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A rare earth up-conversion luminescent nanomaterial with controllable synthesis of core-shell structure and its preparation method and application

A rare earth up-conversion and nano-material technology, which is applied in the field of nano-materials to achieve the effects of good up-conversion luminescence performance, broad application prospects and high luminous efficiency

Active Publication Date: 2020-05-15
CAPITAL NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Efficient synthesis of rare-earth upconversion luminescent nanomaterials with controlled core-shell structure remains a challenge

Method used

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  • A rare earth up-conversion luminescent nanomaterial with controllable synthesis of core-shell structure and its preparation method and application
  • A rare earth up-conversion luminescent nanomaterial with controllable synthesis of core-shell structure and its preparation method and application
  • A rare earth up-conversion luminescent nanomaterial with controllable synthesis of core-shell structure and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Example 1, NaGdF 4 Preparation of small nanoparticles

[0061] (1) Add GdCl to a 100mL three-necked flask 3 0.830mmol, then add 8mL oleic acid, 8mL oleylamine and 16mL octadecene, pump the system to vacuum, stir at 70°C for 0.5h, inflate twice with argon during this period, and completely exhaust the air in the system. It was then heated to 120 °C to obtain a clear solution and kept for 45 min. Cool to room temperature.

[0062] (2) 4mmol NH 4 F and 2.5mmol NaOH were added to the above mixed solution. The system was evacuated again with an oil pump, and stirred at 70°C for 2.5 hours to obtain a clear solution. During this period, the system was inflated twice with argon to completely discharge the air in the system.

[0063] (3) Then close the air valve, slowly heat to 300°C at a rate of 10°C / min, and keep for 1.5h. Then continue to heat up to 320°C, and keep it for 20min until it cools down to room temperature naturally.

[0064] (4) Pour into a centrifuge tube...

Embodiment 2

[0066] Example 2, NaYF 4 Preparation of :Yb:Er Core Nanoparticles

[0067] (1) Add YCl to a 100mL three-necked flask 3 0.83mmol, YbCl 3 0.15mmol, ErCl 3 0.02mmol (Y:Yb:Er=0.83:0.15:0.02), then add 6mL oleic acid and 15mL octadecene, pump the system to vacuum, stir at 70°C for 0.5h, inflate twice with argon , completely exhaust the air in the system. It was then heated to 125°C to obtain a clear solution and maintained for 45 min. Cool to room temperature.

[0068] (2) 4mmol NH 4 F and 2.5mmol NaOH were added to the above mixed solution. The system was evacuated again with an oil pump, and stirred at 70°C for 2.5 hours to obtain a clear solution. During this period, the system was inflated twice with argon to completely discharge the air in the system. Then slowly heat up to 300°C at a rate of 10°C / min, close the gas valve, and keep for 1h.

[0069] (3) After cooling down to room temperature naturally, pour it into a centrifuge tube and centrifuge at high speed (12,...

Embodiment 3

[0071] Example 3, NaYF 4 :Yb:Er@NaGdF 4 Preparation of single-shell nanoparticles

[0072] (1) Add YCl to a 100mL three-necked flask 3 0.83mmol, YbCl 3 0.15mmol, ErCl 3 0.02mmol (Y:Yb:Er=0.83:0.15:0.02), then add 6mL oleic acid and 15mL octadecene, pump the system to vacuum, stir at 70°C for 0.5h, inflate twice with argon, Completely remove air from the system. It was then heated to 125°C to obtain a clear solution and kept for 45min. Cool to room temperature.

[0073] (2) 4mmol NH 4 F and 2.5mmol NaOH were added to the above mixed solution. The system was evacuated again with an oil pump, and stirred at 70°C for 2.5 hours to obtain a clear solution. During this period, the system was inflated twice with argon to completely discharge the air in the system. Then slowly heat up to 300°C at a rate of 10°C / min, close the gas valve, and keep for 1h.

[0074] (3) Take out the above step (2) with a 1mL stainless steel tube syringe to obtain 1mL of the mixture, and then i...

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Abstract

The invention discloses a controllable synthetic core-shell structured rare-earth up-conversion luminescence nano material as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) in an inert gas, enabling products obtained after raw material treatment to react so as to obtain small nano rare-earth granules; (2) under a vacuum condition, mixing a rare-earth compound with a high melting point organic solvent and an anionic surfactant, performing a heating reaction, cooling to room temperature, further mixing with hydroxide and fluoride,and enabling the components to react under the protection of inert gas so as to obtain a system with large nano rare-earth granules; and (3) in an organic solvent of a high melting point, mixing the system with large nano rare-earth granules with the small nano rare-earth granules at least once, and performing repeated reactions, thereby obtaining the rare-earth up-conversion luminescence nano material. The method disclosed by the invention is low in cost, and is simple and convenient and universal, nano granules with controllable layer thicknesses, layer numbers and layer types can be prepared, and the rare-earth nano material is good in up-conversion luminescence property.

Description

technical field [0001] The invention relates to a rare earth up-conversion luminescent nanomaterial with a controllable synthesis of a core-shell structure, a preparation method and an application thereof, and belongs to the field of nanomaterials. Background technique [0002] Rare earth up-conversion luminescent nanomaterials can absorb 980nm, 808nm or other long-wavelength photons and then emit ultraviolet and visible light. This special property makes them have potential applications in many fields, such as cell imaging, anti-counterfeiting, printing and other fields. Restricted by the characteristics of rare earth up-conversion luminescent nanomaterials, their luminescent performance has great defects. In order to improve their luminous efficiency, the construction of rare earth up-conversion luminescent nanomaterials with a core-shell structure can effectively improve their luminescent performance. The effective synthesis of rare-earth upconversion luminescent nanomate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/02C09K11/85B82Y20/00G01N21/63B42D25/36
CPCB42D25/36B82Y20/00C09K11/02C09K11/7773G01N21/63
Inventor 周晶马李益陈妙
Owner CAPITAL NORMAL UNIVERSITY
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