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Oxide up-conversion luminescent material and preparation method thereof

A technology of luminescent materials and oxides, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of improper control of doping concentration, difficulty in realization, and inability to obtain high-purity monoclinic MO

Active Publication Date: 2021-07-30
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Therefore, the micron-sized large-scale rare-earth-doped MOs studied in the literature 2 Most of the luminescent materials have the characteristics of miscibility, such as monoclinic and tetragonal, monoclinic and cubic, which are due to improper control of doping concentration, resulting in incomplete phase transition.
For up-conversion luminescence, in order to enhance light absorption, it is often necessary to dope a high concentration sensitizer Yb 3+ ions, which will directly induce its phase change to tetragonal or cubic phase, that is, although high doping concentration is one of the necessary conditions for obtaining efficient luminescence, monoclinic MO under high rare earth doping concentration 2 However, it is difficult to achieve, and it is impossible to obtain high-purity monoclinic MO at high doping concentration. 2

Method used

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  • Oxide up-conversion luminescent material and preparation method thereof
  • Oxide up-conversion luminescent material and preparation method thereof
  • Oxide up-conversion luminescent material and preparation method thereof

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preparation example Construction

[0042] The present invention also provides a method for preparing the above-mentioned oxide up-conversion luminescent material, comprising the following steps:

[0043] Weighing solid compounds containing M element, Ln element, Li element and N element respectively according to the stoichiometric ratio, mixing uniformly, and grinding to obtain the mixture;

[0044] Calcining the mixture at 1200-1600°C for 3-5 hours to obtain a sintered body;

[0045] After grinding the sintered body, the oxide up-conversion luminescent material is obtained.

[0046] Wherein, the solid compound includes oxide, carbonate, nitrate and halide, and the solid compound containing M element, Ln element, Li element and N element is an oxide compound containing M element, Ln element, Li element and N element. at least one of compounds, carbonates, nitrates or halides. The grinding is preferably wet mechanical ball milling for 10 hours, and the calcination temperature is preferably 1300-1450°C.

[004...

Embodiment 1

[0050] Zr 0.77 Ho 0.01 Yb 0.1 Nb 0.12 o 2 Oxide up-conversion phosphor, the preparation process is as follows:

[0051] Weigh high-purity ZrO according to stoichiometric ratio 2 、Ho 2 o 3 , Yb 2 o 3 and Nb 2 o 5 (In order to avoid impurity phases due to uneven grinding, the Nb element is in excess of ~9% relative to the rare earth ions when weighing), put it in a zirconia ball mill jar, add an appropriate amount of alcohol, use zirconia balls as the grinding medium, and use a planetary ball mill Grind for 10 hours, then dry in an electric oven for 10 hours, and collect a fine powder sample that is uniformly mixed by vibrating sieving;

[0052] Put it into a high-purity corundum crucible, and keep it warm at 1450°C for 4 hours in the air;

[0053] After the material is cooled and discharged, it is slightly ground to obtain a high-efficiency oxide up-conversion luminescent material.

Embodiment 2

[0055] Zr 0.77 Ho 0.01 Yb 0.1 Ta 0.12 o 2 Oxide up-conversion phosphor, the preparation process is as follows:

[0056] Weigh high-purity ZrO according to stoichiometric ratio 2 、Ho 2 o 3 , Yb 2 o 3 and Ta 2 o 5 (In order to avoid impurity phases due to uneven grinding, the Ta element is in excess of ~9% relative to the rare earth ions when weighing), put it in a zirconia ball mill jar, add an appropriate amount of alcohol, use zirconia balls as the grinding medium, and use a planetary ball mill Grind for 10 hours, then dry in an electric oven for 10 hours, and collect a fine powder sample that is uniformly mixed by vibrating sieving;

[0057] Put it into a high-purity corundum crucible, and keep it warm at 1450°C for 4 hours in the air;

[0058] After the material is cooled and discharged, it is slightly ground to obtain a high-efficiency oxide up-conversion luminescent material.

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Abstract

The invention provides an oxide up-conversion luminescent material, and belongs to the technical field of luminescent material preparation and application, the chemical general formula of the oxide up-conversion luminescent material is M1-x-y LnxNyLizO2, M is at least one of Zr and Hf; Ln is an Ho < 3 + > and Yb < 3 + > ion pair or an Er < 3 + > and Tm < 3 + > ion pair; N is at least one of Nb < 5 + > and Ta < 5 + >; and 0 < x < = 0.15, 0 < y < = 0.18, x < = y < = 1.2 x, and 0 < = z < = 0.05. The invention also provides a preparation method of the material, the material is synthesized by adopting a solid-phase method and is prepared by roasting in air, a reducing atmosphere does not need to be provided, the operation is simple, the requirement on equipment is low, the production cost is low, and the material is environment-friendly. According to the oxide up-conversion luminescent material, a monoclinic crystal phase MO2 (M is at least one of Zr and Hf) oxide is used as a matrix of doping ions (Ho < 3 + > / Yb < 3 + >, Tm < 3 + > / Yb < 3 + >, Li < + >, Nb < 5 + > or Ta < 5 + >), the doping ions Li < + >, Nb < 5 + > or Ta < 5 + > are charge compensation agents of rare earth ions Ln < 3 + >, the matrix can be stabilized to be a monoclinic phase when high-concentration rare earth ions are doped, and adjustable bright visible light up-conversion emission can be realized under near-infrared light excitation (such as 980nm).

Description

technical field [0001] The invention belongs to the technical field of preparation and application of luminescent materials, and relates to an oxide up-conversion luminescent material and a preparation method. Background technique [0002] Up-conversion luminescence has potential applications in laser, display, fluorescence imaging, disease diagnosis and treatment, information anti-counterfeiting and other fields. Among them, the rare earth ion Ho 3+ 、Tm 3+ and Yb 3+ Doped upconverting micro / nanoluminescent materials have been extensively studied. To develop new up-conversion luminescent materials and obtain high-efficiency up-conversion luminescence has always been the goal pursued by researchers. The choice of the matrix is ​​crucial, and the matrix composition determines the phonon energy of the material and the lattice symmetry environment occupied by the doped rare earth ions. Low phonon energy helps to reduce the non-radiative relaxation rate, improve the luminesc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/78
CPCC09K11/7769
Inventor 潘国徽武华君张家骅张亮亮吴昊
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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