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a la 2 zr 2 o 7 Up-conversion luminescent material and preparation method thereof

A technology of luminescent materials and solutions, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of reducing the performance of luminescent materials, bulk lattice defects, increasing particle surface, etc. Ask for simple effects

Active Publication Date: 2021-06-29
GUIZHOU NORMAL UNIVERSITY
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Problems solved by technology

Currently, La 2 Zr 2 o 7 It is mainly prepared by high-temperature solid-phase synthesis method, co-precipitation method, and sol-gel method. The synthesis temperature of high-temperature solid-phase method is relatively high (1550°C-1650°C), and the prepared product has a large particle size and low product purity. High, the product needs to be ball milled to increase the surface defects of the particles, the bulk lattice defects are difficult to control, and it is difficult to perform uniform doping, which reduces the performance of its luminescent material

Method used

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  • a la <sub>2</sub> zr <sub>2</sub> o <sub>7</sub> Up-conversion luminescent material and preparation method thereof
  • a la <sub>2</sub> zr <sub>2</sub> o <sub>7</sub> Up-conversion luminescent material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: polymer network gel method prepares La 1.7 Zr 2 o 7 :Er 0.1 , Yb 0.2 Up-conversion luminescent material: La(NO 3 ) 3 ·6H 2 O, Er(NO 3 ) 3 ·6H 2 O, Yb(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 2H 2 O was used as the main raw material to prepare solutions containing La, Er, Yb and Zr at concentrations of 1.0 mol / L, 0.2 mol / L, 0.2 mol / L and 1.0 mol / L, respectively. Take La at a concentration of 1.0 mol / L 3+ Solution 42.50 mL, 0.2 mol / L Er 3+ Solution 12.50 mL, 0.2 mol / L Yb 3+ Solution 25.00 mL, 1.0 mol / L Zr 4+ Solution 50.00 mL and 100.00 mL H 2 0 to a 500 mL beaker and mix evenly to obtain a mixed ion solution; respectively weigh 12 g of acrylamide and 2 g of N,N-methylenebisacrylamide at a mass ratio of 6:1 and add them to the mixed ion solution, and magnetically Stir for 1 h; then place the solution at 80 o Stir in the water bath for 0.5 h in the C water bath, add 1.00 mL of the newly prepared ammonium persulfate solution with a mass fraction ...

Embodiment 2

[0026] Embodiment 2: polymer network gel method prepares La 1.86-2y Zr 2 o 7 :Er 0.14 , Yb 2y ( y = 0.16, 0.20,0.24) series of up-conversion luminescent materials: LaCl 3 ·6H 2 O, ErCl 3 ·6H 2 O, YbCl 3 ·6H 2 O and ZrOCl 2 ·8H 2 O was used as the main raw material, and the solutions containing La, Er, Yb and Zr at concentrations of 0.5 mol / L, 0.1 mol / L, 0.2 mol / L and 1.0 mol / L were prepared, respectively. Take three parts of Er with a concentration of 0.1 mol / L 3+ Solution 28.00 ml and 1.0 mol / L Zr 4+ Solution 40.00 mL to 100 mL H 2 O in the 500 mL beaker A, beaker B and beaker C, according to Yb 3+ The doping amount was designed to be 16%, 20% and 24%, and 0.5 mol / L of La was added to beaker A, beaker B and beaker C respectively 3+ solution 61.6 mL, 58.4 mL and 55.2 mL, then add 0.2 mol / L Yb in beaker A, beaker B and beaker C respectively 3+ 32.00 mL, 40 mL, and 48 mL of the solution were stirred evenly to obtain a mixed ion solution; 10 g of acrylamide and...

Embodiment 3

[0027] Embodiment 3: polymer network gel method prepares La 1.7 Zr 2 o 7 :Er 0.1 , Yb 0.2 Up-conversion luminescent material: La 2 o 3 、Er 2 o 3 , Yb 2 o 3 and ZrOCl 2 ·8H 2 O is the main raw material. A certain amount of rare earth oxides is weighed and dissolved in concentrated nitric acid. The corresponding rare earth-containing solutions are obtained after heating and decomposing excess concentrated nitric acid. The concentrations of La, Er, Yb and Zr solutions are respectively prepared to be 1.0 mol / L, 0.2 mol / L, 0.2 mol / L, 1.0 mol / L solutions. Take La at a concentration of 1.0 mol / L 3+ Solution 42.50 mL, 0.2 mol / L Er 3+ Solution 12.50 mL, 0.2 mol / L Yb 3+ Solution 25.00 mL, 1.0 mol / L Zr 4+ Solution 50.00 mL and 100.00 mL H 2 0 to a 500 mL beaker and mix evenly to obtain a mixed ion solution; respectively weigh 12 g of acrylamide and 2 g of N,N-methylenebisacrylamide at a mass ratio of 6:1 and add them to the mixed ion solution, and magnetically Stir for ...

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Abstract

The invention discloses a La 2 Zr 2 o 7 Up-conversion luminescent material and preparation method thereof, the general chemical formula of the material is La 2‑2x‑ 2y Zr 2 o 7 :Er 2x ,Yb 2y ,in: x is the molar ratio of Er ions replacing La ions, x The value range is 0< x ≤0.3, y is the molar ratio of Yb ions replacing La ions, y The value range is 0< y ≤0.5. Utilizing the hindering effect of polymer gel to form a network, the movement of particles in the solution is restricted, the chance of contact and agglomeration is greatly reduced, and the particles can be evenly dispersed in the network, which is conducive to the formation of small average particle size, uniform dispersion, Powder material with less agglomeration; the gel formed by this method can be sintered at a lower temperature to obtain a uniformly dispersed powder material. The calcination temperature is low, there is no impurity phase, and the crystallinity is high. The calcination temperature is lower than that of the traditional solid-phase synthesis method. The temperature is higher than 500°C, and the preparation process is simple, the cost is low, and it is easy to scale up and put into mass production, and has achieved good results.

Description

technical field [0001] The invention relates to an up-conversion luminescent material, in particular to a La 2 Zr 2 o 7 An up-conversion luminescent material and a preparation method thereof belong to the technical field of rare earth materials. Background technique [0002] La 2 Zr 2 o 7 for A 2 B 2 o 7 type structure crystal, which has the characteristics of low phonon energy, so that it can be used as an up-conversion luminescent material matrix to excite luminescence under a low-energy excitation source, and it has excellent chemical stability and thermal stability, making it expected to become a high-quality Upconverting luminescent material matrix. Will Er 3+ Yb acts as an activator 3+ Co-doped into La as a sensitizer 2 Zr 2 o 7 lattice, will be observable in Yb 3+ Enhanced Er under the action of sensitizer 3+ upconversion luminescence. Currently, La 2 Zr 2 o 7 It is mainly prepared by high-temperature solid-phase synthesis method, co-precipitation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/78
CPCC09K11/7766
Inventor 杨锦瑜朱莉萍黄一男
Owner GUIZHOU NORMAL UNIVERSITY
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