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Synthesis method of rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline

A technology doping with sodium cerium fluoride and rare earth, which is applied in the field of synthesizing rare earth doped inorganic nanocrystals. It can solve the problems of long reaction time, large particle size, and limited development of solvothermal method, and the synthesis conditions are easy to control and prepare. The process is simple and the effect of good application potential

Inactive Publication Date: 2013-05-08
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Problems solved by technology

Recently, the research groups of Jeong and Li Yadong respectively reported the synthesis of rare earth doped NaCeF by solvothermal method. 4 However, the reaction time of the solvothermal method is longer (usually 24 hours), so the energy consumption is higher. The particles obtained by this method are not only large in size, but also easy to agglomerate. These factors limit the rare earth doping NaCeF 4 Further development and application of nanomaterials (reference: Jeong et al., Controlled Fabrication and Shape-Dependent Luminescence Properties of Hexagonal NaCeF 4 , NaCeF 4 :Tb 3+ Nanorods via Polyol-Mediated Solvothermal Route. Inorganic Chemistry, 2011, 50, 3387-3393; Li et al., Nucleation and Growth of CeF 3 and NaCeF 4 Nanocrystals. Chemistry-a European Journal, 2009, 15, 2512-2517)

Method used

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  • Synthesis method of rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline
  • Synthesis method of rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline
  • Synthesis method of rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline

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example 1

[0018] Example 1: NaCeF 4 : The preparation of 0.02Eu nanocrystals, first weigh 0.348 g CeCl 3 ·6H 2 O and 0.007 g EuCl 3 ·6H 2 O was dissolved in a mixed solvent of 4 mL oleic acid and 16 mL octadecene, and then 2 Heated to 160 °C under atmosphere, stirred to form a clear solution and cooled to room temperature; additionally weighed 0.148 g NH 4 F and 0.1 g NaOH were dissolved in 10 mL of methanol, stirred to form a clear solution, then added dropwise to the above solution, and stirred at room temperature for 30 min; 2 Heat the solution to 60 °C under the atmosphere to remove methanol, then heat to 300 °C at a heating rate of 10-15 °C / min, and keep for 1 h; cool to room temperature, a white precipitate appears, centrifuge to separate the supernatant from the precipitate , the obtained precipitate was washed several times with cyclohexane and absolute ethanol to remove the by-products of the reaction; the precipitate was vacuum-dried at 50 °C to obtain the hexagonal pha...

example 2

[0019] Example 2: NaCeF 4 : For the preparation of 0.1Dy nanocrystals, first weigh 0.319 g CeCl 3 ·6H 2 O and 0.037 g DyCl 3 ·6H 2 O was dissolved in a mixed solvent of 5 mL oleic acid and 15 mL octadecene, and then 2 Heated to 150 °C under atmosphere, stirred to form a clear solution and cooled to room temperature; additionally weighed 0.148 g NH 4 F and 0.1 g NaOH were dissolved in 10 mL of methanol, stirred to form a clear solution, then added dropwise to the above solution, and stirred at room temperature for 30 min; 2 Heat the solution to 60 °C under the atmosphere to exclude methanol, then heat to 310 °C at a heating rate of 10-15 °C / min, and keep warm for 0.5 h; cool to room temperature, a white precipitate appears, centrifuge to separate the supernatant from the precipitate , the obtained precipitate was washed several times with cyclohexane and absolute ethanol to remove the by-products of the reaction; the precipitate was vacuum-dried at 50 °C to obtain the he...

example 3

[0020] Example 3: NaCeF 4 : For the preparation of 0.05Tb nanocrystals, first weigh 0.337 g CeCl 3 ·6H 2 O and 0.019 g TbCl 3 ·6H 2 O was dissolved in a mixed solvent of 6 mL oleic acid and 14 mL octadecene, and then 2 Heated to 120 °C under atmosphere, stirred to form a clear solution and cooled to room temperature; additionally weighed 0.148 g NH 4 F and 0.1 g NaOH were dissolved in 10 mL of methanol, stirred to form a clear solution, then added dropwise to the above solution, and stirred at room temperature for 30 min; 2 Heat the solution to 60 °C under atmosphere to exclude methanol, then heat to 290 °C at a heating rate of 10-15 °C / min, and keep warm for 2 h; cool to room temperature, a white precipitate appears, centrifuge to separate the supernatant from the precipitate , the obtained precipitate was washed several times with cyclohexane and absolute ethanol to remove the by-products of the reaction; the precipitate was vacuum-dried at 50 °C to obtain the hexagon...

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Abstract

The invention provides a synthesis method of rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline. The synthesis method comprises the following steps of: using oleic acid and octadecene as solvents, mixing the cerium chloride and rare-earth chloride under the atmosphere of nitrogen, maintaining the temperature at 120-160 DEG C, stirring for a certain peroid of time, cooling the mixture to the room temperature, adding a methanol solution containing sodium hydroxide and ammonium fluoride to the cooled mixture, stirring for a certain peroid of time, heating the stirred mixture under the atmosphere of nitrogen so as to remove methanol, heating to 250-320 DEG C under the atmosphere of nitrogen to react for a certain peroid of time, cooling to room temperature, carrying out centrifugal separation to obtain a reactant, and washing and drying the reactant to obtain the rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline. The rare earth doped hexagonal-phase cerium sodium fluoride nanocrystalline prepared by using the synthesis method is better in uniform dispersity and excellent in down-conversion and up-conversion luminescence properties.

Description

technical field [0001] The invention relates to a method for synthesizing rare earth-doped inorganic nanocrystals, in particular to a method for synthesizing rare earth-doped hexagonal sodium cerium fluoride nanocrystals. Background technique [0002] Rare-earth-doped inorganic nanocrystals have been used in the green field for more than half a century due to their comprehensive advantages such as high photochemical stability, narrow emission linewidth, long fluorescence lifetime, high luminous efficiency, almost non-toxicity and tunable fluorescence emission wavelength. It can be widely used in lighting source, nano optoelectronic device, flat panel display, biomarker and other fields. With the rapid development of nanotechnology, especially the emergence of new materials and new synthesis methods, people are more and more interested in rare earth doped nanoluminescent materials. [0003] In recent years, a large number of literatures have reported the synthesis and spectr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 刘丽琴陈学元涂大涛刘永升朱浩淼
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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