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Preparation method of up-conversion luminescence coding nano-composite particle based on mesoporous silica and coding method

A mesoporous silica and nanocomposite technology is applied in the field of preparation of upconversion luminescence coding microspheres, and can solve the problems of complex operation steps, high biological toxicity, difficult surface modification and the like

Pending Publication Date: 2021-09-07
JIHUA LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Up-conversion luminescent materials need rare earth doping and high crystallization to ensure their photoluminescence performance and efficiency, but also lead to problems such as high biological toxicity, difficult surface modification and difficult realization of functional recombination when they are applied.
At present, the most commonly used improvement method is to coat a layer of silicon oxide or mesoporous silicon oxide on the surface of the up-conversion luminescent material by the sol-gel method. The implementation of this method is complicated and the thickness and consistency of the surface shell layer are not easy to control.

Method used

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  • Preparation method of up-conversion luminescence coding nano-composite particle based on mesoporous silica and coding method
  • Preparation method of up-conversion luminescence coding nano-composite particle based on mesoporous silica and coding method
  • Preparation method of up-conversion luminescence coding nano-composite particle based on mesoporous silica and coding method

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Experimental program
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Embodiment 1

[0047] The mesoporous silica nanoparticle template with radial pore structure was prepared by microemulsion method: 100 mg CTAB was dissolved in 30 mL deionized water, and heated and stirred in an oil bath at 60 ℃ for 30 minutes. Then 25.5 mL of n-octane, 1.8 mL of styrene, 22 mg of lysine, 1 mL of TEOS and 46.3 mg of AIBA were added, and stirred at 350 rpm for 3 hours. The product was collected by ethanol washing and centrifugation for several times, dried in an oven at 80°C for 4 hours, and sintered at 550°C to remove the organic template. figure 1 The mesoporous silica template shown.

[0048] Preparation of calcium fluoride precursor sol co-doped with ytterbium and holmium: dissolve 5.2854 g of calcium acetate monohydrate in 68 mL of water, add 2.5334 g of ytterbium acetate and 0.2052 g of holmium acetate, that is, the rare earth doping ratio is Yb 3+ / Ho 3+ (20 / 2 mol%), adding 12 mL of trifluoroacetic acid and stirring at room temperature for 24 hours, a clear and trans...

Embodiment 2

[0055] The method of preparing zinc fluoride precursor sol co-doped with ytterbium and erbium by using metal alkoxide and rare earth alkoxide: Weigh 3.8238g of zinc methoxide and dissolve it in 68 mL of water, add 2.1018 g of ytterbium isopropoxide and 0.1034 g of erbium isopropoxide, That is, the rare earth doping ratio is Yb3+ / Er3+= 20 / 1 mol%, adding 12 mL of trifluoroacetic acid and stirring at room temperature for 24 hours, a clear and transparent up-conversion luminescence precursor solution is obtained. Add 100 mg of mesoporous silica with radial pore structure prepared in advance to 20 mL of the above precursor sol, and stir thoroughly at a constant temperature and low speed in a 40°C water bath for 12 hours. After centrifugation at 8000 rpm for 2 and a half minutes, the supernatant was discarded, and 200 μL of precursor sol was added again, and the adherent particles were redispersed by vortexing. After standing at room temperature for half an hour, add 20 mL of deioni...

Embodiment 3

[0057] Method for preparing lanthanum fluoride or cerium fluoride precursor sol co-doped with ytterbium and holmium by using trivalent metal acetate and rare earth acetate: Weigh 5.01 g of lanthanum (Ⅲ) acetate hydrate or 4.76 g of cerium (Ⅲ) acetate The hydrate was dissolved in 34 mL of water, and 1.2667 g of ytterbium acetate and 0.1026 g of holmium acetate were added, that is, the rare earth doping ratio was Yb 3+ / Ho 3+ (20 / 2 mol%), adding 6 mL of trifluoroacetic acid and stirring at room temperature for 24 hours, a total volume of 40 mL of ytterbium holmium co-doped LaF 3 or CeF 3 Precursor sol.

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Abstract

The invention discloses a preparation method of up-conversion luminescence coding nano composite particles based on mesoporous silica, which comprises the following steps: preparing metal fluoride precursor sol containing rare earth elements, stirring to enable the sol to enter pore channels of the mesoporous silica through a capillary effect, centrifuging at a low speed to remove a supernate, adding water, and carrying out soft vortex oscillation , and washing off the precursor sol on the surfaces of the particles, centrifugally collecting a sample at a low speed, drying the sample in a drying oven to form xerogel of metal fluoride in the pore channels of the mesoporous silica, and sintering the xerogel after drying to obtain the up-conversion luminescent mesoporous silica composite nanoparticles. According to the method, the up-conversion luminescent nanocrystals can only nucleate and grow in silicon oxide mesopores, the biotoxicity of the up-conversion luminescent nanocrystal encoding microspheres can be greatly reduced, and further modification of the encoding microspheres is facilitated; the invention also provides a corresponding coding method, so that the types or contents of rare earth elements contained in the up-conversion luminescent nanocrystals in different composite particle pore channels are different.

Description

technical field [0001] The invention relates to a preparation method of up-conversion luminescence encoded microspheres, in particular to a preparation method of up-conversion luminescence encoded nanocomposite particles based on mesoporous silicon oxide and an encoding method thereof. Background technique [0002] Driven by the demand for large-scale analysis and detection of biomolecules in the fields of clinical diagnosis and drug screening, various high-throughput analysis methods such as solid-phase chips and liquid-phase chips have emerged as the times require. On the one hand, high-throughput detection technology can integrate multiple variables for analysis, overcoming the limitations of single variable analysis; on the other hand, it can greatly reduce time, labor and economic costs. Compared with traditional single-variable detection and analysis methods, the key to achieving high-throughput analysis lies in how to effectively address each variable so that each var...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/61C09K11/85
CPCC09K11/025C09K11/7791C09K11/779C09K11/7772C09K11/7773
Inventor 顾桐旭褚春旭钟嘉俊白鹏利
Owner JIHUA LAB
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