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Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid material and preparation method

A technology of calcium heterofluoride and nanoparticles, which is applied in the field of hybrid material preparation, can solve problems such as uneven doping, achieve good luminescence performance, prolong luminescence life, and overcome the effects of uneven doping and phase separation

Active Publication Date: 2022-01-21
XIAN UNVERSITY OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention grafts the rare earth doped nanoparticles onto the skeleton of the sol-gel matrix through strong interaction covalent bonds, realizes the doping at the molecular level, and overcomes the shortcomings of uneven doping and phase separation

Method used

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  • Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid material and preparation method
  • Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid material and preparation method
  • Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid material and preparation method

Examples

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Embodiment 1

[0045] A preparation method of terbium-doped calcium fluoride nanoparticles, comprising the following steps:

[0046] S1. Preparation of bonded ligands

[0047]

[0048] Weigh 0.274g (2mmol) m-aminobenzoic acid into a three-necked flask, add 25mL of treated chloroform, stir to dissolve; then weigh 1.120g (4.5mmol) 3-isocyanatopropyltriethoxysilane, drop Add it to the reaction system, the dropwise addition time is not less than 15-30min; then raise the temperature to 65°C for a stirring reaction for 12h, after the reaction is completed, let it stand and cool to room temperature, centrifuge, remove the supernatant, and set the water-alcohol volume ratio to 4 : 1 mixed solvent, washed twice, and dried at 50° C., to obtain the bonded ligand in the form of white powder. 1 H-NMR (DMSO-d6, 400MHz): δ0.58ppm (4H), δ1.04-1.55ppm (18H), δ2.51ppm (4H), δ3.01-3.41ppm (12H), δ6.24ppm (1H ), δ7.46ppm (1H), δ7.94ppm (1H), δ8.62ppm (1H) and δ12.65ppm (1H).

[0049] S2. Preparation of te...

Embodiment 2

[0053] A preparation method of terbium-doped calcium fluoride nanoparticles is basically the same as the preparation method of Example 1, the difference is that in S2, NH 4 After F ethylene glycol solution, stirring was continued at 120 °C for 6 h.

Embodiment 3

[0055] A preparation method of terbium-doped calcium fluoride nanoparticles is basically the same as the preparation method of Example 1, the difference is that in S2, NH 4 After F ethylene glycol solution, stirring was continued at 120 °C for 10 h.

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Abstract

The invention provides terbium-doped calcium fluoride nanoparticles, a sol-gel hybrid material and a preparation method. The preparation method comprises the following steps: S1, preparing a bonded ligand; S2, heating and mixing the bonded ligand, soluble Ca salt and soluble Tb salt in ethylene glycol, then adding a fluorine source solution, and continuing heating reaction to obtain terbium-doped calcium fluoride nanoparticles; S3, dissolving the terbium-doped calcium fluoride nanoparticles in DMF, and obtaining a solution A; dissolving tetraethoxysilane in an ethanol water solution to obtain a solution B; S4, adding the solution A into the solution B, adjusting the pH value to 2-3, adding an alkaline condensation catalyst, carrying out a catalytic condensation reaction, reducing the pH value, and carrying out an aging reaction at 40 DEG C to obtain the sol-gel hybrid material. Rare earth doped nanoparticles are grafted to a skeleton of a sol-gel matrix through relatively strong interaction covalent bonds, so that doping on a molecular level is realized, and the defects of non-uniform doping and phase separation are overcome.

Description

technical field [0001] The invention relates to the technical field of hybrid material preparation, in particular to a terbium-doped calcium fluoride nanoparticle, a sol-gel hybrid material and a preparation method. Background technique [0002] In the research of rare earth functional materials, rare earth luminescent materials have always been an important research direction. Rare earth-doped luminescent nanomaterials use rare earth ions as the luminescent center and inorganic nanocrystals as the matrix. They have both the unique physical and chemical properties of nanomaterials and the good luminescent performance of rare earth ions. Compared with rare earth organic complexes and quantum dots (QDs) and organic dye molecules have the advantages of larger Stokes shift, sharper emission spectrum, longer lifetime, higher chemical / optical stability, lower toxicity, less photobleaching, etc. With the continuous development of rare earth-doped luminescent nanoparticles, their a...

Claims

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Application Information

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IPC IPC(8): C09K11/61C01F11/22B82Y30/00B82Y40/00
CPCC09K11/7748B82Y30/00B82Y40/00C01F11/22C01P2002/72C01P2002/82C01P2004/04C01P2004/64
Inventor 宋立美贾悦悦高建华
Owner XIAN UNVERSITY OF ARTS & SCI
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