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Preparation method of magnesium borate microspheres doped with europium red fluorescent powder with flower-like structure

A technology of red fluorescent powder and flower-like structure, which is applied in the field of red fluorescent powder, can solve the problems of impure red fluorescent pink, difficult to control shape and size, low yield and quality, and achieve high yield, complete crystal form, The effect of high luminous intensity

Active Publication Date: 2014-10-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of flower-shaped magnesium borate microspheres doped with europium red fluorescent powder, which solves the problems of impure red fluorescent pink, weak brightness, difficult control of shape and size, poor dispersion, and low yield and quality in the background technology. And technical issues such as high energy consumption for preparation

Method used

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  • Preparation method of magnesium borate microspheres doped with europium red fluorescent powder with flower-like structure
  • Preparation method of magnesium borate microspheres doped with europium red fluorescent powder with flower-like structure
  • Preparation method of magnesium borate microspheres doped with europium red fluorescent powder with flower-like structure

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Experimental program
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Effect test

Embodiment 1

[0028] Weigh 0.21g Eu 2 o 3 In a beaker, add a 10% mass concentration of dilute nitric acid solution and heat to dissolve it completely. Slowly evaporate to remove excess nitric acid until it becomes viscous. After cooling to room temperature (20°C), add deionized water to make 0.12mol / L Eu (NO 3 ) 3 Aqueous solution 10ml. Dissolve 1.41g (0.025mmol) of PVP (K30) in 50mL of deionized water to prepare a 0.0282g / ml PVP aqueous solution; at room temperature (20°C), add 0.12mol / L of Eu ( NO 3 ) 3 aqueous solution 1ml, add 0.61g (0.0024mol) Mg(NO 3 ) 2 ·6H 2 O, stir and mix to obtain a mixed solution, so that Mg in the mixed solution 2+ with Eu 3+ The total concentration of ions is 0.05mol / L, where n(Eu 3+ ) / n(Mg 2+ +Eu 3+ )=5%, n(Mg 2+ +Eu 3+ ) / n(PVP)=1:0.01, add 0.6mol / L Na at room temperature 2 B 4 o 7 10H 2 O aqueous solution 4ml, continue to stir for 3h to obtain a white turbid solution, and age the white turbid solution at 80°C for 24h at a constant temperat...

Embodiment 2

[0031] Weigh 14.5g (2.6mmol) PVP (K30) and dissolve it in 150mL deionized water, add 0.12mol / L Eu(NO 3 ) 3 Aqueous solution 1ml (preparation method is the same as Example 1), at room temperature (20 ℃), add 0.34g (0.00132mol) of Mg (NO 3 ) 2 ·6H 2 O, stir and mix to obtain a mixed solution, so that Mg in the mixed solution 2+ with Eu 3+ The total concentration of ions is 0.01mol / L, where n(Eu 3+ ) / n(Mg 2+ +Eu 3+ )=10%, n(Mg 2+ +Eu 3+ ) / n(PVP)=1:0.2, add 0.2mol / L Na 2 B 4 o 7 10H 2 O aqueous solution 7.5ml, continue stirring for 3h to obtain a white turbid solution, age the white turbid solution at 20°C for 72h at a constant temperature, after the aging is completed, obtain a precipitated mixture, filter the precipitated mixture to obtain a white filter cake, and separate the white filter cake in turn After washing with distilled water and absolute ethanol for 3 times, the filter cake was dried at 100°C for 24 hours, and then calcined at 300°C for 12 hours to obtai...

Embodiment 3

[0033] Weigh 11.2g (2mmol) PVP (K30) and dissolve it in 100mL deionized water, add 0.12mol / L Eu(NO 3 ) 3 1ml of aqueous solution, add 4.9g (0.02mol) of MgSO at room temperature (20°C) 4 ·7H 2 O, stir and mix to obtain a mixed solution, so that Mg in the mixed solution 2+ with Eu 3+ The total concentration of ions is 0.2mol / L, where n(Eu 3+ ) / n(Mg 2+ +Eu 3+ )=1%, n(Mg 2+ +Eu 3+ ) / n(PVP)=1:0.01, add 0.01mol / LNa 2 B 4 o 7 10H 2 O aqueous solution 180ml, continue stirring for 3h to obtain a white turbid solution, age the white turbid solution at 100°C for 2h at a constant temperature, after the aging is completed, obtain a precipitated mixture, filter the precipitated mixture to obtain a white filter cake, and use After washing with distilled water and absolute ethanol for 3 times, the filter cake was dried at 100°C for 24 hours, and then calcined at 800°C for 2 hours to obtain a white powder sample. The X-ray diffraction spectrum, morphology and fluorescence spectrum...

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Abstract

The invention discloses a preparation method of flower-structure magnesium borate microsphere europium-doped red fluorescent powder. The method comprises the following steps of: taking aqueous solution of inorganic magnesium salt and europium nitrate as well as a borax aqueous solution with molar concentration of 0.01-0.6mol / L as raw materials, stirring in polyvinylpyrrolidone aqueous solution with mass concentration of 2-36% for 2-5 hours at room temperature to obtain mixed solution; aging the mixed solution for 2-72 hours at a temperature of 20-120 DEG C to obtain a precipitate mixture; filtering the precipitate mixture; washing and drying a filter cake; and roasting the filter cake at a temperature of 300-800 DEG C in an air atmosphere to obtain the flower-structure magnesium borate microsphere europium-doped red fluorescent powder. The preparation method disclosed by the invention can be used for preparing the flower-structure magnesium borate microsphere europium-doped red fluorescent powder, and has the advantages of being simple in technology, low in energy consumption and high in yield; and the flower-structure magnesium borate microsphere europium-doped red fluorescent powder has a complete crystal form, is relatively uniform in size distribution, good in luminous purity and high in luminous intensity, and is particularly suitable for a fluorescent luminous material used by a PDP (plasma display panel) coating screen.

Description

(1) Technical field [0001] The invention relates to a red fluorescent powder, in particular to a preparation method of a flower-like structured magnesium borate microsphere doped with europium red fluorescent powder. (2) Background technology [0002] With the rapid development of flat panel display technology, the market demand for high-efficiency phosphors is increasingly strong. Red phosphor plays an important role in adjusting color temperature and improving color rendering, but compared with green and blue phosphors, the development of red phosphors is relatively lagging behind, mainly due to poor stability and low luminous intensity. , High prices. Borate is considered to be one of the luminescent host materials with practical value because of its simple synthesis, low sintering temperature, high luminous brightness and stable chemical properties. Eu 3+ The red light emitting function of ions has been widely used in color TVs, flat panel displays, cathode ray tubes,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/63
Inventor 陈爱民顾培
Owner ZHEJIANG UNIV OF TECH
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