A kind of terbium ion doped up-conversion nanomaterial and its preparation method

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 limited biological application, fluorescence quenching, etc., and achieves short preparation period, low equipment cost, Simple preparation process

Active Publication Date: 2022-04-29
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of terbium ion doped up-conversion nanomaterial and its preparation method
  • A kind of terbium ion doped up-conversion nanomaterial and its preparation method
  • A kind of terbium ion doped up-conversion nanomaterial and its preparation method

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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, in particular to a terbium ion-doped Ho 3+ Upconversion nanomaterials and preparation methods thereof. The upconversion nanomaterials are based on NaHoF 4 It is the core layer, and it is coated with NaYF in turn 4 : Tb shell, NaYbF 4 :Tb shell and NaYF 4 passivation layer, in turn utilizing Tb 3+ : 5 D. 4 Energy transfer between energy levels and Tb 3+ : 5 D. 4 Energy level versus Ho 3+ : 5 S 2 / 5 f 4 The interfacial energy transfer of the energy level transfers the excitation energy from the second shell to the core and causes the Ho 3+ The cross-relaxation effect between ions ( 5 S 2 / 5 f 4 + 5 I 7 → 5 f 5 + 5 I 6 ), and finally get Ho 3+ Based on up-converted red emission. The up-conversion nanometer material has simple preparation process, low equipment cost, easy operation and short preparation period, and is 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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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85C09K11/02B82Y30/00
CPCC09K11/7773C09K11/02B82Y30/00
Inventor 林浩郑雪刚
Owner GUANGZHOU UNIVERSITY
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