Preparation method of rare earth upconversion nanomaterial controlled by transition metal ion in morphology

A transition metal ion, rare earth upconversion technology, applied in the field of nanomaterials, to achieve the effect of good size

CN107312541AInactive Publication Date: 2017-11-03DALIAN UNIV OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2017-11-03
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a preparation method of a rare earth upconversion nanomaterial controlled by a transition metal ion in morphology and belongs to the technical field of nanometer material science. According to the preparation method disclosed by the invention, the rare earth upconversion nanomaterial, namely NaY(Ag)F4:Yb, Er doped with a series of silver ions with different concentrations and gradients is prepared by adopting a solvothermal / hydrothermal method. The result shows that the size, crystal appearance and surface morphology of the prepared rare earth upconversion nanomaterial NaY(Ag)F4:Yb, Er obviously and regularly change along with gradient change of the concentration of the silver ions. Therefore, the morphology change of the rare earth upconversion nanomaterial NaY(Ag)F4:Yb, Er can be controlled by controlling the concentration of the silver ions. The method for controlling the rare earth upconversion nanomaterial has the advantages that one kind of ions is needed, and selected control factors are few; and simplicity and convenience in operation are realized, so the method is a relatively-simple and excellent method for controlling the rare earth upconversion nanomaterial.
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Description

technical field

[0001] The invention belongs to the technical field of nanomaterials, and mainly relates to a preparation method for regulating the morphology of rare earth upconversion nanomaterials by transition metal ions. Background technique

[0002] Rare-earth up-conversion luminescent nanoparticles (UCNPs) are a kind of rare-earth ion doping that can continuously absorb two or more long-wavelength low-energy photons through a multi-photon mechanism under excitation at near-infrared wavelengths, and emit a short-wavelength photon. Photons of high energy wavelength, that is, fluorescent nanomaterials that emit visible light. This phenomenon belongs to the anti-Stokes luminescence displacement phenomenon. Rare-earth upconversion luminescent nanoparticles usually consist of three parts, namely matrix material, sensitizer and activator. Among the rare earth nanoparticles doped with lanthanide metal ions that have developed rapidly in recent years, NaYF 4 Rare-earth up-c...

Examples

Embodiment 1

[0020] (1) Prepare 0.5mol / L of Y(NO 3 ) 3 , 0.2mol / L of Yb(NO 3 ) 3 and Er(NO 3 ) 3 Solution, the AgNO of 0.1mol / L used 3 Standard solutions are purchased.

[0021] (2) Preparation of Ag by solvothermal / hydrothermal method + Doped NaYF 4 : Yb, Er rare earth up-conversion nanoparticles.

[0022] (3) Calculated according to the molar ratio of elements, Ag:Y:Yb:Er=1:79:18:2; measure 3.16mL of 0.5mol / L Y(NO 3 ) 3 solution, 1.4mL of 0.1mol / L AgNO 3 Standard solution, 1.8mL of 0.2mol / L Yb(NO 3 ) 3 solution and 0.2mL of 0.2mol / L Er(NO 3 ) 3 The solution was sequentially added to a mixed solution containing 0.6g NaOH solid, 3mL deionized water, 10mL oleic acid and 20mL ethanol, and was under magnetic stirring, and then 4mL deionized water containing 8mmol NaF was added dropwise to the above mixed solution middle.

[0023] (4) After 30 min of magnetic stirring at room temperature, the gel solution formed in step (3) was transferred to a 75 mL polytetrafluoroethylene rea...

Embodiment 2

[0026] (1) Prepare 0.5mol / L of Y(NO 3 ) 3 , 0.2mol / L of Yb(NO 3 ) 3 and Er(NO 3 ) 3Solution, the AgNO of 0.1mol / L used 3 Standard solutions are purchased.

[0027] (2) Preparation of Ag by solvothermal / hydrothermal method + Doped NaYF 4 : Yb, Er rare earth up-conversion nanoparticles.

[0028] (3) Calculated according to the molar ratio of elements, Ag:Y:Yb:Er=7:73:18:2; measure 2.92mL of 0.5mol / L Y(NO 3 ) 3 solution, 2.0mL of 0.1mol / L AgNO 3 Standard solution, 1.8mL of 0.2mol / L Yb(NO 3 ) 3 solution and 0.2mL of 0.2mol / L Er(NO 3 ) 3 The solution was sequentially added to a mixed solution containing 0.6g NaOH solid, 3mL deionized water, 10mL oleic acid and 20mL ethanol, and was under magnetic stirring, and then 4mL deionized water containing 8mmol NaF was added dropwise to the above mixed solution middle.

[0029] (4) After 30 min of magnetic stirring at room temperature, the gel solution formed in step (3) was transferred to a 75 mL polytetrafluoroethylene reac...

Embodiment 3

[0032] (1) Prepare 0.5mol / L of Y(NO 3 ) 3 , 0.2mol / L of Yb(NO 3 ) 3 and Er(NO 3 ) 3 Solution, the AgNO of 0.1mol / L used 3 Standard solutions are purchased.

[0033] (2) Preparation of Ag by solvothermal / hydrothermal method + Doped NaYF 4 : Yb, Er rare earth up-conversion nanoparticles.

[0034] (3) Calculated according to the molar ratio of elements, Ag:Y:Yb:Er=11:69:18:2; measure 2.76mL of 0.5mol / L Y(NO 3 ) 3 solution, 2.4mL of 0.1mol / L AgNO 3 Standard solution, 1.8mL of 0.2mol / L Yb(NO 3 ) 3 solution and 0.2mL of 0.2mol / L Er(NO 3 ) 3 The solution was sequentially added to a mixed solution containing 0.6g NaOH solid, 3mL deionized water, 10mL oleic acid and 20mL ethanol, and was under magnetic stirring, and then 4mL deionized water containing 8mmol NaF was added dropwise to the above mixed solution middle.

[0035] (4) After 30 min of magnetic stirring at room temperature, the gel solution formed in step (3) was transferred to a 75 mL polytetrafluoroethylene re...