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Terbium ion doped up-conversion nano material and preparation method thereof

A nanomaterial and ion doping technology is applied in the field of terbium ion-doped Ho3+-based up-conversion nanomaterials and their preparation, which can solve the problems of fluorescence quenching, limited application in the biological field, etc., and achieves low equipment cost, short preparation period, Simple preparation process

Active Publication Date: 2021-06-04
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Ho 3+ The biggest problem with the base material is the high concentration of Ho 3+ Fluorescence quenching induced by doping
In addition, the larger size also limits its application in the biological field

Method used

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  • Terbium ion doped up-conversion nano material and preparation method thereof
  • Terbium ion doped up-conversion nano material and preparation method thereof
  • Terbium ion doped up-conversion nano material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] This embodiment provides a NaHoF 4 @NaYF 4 :75%Tb@NaYbF 4 :30%Tb@NaYF 4 Preparation methods of upconversion nanomaterials.

[0076] (1)NaHoF 4 Nuclear layer preparation: put 15mL oleic acid and 20mL octadecene into a 100mL three-necked flask, mix and stir evenly. Then add 1mL concentration of 1mol L -1 Holmium chloride solution, mix and stir evenly, then raise the temperature to 105°C and keep it for 40min to remove water. Then the temperature was raised to 150°C and kept for 40 minutes to form a rare earth-oleic acid chelate. Then the temperature was naturally cooled to room temperature, 0.1 g of sodium hydroxide (2.5 mmol) and 0.148 g of ammonium fluoride (4 mmol) in methanol (10 mL in total) were added to the above mixture and stirred, then the temperature was raised to 90 °C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 280° C. for 1 h. Finally, the cloudy solution after the reaction was nat...

Embodiment 2

[0081] This embodiment provides a NaHoF 4 @NaYF 4 :73.5%Tb@NaYbF 4 :28.5%Tb@NaYF 4 Preparation methods of upconversion nanomaterials.

[0082] (1)NaHoF 4 Nuclear layer preparation: put 13.6mL oleic acid and 20mL octadecene into a 100mL three-necked flask, mix and stir evenly. Then add 1mL concentration of 1mol L -1 Holmium chloride solution, mix and stir evenly, then raise the temperature to 98°C and keep it for 40min to remove water. Then the temperature was raised to 148° C. and kept for 40 minutes to form a rare earth-oleic acid chelate. Then the temperature was naturally cooled to room temperature, 0.1 g of sodium hydroxide (2.5 mmol) and 0.148 g of ammonium fluoride (4 mmol) in methanol (10 mL in total) were added to the above mixture and stirred, then the temperature was raised to 88 °C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 278° C. for 1 h. Finally, the cloudy solution after the reaction wa...

Embodiment 3

[0087] This embodiment provides a NaHoF 4 @NaYF 4 :76.5%Tb@NaYbF 4 :31.5%Tb@NaYF 4 Preparation methods of upconversion nanomaterials.

[0088] (1)NaHoF 4 Nuclear layer preparation: put 16.4mL oleic acid and 20mL octadecene into a 100mL three-necked flask, mix and stir evenly. Then add 1mL concentration of 1mol L -1 Holmium chloride solution, mix and stir evenly, then raise the temperature to 112°C and keep it for 40min to remove water. Then the temperature was raised to 152° C. and kept for 40 minutes to form a rare earth-oleic acid chelate. Then the temperature was naturally cooled to room temperature, 0.1 g of sodium hydroxide (2.5 mmol) and 0.148 g of ammonium fluoride (4 mmol) in methanol (10 mL in total) were added to the above mixture and stirred, then the temperature was raised to 92 °C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 282° C. for 1 h. Finally, the cloudy solution after the reaction...

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Abstract

The invention belongs to the technical field of luminescent materials, and particularly relates to a terbium ion doped Ho < 3 + >-based up-conversion nano material for red light emission and a preparation method thereof. The up-conversion nano material takes NaHoF4 as a core layer, a NaYF4: Tb shell layer, a NaYbF4: Tb shell layer and a NaYF4 passivation layer are sequentially coated outside the core layer, excitation energy is transmitted to the core layer from a second shell layer by sequentially utilizing energy migration between Tb < 3 + >: 5D4 energy levels and interface energy transmission of the Tb < 3 + >: 5D4 energy levels to Ho < 3 + >: 5S2 / 5F4 energy levels, a cross relaxation effect (5S2 / 5F4 + 5I7-5F5 + 5I6) between Ho < 3 + > ions is caused, and finally Ho < 3 + >-based up-conversion red light emission is obtained. The up-conversion nano material is simple in preparation process, low in equipment cost, easy to operate, short in preparation period and suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, in particular to a terbium ion-doped Ho 3+ Upconversion nanomaterials and preparation methods thereof. Background technique [0002] Upconversion luminescence, also known as anti-Stokes luminescence, refers to the process of converting excitation light with a longer wavelength into emitted light with a shorter wavelength through multiphoton absorption. Up-conversion nanomaterials have the advantages of narrow emission bands, rich emission levels, high chemical stability, and low toxicity. In the range of visible light, red light (600-700nm) has a strong penetrability to biological tissues due to its longer wavelength, and is known as the "optical window". In addition, Ho 3+ As an excellent active ion, ions have outstanding performance in the field of biomedicine for their up-conversion red light emission. However, Ho 3+ The biggest problem with the base material is the high con...

Claims

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Application Information

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IPC IPC(8): C09K11/85C09K11/02B82Y30/00
CPCC09K11/7773C09K11/02B82Y30/00
Inventor 林浩郑雪刚
Owner GUANGZHOU UNIVERSITY
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