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Preparation method of water-soluble red-green light tunable rare-earth doped up-conversion nano-material

A nano-material, water-soluble technology, applied in the direction of luminescent materials, material excitation analysis, chemical instruments and methods, etc., can solve the problems of limited application, large particle size, complex operation, etc., easy to achieve surface functionalization, and low synthesis temperature , the effect of fluorescence enhancement

Inactive Publication Date: 2014-08-13
TIANJIN NORMAL UNIVERSITY
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Problems solved by technology

[0006] In recent years, the solvothermal method has received more and more attention. Most of the classic organic phase synthesis uses organic solvents such as octadecane and ethylene glycol, and oleic acid as a ligand. The synthesized particles have uniform particle size and small particles. And the fluorescence is strong, but the conditions of the synthesis process are harsh, the temperature is high and the environment is not friendly, the biocompatibility of the synthesized particles is poor, and the exchange or oxidation of the ligand is required. However, this process is complicated to operate and the cost is high.
The particles synthesized by using water as a solvent method have large particle size, uneven size, insoluble in water, and difficult surface functionalization, which limits its further application

Method used

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  • Preparation method of water-soluble red-green light tunable rare-earth doped up-conversion nano-material
  • Preparation method of water-soluble red-green light tunable rare-earth doped up-conversion nano-material
  • Preparation method of water-soluble red-green light tunable rare-earth doped up-conversion nano-material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Yttrium oxide Y 2 0 3 (0.4mmol, Mr=224.81), Ytterbium oxide Yb 2 0 3 (0.09mmol, Mr=394.08), Erbium oxide 2 O 3 (0.01mmol, Mr=382.52), that is Y, 0.8mmol, Yb, 0.18mol, Er, 0.02mmol, the ratio of the amount of ytterbium to erbium Yb / Er=9 / 1, Y+Yb+Er=1mmol, F / Y+Yb+Er=4 / 1, 0.15g polyethyleneimine PEI, solvent: 15ml ethylene glycol, temperature 200oC.

[0038] First, add 0.0903g yttrium oxide Y 2 0 3 , 0.0355g ytterbium oxide Yb 2 0 3 ,0.0038g Erbium oxide Er 2 0 3 (The ratio of the amount of ytterbium to erbium substance Yb / Er=9 / 1) Put into a 50ml beaker, add 1.5ml concentrated nitric acid, 4ml high purity water, in a fume hood, adjust the temperature of the heating mantle to 100oC, and the solid powder after 5min It will dissolve and evaporate to dryness. When placed in the sun, a crystal film can be seen at the bottom of the beaker. Add 4ml of high-purity water and evaporate to dryness.

[0039] Secondly, weigh 0.1680g sodium fluoride NaF (F / Y+Yb+Er=4 / 1), add 9ml ethylene...

Embodiment 2

[0044] Yttrium oxide Y 2 0 3 (0.4mmol, Mr=224.81), Ytterbium oxide Yb 2 0 3 (0.09mmol, Mr=394.08), Erbium oxide 2 O 3 (0.01mmol, Mr=382.52), that is Y, 0.8mmol, Yb, 0.18mol, Er, 0.02mmol, the ratio of the amount of ytterbium to erbium Yb / Er=9 / 1, Y+Yb+Er=1mmol, F / Y+Yb+Er=4 / 1, 0.15g polyethyleneimine PEI, solvent: 12ml ethylene glycol + 3ml high purity water, temperature 180oC.

[0045] First, add 0.0903g yttrium oxide Y 2 0 3 , 0.0355g ytterbium oxide Yb 2 0 3 ,0.0038g Erbium oxide Er 2 0 3 (The ratio of the amount of ytterbium to erbium substance Yb / Er=9 / 1) Put into a 50ml beaker, add 2ml concentrated nitric acid, 4ml high purity water, in a fume hood, adjust the temperature of the electric heating mantle to 100oC, the solid powder will be It will dissolve and evaporate to dryness. A crystal film can be seen at the bottom of the beaker in the sun. Add 4ml of high-purity water and evaporate to dryness.

[0046] Secondly, weigh 0.1680g (F / Y+Yb+Er=4 / 1) NaF, add 9ml ethylene glyc...

Embodiment 3

[0050] Yttrium oxide Y 2 0 3 (0.4mmol, Mr=224.81), Ytterbium oxide Yb 2 0 3 (0.09mmol, Mr=394.08), Erbium oxide 2 O 3 (0.01mmol, Mr=382.52), that is Y, 0.8mmol, Yb, 0.18mol, Er, 0.02mmol, the ratio of the amount of ytterbium to erbium Yb / Er=9 / 1, Y+Yb+Er=1mmol, F / Y+Yb+Er=4 / 1, 0.15g polyethyleneimine PEI, solvent: 6ml ethylene glycol + 9ml high purity water, temperature 160oC.

[0051] First, add 0.0903g yttrium oxide Y 2 0 3 , 0.0355g ytterbium oxide Yb 2 0 3 ,0.0038g Erbium oxide Er 2 0 3 (The ratio of the amount of ytterbium to erbium substance Yb / Er=9 / 1) Put it in a 50ml beaker, add 3ml concentrated nitric acid, 4ml high purity water, in a fume hood, adjust the temperature of the electric heating mantle to 100oC, the solid powder will be It will dissolve and evaporate to dryness. When placed in the sun, a crystal film can be seen at the bottom of the beaker. Add 4ml of high-purity water and evaporate to dryness.

[0052] Secondly, weigh 0.1680g (F / Y+Yb+Er=4 / 1) sodium fluori...

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Abstract

The invention discloses a preparation method of a water-soluble red-green light tunable rare earth-doped up-conversion nanomaterial, which mainly uses ethylene glycol-high-purity water solvent system in Y (0.8mol), Y+Yb+Er=1mmol, Under the ratio of Yb / Er=1 / 1-9 / 1, F / Y+Yb+Er=4 / 1-16 / 1, the dosage of PEI is 0.15-0.25g, pH is 8-9, temperature is 160-200oC, Under the condition of reaction for 1-8h, the particles with a particle size of 40-80nm and tunable red and green light were synthesized, which have certain water solubility. After further simple treatment, the surface PEI was functionalized to achieve excellent water solubility. It can be applied to detect folic acid with high sensitivity and high selectivity. Compared with the traditional oil-phase method, the method for solvothermally synthesizing water-soluble nanoparticles provided by the present invention has the advantages of low cost, green, simple and safe process, low synthesis temperature and easier surface functionalization.

Description

[0001] This patent is funded by the General Project 21375095 of the National Natural Science Foundation of China, the National Excellent Doctoral Dissertation Author Special Fund FANEDD-201023, and the Tianjin Applied Basic Research Program Key Project 12JCZDJC21700. technical field [0002] The invention belongs to the field of preparation of fluorescent nanomaterials, in particular to a preparation method of a water-soluble red-green light tunable rare earth-doped up-conversion nanomaterial, which is applied to the detection of folic acid. Background technique [0003] Rare earth ions have rich energy level structures and excellent optical properties. In recent years, rare earth doped upconversion nanomaterials have shown important application prospects in the fields of biomolecular labeling and bioimaging. Traditional down-converting fluorescent materials (high-energy short-wave excitation, low-energy long-wave emission) such as organic dyes and II-VI semiconductor quantum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85G01N21/64
Inventor 李妍孙玉绣胡悦立
Owner TIANJIN NORMAL UNIVERSITY
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