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A core-shell structure up-conversion nanomaterial and its preparation method

A nanomaterial and core-shell structure technology, which is applied in the field of red light-emitting core-shell structure up-conversion nanomaterials and their preparation, can solve problems such as concentration quenching, and achieve the effects of low equipment cost, easy operation and 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, NaHoF 4 base material due to the high concentration of Ho 3+ concentration quenching

Method used

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  • A core-shell structure up-conversion nanomaterial and its preparation method
  • A core-shell structure up-conversion nanomaterial and its preparation method
  • A core-shell structure up-conversion nanomaterial and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0083] This embodiment provides a NaHoF 4 @NaGdF 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 solution after the reaction w...

Embodiment 2

[0089] This embodiment provides a NaHoF 4 @NaGdF 4 :72%Tb@NaGdF 4 :45%Yb,0.7%Tm@NaYF 4 Preparation methods of upconversion nanomaterials.

[0090] (1)NaHoF 4 Nuclear layer preparation: put 13mL 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 95°C and keep it for 40min to remove water. Then the temperature was raised to 145° 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 80 ° C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 270° C. for 1 h. Finally, the cloudy solution after the reacti...

Embodiment 3

[0095] This embodiment provides a NaHoF 4 @NaGdF 4 :78%Tb@NaGdF 4 :55%Yb,1.3%Tm@NaYF 4 Preparation methods of upconversion nanomaterials.

[0096] (1)NaHoF 4 Nuclear layer preparation: put 17mL 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 115°C and keep it for 40min to remove water. Then the temperature was raised to 155° 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 100 ° C and kept for 1 h , to remove excess methanol. Then, under the protection of argon, the temperature was raised to 290° C. for 1 h. Finally, the cloudy liquid after the re...

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Abstract

The invention belongs to the technical field of luminescent materials, and in particular relates to a core-shell structure up-conversion nano material emitting red light and a preparation method thereof. The upconversion nanomaterials are based on NaHoF 4 It is the core layer, and it is coated with NaGdF in turn 4 : Tb shell, NaGdF 4 :Yb, Tm shell and NaYF 4 passivation layer, in turn utilizing Gd 3+ : 6 P 7 / 2 Energy transfer between energy levels, 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 NaHoF 4 based up-conversion red emission. The preparation process of the up-conversion nanometer material is simple, the cycle is short, the equipment cost is low, the operation is simple, and it is suitable for mass production.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a core-shell structure up-conversion nano material emitting red light and a preparation method thereof. Background technique [0002] Photon upconversion refers to the anti-Stokes process that converts two or more low-energy photons into a single high-energy photon. Rare earth-doped upconversion nanomaterials have the advantages of high photochemical stability, long fluorescence lifetime, and low toxicity, and have great application prospects in the fields of biological imaging, optical temperature sensors, anti-counterfeiting, and 3D displays. Compared with the short-wavelength blue light and green light, the longer-wavelength red light (600-700nm) is known as the "biological window of visible light" because of its deeper penetration into biological tissues. As we all know, NaHoF 4 Based on upconversion nanomaterials have excellent performance in biom...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
CPCC09K11/7773
Inventor 林浩郑雪刚
Owner GUANGZHOU UNIVERSITY
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