Preparation method of small-sized NaYF4 nano substrate material with hexagonal phase by inducement

Abstract

The invention belongs to the technical field of a nano up-conversion luminescent material, in particular relates to a preparation method for a small-sized NaYF4 nano substrate material with a hexagonal phase by inducement with rare earth nano crystal nucleus. In the method, rare earth ions are doped in the NaYF4 nano substrate material so as to obtain a nano material with a low up-conversion luminescence threshold and high luminescence strength. In the method, the small-sized beta-NaYF4 nano substrate material is generated by inducement with a hydrothermal (solvent) process in the presence of rare earth fluoride nano crystal nucleus, wherein the size of the particle is from 20nm to 200nm, and distribution of the size is even. According to the invention, a preparation method of the small-sized NaYF4 nano substrate material with the hexagonal phase is expanded, and the problem that the NaYF4 nano substrate material, especially water-soluble NaYF4 nano substrate material is difficultly generated at low temperature, is solved. By using the nano up-conversion luminescent material, the demand on biological fluorescent identification probes and disease diagnosis and treatment materials is met, and a foundation is established for the practicable application of the up-conversion luminescent material.

Description

technical field

[0001] The invention belongs to the technical field of nanoscale up-conversion luminescent materials, and in particular relates to a method for preparing small-sized hexagonal phase NaYF by induction of rare earth fluoride nanocrystals as nuclei 4 nano-matrix material approach, the NaYF 4 After the nano-matrix material is doped with rare earth ions, nano-materials with low up-conversion luminescence threshold and high luminous intensity can be obtained. Background technique

[0002] Up-conversion luminescent materials refer to materials that can absorb low-frequency photons and emit high-frequency photons. Up-conversion luminescent materials have very important application prospects in laser, communication, energy, medical, military, aerospace and people's daily life. In recent years, with the development of micro- and nano-technology, up-conversion micro- and nano-materials have been gradually applied in fields such as energy, anti-counterfeiting, biology,...

Examples

Embodiment 1

[0038] (1) Prepare various reaction reagent solutions. Weigh 12.1306 grams of yttrium chloride, add 80ml of ethylene glycol, and stir until dissolved. The ethylene glycol solution of yttrium chloride prepared at this time is preserved as a storage solution, and the concentration of yttrium ions in the solution is 0.5mol / L. As above, weigh 1.528 grams of erbium chloride, 7.7472 grams of ytterbium chloride, 3.0663 grams of thulium chloride, 31.16 grams of lutetium chloride, and 4.675 grams of sodium chloride, and add 80ml of ethylene glycol to make the concentration 0.05mol / L respectively , 0.25mol / L, 0.1mol / L, 1mol / L, 1mol / L ethylene glycol solutions of various chlorides.

[0039] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Take by weighing 0.5 gram of surfactant PVP, add 8ml of ethylene glycol, stir until dissolving, take lutetium chloride solution 1ml prepared in step (1) in proportion, sodium c...

Embodiment 2

[0043] (1) With embodiment 1 step (1).

[0044] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Weigh 0.5 gram of surfactant PVP, add 8ml of ethylene glycol, stir until dissolved, take 1ml of lutetium chloride solution and 1ml of sodium chloride solution prepared in step (1) in proportion and add it to the PVP solution, and stir magnetically at room temperature 1 hour. Add 8 ml of ethylene glycol solution containing 0.56 g of potassium fluoride, and stir for 30 minutes. The above mixed solution was transferred to a reaction kettle, the temperature was 180 degrees Celsius, and the reaction time was 24 hours. After the reaction, the dispersed NaLuF 4 Ethylene glycol solution of nanocrystals. NaLuF 4 The nanocrystals are pure cubic phase with an average particle size of 25nm.

[0045] (3) The rare earth fluoride nanocrystal nucleus prepared in step (2) induces the generation of small-sized, hexagon...

Embodiment 3

[0048] (1) With embodiment 1 step (1).

