Preparation of laser excitation rare earth doped calcium silicon-phosphate high-brightness three-primary-color nano phosphor powder as well as product and application thereof

A nano-fluorescent powder and rare earth doping technology, which is applied in the direction of luminescent materials, chemical instruments and methods, electrical components, etc., can solve the problems of low preparation purity and few types of laser-excited white light LD phosphors, etc., and achieve simple process and structure The effect of easy control and high powder purity

Inactive Publication Date: 2018-07-20
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Aiming at the problem that there are few types of white light LD phosphors excited by lasers and the preparation purity is not high, the purpose of the present invention is to provide a method for preparing laser-excited rare earth-doped silicon phosphate high-brightness trichromatic nano-phosphors

Method used

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  • Preparation of laser excitation rare earth doped calcium silicon-phosphate high-brightness three-primary-color nano phosphor powder as well as product and application thereof
  • Preparation of laser excitation rare earth doped calcium silicon-phosphate high-brightness three-primary-color nano phosphor powder as well as product and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Weigh calcium oxide: calcium phosphate: tetraethyl orthosilicate in a molar ratio of 0.5mol:0.2mol:0.1mol to weigh the powder, then weigh 0.02mol of erbium nitrate and dissolve it in deionized water, stir and add 0.001mol of citric acid Stir for 30 minutes and move to an electric furnace until the liquid burns. After burning, the powder is ground and loaded into an alumina boat and placed in a muffle furnace. Oxygen is introduced to raise the temperature to 600°C for 100 minutes, keep it warm for 8 hours, and then cool down to room temperature. Calcined, ball milled and granulated to obtain rare earth doped silicon calcium phosphate phosphor. Luminescent properties were tested using a Flog-3 fluorescence spectrometer. Under 980nm laser excitation, there is an obvious luminescence peak in red light.

Embodiment 2

[0025] Weigh strontium nitrate: calcium phosphate: tetraethyl orthosilicate ratio 0.5mol:0.2mol:0.1mol to weigh the powder, then weigh 0.001mol of samarium nitrate and 0.0025mol of ytterbium nitrate, dissolve them in deionized water and add 0.025mol of Stir the citric acid for 30 minutes and move it to an electric heating furnace until the liquid burns. After the combustion, the powder is ground and loaded into an alumina boat and put into a muffle furnace. The temperature is raised to 1000°C after passing in argon for 100 minutes, kept for 2 hours, and then lowered to room temperature. Calcined, ball milled and granulated to obtain rare earth doped silicon calcium phosphate phosphor. Luminescent properties were tested using a Flog-3 fluorescence spectrometer. Under 980nm laser excitation, there is an obvious luminescence peak in blue light.

Embodiment 3

[0027] Weigh barium chloride: calcium phosphate: tetraethyl orthosilicate ratio 0.5mol:0.2mol:0.1mol to weigh the powder, then weigh 0.01mol of thulium nitrate and 0.005mol of ytterbium nitrate, dissolve in deionized water and stir to add 0.005mol The citric acid was stirred for 30 minutes and moved to the electric furnace until the liquid was burned. After the combustion, the powder was ground and loaded into an alumina boat and placed in a muffle furnace. Air was introduced to raise the temperature to 800°C for 100 minutes, kept for 5 hours, and then dropped to room temperature. Calcined, ball milled and granulated to obtain rare earth doped silicon calcium phosphate phosphor. Luminescent properties were tested using a Flog-3 fluorescence spectrometer. Under 980nm laser excitation, there is an obvious luminescence peak in green light.

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Abstract

The invention discloses preparation of laser excitation rare earth doped calcium silicon-phosphate high-brightness three-primary-color nano phosphor powder as well as a product and application thereof. The preparation comprises the following steps: weighing raw materials according to a stoichiometric ratio of a chemical formula M5(PO4)2SiO4: Re, B, dissolving the materials into deionized water, adding an igniter composition, stirring for 30 minutes, transferring onto an electro-thermal furnace until liquid is burning, and grinding the powder to be put into a muffle furnace after burning; introducing one or a mixed gas atmosphere of air, oxygen or argon into the muffle furnace to be heated and calcined; ball-milling and granulating after calcining, thereby obtaining the rare earth doped calcium silicon-phosphate phosphor powder. The phosphor powder disclosed by the invention has up-conversion luminescence characteristics; different rare earth elements or rare earth of different concentrations is doped in a matrix, so that a fluorescent material with strong emission in a visible spectral region under laser excitation can be obtained. The fluorescent material can be applied to high-brightness LD lighting.

Description

technical field [0001] The invention belongs to the field of fluorescent powder materials, and specifically relates to the preparation, product and application of laser-excited rare earth-doped silicon calcium phosphate high-brightness trichromatic nano fluorescent powder. It belongs to the field of high-brightness white LD lighting. Background technique [0002] LED has become a new generation of lighting source. Developed countries such as Japan and the United States have invested a lot of manpower and material resources in development, and my country has also listed it as a development focus since the "Eleventh Five-Year Plan". At present, the main problems that limit the large-scale replacement of traditional lighting devices by LEDs are the high cost and low brightness. Despite the rapid development of LEDs in recent years, the luminous efficiency of a single LED is still far lower than that of fluorescent lamps. In order to obtain a light source with sufficient brigh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/71H01L33/50
CPCC09K11/7778H01L33/502
Inventor 何丹农张芳吴晓燕段磊卢玉英金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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