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A three-dimensional nayf 4 Upconversion luminescent micro flower and preparation method thereof

A micro-flower, three-dimensional technology, applied in luminescent materials, chemical instruments and methods, photovoltaic power generation, etc., can solve the problems of difficult to obtain three-dimensional three-dimensional micro-particles, environmental pollution by surfactants, and troublesome post-processing of products. , to achieve the effect of good effect, lower energy consumption and shorter time.

Active Publication Date: 2022-07-08
HUBEI UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organic thermal decomposition method generally uses expensive organic metal salts and high-boiling organic solvents and surfactants to react at higher temperatures under the protection of inert gases. This method requires anhydrous and oxygen-free pretreatment of the reaction solution, and the post-processing of the product is troublesome. , and the cost of raw materials is high; high-temperature solid-phase method is also commonly used to prepare rare earth doped NaYF 4 Up-conversion materials, but the morphology of the prepared materials is uncontrollable and the reaction temperature is high
The luminescent properties of the samples prepared by the hydrothermal solvothermal method are good, but in general, the hydrothermal reaction to prepare the hexagonal phase NaYF 4 The cycle of up-conversion materials is long, and the participation of surfactants is required to pollute the environment to a certain extent
At the same time, due to NaYF 4 Its own crystallographic growth characteristics, three-dimensional micron particles are not easy to make

Method used

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  • A three-dimensional nayf  <sub>4</sub> Upconversion luminescent micro flower and preparation method thereof
  • A three-dimensional nayf  <sub>4</sub> Upconversion luminescent micro flower and preparation method thereof
  • A three-dimensional nayf  <sub>4</sub> Upconversion luminescent micro flower and preparation method thereof

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preparation example Construction

[0042] see figure 1 , in this example, the three-dimensional NaYF 4 The preparation method of the upconversion luminescent microflora comprises the following steps:

[0043] Step S10, to the containing Y 3+ , Yb 3+ and Er 3+ Ethanolamine was added to the initial solution to obtain a precursor solution.

[0044] wherein, in the initial solution, the Y 3+ provided by at least one of yttrium nitrate and yttrium chloride, and / or the Yb 3+ provided by at least one of ytterbium nitrate and ytterbium chloride; and / or, the Er 3+ Provided by at least one of erbium nitrate and erbium chloride. That is, Y 3+ It can be provided for yttrium nitrate dissolved in water, also can be provided for yttrium chloride dissolved in water, and can also be provided for yttrium nitrate and yttrium chloride dissolved in water at the same time. Yb 3+ and Er 3+ The principle is the same as the above, and will not be repeated here. In a preferred embodiment, the initial solution is obtained by ...

Embodiment 1

[0057] Press Y 3+ : Yb 3+ : Er 3+ The molar ratio is 78:20:2. Weigh 1 mmol of yttrium nitrate, ytterbium nitrate and erbium nitrate and dissolve them in 10 mL of water to form an initial solution. Add 1.5 mL of ethanolamine to the initial solution under magnetic stirring at 600 r / min, and stir for 5 min to obtain the precursor solution. Under magnetic stirring at 600 r / min, 24 mmol NaBF was 4 The reaction solution is added to the precursor solution, and concentrated hydrochloric acid is added to the reaction solution to adjust the pH to 9 to obtain a colloidal solution. The colloidal solution was added to the autoclave and heated in an oven at 100 °C for 60 min. After the reaction kettle was cooled to room temperature, centrifuged, washed three times with absolute ethanol and water ultrasonically, and dried at 80 °C to obtain a three-dimensional flower-shaped yellow luminescent NaYF. 4 : 20% Yb 3+ / 2%Er 3+ Up-converting microcrystalline.

Embodiment 2

[0059] Press Y 3+ : Yb 3+ : Er 3+ The molar ratio is 78:20:2. Weigh 1 mmol of yttrium nitrate, ytterbium nitrate and erbium nitrate and dissolve them in 10 mL of water to form an initial solution. Add 1.5 mL of ethanolamine to the initial solution under magnetic stirring at 600 r / min, and stir for 5 min to obtain the precursor solution. Under magnetic stirring at 600 r / min, 24 mmol NaBF was 4 adding concentrated hydrochloric acid to the reaction solution to adjust the pH to 10 to obtain a colloidal solution. The colloidal solution was added to the autoclave and heated in an oven at 100 °C for 60 min. After the reaction kettle was cooled to room temperature, centrifuged, washed three times with absolute ethanol and water ultrasonically, and dried at 80 °C to obtain a three-dimensional flower-shaped orange luminescent NaYF. 4 : 20% Yb 3+ / 2%Er 3+ Up-converting microcrystalline.

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Abstract

The invention discloses a three-dimensional NaYF 4 Upconversion luminescent microflora and preparation method thereof, wherein three-dimensional NaYF 4 The preparation method of the up-conversion luminescent microflora comprises the following steps: S10, to the Y-containing 3+ , Yb 3+ and Er 3+ Add ethanolamine to the initial solution of , to get the precursor solution; S20, add NaBF to the precursor solution 4 , and adjust the pH value to 9-10 to obtain a colloidal solution; S30, heat the colloidal solution at 100-120 °C for 40-60 min, then separate, wash and dry to obtain three-dimensional NaYF 4 Upconverting luminescent micron flowers. The preparation method requires short time and low reaction temperature, and is suitable for large-scale production; and finally, three-dimensional NaYF with uniform particle size, good luminescence performance and adjustable color is prepared. 4 Upconversion luminescent micro-flowers, because of the large specific surface area and complex structure of the three-dimensional micro-particles, are more easily attached to the surface of biological cells and viruses. Therefore, they are applied in the fields of bioimaging and photodynamic therapy, and the effect is better.

Description

technical field [0001] The invention relates to the technical field of up-conversion materials, in particular to a three-dimensional NaYF 4 Upconversion luminescent microflora and preparation method thereof. Background technique [0002] Upconversion luminescence is an anti-Stokes process that achieves a short visible light emission by absorbing two or more low-energy near-infrared light long-wavelength photons. From the first conceptual infrared quantum counter device proposed by Bloembergen N. in 1959, upconversion luminescent materials have shown potential applications in the fields of sensors, photodynamic therapy, solar cells, biomarkers, and imaging. [0003] Sodium yttrium fluoride (NaYF 4 ) is currently recognized as one of the host materials with high-efficiency upconversion luminescence. 4 Upconversion materials are of great significance. Under normal conditions, NaYF 4 There are two crystal structures, one is a cubic phase and the other is a hexagonal phase, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85
CPCC09K11/7773Y02E10/52
Inventor 王松赵琦胡雍诗玲张莹钟志成梁桂杰程晓红
Owner HUBEI UNIV OF ARTS & SCI