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Preparation method of manganese-doped fluoride luminescent material controllable in morphology and particle size

A technology of luminescent materials and manganese doping, which is applied in the direction of luminescent materials, chemical instruments and methods, etc. It can solve problems such as difficult to achieve continuous production in large quantities, volatilization of HF, and difficulty in controlling the shape of product particles.

Active Publication Date: 2017-01-11
BEIJING YUJI SCI & TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

mn 4+ Doped A 2 MF 6 Among fluoride luminescent materials, patent WO2012 / 128837 reported about A 2 MF 6 :Mn 4+ Methods such as multi-temperature crystallization and isothermal crystallization are used in the synthesis method. In this method, a solution with a high concentration of HF will be used, and the synthesis process will cause HF to volatilize, the operation safety is low, and high-concentration hydrogen fluoride is very harmful and difficult to handle. The particle shape of the product is difficult to control, and it is difficult to achieve continuous production in large quantities;

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  • Preparation method of manganese-doped fluoride luminescent material controllable in morphology and particle size
  • Preparation method of manganese-doped fluoride luminescent material controllable in morphology and particle size
  • Preparation method of manganese-doped fluoride luminescent material controllable in morphology and particle size

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preparation example Construction

[0046] Preparation of tetravalent manganese ions: Weigh the required hydrofluoric acid solution with a graduated cylinder, and weigh the calculated amount of fluoride containing A and KMnO 4 Make it slowly dissolve in the hydrofluoric acid solution, control the reaction temperature to be less than 20°C, slowly add 30wt% H 2 o 2 Solution, when the color of the bottom solution starts to change from purple to golden yellow, stop adding H 2 o 2 , adopt the solid-liquid separation method to extract the required precipitate, and obtain the yellow powder K containing tetravalent manganese ions 2 MnF 6 ;

[0047] The first step is to prepare the original crystal of manganese-doped fluoride luminescent material with a particle size of 2 MnF 6 Dissolved in hydrofluoric acid as the bottom liquid, control the synthesis temperature. The compound containing M and or N is weighed and dissolved in an appropriate amount of hydrofluoric acid as a drop solution. Stir the bottom liquid and...

Embodiment 1

[0057] Two-step preparation of spherical K with controllable morphology and particle size 2 Ge 0.95 f 6 : 0.05 mn 4+ Fluoride red luminescent material

[0058] In a polytetrafluoro beaker, weigh 100ml of 40wt% hydrofluoric acid solution in a polytetrafluoro beaker with a measuring cylinder, and weigh 30.00gKHF 2 and 1.50 g KMnO 4 It is slowly dissolved in hydrofluoric acid solution, and the temperature is controlled within the range of 25-30°C. Place the polytetrafluoro beaker in the water bath of the cooler and start to cool down to below 20°C, slowly add 30wt% H 2 o 2 Solution, the color of the bottom solution starts to change from purple to golden yellow, stop adding H 2 o 2 , after a stable reaction for 15 minutes, filter with suction, rinse with a small volume of acetone three times, put the filter cake in an oven and dry at 100°C for 2 hours, break it through a 100-mesh sieve at room temperature, and obtain K 2 MnF 6 Yellow powder ready for use;

[0059] Accu...

Embodiment 2

[0065] Two-step preparation of spherical K with controllable morphology and particle size 2 Ti 0.95 f 6 : 0.05 mn 4+ Fluoride red luminescent material

[0066] Accurately weigh 10ml of 49wt% HF solution and place it in a Teflon beaker, weigh 5.00g of KHF 2 and 0.16g K 2 MnF 6 Dissolve in hydrofluoric acid and control the temperature to 25°C as the reaction bottom solution. Weigh 1.00g TiO2 2 Dissolve in 5ml of 49wt% HF as a drop solution, control the temperature of the drop solution to 25°C, stir the bottom solution, add the drop solution dropwise to the bottom solution, and stir for 30 minutes after the dropwise addition. The color of the reaction bottom solution gradually changed from initial golden yellow to light, and precipitates were precipitated during the process. Suction filter the bottom liquid of the reaction, rinse it with a small volume of acetone three times, then place it in an oven at 100°C and dry it for 2 hours, take out the dry cake and crush it thr...

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Abstract

The invention relates to a preparation method of a manganese-doped fluoride luminescent material controllable in morphology and particle size, and belongs to the field of preparation of LED luminescent materials. The method is mainly characterized in that the manganese-doped fluoride luminescent material Ax(M1-zNw)Fy:Mn4+ uniform in morphology and controllable in particle size can be prepared through two-step synthesis. The two-step synthesis is characterized in that firstly, a liquid phase synthesis mode is adopted to prepare a manganese-doped fluoride luminescent material raw crystal with the particle size smaller than 10 micrometers; secondly, the raw crystal is put into the reaction solution in the first step, the saturability and the proportion are controlled to control the growth amount of a secondary crystal, and the sphere-like product controllable in particle size and uniform in morphology is obtained. By carrying out surface treatment on the manganese-doped fluoride luminescent material with organosilicone, the stability performance of the manganese-doped fluoride luminescent material in a high-temperature and high-humidity environment is improved.

Description

technical field [0001] The invention relates to a tetravalent manganese (Mn 4+ ) doped fluoride luminescent material, the main feature of which is that a spherical manganese-doped fluoride luminescent material with uniform appearance, controllable particle size and high stability can be prepared through two-step synthesis, which belongs to the field of functional materials. Background technique [0002] In the mid-1990s, humans broke through the key technology of manufacturing blue light-emitting diodes (LEDs), and developed a technology that uses blue light to excite yellow light-emitting materials to mix and synthesize white light; semiconductor lighting is environmentally friendly, energy-saving and efficient, and simple in structure. It is known as the fourth-generation lighting source after incandescent lamps, fluorescent lamps and energy-saving lamps due to its small size and other advantages; today's white LED lighting has been widely used in many fields such as gener...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/61C09K11/66C09K11/67
CPCC09K11/025C09K11/616C09K11/665C09K11/675
Inventor 王超张琳毛建解荣军
Owner BEIJING YUJI SCI & TECH
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