Preparation method for Er<3+>-Yb<3+>-co-doped NaYF4 fluorescent powder

A fluorescent powder and tetragonal phase technology, applied in the field of Er3+

Active Publication Date: 2015-12-02
FUZHOU UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102382654A discloses an up-conversion fluorescent nanocrystal with NaYF4 as the substrate and doped with Er3+ and Yb3+ ions A preparation method, which uses a solvothermal method to prepare a single pure hexagonal phase of NaYF4:Yb3+, Er3+ nano Particles, although the luminescence performance of the sample is good, but the reaction cycle is long, the luminescence color is single, and it is not easy to obtain samples with different luminescence colors by changing the process parameters
In addition, precipitation method and high-temperature solid-state method are often used to synthesize NaYF4 nanocrystals doped with rare earth ions, but the crystal phase and luminous color of the synthesized phosphor are relatively single.

Method used

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  • Preparation method for Er&lt;3+&gt;-Yb&lt;3+&gt;-co-doped NaYF4 fluorescent powder
  • Preparation method for Er&lt;3+&gt;-Yb&lt;3+&gt;-co-doped NaYF4 fluorescent powder

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Experimental program
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Effect test

Embodiment 1

[0025] 1) Weigh 0.27g solid powder yttrium acetate tetrahydrate, 0.072g solid powder ytterbium acetate tetrahydrate, 0.012g solid powder erbium acetate tetrahydrate and 0.04g solid sodium hydroxide;

[0026] 2) Measure 4mL of isopropanol, 4mL of ethanol, 1mL of trifluoroacetic acid and 3mL of water, add the solid powder into it, and stir for 3 hours to obtain transparent sol A;

[0027] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0028] 4) Put the colloidal substance B in a high-temperature furnace, raise the furnace temperature from room temperature to 300 °C at a rate of 4 °C / min., keep it warm for 1 hour, and take it out after cooling to room temperature with the furnace;

[0029] 5) Grinding to obtain Er that emits green light under 980nm laser excitation 3+ , Yb 3+ double doped YF 3 , hexagonal, tetragonal NaYF 4 Up-conversion phosphors with three-phase coexistence.

Embodiment 2

[0031] 1) Weigh 0.27g solid powder yttrium acetate tetrahydrate, 0.072g solid powder ytterbium acetate tetrahydrate, 0.012g solid powder erbium acetate tetrahydrate and 0.04g solid sodium hydroxide;

[0032] 2) Measure 4mL of isopropanol, 4mL of ethanol, 1mL of trifluoroacetic acid and 3mL of water, add the solid powder into it, and stir for 3 hours to obtain transparent sol A;

[0033] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0034] 4) Put the colloidal substance B in a high-temperature furnace, raise the temperature of the furnace from room temperature to 400 °C at a rate of 4 °C / min., keep it for 1 hour, and take it out after cooling to room temperature with the furnace;

[0035] 5) Grinding to obtain Er that emits green light under 980nm laser excitation 3+ , Yb 3+ double doped YF 3 , hexagonal, tetragonal NaYF 4 Up-conversion phosphors with three-phase coexistence.

Embodiment 3

[0037] 1) Weigh 0.27g solid powder yttrium acetate tetrahydrate, 0.072g solid powder ytterbium acetate tetrahydrate, 0.012g solid powder erbium acetate tetrahydrate and 0.04g solid sodium hydroxide;

[0038] 2) Measure 4mL of isopropanol, 4mL of ethanol, 1mL of trifluoroacetic acid and 3mL of water, add solid powder to it, stir for 1 hour, and obtain transparent sol A;

[0039] 3) Transfer transparent sol A to a high-temperature-resistant crucible, and dry in an oven for 3 hours to obtain colloidal substance B;

[0040] 4) Put the colloidal substance B in a high-temperature furnace, raise the furnace temperature from room temperature to 500 °C at a rate of 4 °C / min., keep it for 1 hour, and take it out after cooling to room temperature with the furnace;

[0041] 5) Grinding to obtain Er that emits green light under 980nm laser excitation 3+ , Yb 3+ double doped YF 3 , hexagonal, tetragonal NaYF 4 Up-conversion phosphors with three-phase coexistence.

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Abstract

The invention discloses a preparation method for Er<3+>-Yb<3+>-co-doped NaYF4 fluorescent powder of which the crystalline phase can be controllably synthesized. The method comprises the following steps that yttrium acetate, ytterbium acetate, erbium acetate and sodium hydroxide are batched and mixed, isopropanol, ethyl alcohol and water serve as solvent, trifluoroacetic acid is added, and transparent sol A is obtained after the mixture is stirred evenly; heat treatment is performed on colloidal matter obtained by drying the transparent sol A, the temperature is increased to 300-800 DEG C from the room temperature, heat preservation is performed for a certain time, and the colloidal matter is cooled to the room temperature along with a furnace and then ground to obtain the Er<3+>-Yb<3+>-co-doped up-conversion fluorescent powder with different crystalline phase compositions and multiple light emitting colors. The preparation method is simple in synthesis technology, short in production cycle and capable of easily achieving scale production; the synthesized Er<3+>-Yb<3+>-co-doped up-conversion fluorescent powder is controllable in crystalline phase, diverse in light emitting colors and wide in application.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth doped luminescent materials, in particular to an Er 3+ , Yb 3+ Co-doped NaYF 4 Preparation method of fluorescent powder. Background technique [0002] An up-conversion luminescent material is a luminescent material that can convert near-infrared light into visible light. NaYF doped with rare earth ions 4 It is widely used in biomedicine, anti-counterfeiting marks, photoluminescent devices and other fields due to its high-efficiency luminescence performance. To obtain up-conversion phosphors with multiple luminescent colors, it is often necessary to prepare substances with different chemical compositions. With the maturity of phosphor preparation technology, the effective and simple preparation of phosphors with different crystal phases and different luminescent colors can bring great convenience to the application in production. At present, the preparation of NaYF doped wit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 李凌云孙李珍于岩潘坚福
Owner FUZHOU UNIV
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