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Micro/nano potassium yttrium tungstate near-spherical particles and preparation method thereof

A technology of yttrium potassium tungstate and spherical particles, which is applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve problems such as limited scope of application, expensive raw materials, difficulty in powder collection, etc., and achieve broad application prospects. Uniform particle size distribution and improved luminous efficiency

Active Publication Date: 2013-10-02
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But different methods have their own limitations, such as the disadvantages of the combustion method: the reaction is uncontrollable, and the powder collection is difficult; the raw materials used in the sol-gel method are relatively expensive, and some raw materials are organic matter, which is harmful to health. Secondly, the entire sol - The gel process takes a long time; the most obvious defect of the hydrothermal method is: the scope of application is limited to the preparation and treatment of oxide materials or a small number of sulfides that are not very sensitive to water, and some easily hydrolyzed compounds are not suitable. small range
[0005] At present, people's reports on yttrium potassium tungstate mainly focus on the growth of bulk single crystals, spectral properties, and optical waveguide characteristics. Patent reports involve the preparation of tungstate single crystals (02802513.X), tungstate nano The preparation of thin films (200810032456.0, 200510026632.6), the luminescence of tungstate (200910067493.X, 200910067492.5, 200910114933.2, etc.), and the research on the low-dimensional nanoscale and shape control of compound tungstate and the synthesis process of micro-nano structure materials Research less involved

Method used

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  • Micro/nano potassium yttrium tungstate near-spherical particles and preparation method thereof
  • Micro/nano potassium yttrium tungstate near-spherical particles and preparation method thereof
  • Micro/nano potassium yttrium tungstate near-spherical particles and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh a certain amount of hydrated K 2 WO 4 , Y 2 o 3 Dissolve in deionized water and dilute nitric acid respectively, and prepare WO 4 2- Solution and Y 3+ Ionic solution; adjust the pH values ​​of the two solutions, then mix and stir, then adjust the pH value of the mixed solution to 5, and then add acetylacetone with a volume fraction of 20% of the mixed solution to the mixed solution and ultrasonically vibrate for half an hour to obtain a precursor solution . Put the prepared precursor solution in a hydrothermal kettle at 180°C for 20 hours, filter the solution after hydrothermal insulation, clean the filter, put it into a crucible, transfer it to a high-temperature furnace and heat it at 800°C for 8 hours to obtain Micronano potassium yttrium tungstate particles. Depend on figure 1 As shown, the particle size is between 0.100 and 1 μm, and its powder diffraction pattern is shown in Figure 5 Shown in Example 1.

Embodiment 2

[0025] Weigh a certain amount of hydrated K 2 WO 4 , Y(NO 3 ) 3 Dissolve in deionized water and dilute nitric acid respectively, and prepare WO 4 2- Solution and Y 3+ Ionic solution; adjust the pH values ​​of the two solutions, then mix and stir, then adjust the pH value of the mixed solution to 6, and then add acetylacetone with a volume fraction of 20% of the mixed solution to the mixed solution and ultrasonically vibrate for half an hour to obtain a precursor solution . Put the prepared precursor solution in a hydrothermal kettle at 180°C for 20 hours, filter the solution after hydrothermal insulation, clean the filter, put it into a crucible, transfer it to a high-temperature furnace and heat it at 800°C for 8 hours to obtain Micronano potassium yttrium tungstate particles. Depend on figure 2 As shown, the particle size is between 0.3 and 1 μm, and its powder diffraction pattern is shown in Figure 5 Shown in Example 2.

Embodiment 3

[0027] Weigh a certain amount of hydrated (NH 4 ) 2 WO 4 , Y 2 o 3 Dissolve in deionized water and dilute nitric acid respectively, and prepare WO 4 2- Solution and Y 3+ Ionic solution; adjust the pH values ​​of the two solutions, then mix and stir, then adjust the pH value of the mixed solution to 7, and then add acetylacetone with a volume fraction of 15% of the mixed solution to the mixed solution and ultrasonically vibrate for half an hour to obtain a precursor solution . Put the prepared precursor solution in a hydrothermal kettle at 180°C for 20 hours, filter the solution after hydrothermal insulation, clean the filter, put it into a crucible, transfer it to a high-temperature furnace and heat it at 800°C for 4 hours to obtain Micronano yttrium potassium tungstate particles. Depend on image 3 As shown, the particle size is between 0.1 and 0.7 μm, and its powder diffraction pattern is shown in Figure 5 Shown in Example 3.

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Abstract

The invention discloses micro / nano potassium yttrium tungstate near-spherical particles and a preparation method thereof. The preparation method comprises the following steps: regulating the pH value of a soluble tungstate solution to 7-8.5 and the pH value of Y<3+> of the yttrium ion solution to 5-6.5, mixing according to the tungstate ion:yttrium ion mol ratio of 2:1, regulating the pH value of the mixed solution to 5-7.5, uniformly stirring, adding acetylacetone accounting for 10-20 vol% of the mixed solution, and carrying out ultrasonic vibration to obtain a precursor solution; holding the precursor solution by hydrothermal sealing to obtain a white precipitate, wherein the hydrothermal temperature is 140-180 DEG C, and the holding time is 20-24 hours; and centrifuging the white precipitate, and carrying out heat treatment to obtain the micro / nano potassium yttrium tungstate near-spherical particles. The micro / nano potassium yttrium tungstate near-spherical particles are composed of KY(WO4)2 particles, the particle size is 0.100-1 mu m, and the particle shape is near-spherical. The invention enhances the luminescence efficiency of the powder, can be used as a luminescent material, and can be widely used in the fields of road signs, various energy-saving illuminators, biomedical labels, aviation display devices, various meters and computers, and the like.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, in particular to an inorganic luminescent material compound tungstate and a preparation method thereof. Background technique [0002] The traditional preparation method of phosphorescent materials is a high-temperature solid-phase method. The traditional preparation method usually requires high temperature or complex equipment, and the reaction time is relatively long. With the rapid update of new technologies, the improvement of the performance indicators of phosphorescent materials needs to overcome the classic synthesis method. Due to the inherent defects, some new methods have emerged, such as combustion method, sol-gel method, hydrothermal precipitation method, microwave method and so on. But different methods have their own limitations, such as the disadvantages of the combustion method: the reaction is uncontrollable, and the powder collection is difficult; the raw materials ...

Claims

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Application Information

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IPC IPC(8): C01G41/00
Inventor 唐丽永刘玲沈彬彬王永刚周海鉴刘琳
Owner JIANGSU UNIV
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