Preparation method of gadolinium tungstate fluorescent powder

A fluorescent powder, gd2-xw2o9 technology, applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems of inability to meet market demand, low luminous intensity of products, harsh synthesis conditions, etc., and achieve easy market promotion and application, uniform size , the effect of easy operation

Inactive Publication Date: 2019-02-01
CHONGQING UNIV OF ARTS & SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the preparation of Gd by high-temperature solid-phase method 2-x W 2 o 9 :xEu 3+ There are still technical problems such as low luminous intensity of the product, unable to meet market demand, harsh synthesis conditions, and high product cost that need to be resolved urgently

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  • Preparation method of gadolinium tungstate fluorescent powder
  • Preparation method of gadolinium tungstate fluorescent powder
  • Preparation method of gadolinium tungstate fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1 Gd 1.5 W 2 o 9 :0.5Eu 3+ Preparation of:

[0019] Weigh Gd separately 2 o 3 0.6788g, WO 3 1.1602g, Eu 2 o 3 0.2201g, then take by weighing the surfactant of 1.4wt% of the above raw material gross mass (hexadecyltrimethylammonium bromide: sodium dodecylbenzenesulfonate: the mass ratio of Polyethylene Glycol 200 is 1: 2:0.8); Gd to be weighed 2 o 3 , WO 3 , Eu 2 o 3 , mixed with surfactants, according to the ball-to-material ratio of 7:1, put in agate balls, add alcohol, the amount of lubricant added is limited to be kept dispersed by the ball mill system, and the ball mill is mixed for 4 hours to obtain a mixed powder.

[0020] (3) Put the mixed powder into a corundum crucible, place it in a high-temperature furnace for calcination, raise the temperature to 200°C at a heating rate of 10°C per minute, keep it warm for 19 minutes, and then raise the temperature to 800°C at a heating rate of 10°C per minute Calcination at heat preservation for 1.5...

Embodiment 2

[0022] Example 2 Gd 1.9 W 2 o 9 :0.1Eu 3+ Preparation of:

[0023] Weigh Gd separately 2 o 3 0.8596, WO 3 1.1600g, Eu 2 o 3 0.0441g, then take by weighing the surfactant of 1.3wt% of the above raw material gross mass (hexadecyltrimethylammonium bromide: sodium dodecylbenzenesulfonate: the mass ratio of Polyethylene Glycol 200 is 1: 3:0.7); Gd to be weighed 2 o 3， WO 3， Eu 2 o 3， Surfactants are mixed, according to the ball-to-material ratio of 8:1, agate balls are added, acetone is added, the amount of lubricant added is limited to be kept dispersed by the ball mill system, and the ball mill is mixed for 5 hours to obtain a mixed powder.

[0024](3) Put the mixed powder into a corundum crucible, place it in a high-temperature furnace for calcination, raise the temperature to 210°C at a heating rate of 12°C per minute, and heat it for 18 minutes, then raise the temperature to 850°C at a heating rate of 12°C per minute Calcination at heat preservation for 1h, af...

Embodiment 3

[0026] Example 3 Gd 1.8 W 2 o 9 :0.2Eu 3+ Preparation of:

[0027] Weigh Gd separately 2 o 3 0.8147, WO 3 1.1603g, Eu 2 o 3 0.0881g, then take by weighing the surfactant of 1.5wt% of the above raw material gross mass (hexadecyltrimethylammonium bromide: sodium dodecylbenzenesulfonate: the mass ratio of Polyethylene Glycol 200 is 1: 1:0.9); Gd to be weighed 2 o 3， WO 3， Eu 2 o 3， Surfactants are mixed, according to the ball-to-material ratio of 3:1, put in agate balls, add alcohol, the amount of lubricant added is limited to be kept dispersed by the ball mill system, and the ball mill is mixed for 2 hours to obtain a mixed powder.

[0028] (3) Put the mixed powder into a corundum crucible, place it in a high-temperature furnace for calcination, raise the temperature to 190°C at a heating rate of 8°C per minute, keep it warm for 22 minutes, and then raise the temperature to 700°C at a heating rate of 8°C per minute Calcination at heat preservation for 2h, after ...

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Abstract

The invention relates to a preparation method of Gd2-xW2O9:xEu<3+> fluorescent powder. Gd2O3, WO3, Eu2O3, a surfactant and a lubricant are adopted as the raw materials, and ball milling, high temperature solid phase process and other steps are carried out respectively to obtain the fluorescent powder. The fluorescent powder provided by the invention has spherical particle shape, is smooth in surface, has a diameter distribution in the range of 9-20nm, is uniform in size, disperse and non-agglomerated, the product has high luminescent intensity, and under 395nm excitation, the emission spectrumis mainly composed of several characteristic emission peaks of Eu<3+> ions, wherein the strongest emission peak is located at 616nm, and under a monitoring wavelength of 613nm, the excitation spectrum of the sample has six obvious excitation peaks, respectively located at 254nm, 311nm, 362nm, 395nm, 466nm and 536nm. The fluorescent powder prepared by the method provided by the invention has highluminescent intensity, and the emission peak intensity is as high as 8700. The preparation method provided by the invention has the characteristics of simple process, simple operation, relatively lowtemperature and low cost, and is convenient for market popularization and application.

Description

technical field [0001] The present invention relates to a kind of preparation method of fluorescent powder, relate in particular to a kind of Gd 2-x W 2 o 9 :xEu 3+ Preparation method of fluorescent powder. Background technique [0002] Tungsten and rare earth elements are abundant elements in my country. In order to make full use of tungsten and rare earth resources, enrich the content of solid chemistry, find new solid luminescent materials and catalysts with high catalytic activity, the synthesis, properties, reaction mechanism and application of tungstate, especially The application of polytungstate has received extensive attention and the research is very active. [0003] In the past few decades, crystals, glasses, ceramics, and fluorescent materials prepared by doping rare earth ions have played a significant role in the development of new optical devices, such as solid-state lasers, fiber amplifiers, displays, and biosensors. Therefore, the research on rare earth ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/78
CPCC09K11/7787
Inventor 曹仕秀韩涛彭玲玲刘碧桃李夫
Owner CHONGQING UNIV OF ARTS & SCI
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