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a kind of yb 3+ /er 3+ co-doped mnf 2 Preparation method of inner hollow sphere

A hollow sphere, co-doping technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems that the preparation method with specific morphology is less involved, and the preparation method of inner hollow sphere has not been reported, and achieves uniform morphology and synthesis. The process is easy to realize and the effect of high luminous efficiency

Inactive Publication Date: 2016-08-31
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, most of the existing preparation methods are based on the preparation method of nanocrystals, and rarely involve the preparation method with specific morphology, and the specific preparation method of the inner hollow sphere has not yet been reported.

Method used

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  • a kind of yb  <sup>3+</sup> /er  <sup>3+</sup> co-doped mnf  <sub>2</sub> Preparation method of inner hollow sphere
  • a kind of yb  <sup>3+</sup> /er  <sup>3+</sup> co-doped mnf  <sub>2</sub> Preparation method of inner hollow sphere
  • a kind of yb  <sup>3+</sup> /er  <sup>3+</sup> co-doped mnf  <sub>2</sub> Preparation method of inner hollow sphere

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Experimental program
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Embodiment 1

[0027] First provide an ethylene glycol solution containing PEI, the mass fraction of PEI is 5%; then dissolve ytterbium acetate (0.36mmol), manganese acetate (1.6mmol), and erbium acetate (0.04mmol) in the above solution, and stir well Finally, solution A is formed; while stirring the solution A, ammonium fluoride is added, and the mixed solution B is formed after stirring evenly, wherein the ratio of the total moles of ytterbium acetate, manganese acetate, and erbium acetate to the moles of ammonium fluoride The ratio is 1:2, the mixture B is put into a 25ml autoclave, the filling degree of the autoclave is 70%, and the product is obtained after the autoclave is placed in a temperature environment of 180°C for 12 hours; Finally, the product was washed several times with absolute ethanol and water, and dried in a vacuum oven at 80°C for several hours to obtain the Yb 3+ / Er 3+ co-doped MnF 2 Inner hollow ball. The product was identified as MnF by X-ray powder diffraction ...

Embodiment 2

[0029] First provide an ethylene glycol solution containing PEI, the mass fraction of PEI is 7%; then dissolve ytterbium acetate (0.40mmol), manganese acetate (1.6mmol), and erbium acetate (0.04mmol) in the above solution, and stir well Finally, solution A is formed; while stirring the solution A, ammonium fluoride is added, and the mixed solution B is formed after stirring evenly, wherein the ratio of the total moles of ytterbium acetate, manganese acetate, and erbium acetate to the moles of ammonium fluoride The ratio is 1:2.2; the mixture B is put into a 25ml autoclave, the filling degree of the autoclave is 80%, and the product is obtained after the autoclave is placed in a temperature environment of 190°C for 10 hours; Finally, the product was washed several times with absolute ethanol and water, and dried in a vacuum oven at 80°C for several hours to obtain the Yb 3+ / Er 3+ co-doped MnF 2 Inner hollow ball. The morphology of the material was obtained from the results ...

Embodiment 3

[0031] First provide an ethylene glycol solution containing PEI, the mass fraction of PEI is 7%; then dissolve ytterbium acetate (0.32mmol), manganese acetate (1.6mmol), and erbium acetate (0.04mmol) in the above solution, and stir well Finally, solution A is formed; while stirring the solution A, ammonium fluoride is added, and the mixed solution B is formed after stirring evenly, wherein the ratio of the total moles of ytterbium acetate, manganese acetate, and erbium acetate to the moles of ammonium fluoride The ratio is 1:1.8; the mixture B is put into a 25ml autoclave, the filling degree of the autoclave is 60%, and the product is obtained after the autoclave is placed in a temperature environment of 200°C for 10 hours; Finally, the product was washed several times with absolute ethanol and water, and dried in a vacuum oven at 80°C for several hours to obtain the Yb 3+ / Er 3+ co-doped MnF 2 Inner hollow ball. And the obtained product was identified by X-ray powder diffr...

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Abstract

The invention relates to the field of preparation methods of upconversion materials, particularly a preparation method of an Yb<3+> / Er<3+>-codoped MnFe internally-hollow sphere. The preparation method comprises the following steps: providing a PEI (polyetherimide)-containing ethylene glycol; uniformly stirring reaction raw materials to form a mixed solution; putting the mixed solution into a high-pressure reaction kettle, wherein the compactness of the high-pressure reaction kettle is 60-80%; and putting the high-pressure reaction kettle in a 180-200-DEG C environment to react for 8-12 hours, thereby obtaining the product. The Yb<3+> / Er<3+>-codoped MnFe is an internally-hollow sphere structure, and has the advantages of uniform size and shape and high luminescence efficiency.

Description

technical field [0001] The invention relates to the field of preparation methods of up-conversion materials, in particular to a Yb 3+ / Er 3+ co-doped MnF 2 The preparation method of the inner hollow sphere. Background technique [0002] Rare-earth-doped upconversion fluorescent nanomaterials have unique luminescent properties, which aroused people's extensive research interest at the end of the 20th century, especially at the beginning of the 21st century. The up-conversion process is a nonlinear optical process, which is characterized by the continuous absorption of more than two pump photons, and the generation of radiation with a shorter wavelength than the pump light through the metastable energy level. Due to the effective shielding effect of the 5s and 5p orbitals, the absorption and emission lines generated by the transition between the inner 4f electron levels of rare earth ions have high quantum yield, long lifetime and high stability. Therefore, rare earth-dope...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/61
Inventor 赵丰华侯婷婷王立开李志坚
Owner GUANGDONG UNIV OF TECH
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