so that they have moisture resistance. Background technique [0002] In the 1990s, breakthroughs in blue light-emitting diode (LED) technology laid the foundation for the emergence of white LEDs. At present, there are three main methods of using LED technology to realize white light: light conversion type, multi-color combination type and multi-quantum well type. Today, the mainstream solution for solid-state lighting white LEDs is phosphor light conversion, in which high-efficiency phosphors become the key. Because phosphors determine the important characteristics and parameters of white LEDs such as light conversion efficiency, lumen efficiency, luminous flux, correlated color temperature (Tc), chromaticity coordinates, and color rendering index (R...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61C09K11/02
Inventor 权恒道张琳王超鲁路吴振雄
Owner BEIJING YUJI SCI & TECH
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