An oxide up-conversion luminescent material and its preparation method

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

Active Publication Date: 2022-06-21
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

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  • An oxide up-conversion luminescent material and its preparation method
  • An oxide up-conversion luminescent material and its preparation method
  • An oxide up-conversion luminescent material and its preparation method

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preparation example Construction

[0042] The present invention also provides a preparation method of the above-mentioned oxide up-conversion light-emitting material, comprising the following steps:

[0043] Weigh the solid compounds containing M element, Ln element, Li element and Ta element respectively according to the stoichiometric ratio, mix uniformly, and grind to obtain a 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 light-emitting material is obtained.

[0046] Wherein, the solid compounds include oxides, carbonates, nitrates and halides, and the solid compounds containing M element, Ln element, Li element and Ta element are oxides containing M element, Ln element, Li element and Ta element at least one of carbonate, nitrate, or halide. The grinding is preferably wet mechanical ball milling for 10 hours, and the firing temperature is preferably 1300-1450°C.

[0047] The preparation me...

Embodiment 1

[0050] Zr 0.77 Er 0.02 Yb 0.09 Ta 0.12 O 2 The oxide up-conversion phosphor, the preparation process is as follows:

[0051] Weigh high-purity ZrO according to stoichiometric ratio 2 , Er 2 O 3 , Yb 2 O 3 and Ta 2 O 5 (In order to avoid the generation of impurity due to uneven grinding, Ta element is in excess of ~9% relative to rare earth ions when weighing), put it in a zirconia ball mill, 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 heating drying oven for 10 hours, and collect fine powder samples uniformly mixed by vibrating sieving;

[0052] Put it into a high-purity corundum crucible and keep it at 1450℃ for 4h under air;

[0053] After cooling and discharging, a little grinding is performed to obtain a high-efficiency oxide up-conversion luminescent material.

Embodiment 2

[0055] Zr 0.385 hf 0.385 Er 0.02 Yb 0.09 Ta 0.12 O 2 The oxide up-conversion phosphor, the preparation process is as follows:

[0056] Weigh high-purity ZrO according to stoichiometric ratio 2 , HfO 2 , Er 2 O 3 , Yb 2 O 3 and Ta 2 O 5 (In order to avoid the generation of impurity due to uneven grinding, Ta element is in excess of ~9% relative to rare earth ions when weighing), put it in a zirconia ball mill, 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 heating drying oven for 10 hours, and collect fine powder samples uniformly mixed by vibrating sieving;

[0057] Put it into a high-purity corundum crucible and keep it at 1450℃ for 4h under air;

[0058] After cooling and discharging, a little grinding is performed to obtain a high-efficiency oxide up-conversion luminescent material.

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Abstract

The invention provides an oxide up-conversion light-emitting material, belonging to the technical field of light-emitting material preparation and application, and its general chemical formula is M 1‑x‑y Ln x Ta y Li z O 2 , where M is at least one of Zr and Hf; Ln is Er 3+ , or for Er 3+ and Yb 3+ ; and 0<x≤0.15, 0<y≤0.18, x≤y≤1.2x, 0≤z≤0.05. The invention also provides a method for preparing an oxide up-conversion luminescent material, which is synthesized by a solid-phase method and prepared by calcining in the air without providing a reducing atmosphere, with simple operation, low equipment requirements, low production cost and environmental friendliness. . The oxide up-conversion light-emitting material of the present invention utilizes monoclinic phase MO 2 (M is one or both of Zr or Hf) oxides as doping ions (Er 3+ ,Er 3+ / Yb 3+ , Li + ,Ta 5+ ) matrix, in which the doping ionic Li + ,Ta 5+ is the rare earth ion Ln 3+ The charge compensator can stabilize the matrix to a monoclinic phase when a high concentration of rare earth ions is doped; the oxide upconversion luminescent material of the present invention has tunable bright visible light under near-infrared light excitation (such as 808 or 980 nm) up-converted emission.

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] Upconversion luminescence has potential applications in the fields of laser, display, fluorescence imaging, disease diagnosis and treatment, and information anti-counterfeiting. Among them, the rare earth ion Er 3+ , Yb 3+ Doped upconversion micro / nanoluminescent materials have been extensively studied. The development of new up-conversion luminescent materials to obtain high-efficiency up-conversion luminescence has always been the pursuit of researchers. The choice of the matrix is ​​crucial, and the composition of the matrix determines the phonon energy of the material and the lattice site symmetry environment occupied by the doped rare-earth ions. The low phonon energy helps to reduce the radiation-free relaxation rate and increase...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/67
CPCC09K11/7769C09K11/7701
Inventor 潘国徽张家骅武华君张亮亮吴昊
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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