A method for preparing cubic pyrochlore structured nanoparticles based on a sol-gel process and applications of the nanoparticles

A cubic pyrochlore, nanoparticle technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low mechanical strength of fluoride, limited application of anti-laser damage, poor chemical stability, etc., and achieves a simple, feasible and simplified preparation method. Double-doping or multi-doping process, good repeatability

Inactive Publication Date: 2019-04-02
SHAANXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although fluoride up-conversion materials have high efficiency, fluoride has low mechanical strength, poor chemical stability, and low threshold of resistance to laser damage, which limits its application in biological immunoassays and anti-counterfeiting marking materials to a certain extent.

Method used

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  • A method for preparing cubic pyrochlore structured nanoparticles based on a sol-gel process and applications of the nanoparticles
  • A method for preparing cubic pyrochlore structured nanoparticles based on a sol-gel process and applications of the nanoparticles
  • A method for preparing cubic pyrochlore structured nanoparticles based on a sol-gel process and applications of the nanoparticles

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preparation example Construction

[0032] A kind of preparation method of the cubic pyrochlore structure nano-particle based on sol-gel method of the present invention, comprises the following steps:

[0033] S1, using 10-100ml acetic acid as a solvent and as solution A;

[0034] S2, under the condition of fast stirring, be (1~9):1 mass ratio bismuth nitrate and erbium nitrate to join in solution A rapidly, and obtain solution B;

[0035] S3. Under rapid stirring, tetrabutyl titanate with a mass ratio of (0.1-0.2): 1 to the above solution is quickly added to solution B to obtain solution C;

[0036] S4. Put the solution C in a water bath at a temperature of 10-18° C. and add 13-15 mL of ammonia water to adjust the pH value of the solution to neutral to obtain a milky white solution D;

[0037] S5. Control the centrifugal rate to 5000-10000 rpm, and centrifuge the milky white solution D to obtain white powder E;

[0038] S6. Dry powder E at 80°C for 6-12 hours, and then calcine at 650-900°C to obtain Bi 2 Ti ...

Embodiment 1

[0044] Dissolve bismuth nitrate and erbium nitrate in 10 ml of acetic acid at a mass ratio of 1:1, and form a transparent solution by magnetic stirring in a water bath; adjust the temperature of the water bath to 10°C, and slowly add 13 ml of ammonia water to the transparent solution In the solution, a milky white product is produced, and the pH of the whole system is neutral, and the reaction is completed. Subsequently, the reacted solution was subjected to solid-liquid separation with a centrifuge at a centrifugation rate of 5000 rpm to obtain a white powder. The white powder was dried at 80°C for 6 hours, then transferred to a muffle furnace and calcined at 800°C for 1 hour to obtain Bi 2 Ti 2 o 7 : Er nano powder.

[0045] figure 1 The near-infrared light source with a wavelength of 980nm is given as the excitation source, and the obtained up-conversion luminescence performance is obtained. The test wavelength range is 200-900nm, and the integration time is 10ms. It ...

Embodiment 2

[0047] Dissolve bismuth nitrate and erbium nitrate in 40 ml of acetic acid at a mass ratio of 9:1, and form a transparent solution by magnetic stirring in a water bath; adjust the temperature of the water bath to 12°C, and slowly add 15 ml of ammonia water to the transparent solution In the solution, a milky white product is produced, and the pH of the whole system is neutral, and the reaction is completed. Subsequently, the reacted solution was subjected to solid-liquid separation with a centrifuge at a centrifugation rate of 8000 rpm to obtain a white powder. The white powder was dried at 80°C for 8 hours, then transferred to a muffle furnace and calcined at 800°C for 1 hour to obtain Bi 2 Ti 2 o 7 : Er nano powder.

[0048] figure 2 Given that the laser with a wavelength of 980nm is used as the excitation source, the obtained up-conversion luminescence performance is obtained. The test wavelength range is 200-900nm, and the integration time is 10ms. It can be seen fr...

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Abstract

A method for preparing cubic pyrochlore structured nanoparticles based on a sol-gel process and applications of the nanoparticles are disclosed. Acetic acid is adopted as a solvent. Through rigidly controlling the mass ratio of bismuth, erbium and titanium and by utilizing atomic-scale mixing thereof, an objective of precisely controlling the stoichiometric ratio of the bismuth, erbium and titanium is achieved. The pure cubic pyrochlore-phase Bi2Ti2O7:Er nanopowder having good crystallization performance can be obtained by drying, heating, temperature maintaining and cooling. Through excitation (980 nanometer) of a near-infrared light source, up-conversion red-green luminescence which can be observed with naked eyes is obtained for the first time without doping with other rare earth elements, and the up-conversion luminescence obtained is expected to exert important roles in the fields of biological detection, photo-thermal treatment, display, counterfeiting preventing, medical diagnosis, and the like.

Description

technical field [0001] The present invention belongs to ternary Bi 2 Ti 2 o 7 The field of compound nanoparticle preparation and luminescence technology, specifically relates to a preparation method and application of cubic pyrochlore structure nanoparticle based on sol-gel method. Background technique [0002] Near-infrared conversion visible light up-conversion material is a new type of functional material that can convert invisible infrared light into visible light with naked eyes. From the perspective of luminescence physics, it is a process of converting lower energy photons into higher energy photons, which is called the anti-Stoke effect. In recent years, rare earth up-conversion nano-luminescent materials are increasingly showing attractive application prospects in the fields of bioluminescent imaging, photothermal therapy, infrared detection, solar photovoltaic devices, optical anti-counterfeiting, etc., making it a hot spot in the current research of nano-lumine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/67
CPCC09K11/77
Inventor 葛万银徐美美焦思怡常哲
Owner SHAANXI UNIV OF SCI & TECH
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