Method for synthesizing rare-earth metal codoped yttrium potassium pentafluoride nano crystal from waste fluorescent powder

A rare earth metal and yttrium potassium pentafluoride technology, which is applied in the field of solid waste resource utilization, can solve the problems of insufficient luminescence performance of rare earth fluorescent up-conversion materials, insufficient uniform dispersion, large nanocrystalline size, etc., and achieves good down-conversion. The effect of luminous performance, good luminous performance and simple process flow

Inactive Publication Date: 2015-08-26
WUHAN UNIV OF TECH
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Problems solved by technology

[0006] CN104388087A discloses a method for preparing rare-earth fluorescent up-conversion materials with waste fluorescent powder. The method adopts ammonia precipitation and liquid separation-oxalic acid secondary precipitation process for rare earth leaching, but for extremely small amounts of elements such as lead and zinc in waste fluorescent powder Fail to effectively remove; meanwhile, CN104388087A adopts the mixture of anhydrous yttrium chloride and anhydrous europium chloride, MOH solid and MHF2 fine powder and RmF3 or RmCl3 solids are mixed in all solid phases, and the reaction is carried out, and the obtained nanocrystalline Large, with a particle size of more than 100nm, the dispersion is not uniform enough, and the rare earth ions cannot be fully doped into the lattice of the matrix material, resulting in insufficient luminescence performance of the rare earth fluorescent upconversion material, which limits its application in biomedicine, solar cells and other fields
Preparation of Eu from Waste Phosphors 3+ , Yb 3+ 、Er 3+ Doped alone or co-doped with K 2 YF 5 There is no corresponding report on the process of nanocrystal

Method used

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  • Method for synthesizing rare-earth metal codoped yttrium potassium pentafluoride nano crystal from waste fluorescent powder
  • Method for synthesizing rare-earth metal codoped yttrium potassium pentafluoride nano crystal from waste fluorescent powder
  • Method for synthesizing rare-earth metal codoped yttrium potassium pentafluoride nano crystal from waste fluorescent powder

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Embodiment 1

[0036] The embodiment of the rare earth metal three-doped yttrium potassium pentafluoride nanocrystals with a particle size below 20nm prepared by using waste fluorescent powder as a raw material is as follows:

[0037] 1) Take 10g of waste fluorescent powder, add sulfuric acid and hydrochloric acid mixed acid solution (2mol / L sulfuric acid solution and 4mol / L hydrochloric acid solution are prepared at a volume ratio of 1:1) 100ml to leach the fluorescent powder, the speed is 1000rpm / min, add 0.6 ml of 20% H 2 o 2 , temperature 70°C-90°C, leaching for 4h;

[0038] 2) The leached solution is put into a centrifuge for solid-liquid separation to obtain a leaching solution. The leaching solution is mixed with ammonia water, a very dilute potassium sulfide solution and a very dilute potassium sulfate solution to adjust the pH value to 3.5-4, and then put it into a centrifuge for further processing. Solid-liquid separation to obtain the filtrate that removes most of the aluminum, ...

Embodiment 2

[0050] The embodiment of the potassium pentafluoride yttrium potassium pentafluoride double-doped with europium and erbium doped with particle size is prepared as raw material with waste fluorescent powder as follows:

[0051] 1) Take 10g of waste fluorescent powder, add sulfuric acid and hydrochloric acid mixed acid solution (2mol / L sulfuric acid solution and 4mol / L hydrochloric acid solution are prepared at a volume ratio of 1:1) 100ml to leach the fluorescent powder, the speed is 1000rpm / min, add 0.6 ml of 20% H 2 o 2 , temperature 70°C-90°C, leaching for 4h;

[0052] 2) The leached solution is put into a centrifuge for solid-liquid separation to obtain a leaching solution. The leaching solution is mixed with ammonia water, a very dilute potassium sulfide solution and a very dilute potassium sulfate solution to adjust the pH value to 3.5-4, and then put it into a centrifuge for further processing. Solid-liquid separation to obtain the filtrate that removes most of the alu...

Embodiment 3

[0061] The implementation mode of preparing europium monodoped yttrium potassium pentafluoride nanocrystals with waste fluorescent powder as raw material is as follows:

[0062] 1) Take 10g of waste fluorescent powder, add sulfuric acid and hydrochloric acid mixed acid solution (2mol / L sulfuric acid solution and 4mol / L hydrochloric acid solution are prepared at a volume ratio of 1:1) 100ml to leach the fluorescent powder, the speed is 1000rpm / min, add 0.6 ml of 20% H 2 o 2 , temperature 70°C-90°C, leaching for 4h;

[0063] 2) The leached solution is put into a centrifuge for solid-liquid separation to obtain a leaching solution. The leaching solution is mixed with ammonia water, a very dilute potassium sulfide solution and a very dilute potassium sulfate solution to adjust the pH value to 3.5-4, and then put it into a centrifuge for further processing. Solid-liquid separation to obtain the filtrate that removes most of the aluminum, iron, silicon, magnesium and other impurit...

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Abstract

The invention discloses a method for synthesizing rare-earth metal codoped yttrium potassium pentafluoride nano crystal from waste fluorescent powder. The method comprises the following steps: heating to disperse rare-earth ions, potassium bifluoride and potassium hydroxide in oleic acid so as to form a homogenized solution, and enabling the mixed components to react under a high temperature condition so as to generate ytterbium, europium and erbium codoped yttrium potassium pentafluoride nano crystal. By controlling the factors such as the concentration of rare-earth doped ions and the ratio of additives such as a potassium source, a fluorine source and oleic acid, the particle size and the intensity of visible light can be adjusted and controlled, and conversion of ultraviolet light and near-infrared light to visible light of multiple wavelengths can be achieved. The product prepared by using the method is uniform in morphology, controllable in size, high in light emission intensity, and can be used in fields such as photo-electron devices, electric light source illumination, solar batteries and biological fluorescent markers. The method is simple in preparation process, free of special equipment, low in cost, green and environment-friendly, and applicable to preparation and large-scale industrial production of multiple types of rare-earth up-conversion luminescence nano crystals.

Description

technical field [0001] The invention relates to a new technology for resource utilization of solid waste, especially suitable for the green high-value resource utilization of rare earth three-primary-color fluorescent powder waste, in particular to a rare earth secondary resource for preparing rare earth metal co-doped yttrium pentafluoride Methods for Potassium Nanomaterials. Background technique [0002] Rare-earth fluorescent up-conversion fluorescent materials refer to materials that can absorb long-wave radiation with low photon energy and emit short-wave radiation with high photon energy based on a two-photon or multi-photon mechanism when the material is excited by light. It is essentially an anti-Stokes glow. In recent years, up-conversion luminescent materials have broad application prospects in solid-state laser, three-dimensional display, infrared imaging, solar cells, especially as a new type of fluorescent marker in biomacromolecule analysis and biomedical clin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/01B82Y20/00B82Y40/00
CPCY02W30/50
Inventor 王友法熊真敏丁奕丹梅光军李正赵书文
Owner WUHAN UNIV OF TECH
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