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Rare-earth upconversion luminescent nanosphere having hollow core-shell structure as well as preparation method and use of nanosphere

A technology of rare earth up-conversion and core-shell structure, which is applied in the field of hollow core-shell structure rare earth up-conversion luminescent nanospheres and its preparation, can solve the problems of cumbersome steps, poor dispersion, and easy aggregation of particles, and achieve a simple preparation method. Effect

Active Publication Date: 2016-02-03
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Claims
  • Application Information

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Problems solved by technology

The steps of this method are relatively cumbersome, and the co-precipitation or high-temperature thermal decomposition methods used to synthesize nanocrystals require a large amount of high-boiling organic solvents.
And the method of "core first and then shell" is adopted. On the one hand, when the fluoride core is too large, the dispersion is not good, and it is not easy to coat with silica; on the other hand, when the silica coating is too thick, the particles are easy to agglomerate, so the obtained The size of the UCNP-MS hollow core-shell structure material does not exceed 150nm, the adjustable range is limited, and the obtained luminescent nanospheres cannot reach the size of several hundred nanometers

Method used

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  • Rare-earth upconversion luminescent nanosphere having hollow core-shell structure as well as preparation method and use of nanosphere
  • Rare-earth upconversion luminescent nanosphere having hollow core-shell structure as well as preparation method and use of nanosphere
  • Rare-earth upconversion luminescent nanosphere having hollow core-shell structure as well as preparation method and use of nanosphere

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preparation example Construction

[0046] As mentioned above, in order to solve the cumbersome steps in the preparation of rare earth up-conversion luminescent nanospheres with hollow core-shell structure in the prior art using the method of "core first and then shell", a large amount of high-boiling organic solvents are required for the synthesis of nanocrystals, and the size of the final luminescent nanospheres Due to problems such as limited adjustable range, the present invention provides a method for preparing rare earth up-conversion luminescent nanospheres with a hollow core-shell structure, such as figure 1 As shown, the method includes the following steps:

[0047] (1) preparing hollow mesoporous silica nanospheres;

[0048] (2) introducing the precursor of the rare earth-doped ternary fluoride into the cavity of the hollow mesoporous silica nanosphere prepared in step (1);

[0049] (3) Calcining the mesoporous silica nanospheres filled with precursors in the cavity, so that the precursors can generat...

Embodiment 1

[0074] Preparation of Luminescent Nanosphere HMS-NaYF with a Size of 200nm 4 :Yb / Er

[0075] (1) A cationic surfactant-assisted selective etching method (Nanoscale, 2011, 3, 1632) was used to prepare hollow inorganic mesoporous silica nanosphere solid powder with a size of 200 nm and a shell thickness of 35 nm. Its specific surface area is 318cm 2 / g, the pore volume is 0.5cm 3 / g.

[0076] (2) Under vacuum conditions, 5mL of CF 3 COONa, Y(CF 3 COO) 3 , Yb(CF 3 COO) 3 and Er(CF 3 COO) 3 The mixed solution (the concentration of the mixed solution is 1.05mmol / L, the molar ratio of each element is Y:Na:Yb:Er=0.78:2.5:0.2:0.02) is injected into 25mg of the hollow inorganic medium prepared in the above step (1). Porous silica nanosphere solid powder, stirred for 1 hour, continued to stir for 1 hour after removing the vacuum, collected the solid after centrifugation, and dried overnight at 110° C. to obtain a dry solid.

[0077] (3) Put the dry solid obtained in step (2) ...

Embodiment 2

[0083] Preparation of Luminescent Nanosphere HPMO-NaLuF with a Size of 80nm 4 :Yb / Er

[0084] (1) Use the polymer bead template method (J.Mater.Chem., 2012,22,17636), and replace it with a mixture of 1,4-bis(triethoxysilyl)benzene and aminopropylethoxysilane Ethyl orthosilicate, and a hollow organic mesoporous silica nanosphere solid powder with a size of 80nm and a shell thickness of about 15nm was prepared. 13 C and 29 Si solid NMR confirmed its organosilicon composition (such as Figure 5 ).

[0085] (2) Under vacuum conditions, 2mL of CF 3 COONa, Lu(CF 3 COO) 3 , Yb(CF 3 COO) 3 and Er(CF 3 COO) 3 The mixed solution (concentration is 0.9mmol / L, the molar ratio of each element is Gd:Na:Yb:Er=0.78:2.5:0.2:0.02) is injected into 10mg of hollow organic mesoporous silica prepared in step (1) In the nanosphere solid powder, stir for 0.5 hour, and continue to stir for 6 hours after removing the vacuum. The solid was collected after centrifugation and dried overnight at...

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Abstract

The invention discloses a preparation method of a rare-earth upconversion luminescent nanosphere having a hollow core-shell structure as well as a product and use of the nanosphere. The preparation method comprises the following steps: (1) preparing a hollow mesoporous silica nanosphere; (2) introducing a precursor of rare-earth doped ternary fluoride to a cavity of the hollow mesoporous silica nanosphere prepared in the step (1); (3) roasting the silica nanosphere the cavity of which has been filled with the precursor, so that the precursor generates the rare-earth ternary fluoride, thus obtaining the rare-earth upconversion luminescent nanosphere having the hollow core-shell structure. According to the synthesis method disclosed by the invention, a high-boiling-point organic solvent is not needed, and the pure-phase rare-earth doped ternary fluoride can be obtained just by simple high-temperature roasting; the preparation method is relatively simple. The nanosphere prepared by using the preparation method not only has high upconversion luminescence capability, but also has relatively high drug loading capability, and can be applied to drug sustained release and the like.

Description

technical field [0001] The invention belongs to the technical field of nanocomposite materials, and in particular relates to a rare earth up-conversion luminescent nanosphere with a hollow core-shell structure and a preparation method and application thereof. Background technique [0002] Rare-earth-doped upconversion nanoparticles (upconversion nanoparticles, UCNPs) can convert near-infrared light into visible light, and have the advantages of no background fluorescence, low toxicity, high photostability, and deep light penetration depth, so they have attracted attention in various biological applications. extensive attention. Recognized as one of the best carriers, mesoporous silica (mesoporous silica, MS) is often used to bind UCNP due to its adjustable pore structure and surface properties, enabling it to obtain drug loading and bioconjugation, etc.More Function. In recent years, many UCNP-MS composite materials have been developed at home and abroad, which are applied...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85C09K11/02B82Y20/00B82Y30/00B82Y40/00A61K47/02A61K31/704A61P35/00
Inventor 陈学元卢珊涂大涛李幸俊李仁富
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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