[0049] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Take by weighing 0.5 gram of surfactant PVP, add 8ml ethylene glycol, stir until dissolving, take lutetium chloride solution 1ml prepared in step (1), sodium chloride solution 1ml in proportion and add in the PVP solution, under normal temperature magnetic stirring 1 Hour. Add 8 ml of a solution of 0.56 g of potassium fluoride in 4 ml of ethylene glycol and stir for 30 minutes. The above mixed solution was transferred to a reaction kettle, the temperature was 180 degrees Celsius, and the reaction time was 24 hours. After the reaction, the dispersed NaLuF 4 Ethylene glycol solution of nanocrystals. NaLuF 4 The nanocrystals are pure cubic phase with an average particle size of 25nm.

[0050] (3) The rare earth fluoride nanocrystal nucleus prepared in step (2) induces the generation of small-sized, hexag...

technical field

[0001] The invention belongs to the technical field of nanoscale up-conversion luminescent materials, and in particular relates to a method for preparing small-sized hexagonal phase NaYF by induction of rare earth fluoride nanocrystals as nuclei 4 nano-matrix material approach, the NaYF 4 After the nano-matrix material is doped with rare earth ions, nano-materials with low up-conversion luminescence threshold and high luminous intensity can be obtained. Background technique

[0002] Up-conversion luminescent materials refer to materials that can absorb low-frequency photons and emit high-frequency photons. Up-conversion luminescent materials have very important application prospects in laser, communication, energy, medical, military, aerospace and people's daily life. In recent years, with the development of micro- and nano-technology, up-conversion micro- and nano-materials have been gradually applied in fields such as energy, anti-counterfeiting, biology,...

Examples

Embodiment 1

[0038] (1) Prepare various reaction reagent solutions. Weigh 12.1306 grams of yttrium chloride, add 80ml of ethylene glycol, and stir until dissolved. The ethylene glycol solution of yttrium chloride prepared at this time is preserved as a storage solution, and the concentration of yttrium ions in the solution is 0.5mol / L. As above, weigh 1.528 grams of erbium chloride, 7.7472 grams of ytterbium chloride, 3.0663 grams of thulium chloride, 31.16 grams of lutetium chloride, and 4.675 grams of sodium chloride, and add 80ml of ethylene glycol to make the concentration 0.05mol / L respectively , 0.25mol / L, 0.1mol / L, 1mol / L, 1mol / L ethylene glycol solutions of various chlorides.

[0039] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Take by weighing 0.5 gram of surfactant PVP, add 8ml of ethylene glycol, stir until dissolving, take lutetium chloride solution 1ml prepared in step (1) in proportion, sodium c...

Embodiment 2

[0043] (1) With embodiment 1 step (1).

[0044] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Weigh 0.5 gram of surfactant PVP, add 8ml of ethylene glycol, stir until dissolved, take 1ml of lutetium chloride solution and 1ml of sodium chloride solution prepared in step (1) in proportion and add it to the PVP solution, and stir magnetically at room temperature 1 hour. Add 8 ml of ethylene glycol solution containing 0.56 g of potassium fluoride, and stir for 30 minutes. The above mixed solution was transferred to a reaction kettle, the temperature was 180 degrees Celsius, and the reaction time was 24 hours. After the reaction, the dispersed NaLuF 4 Ethylene glycol solution of nanocrystals. NaLuF 4 The nanocrystals are pure cubic phase with an average particle size of 25nm.

[0045] (3) The rare earth fluoride nanocrystal nucleus prepared in step (2) induces the generation of small-sized, hexagon...

Embodiment 3

[0048] (1) With embodiment 1 step (1).

[0049] (2) Preparation Using ethylene glycol as a solvent to prepare rare earth fluoride nanocrystal nuclei by solvothermal method. Take by weighing 0.5 gram of surfactant PVP, add 8ml ethylene glycol, stir until dissolving, take lutetium chloride solution 1ml prepared in step (1), sodium chloride solution 1ml in proportion and add in the PVP solution, under normal temperature magnetic stirring 1 Hour. Add 8 ml of a solution of 0.56 g of potassium fluoride in 4 ml of ethylene glycol and stir for 30 minutes. The above mixed solution was transferred to a reaction kettle, the temperature was 180 degrees Celsius, and the reaction time was 24 hours. After the reaction, the dispersed NaLuF 4 Ethylene glycol solution of nanocrystals. NaLuF 4 The nanocrystals are pure cubic phase with an average particle size of 25nm.

[0050] (3) The rare earth fluoride nanocrystal nucleus prepared in step (2) induces the generation of small-sized, hexag...

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