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Holmium-based up-conversion nano material and preparation method thereof

A nanomaterial and nanoparticle technology, which is applied to the field of small-sized holmium-based up-conversion nanomaterials and their preparation, can solve problems such as fluorescence quenching, and achieve the effects of low equipment cost, simple preparation process and short preparation period.

Pending Publication Date: 2021-06-01
GUANGZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, high concentrations of holmium ion doping can easily cause fluorescence quenching

Method used

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  • Holmium-based up-conversion nano material and preparation method thereof
  • Holmium-based up-conversion nano material and preparation method thereof
  • Holmium-based up-conversion nano material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0083] This embodiment provides a NaHoF 4 @NaYF 4 :75%Tb@NaGdF 4 :49%Yb,1%Tm@NaYF 4 Preparation methods of upconversion nanomaterials.

[0084] (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 liquid after the reaction was...

Embodiment 2

[0089] This embodiment provides a NaHoF 4 @NaYF 4 :70%Tb@NaGdF 4 :46%Yb,0.75%Tm@NaYF 4 Preparation methods of upconversion nanomaterials.

[0090] (1)NaHoF 4 Nuclear layer preparation: put 14mL 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 100°C and keep it for 40min to remove water. Then the temperature was raised to 140° C. and kept for 40 minutes to generate 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 85 ° C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 275° C. for 1 h. Finally, the cloudy solution after the r...

Embodiment 3

[0095] This embodiment provides a NaHoF 4 @NaYF 4 :80%Tb@NaGdF 4 :52%Yb,1.25%Tm@NaYF 4 Preparation methods of upconversion nanomaterials.

[0096] (1)NaHoF 4 Nuclear layer preparation: put 16mL 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 110°C and keep it for 40min to remove water. Then the temperature was raised to 160° 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 95 ° C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 285° C. for 1 h. Finally, the cloudy solution after the react...

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Abstract

The invention belongs to the technical field of luminescent materials, and particularly relates to a small-size holmium-based up-conversion nano material with red light emission and a preparation method thereof. According to the up-conversion nano material, NaHoF4 serves as a core layer, a NaYF4: Tb shell layer, a NaGdF4: Yb, a Tm shell layer and a NaYF4 passivation layer sequentially coat the core layer, excitation energy is transmitted to the core layer from the second shell layer by sequentially utilizing interface energy transmission of a Gd<3+>: 6P7 / 2 energy level to a Tb<3+>: 5D4 energy level, energy migration between Tb<3+>: 5D4 energy levels and interface energy transmission of the Tb<3+>: 5D4 energy level to Ho<3+>: 5S2 / 5F4 energy level, a cross relaxation effect (5S2 / 5F4 + 5I7 -> 5F5 + 5I6) between Ho<3+> ions is caused, and finally Ho<3+>-based red up-conversion luminescence is obtained. The preparation process of the up-conversion nano material is simple, short in period, low in equipment cost, simple to operate and suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a small-sized holmium-based up-conversion nanometer material with red light emission and a preparation method thereof. Background technique [0002] Through multiphoton absorption, upconversion nanomaterials can convert low-energy excitation light into high-energy emission light. Compared with down-conversion fluorescent materials, up-conversion nanomaterials have the advantages of low toxicity, large Stokes shift and sharp emission peaks, and have application value in information security, solar cells, biomedical imaging, super-resolution nano-microscopy and other fields. Compared with blue light and green light, red light has deep biological tissue penetration due to its longer wavelength (600-700nm), and is known as the "optical window of visible light". Besides erbium and thulium ions, holmium ions are considered to be another important upconversion...

Claims

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Application Information

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