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a mn 4+ Preparation method of ion-activated fluoride phosphor

A fluorescent powder and fluoride technology, which is applied in the field of preparation of fluoride fluorescent powder, can solve the problems of difficult control of the preparation process, unsuitability for industrial production, and volatilization of hydrogen fluoride gas, and achieve the goals of short time consumption, convenient synthesis, and reduced dosage requirements Effect

Active Publication Date: 2020-08-28
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Much research work has been done on this, patent WO 2007 / 100824 discloses that Mn 4+ Activated A 2 MF 6 (A is K, Na, Rb, etc.; M is Ti, Si, Sn, Ge, etc.) red fluorescent powder; its preparation method is to dissolve the raw materials in high-concentration hydrofluoric acid, and then heat and volatilize to dryness. A large amount of toxic hydrogen fluoride gas volatilizes during the preparation process, and the preparation process is difficult to control, so it is not suitable for industrial production; the preparation method disclosed in the patent CN 102732249 A is to combine the first solution of fluoride containing tetravalent metal M with the first solution containing alkali metal A The second solution or the compound of A in solid form is mixed, and after the reaction, a precipitate is formed to obtain the product, but this preparation method needs to control the concentration of the two solutions, the speed of mixing, the temperature and other factors, and it is difficult to obtain a compound with better luminous efficiency. product

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  • a mn <sup>4+</sup> Preparation method of ion-activated fluoride phosphor
  • a mn <sup>4+</sup> Preparation method of ion-activated fluoride phosphor
  • a mn <sup>4+</sup> Preparation method of ion-activated fluoride phosphor

Examples

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Effect test

Embodiment 1

[0044] Example 1: K 2 MnF 6 preparation of

[0045] Prepare K according to the method described in the literature Angew. 2 MnF 6 crystals.

[0046] 0.45g KMnO 4 and 9g KHF 2 Dissolve in 30mL hydrofluoric acid (49%), stir for 20 minutes, then gradually drop into about 1.2mL hydrogen peroxide (30wt.%), gradually form a yellow precipitate in the solution, filter the solution to obtain the precipitate, wash with acetone Bake at 60°C for 2 hours to get K 2 MnF 6 .

Embodiment 2

[0047] Example 2: K 2 NaAlF 6 :Mn 4+ Preparation of Fluoride Phosphor Powder

[0048] The K prepared by 0.00741g embodiment 1 2 MnF 6 , 0.8197g NaAlO 2 , 0.1182g KHF 2 Dissolve in 10mL of hydrofluoric acid (49wt.%) solution, stir for 5 minutes to fully dissolve, then add 10mL of precipitant methanol dropwise at a rate of 0.2 mL / s, after all 10mL of methanol has been added dropwise, continue stirring at room temperature For 5 minutes, stop stirring to take out the precipitate, centrifuge, wash twice with acetone, and dry at 60°C in an air atmosphere to obtain the product K 2 NaAlF 6 :Mn 4+ Fluoride phosphor.

[0049] figure 1 for K 2 NaAlF 6 :Mn 4+ X-ray powder diffraction pattern of fluoride phosphor, indicating that the synthesized product is a square phase K 2 NaAlF 6 ; figure 2 for K 2 NaAlF 6 :Mn 4+ Scanning electron microscope image of fluoride phosphor powder, it can be seen that the particle size of the powder is about 1 μm; image 3 for K 2 NaAlF ...

Embodiment 3

[0051] Example 3: K 2 TiF 6 :Mn 4+ Preparation of Fluoride Phosphor Powder

[0052] The K prepared by 0.00741g embodiment 1 2 MnF 6 , 0.2401g K 2 TiF 6 Dissolve in 10mL of hydrofluoric acid (49wt.%) solution, stir for 5 minutes to fully dissolve, then add 10mL of precipitant methanol dropwise at a rate of 0.2mL / s, after all 10mL of methanol has been added dropwise, continue stirring at room temperature For 5 minutes, stop stirring to take out the precipitate, centrifuge, wash twice with acetone, and dry at 60°C in an air atmosphere to obtain the product K 2 TiF 6 :Mn 4+ Fluoride red phosphor.

[0053] Figure 4 for K 2 TiF 6 :Mn 4+ X-ray powder diffraction pattern of fluoride phosphor, indicating that the synthesized product is a hexagonal phase K 2 TiF 6 ; Figure 5 for K 2 TiF 6 :Mn 4+ Scanning electron microscope image of fluoride phosphor powder, the powder particle size is about 10 μm; Figure 6 for K 2 TiF 6 :Mn 4+ Excitation and emission spectra o...

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Abstract

The invention provides a preparation method of Mn<4+>-activated fluoride fluorescent powder. The preparation method provided by the invention does not need to form a saturated solution of A2MF6, so that the requirement of the use amount of raw materials is greatly reduced; in the preparation process, the target product can be synthesized at room temperature and is convenient to synthesize; a precipitating agent is added, so that the preparation is more convenient, the operation is simpler, the synthetic steps are simplified, and the prepared fluorescent powder has better optical properties; the fluoride fluorescent powder can be well excited by ultraviolet light to blue light, especially the blue light, and has strong red light emission, wherein the red light emission peak is in the wavelength range from 600 to 650 nm; the method has the advantages of a simple preparation process and short consumed time; and the prepared material has a high luminescence quantum yield and is suitable for industrial large-scale preparation.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a Mn 4+ Preparation method of ion-activated fluoride phosphor. Background technique [0002] In recent decades, White Light-Emitting Diode (WLED for short) has attracted great attention due to its advantages of energy saving, environmental protection, and long life, and has gradually replaced traditional incandescent and fluorescent lamps. At present, the most common method for preparing WLEDs on the market is to combine blue GaN chips with yellow YAG:Ce 3+ Phosphor powder is combined, wherein the yellow light phosphor absorbs part of the blue light emitted by the GaN chip and emits yellow light, which is mixed with the unabsorbed blue light to form white light. Due to the lack of red light components in the emission spectrum of the yellow phosphor, the WLED prepared by this method is a cool white light device, and its correlated color temperature (Correlated Colo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67C09K11/61C09K11/66C09K11/64C09K11/85C09K11/62
CPCC09K11/616C09K11/628C09K11/645C09K11/665C09K11/675C09K11/772
Inventor 朱浩淼易小东陈学元
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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