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Preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles

A nanoparticle and calcium fluoride technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of limiting breadth and depth, and achieve the effect of low cost, easy source and easy implementation

Inactive Publication Date: 2016-02-03
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the huge specific surface area of ​​nanoparticles, it is easy to form agglomerates, which limits the breadth and depth of its application fields.
Although people have made certain improvements to this problem, there are few reports that can have excellent colloidal dispersion in water systems while maintaining good fluorescence properties.

Method used

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  • Preparation method of water-soluble Eu&lt;3+&gt;-doped calcium fluoride nano particles
  • Preparation method of water-soluble Eu&lt;3+&gt;-doped calcium fluoride nano particles
  • Preparation method of water-soluble Eu&lt;3+&gt;-doped calcium fluoride nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Blend 10 mL of 0.01 mol / L europium nitrate solution and 10 mL of 1 mol / L calcium nitrate solution;

[0040] 2) Add 10 mL of 0.67 mol / L sodium citrate solution to the mixed solution in step 1) dropwise, and stir for 15 min;

[0041] 3) Add 10 mL of 2.03 mol / L sodium fluoride solution dropwise to the mixed solution in step 2) at room temperature, and stir for 15 min;

[0042] 4) Transfer the mixed liquid in step 3) to a closed reactor, react at 150° C. for 12 hours, and then naturally cool to room temperature to obtain a reaction liquid;

[0043] 5) Use a high-speed centrifuge to centrifuge the reaction solution in step 4) to obtain a precipitate, and use deionized water and absolute ethanol to alternately centrifuge and wash 3 times to remove excess electrolyte in the system, then redisperse in water, adjust the pH to 9.5, water-soluble Eu 3+ Doped with calcium fluoride nanoparticles.

[0044] The resulting water-soluble Eu 3+ The X-ray diffraction pattern of dope...

Embodiment 2

[0046] 1) Blend 10 mL of 0.03 mol / L europium chloride solution and 10 mL of 1 mol / L calcium chloride solution;

[0047] 2) Add 10 mL of 0.8 mol / L sodium citrate solution dropwise to the mixed solution in step 1), and stir for 15 min;

[0048] 3) Add 10 mL of 2.09 mol / L potassium fluoride solution dropwise to the mixed solution in step 2) at room temperature, and stir for 15 min;

[0049] 4) Transfer the mixed solution in step 3) to a closed reactor, react at 180° C. for 6 hours, and then naturally cool to room temperature to obtain a reaction solution;

[0050] 5) Use a high-speed centrifuge to centrifuge the reaction solution in step 4) to obtain a precipitate, and use deionized water and absolute ethanol to alternately centrifuge and wash 3 times to remove excess electrolyte in the system, then redisperse in water, adjust the pH to 9, water-soluble Eu 3+Doped with calcium fluoride nanoparticles.

[0051] The resulting water-soluble Eu 3+ The X-ray diffraction pattern of ...

Embodiment 3

[0053] 1) Blend 10 mL of 0.05 mol / L europium chloride solution and 10 mL of 1 mol / L calcium acetate solution;

[0054] 2) Add 10 mL of 0.85 mol / L potassium citrate solution to the mixed solution in step 1) dropwise, and stir for 15 min;

[0055] 3) Add 10 mL of 2.15 mol / L sodium fluoride solution dropwise to the mixed solution in step 2) at room temperature, and stir for 15 min;

[0056] 4) Transfer the mixed solution in step 3) to a closed reactor, react at 90° C. for 24 hours, and then naturally cool to room temperature to obtain a reaction solution;

[0057] 5) Use a high-speed centrifuge to centrifuge the reaction solution in step 4) to obtain a precipitate, and use deionized water and absolute ethanol to alternately centrifuge and wash 3 times to remove excess electrolyte in the system, then redisperse in water, adjust the pH to 10, water-soluble Eu 3+ Doped with calcium fluoride nanoparticles.

[0058] The resulting water-soluble Eu 3+ The X-ray diffraction pattern o...

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Abstract

The invention relates to a preparation method of water-soluble Eu<3+>-doped calcium fluoride nano particles. The method is characterized in that a soluble europium salting solution and a soluble calcium salting solution are blended; under stirring condition, a soluble citric acid salting solution can be added drop by drop, under stirring condition, a soluble fluorine salting solution is added, the above mixed solution is transferred into an enclosed reactor and reacted for 3-24 hours at temperature of 90-180 DEG C, natural cooling to room temperature is carried out, and a reaction solution is obtained; the above reaction solution is centrifuged to obtain precipitate, deionized water and absolute ethyl alcohol are used for alternative centrifugation and washing for 3 times, excessive electrolyte in the precipitate is removed and is re-dispersed in water, and a pH value is adjusted, then the calcium fluoride water-soluble nano particles with high dispersibility can be obtained. The raw materials have the advantages of non toxicity and environmental protection, abundant source and easy acquisition, low cost, simple synthesis process, and easy operation; products quality is stable and technical repeatability is good, the crystallization degree and stability of the prepared calcium fluoride are good, and the method provides a certain experiment base and technical means in biological fluorescent labeling application.

Description

technical field [0001] The invention belongs to the field of preparation technology of inorganic materials, in particular to a water-soluble Eu 3+ Preparation method of doped calcium fluoride nanoparticles. Background technique [0002] Inorganic nano-fluorescent materials doped with rare earth elements have received more and more attention in recent years because of their stable luminescent properties, no photobleaching, and high fluorescence intensity. Due to its advantages in structure and characteristics, calcium fluoride has attracted much attention as a functional material, and its electrical, magnetic and photoelectric properties have been widely used. However, calcium fluoride nanocrystals doped with rare earth elements, due to their excellent fluorescence properties, are very low. The toxicity and low cost make it a leader in inorganic nano-fluorescent materials. However, due to the huge specific surface area of ​​nanoparticles, they are easy to form agglomerates,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61B82Y30/00
Inventor 谭军军陈小虎金小影胡兵
Owner HUBEI UNIV OF TECH
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