Silicon dioxide coating rare earth core-shell upper conversion fluorescence nano-tube and preparation method thereof

A fluorescent nanocrystal, silicon dioxide technology, applied in chemical instruments and methods, luminescent materials and other directions, to achieve the effects of easy availability of raw materials, simple operation and low price

Inactive Publication Date: 2008-01-09
CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no report on the in situ direct preparation ...

Method used

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Examples

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Embodiment 1

[0015] Example 1: Yb 3+ ions and Er 3+ ion co-doped YVO 4 / SiO 2 Preparation of core-shell upconversion fluorescent nanocrystals, general formula A x B y / SiO 2 A is Y, B is VO 4 , X is 1, Y is 1;

[0016] Concretely comprise the following steps: (a) in conical flask, take 1ml and be dissolved with yttrium nitrate, ytterbium nitrate and erbium nitrate total concentration and be the aqueous solution of 0.2mol / l, 1g hexadecyltrimethylammonium bromide, 12.9 ml of n-octane and 1 ml of n-butanol, and magnetically stirred at 20°C for 20 minutes to form a stable and transparent microemulsion I. (b) Configure microemulsion II in the same proportion, the water phase of microemulsion II is 0.2mol / l sodium vanadate aqueous solution, mix microemulsion I and II, stir for 24h, make sufficient reaction to generate Yb 3+ and Er 3+ Co-doped YVO 4 Nanocrystalline. (c) Add 200 microliters of concentrated ammonia water and 100 microliters of tetraethyl orthosilicate to the solution, an...

Embodiment 2

[0017] Example 2: Yb 3+ Ion and Tm 3+ ion co-doped NaYF 4 / SiO 2 Preparation of core-shell upconversion fluorescent nanocrystals, general formula A x B y / SiO 2 A is Na, B is YF, X is 1, and Y is 4;

[0018] Concretely comprise the following steps: (a) in conical flask, measure 1ml to be dissolved with yttrium nitrate, ytterbium nitrate and thulium nitrate total concentration and be the aqueous solution of 0.2 mole per liter, 2g cetyltrimethylammonium bromide, 15.4 ml of n-heptane and 2 ml of n-hexanol, and magnetically stirred at 20°C for 20 minutes to form a stable and transparent microemulsion. (b) Add 1ml of 0.8mol / l sodium fluoride aqueous solution and stir for 2-12h to fully react to form Yb 3+ and Tm 3+ Co-doped NaYF 4 Nanocrystalline. (c) Get 250 microliters of concentrated ammonia water and 150 microliters of orthosilicate ethyl ester and join in the solution, continue to stir for 24 hours, make SiO 2 shell. (d) Transfer the solution to an autoclave weighe...

Embodiment 3

[0019] Example 3: Yb 3+ ions and Er 3+ ion co-doped LaF 3 / SiO 2 Preparation of core-shell upconversion fluorescent nanocrystals, general formula A x B y / SiO 2 Among them, A is La, B is F, X is 1, and Y is 3;

[0020] Concretely comprise the following steps: (a) in conical flask, measure 0.6ml to be dissolved with lanthanum nitrate, ytterbium nitrate and erbium nitric acid total concentration and be the aqueous solution of 0.2mol / l, 0.6g sodium dodecylsulfonate, 9ml ring Hexylamine and 1.2ml n-butanol were magnetically stirred at 20°C for 10 minutes to form a stable and transparent microemulsion I. (b) Configure microemulsion II in the same proportion as above, the water phase of microemulsion II is 0.6mol / l ammonium fluoride aqueous solution, add microemulsion II in microemulsion I, stir for 12 hours, make sufficient reaction to generate Yb 3+ and Er 3+ Co-doped LaF 3 Nanocrystalline. (c) Add 100 microliters of concentrated ammonia water and 60 microliters of tetra...

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Abstract

A silicon dioxide coated conversion fluorescent nanometer crystal on rare-earth core shell by direct in-situ synthesizing and its production of core-shell nanometer crystal are disclosed. The general formula is AxBy/SiO2. It adopts reversed-phase aggregation micro-emulsion method combined with hydrothermal method. Nanometer crystal of ytterbium and thulium co-doped is used to transmit blue light, co-doped ytterbium and erbium is used to transmit green light and red light under near-infrared excitation. It's convenient and simplified; it has uniform size distribution, dispersion and repeating ability. It can be used as biological-inspecting and analyzing fluorescent marks.

Description

technical field [0001] The invention relates to an up-conversion fluorescent material and a preparation method thereof, in particular to a silicon dioxide-coated rare earth core-shell up-conversion fluorescent nanocrystal and a preparation method thereof. Background technique [0002] Up-conversion luminescence refers to the ability to excite a special medium with low-energy light to obtain high-energy light. In recent years, more and more attention has been paid to upconversion fluorescent materials that can be excited by near-infrared light to obtain visible light, and they are widely used in near-infrared light detection, imaging and lasers. Up-conversion fluorescent materials have special and excellent fluorescence emission properties, narrow fluorescence spectrum, and no photobleaching. In particular, the up-conversion process is excited by infrared light and does not excite background fluorescence, so the detection sensitivity can be significantly improved. These prop...

Claims

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Application Information

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IPC IPC(8): C09K11/77C09K11/02
Inventor 孙雅娟孔祥贵曾庆辉张友林
Owner CHANGCHUN INST OF OPTICS FINE MECHANICS & PHYSICS CHINESE ACAD OF SCI
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