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Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid materials and preparation methods

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: 2022-05-06
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 materials and preparation methods
  • Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid materials and preparation methods
  • Terbium-doped calcium fluoride nanoparticles, sol-gel hybrid materials and preparation methods

Examples

Experimental program
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Effect test

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 a terbium-doped calcium fluoride nanoparticle, a sol-gel hybrid material and a preparation method thereof, comprising the following steps: S1, preparing a bonding ligand; S2, combining the bonding ligand, soluble Ca salt, and soluble After the Tb salt is heated and mixed in ethylene glycol, the fluorine source solution is added, and the heating reaction is continued to obtain terbium-doped calcium fluoride nanoparticles; S3, dissolving the terbium-doped calcium fluoride nanoparticles in DMF to obtain a solution A; Dissolve ethyl orthosilicate in aqueous ethanol solution to obtain solution B; S4, add solution A to solution B, adjust the pH to 2-3, then add an alkaline condensation catalyst to catalyze the condensation reaction, and reduce the pH , aged at 40°C to obtain a sol-gel hybrid material. Rare-earth-doped nanoparticles are grafted onto the skeleton of the sol-gel matrix through strong interactive covalent bonds to achieve doping at the molecular level and overcome the shortcomings of inhomogeneous doping and phase separation.

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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Patent Type & Authority Patents(China)
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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