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Preparation method for europium-doping calcium titanate fluorescent powder

A calcium titanate and phosphor technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of phosphor powder thermal stability and low luminous index, difficult to achieve high-quality packaging of phosphor powder, and luminous efficiency to be further improved , to achieve good application prospects, reduce energy consumption, and low cost

Inactive Publication Date: 2013-02-06
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Sr reported by Jia et al. in Solid State Communication.Vol.126(2003)pp.153~157 1-x Ca x TiO 3 :Pr 3+ Phosphor powder and CaTiO reported by Eric et al. in Alloys andComoouds.Vol.374(2004)pp.202~206 3 :Pr 3+ Phosphors, the problems of thermal stability and low luminescence index of phosphors have been solved, however, the synthesis temperature of these phosphors is too high (1350°C)
Mazzb et al reported the synthesis of CaTiO by hydrothermal method in Optical Materials.Vol.32(2010)pp.990~997 3 :Eu 3+ Phosphor powder, they synthesized phosphor powder at a lower temperature, but the particle size of the phosphor powder obtained by this method is large and piled up in blocks, and the agglomeration is serious, so it is difficult to achieve high-quality packaging of the phosphor powder
Sun et al reported CaTiO in Alloys and Compounds.Vol.493(2010)pp.561~564 3 :Eu 3+ Phosphor powder with a core-shell structure wrapped with silica particles has better luminous performance and a lower synthesis temperature, but the luminous efficiency needs to be further improved

Method used

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  • Preparation method for europium-doping calcium titanate fluorescent powder
  • Preparation method for europium-doping calcium titanate fluorescent powder
  • Preparation method for europium-doping calcium titanate fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 1.74ml of n-tetrabutyl titanate, disperse it in 10ml of absolute ethanol, add dropwise 10ml of 3mol / L ammonia solution to make it all react into a white precipitate, and centrifuge and wash it with deionized water for 3 times. Then add the above precursor to the mixed solution of 15ml ethylene glycol and 15ml ethylenediamine and stir for 50min to fully disperse the mixed solution. Dissolve 2.275g calcium acetate, 0.036g europium nitrate and 3.0g sodium hydroxide solution, 1ml of polyethylene glycol 200, and stirred for 50min at a rotation speed of 200r / min, so that the obtained solution was in the form of a suspension. The above-mentioned reactants were poured into a reaction kettle with a volume of 100ml, and then kept at 180° C. for 12 hours, and then cooled to room temperature. The product was collected by washing and centrifugation, washed twice with ethanol, then washed twice with pH = 1 hydrochloric acid solution, then washed three times with deionized water,...

Embodiment 2

[0027] Take 1.78ml of n-tetrabutyl titanate, disperse it in 12ml of absolute ethanol, add dropwise 15ml of 2mol / L ammonia solution to make it all react into a white precipitate, and centrifuge and wash it with deionized water for 4 times. Then add the above precursor to the mixed solution of 17ml ethylene glycol and 20ml ethylenediamine and stir for 40min to fully disperse the mixed solution. Dissolve the mixed solution of 2.448g calcium acetate, 0.104g europium nitrate, 3.5g sodium hydroxide solution, 2ml of polyethylene glycol 400, and stirred for 40min at a rotation speed of 300r / min to make the obtained solution into a suspension. The above reactant was poured into a reaction kettle with a volume of 100ml, and then kept at 200°C for 10 hours, and then cooled to room temperature. The product was collected by washing and centrifugation, first washed 3 times with ethanol, then washed 3 times with pH = 2 hydrochloric acid solution, and then washed 3 times with deionized water,...

Embodiment 3

[0029] Take 1.85 ml of n-tetrabutyl titanate, disperse it in 15 ml of absolute ethanol, add dropwise 20 ml of 1 mol / L ammonia solution to make it all react into a white precipitate, and centrifuge and wash it with deionized water for 5 times. Then add the mixture of 28ml ethylene glycol and 25ml ethylenediamine to the above precursor and stir for 30min to fully disperse it in the mixture. Dissolve 2.673g calcium acetate, 0.202g europium nitrate and 3.8g hydroxide Sodium solution and 2ml of polyethylene glycol 600 were stirred for 20min at a rotation speed of 500r / min to make the obtained solution into a suspension. The above-mentioned reactant was poured into a reaction kettle with a volume of 100ml, and then kept at 220° C. for 8 hours, and then cooled to room temperature. The product was collected by washing and centrifugation, first washed 3 times with ethanol, then washed 4 times with pH = 3 hydrochloric acid solution, and then washed 5 times with deionized water, and fina...

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Abstract

The invention relates to a preparation method for europium-doping calcium titanate fluorescent powder. The preparation method comprises the following steps of: (1) adding an aqueous ammonia solution into a tetra-n-butyl titanate solution at the room temperature so as to obtain a white precipitant, and washing the white precipitant so as to obtain a precursor; (2) dispersing the precursor in a mixing solution of ethylene glycol and ethylene dimine, and then stirring continuously so as to form a precursor suspending liquid; (3) respectively dissolving calcium acetate, europium nitrate and sodium hydroxide in deionized water, dropping into the precursor suspending liquid, adding polyethylene glycol 200, pouring into an agitated reactor after stirring and heating to 180-220 DEG C and reactingfor 8-12h; and (4) after reaction, cooling to the room temperature, washing and drying a product so as to obtain the fluorescent powder. The preparation method has the advantages that the preparationmethod is simple, the cost is low, required production equipment is simple, the reaction temperature is low, the energy consumption is reduced and the industrial production is facilitated; and the obtained europium-doping calcium titanate fluorescent powder has the advantages of good dispersibility, difficulty in agglomeration, spheroidal structure and good application prospect.

Description

technical field [0001] The invention belongs to the field of preparation of calcium titanate fluorescent powder, in particular to a preparation method of europium-doped calcium titanate fluorescent powder. Background technique [0002] As a new green and environment-friendly solid-state lighting source, white LED is known as the most promising new light source in the 21st century. It has a very broad application prospect in many fields, such as mobile phones, computer backlights, etc. [0003] White LEDs can be realized by using LED chips with phosphors, but currently the most widely used phosphors are YAG:Ce phosphors, which have poor thermal stability and low color rendering index, making it difficult to meet the needs of high-quality lighting. In order to solve this problem, phosphors with good thermal stability and high color rendering index have received extensive attention. For example, Sr reported by Jia et al. in Solid State Communication.Vol.126(2003)pp.153~157 1-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/78
Inventor 王宏志吴斌李耀刚张青红
Owner DONGHUA UNIV
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