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Nanogold shell coated upconversion nanocrystal composite structure material and preparation method thereof

A nanocrystalline composite and structural material technology, applied in nanotechnology, nano-optics, luminescent materials, etc., can solve the problems of incomplete core-shell structure, large nano-particle size, weak biological tissue penetration ability, etc.

Inactive Publication Date: 2018-06-15
CHANGCHUN UNIV OF TECH
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  • Claims
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Problems solved by technology

[0004] In order to solve the technical problems of the rare earth up-conversion luminescent material nanoparticles coated with gold shell in the prior art, the size of the nanoparticles is large, the fluorescence intensity is weakened, the core-shell structure is incomplete, and the penetrating ability of biological tissues is weak, the present invention provides a small size and Nano-gold shell-coated up-conversion nanocrystalline composite structure material with selective enhancement of fluorescence and continuous dense ultra-thin gold shell structure and preparation method thereof

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  • Nanogold shell coated upconversion nanocrystal composite structure material and preparation method thereof
  • Nanogold shell coated upconversion nanocrystal composite structure material and preparation method thereof
  • Nanogold shell coated upconversion nanocrystal composite structure material and preparation method thereof

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preparation example Construction

[0102] The preparation method of the above nano-gold shell-coated up-conversion nanocrystalline composite structure up-conversion luminescent material specifically includes the following steps:

[0103] (1) According to NaMF 4 :xYb,yN@SiO 2 Experimental design of @Au(NSA) composite structure, firstly synthesize pure NaMF 4 :xYb, yN(NYF) matrix, measure Y(NO 3 ) 3 , Yb(NO 3 ) 3 , and measure Tm(NO 3 ) 3 , Er(NO 3 ) 3 、Ho(NO 3 ) 3 One or more of them are placed in a beaker, weigh 0.168g NaF and 10mL H 2 O (centrifuge tube sonicated); weigh 0.3g NaOH, 1.5mL H 2 O, 10mL ethanol and 5mL OA in the above beaker; drop the prepared NaF solution into the beaker, and stir rapidly for 30min; add the solution into the reaction kettle and heat to 200°C for 8-24h; wait for the above solution to cool to room temperature, 10000rpm Centrifuge and wash three times, dry at 60°C for 24 hours, then disperse in appropriate amount of cyclohexane for use;

[0104] Or use another syntheti...

Embodiment 1

[0136] Ⅰ. NYF1 (NaYF 4 : 18%Yb, 2%Er) preparation: (1) weigh 0.2428g YCl 3 , 0.0698gYbCl 3 and 0.0076g ErCl 3 Put the powder in a three-necked flask, (2) dropwise add OA:ODE=14:16mL to the three-necked flask, heat at 160°C for 30min, and cool to room temperature; (3) Take a new beaker and weigh 0.148g NH 4 F and 0.1g NaOH in 10mL methanol solution, ultrasonically disperse for 30min; (4) Add the solution in step (3) dropwise into the three-necked flask, heat to 70°C for 30min; continue to heat to 100°C for 10min; (5) The temperature was raised to 280°C and heated for 1h (N 2 protection, condensed and refluxed); (6) centrifuged and washed with ethanol for 3 times, dried at 60°C for 20 hours, and dispersed in 50 mL of cyclohexane.

[0137] Ⅱ.NS1 (NaYF 4 :18%Yb,2%Er@SiO 2 ) preparation: (1) Take 9 mL of dispersed NYF sample into a beaker, add dropwise 8 mL of cyclohexane and 1 mL of CO-520 for ultrasonic dispersion for 1 min; (2) continue to drop 100 μL of ammonia water, and...

Embodiment 2

[0144]Ⅰ. NYF1 (NaYF 4 : 18%Yb, 2%Er) preparation: (1) weigh 0.2428g YCl 3 , 0.0698gYbCl 3 and 0.0076g ErCl 3 Put the powder in a three-necked flask; (2) Add OA:ODE=14:16mL dropwise to the three-necked flask, heat at 160°C for 30min, and cool to room temperature; (3) Take a new beaker and weigh 0.148g NH 4 F and 0.1g NaOH in 10mL methanol solution, ultrasonically disperse for 30min; (4) Add the solution in step (3) dropwise into the three-necked flask, heat to 70°C for 30min; continue to heat to 100°C for 10min; (5) The temperature was raised to 300°C and heated for 1h (N 2 protection, condensed and refluxed); (6) centrifuged and washed with ethanol for 3 times, dried at 60°C for 20 hours, and dispersed in 50 mL of cyclohexane.

[0145] Ⅱ.NS1 (NaYF 4 :18%Yb,2%Er@SiO 2 ) preparation: (1) Take 9 mL of dispersed NYF sample into a beaker, add dropwise 8 mL of cyclohexane and 1 mL of CO-520 for ultrasonic dispersion for 1 min; (2) continue to drop 100 μL of ammonia water, and ...

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Abstract

The invention belongs to the technical field of luminous materials and relates to a nanogold shell coated upconversion nanocrystal composite structure material and a preparation method of the material. The material solves the technical problems of large nano particle size, low fluorescence intensity, incomplete core-shell structure and poor biological tissue penetration capacity of the existing rare-earth upconversion luminescent material. The invention provides the nanogold shell coated upconversion nanocrystal composite structure material in a fluoride and oxide upconversion nano core-shellstructure. The invention further provides the preparation method of the composite structure material. Compared with the upconversion luminescent material prepared by the traditional method, the nanogold shell coated upconversion nanocrystal composite structure material is small in particle size, regular in pattern, good in dispersity, good in biocompatibility, and easy in surface biological functionalization; a gold shell is ultrathin, complete and consecutive; and selectively reinforced fluorescence emission is obtained by adjusting a position of an SPR (surface plasmon resonance) absorptionpeak. The preparation method of the material has the advantages of good controllability, low reaction temperature, low equipment requirements, simple in-situ synthesis operation technology and the like.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a nano-gold shell-coated up-conversion nano-crystal composite structure material and a preparation method thereof. Background technique [0002] Up-conversion luminescence is a unique nonlinear optical phenomenon. Due to its potential wide application value, it has been used not only in the field of basic scientific research, but also in applications such as nonlinear optical devices, light-emitting devices, solar cells, catalysis, etc. On the one hand, it has also attracted the attention of many scientists. Compared with traditional fluorescent probes such as organic dyes and quantum dots, rare earth-doped upconversion fluorescent nanomaterials have the advantages of good chemical stability, high luminous color purity, low toxicity and large Stokes shift. At the same time, under the excitation conditions of long-wave-near-infrared light (800-1300nm), t...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/80C09K11/02B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C09K11/02C09K11/7773C09K11/7776
Inventor 陈力安西涛李静唐静谢婉莹酒俊霞
Owner CHANGCHUN UNIV OF TECH
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