Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal

A technology of fluoride chloride and nanocrystals, which is applied in the direction of chemical instruments and methods, luminescent materials, etc., can solve the problems that have not been seen to successfully prepare monodisperse alkaline earth fluoride chloride nanocrystals, and achieve uniform shape, high yield, and preparation technically simple effect

Inactive Publication Date: 2012-06-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there has been no report on the successful preparation of monodisperse alkaline earth fluoride chloride nanocrystals so far.

Method used

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  • Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal
  • Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal
  • Preparation method for alkaline earth fluo-chloride up-conversion luminescence nanometer crystal

Examples

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Effect test

example 1

[0016] Example 1: 0.5mmol strontium trifluoroacetate Sr (CF 3 COO) 2 , 10mL oleic acid and 10mL octadecene were added to a 100mL three-neck flask, heated to 100°C for 30 minutes under the protection of nitrogen atmosphere to remove water and oxygen, then continue to heat to 280°C and hold for 2 hours to generate strontium fluoride SrF 2 Nanocrystalline: After cooling to room temperature, quickly add a mixture of 0.5mmol trichloroacetic acid, 10mL oleic acid and 10mL octadecene, and heat to 100°C for 30 minutes under the protection of nitrogen atmosphere to remove water and oxygen. Continue heating to 250°C under protection and keep it warm for 30 minutes to generate strontium fluoride chloride SrFCl nanocrystals; the obtained nanocrystals are washed with a mixture of ethanol and cyclohexane, and dried at 60°C to obtain the final product.

[0017] Powder X-ray diffraction pattern ( figure 1 ) analysis showed that the samples before and after chlorination were SrF 2 and SrFCl...

example 2

[0018] Example 2: 0.1mmol strontium trifluoroacetate Sr (CF 3 COO) 2 , 10mL oleic acid and 10mL octadecene were added to a 100mL three-neck flask, heated to 100°C for 30 minutes under the protection of nitrogen atmosphere to remove water and oxygen, then continue to heat to 280°C and hold for 2 hours to generate strontium fluoride SrF 2 Nanocrystalline: after cooling to room temperature, quickly add a mixture of 0.1mmol trichloroacetic acid, 10mL oleic acid and 10mL octadecene, and heat to 100°C under the protection of nitrogen atmosphere for 30 minutes to remove water and oxygen. Continue heating to 250°C under protection and keep it warm for 30 minutes to generate strontium fluoride chloride SrFCl nanocrystals; the obtained nanocrystals are washed with a mixture of ethanol and cyclohexane, and dried at 60°C to obtain the final product.

[0019] Powder X-ray diffraction analysis showed that the chlorinated product was pure SrFCl phase; transmission electron microscope observ...

example 3

[0020] Example 3: 1.0mmol strontium trifluoroacetate Sr (CF 3 COO) 2 , 10mL oleic acid and 10mL octadecene were added to a 100mL three-neck flask, heated to 100°C for 30 minutes under the protection of nitrogen atmosphere to remove water and oxygen, then continue to heat to 280°C and hold for 2 hours to generate strontium fluoride SrF 2 Nanocrystalline: After cooling to room temperature, quickly add a mixture of 1.0mmol trichloroacetic acid, 10mL oleic acid and 10mL octadecene, and heat to 100°C for 30 minutes under the protection of nitrogen atmosphere to remove water and oxygen. Continue heating to 250°C under protection and keep it warm for 30 minutes to generate strontium fluoride chloride SrFCl nanocrystals; the obtained nanocrystals are washed with a mixture of ethanol and cyclohexane, and dried at 60°C to obtain the final product.

[0021] Powder X-ray diffraction analysis showed that the chlorinated product was pure SrFCl phase; transmission electron microscope observ...

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Abstract

The invention provides a preparation method for an alkaline earth fluo-chloride up-conversion luminescence nanometer crystal, which belongs to the technical field of preparation of inorganic materials. The method comprises the following steps: with an alkaline earth trifluoroacetic acid compound as a raw material, heating the compound in a mixed solvent of oleic acid and octadecene at a temperature of 260 to 310 DEG C under the protection of a nitrogen atmosphere and carrying out insulation for 1 to 6 h so as to prepare an alkaline earth fluoride nanometer crystal; and adding trichloroacetic acid, heating an obtained mixture at a temperature of 120 to 280 DEG C, carrying out insulation for 30 min, chloridizing the resultant fluoride nanometer crystal so as to obtain the monodispersed alkaline earth fluo-chloride nanometer crystal. After doping of rare earth ions like Yb<3+> and Er<3+>, the synthesized fluo-chloride nanometer crystal has good yellow color up-conversion luminescence characteristics and is expected to be used in a wide variety of fields of optical displays, solar cells, biological markers, etc.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic materials, and relates to a method for preparing rare earth ion-doped monodisperse alkaline earth fluoride nanocrystals with excellent up-conversion luminescence characteristics through a seed crystal chlorination method. technical background [0002] In recent years, rare earth ion-doped upconversion luminescent nanomaterials have attracted great attention from the scientific community due to their broad application prospects in the fields of lasers, light displays, solar cells, and biomarkers. Selecting a suitable matrix material is one of the key conditions to achieve high luminescence quantum efficiency of doped rare earth ions. Generally speaking, the lower the energy of the matrix phonon, the lower the non-radiative transition probability of rare earth ions, and the higher the luminescence intensity of the material. Heavy halides such as iodide, bromide and chloride have ve...

Claims

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Application Information

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IPC IPC(8): C09K11/61C09K11/85
Inventor 陈大钦王元生
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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