A rare earth-doped fluorozirconate luminescent material and its preparation method

A fluorozirconate, rare earth doping technology, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of product agglomeration, non-luminescence, inability to enter, etc., and achieve the effect of good crystallinity and easy dispersion of particles

Active Publication Date: 2018-04-06
WENZHOU UNIVERSITY
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  • Abstract
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Problems solved by technology

However, the sintering temperature required for high-temperature solid-phase synthesis is generally higher than 1000°C and repeated grinding and sintering are required. The product agglomerates seriously, and the pulverization process seriously affects the luminous performance of the product.
[0003] In recent years, it has been found that Mn 4+ Doped with fluorosilicates such as K 2 SiF 6 [J.H.Oh, H, Kang, Y.J.Eo, H.K.Park, Y.G.Do, J.Mater.Chem.C, 2015, 3, 607‐615.], BaSiF 6 [X.Y.Jiang, Y.X.Pan, S.M.Huang, X.A.Chen, J.G.Wang, G.K.Liu, J.Mater.Chem.C.2014, 2(13), 2301‐2306.], and fluorotitanates such as BaTiF 6 [X.Y.Jiang, Z.Chen, S.M.Huang, J.G.Wang, Y.X.Pan, Dalton Trans.2014, 43, 9414‐9418.], can emit red light, in which Mn 4+ Replace Si 4+ or Ti 4+ position, without replacing the position of alkaline earth or alkali metal ions, but Mn 4+ In the matrix SrZrF of the present invention 6 does not emit light, and has not been successfully synthesized so far, it may be that Mn 4+ Can't get into SrZrF 6 Zr in 4+ Location

Method used

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Effect test

Embodiment 1

[0024] Mole ratio Sr: [ZrF 6 ]: Eu=0.98:1:0.02, accurately weigh the solid strontium fluoride SrF with an electronic balance 2 (analytical pure) with europium oxide Eu 2 o 3 (4N), put into the polytetrafluoroethylene reactor lining, accurately measure fluozirconic acid with a pipette and add, then add deionized water to make the total volume of the reaction system reach 40mL (accounting for 80% of the inner volume of the reactor), Magnetic stirring was carried out for 15 minutes, and the liner containing the mixture was placed in a closed stainless steel reaction kettle. The reaction kettle was transferred to an oven and kept at 180° C. for 12 hours. After the reaction is completed, it is cooled and dried naturally after suction filtration, and the total product is about 3 grams. The product emits bright red fluorescence under near-ultraviolet irradiation. figure 1 The XRD shows that the product is a pure phase of SrZrF 6 , slightly doped with Eu 3+ The crystal structur...

Embodiment 2

[0027] Mole ratio Sr: [ZrF 6 ]: Eu=0.995:1:0.005, accurately weigh the solid strontium fluoride SrF with an electronic balance 2(analytical pure) with europium oxide Eu 2 o 3 (4N), put into the polytetrafluoroethylene reactor lining, accurately measure fluozirconic acid with a pipette and add, then add deionized water to make the total volume of the reaction system reach 40mL (accounting for 80% of the inner volume of the reactor), Magnetic stirring was performed for 10 minutes, and the liner containing the mixture was placed in a closed stainless steel reaction kettle. The reaction kettle was transferred to an oven and kept at 220° C. for 4 hours. After the reaction is completed, it is cooled and dried naturally after suction filtration, and the total product is about 3 grams. The product emits bright red fluorescence under near-ultraviolet irradiation. Its excitation and emission spectra are image 3 Basically similar.

Embodiment 3

[0029] Mole ratio Sr: [ZrF 6 ]: Eu=0.93:1:0.07, accurately weigh the solid strontium fluoride SrF with an electronic balance 2 (analytical pure) with europium oxide Eu 2 o 3 (4N), put into the polytetrafluoroethylene reactor lining, accurately measure fluozirconic acid with a pipette and add, then add deionized water to make the total volume of the reaction system reach 40mL (accounting for 80% of the inner volume of the reactor), Magnetic stirring was performed for 10 minutes, and the liner containing the mixture was placed in a closed stainless steel reaction kettle. The reaction kettle was transferred to an oven and kept at 220° C. for 4 hours. After the reaction is completed, it is cooled and dried naturally after suction filtration, and the total product is about 3 grams. The product emits bright red fluorescence under near-ultraviolet irradiation. Its excitation and emission spectra are image 3 Basically similar.

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Abstract

The invention discloses a rare earth-doped fluorozirconate luminescent material and a preparation method thereof. The chemical composition of the material is Sr(1‐x)ZrF6:xRE3+, where RE=Eu, Tb, Ce or Dy, 0.5%≤x≤7.0%; its preparation method is as follows: solid strontium fluoride and rare earth oxide The stoichiometric ratio is accurately weighed and put into the lining of the reaction kettle, then the fluozirconic acid and deionized water are added, stirred, the mixture is put into the reaction kettle, and reacted at 120-220°C to obtain a well-crystallized micron rod-shaped luminescent material. The phonon energy of the material is low, the non-radiative relaxation rate of the luminescence center is low, and the luminescence efficiency is high. The material particles are dispersed and not agglomerated, which is conducive to the application of coated pipes. The material has a high degree of crystallinity, a stable matrix, and can be applied in a humid environment without hydrolysis. The material can be used in energy-saving lamps and high-pressure mercury lamps, and has simple preparation process and low equipment requirements.

Description

technical field [0001] The invention relates to an inorganic solid luminescent material, in particular to a luminescent material based on strontium fluorozirconate which can be used in energy-saving lamps and high-pressure mercury lamps and a preparation method thereof. Specifically relates to a strontium fluorozirconate as the matrix, with Eu 3+ (or Tb 3+ 、Ce 3+ with Dy 3+ ) is a luminescent material that activates ions, and its luminous efficiency is equivalent to that of commercial phosphors synthesized by high-temperature solid-phase method. Background technique [0002] Energy-saving lamps (254nm) and high-pressure mercury lamps (365nm) are traditional photo light sources. They are still widely used in people's production and life due to their high color rendering, high efficiency, and durability. They are currently the leading products in the lighting market. In order to obtain white light, it is necessary to uniformly mix three kinds of luminescent materials that ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67
CPCC09K11/7705C09K11/772C09K11/7733C09K11/7748
Inventor 潘跃晓李丽刘桂朱江明吴紫英
Owner WENZHOU UNIVERSITY
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