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A kind of rare earth vanadium niobate red fluorescent material and preparation method thereof
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A vanadium niobate, red fluorescence technology, applied in luminescent materials, chemical instruments and methods, etc., to achieve the effect of reducing energy loss, uniform particle distribution, and good thermal stability
Active Publication Date: 2018-09-28
JIANGXI IONIC RARE EARTH ENG RES CO LTD
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[0004] It can be seen that vanadate-based fluorescent materials have gradually become a research hotspot, but for (Sc,Lu)VO 4 Co-doped Eu in the matrix 3+ , Sm 3+ and Bi 3+ , while using a certain amount of NbO 4 3- to replace part of VO 4 3- To improve the luminous properties and thermal stability of phosphors, no similar reports have been seen.
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Embodiment 1
[0027] The chemical formula of the rare earth vanadate red phosphor product for near-ultraviolet excitation in this embodiment is Sc 0.935 V 0.8 Nb 0.2 o 4 :Eu 3+ 0.05 ,Sm3+ 0.01 , Bi 3+ 0.005 , wherein, x=0.05, y=0.01, z=0.005, n=0.2, A is Sc. Its preparation method is: weigh Sc 2 o 3 8.0761g, Eu 2 o 3 1.0998g, Sm 2 o 3 0.2179g and Bi 2 o 3 0.1456g, then its mixed and dissolved in 40% HNO 3 In, make it dissolve completely to form mixed solution A; then weigh NH 4 VO 3 11.6978g and K 3 NbO 4 4.5001g, dissolve it in ammonia solution, and add 0.7721g of surfactant CTAB to form mixed solution B, then place it in a microwave-ultrasonic combined synthesizer, adjust microwave power 300-900w, ultrasonic power 400-1000w, microwave / ultrasonic power The ultrasonic time mode is 1:1~3:1, and the reaction temperature is 20~80°C; the mixed solution A is added to the solution B at 3~10ml / min controlled by a peristaltic pump to produce a white precipitate, and then aged fo...
Embodiment 2～ Embodiment 15
[0029] Except for weighing relevant raw materials according to their chemical formula composition and stoichiometric measurement, the rest of the preparation steps are the same as in Example 1. The chemical formula composition, color coordinates and relative brightness of the product are shown in Table 1.
[0030] Table 1 Chemical formula, color coordinates and relative brightness of Examples 1-15
[0031]
[0032]
[0033] Note: The above data are tested under the excitation of near ultraviolet (397nm)
Embodiment 16
[0035] The chemical formula of the rare earth vanadate red phosphor product for near-ultraviolet excitation in this embodiment is Lu 0.9 V 0.9 Nb 0.1 o 4 :Eu 3+ 0.07 ,Sm 3+ 0.02 , Bi 3+ 0.01 , wherein, x=0.07, y=0.02, z=0.01, n=0.1, A is Lu. Its preparation method is: weigh Lu(OH) 3 13.5593g, Eu(OH) 3 0.9473g, Sm(OH) 3 0.2685g and Bi(OH) 3 0.1733g, then it is mixed and dissolved in 36% HCl, and it is completely dissolved to form mixed solution A; then weigh NH 4 VO 3 7.0187g and K 3 NbO 4 1. 2000g, dissolve it in ammonia solution, and add surfactant PEG60000.6950g to form a mixed solution B, then place it in a microwave-ultrasonic combined synthesizer, adjust the microwave power 300-900w, ultrasonic power 400-1000w, microwave / ultrasonic The ultrasonic time mode is 1:1~3:1, and the reaction temperature is 20~80°C; the mixed solution A is added to the solution B at 3~10ml / min controlled by a peristaltic pump to produce a white precipitate, and then aged for 0.5~2...
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Abstract
The invention discloses a rare-earth vanadium niobate red fluorescent material and a preparation method thereof. The chemical formula of the material is A[1-x-y-z]V[1-n]Nb[n]O[4]:Eu<3+>x,Sm<3+>y,Bi<3+>z, wherein A represents one or two of Sc and Lu; and 0.005<=x<=0.2, 0.005<=y<=0.1, 0.001<=z<=0.05, 0<n<=0.5, and A:V:Nb:Eu:Sm:Bi=(1-x-y-z):(1-n):n:x:y:z. The preparation method comprises the following steps: S1. weighing metal compounds of Sc, Lu, Eu, Sm and Bi according to the stoichiometric proportion, and dissolving the metal compounds in hydrochloric acid or nitric acid to form a mixed solution A; S2. weighing raw materials ammonium metavanadate and potassium niobate, dissolving the raw materials in aqua ammonia, adding a surfactant to form a mixed solution B, and putting in a microwave-ultrasonic combined synthesizer; S3. dropwisely adding the mixed solution A into the solution B by using a constant-flow peristaltic pump to generate a precipitate, aging, filtering, washing, and drying to obtain a precursor; and S4. igniting the precursor at high temperature, and carrying out after-treatment to obtain the finished product.
Description
technical field [0001] The invention relates to the technical field of fluorescent powder for near-ultraviolet LED excitation, in particular to a rare earth vanadium niobate red fluorescent material and a preparation method thereof. Background technique [0002] Since the advent of white light-emitting diodes (Light~emitting Diodes; LED), because of its high efficiency, environmental protection, energy saving, pollution-free and long life, it has entered the high-tech field at a rapid pace in recent years, and is known as incandescent lamps and fluorescent lamps. , The fourth generation of lighting sources after energy-saving lamps. Currently, commercial "blue LED+YAG:Ce 3+ "White light produced by the combined form, color reproduction and color rendering index all limit its further development due to the lack of red fluorescence. With the gradual commercialization of near-ultraviolet LEDs, the development of "near-ultraviolet LEDs + red, green and blue (RGB) ) Phosphor” r...
Claims
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