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Preparation method of rare-earth-doped polyphosphate nanocrystals

A technology of polyphosphate and nanocrystals, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems that nanomaterials are prone to agglomeration and limit the application of materials, and achieve good fluorescence performance, low reaction temperature, and crystallization. type perfect effect

Inactive Publication Date: 2014-08-27
XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation methods they adopted are all realized under high temperature (400-500°C) heat treatment conditions. Due to the high reaction temperature, the obtained nanomaterials are easily agglomerated, which limits the application of this material in the optical field.

Method used

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  • Preparation method of rare-earth-doped polyphosphate nanocrystals
  • Preparation method of rare-earth-doped polyphosphate nanocrystals
  • Preparation method of rare-earth-doped polyphosphate nanocrystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: LiLa 0.9 PR 0.1 (PO 3 ) 4 Preparation of Nanocrystals

[0040] Mix 0.9mmol of lanthanum oxide, 0.1mmol of praseodymium oxide, 4.25mmol of lithium carbonate and 100mmol of phosphoric acid in a glassy carbon crucible, raise the temperature to 250°C under stirring conditions, and react at this temperature for 10h; then continue at a speed of 15°C / min Raise the temperature to 320°C, react for 8 hours under stirring conditions, and centrifuge the product at 5000 rpm / min for 10 minutes to obtain a precipitate, which is LiLa 0.9 PR 0.1 (PO 3 ) 4 For nanocrystals, the precipitates obtained by centrifugation were washed with deionized water and absolute ethanol in turn, and each washing step was repeated three times; in order to further improve the performance of the obtained nanocrystals, the washed precipitates were evenly dispersed in absolute ethanol A dispersion is formed, which is transferred to a reaction kettle with a filling degree of 80%. After reacti...

Embodiment 2

[0042] Example 2: LiLa 0.75 Nd 0.25 (PO 3 ) 4 Preparation of Nanocrystals

[0043] Mix 0.75mmol of lanthanum oxide, 0.25mmol of neodymium oxide, 3mmol of lithium metaphosphate and 100mmol of phosphoric acid in a glassy carbon crucible, raise the temperature to 240°C under stirring conditions, and react at this temperature for 15h; then continue at a speed of 15°C / min Raise the temperature to 340°C, react for 6 hours under stirring conditions, and centrifuge the product at 5000 rpm / min for 10 minutes to obtain a precipitate, which is LiLa 0.75 Nd 0.25 (PO 3 ) 4 For nanocrystals, the precipitates obtained by centrifugation were washed with deionized water and absolute ethanol in turn, and each washing step was repeated three times; in order to further improve the performance of the obtained nanocrystals, the washed precipitates were evenly dispersed in absolute ethanol A dispersion is formed, which is transferred to a reaction kettle with a filling degree of 80%. After re...

Embodiment 3

[0045] Example 3: KY 0.6 Nd 0.4 (PO 3 ) 4 Preparation of Nanocrystals

[0046] Mix 0.6mmol of yttrium oxide, 0.4mmol of neodymium oxide, 4.25mmol of potassium carbonate and 150mmol of phosphoric acid in a glassy carbon crucible, raise the temperature to 230°C under stirring conditions, and react at this temperature for 20h; then continue at a speed of 15°C / min Raise the temperature to 350°C, react for 5 hours under stirring conditions, and centrifuge the product at 5000rpm / min for 10 minutes to obtain a precipitate, which is KY 0.6 Nd 0.4 (PO 3 ) 4 For nanocrystals, the precipitates obtained by centrifugation were washed with 80°C deionized water, deionized water and absolute ethanol in sequence, and each washing step was repeated three times; in order to further improve the performance of the obtained nanocrystals, the washed precipitates were uniformly Disperse in absolute ethanol to form a dispersion, transfer the dispersion to a reaction kettle with a filling degree...

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Abstract

The invention provides a preparation method of rare-earth-doped polyphosphate nanocrystals, which solves the technical problem of high agglomeration tendency in the nano material. The preparation method comprises the following steps: 1) adding raw materials into a glass carbon crucible, evenly mixing, and reacting at 200-250 DEG C for 10-24 hours while stirring; and 2) heating the reaction system in the step 1) to 320-350 DEG C, reacting for 3-8 hours while stirring, centrifuging the product to obtain a precipitate, and washing the precipitate to obtain the rare-earth-doped polyphosphate nanocrystals. The invention has the advantages of low reaction temperature and mild reaction conditions; the obtained rare-earth-doped polyphosphate nanocrystals can not easily aggregate; and the rare-earth-doped polyphosphate nanocrystals prepared by the low temperature reaction-hydrothermal synthesis method have the advantages of uniform dispersion, perfect crystal form, high doping content and favorable fluorescence.

Description

technical field [0001] The invention belongs to the technical field of optical materials, and in particular relates to a preparation method of rare earth-doped polyphosphate nanocrystals. Background technique [0002] As an important self-activated crystal, rare earth-doped polyphosphate crystal is used in high-energy laser system due to its high doping concentration, low quenching rate and large emission cross section. [0003] At present, polyphosphate crystals used in lasers are mainly prepared by high-temperature pulling method. Because rare earth polyphosphates have complex structures, harsh growth conditions (high temperature, yellow / platinum crucible), and long growth cycles, it is difficult to grow large crystals. At the same time, because the crystal laser material itself is prone to damage, it is difficult to solve the problems of heat accumulation and thermal damage in high repetition rate and high energy laser systems, so that it has not been widely used so far. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/38B82Y30/00
Inventor 韦玮彭波崔晓霞王中跃
Owner XI'AN INST OF OPTICS & FINE MECHANICS - CHINESE ACAD OF SCI
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