an er with blu-ray upconversion 3+ /tm 3+ -mofs fluorescent material and preparation method thereof

A fluorescent material and blue light technology, applied in the field of material chemistry, can solve problems such as unfavorable biological tissue imaging, limited application prospects, tissue fluorescence interference, etc., and achieve the effects of improving energy transfer efficiency, simple process, and low cost

Active Publication Date: 2021-06-18
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional rare earth MOFs materials generally use ultraviolet light as the excitation light source, and ultraviolet light has a small penetration depth in biological tissue and will cause tissue fluorescence interference, which is not conducive to biological tissue imaging
In addition, the luminescence of rare earth ions comes from the transition between forbidden 4f electrons, and the luminescence efficiency is low, which limits its application prospects.

Method used

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  • an er with blu-ray upconversion <sup>3+</sup> /tm <sup>3+</sup> -mofs fluorescent material and preparation method thereof
  • an er with blu-ray upconversion <sup>3+</sup> /tm <sup>3+</sup> -mofs fluorescent material and preparation method thereof
  • an er with blu-ray upconversion <sup>3+</sup> /tm <sup>3+</sup> -mofs fluorescent material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Sodium citrate-based Er with blue light upconversion 3+ / Tm 3+ -MOFs fluorescent material (MOFs-Y 0.92 / Er 0.6 / Tm 0.2 )

[0031] The preparation method is as follows

[0032] 1) Weigh 0.08607g of erbium oxide, 0.08682g of thulium oxide, and 1.0161g of yttrium oxide and dissolve them in concentrated nitric acid respectively, heat and stir to form erbium nitrate, thulium nitrate, and yttrium nitrate solutions, and dilute to 45ml with deionized water respectively to prepare the concentration 0.01mol / L, 0.01mol / L, 0.2mol / L stock solutions of erbium nitrate, thulium nitrate, and yttrium nitrate.

[0033] 2) Weigh 0.14705g (0.5mmol) of sodium citrate dihydrate and mix with 10ml of deionized water, measure 6ml of Er(NO 3 ) 3 solution, 2ml of Tm(NO 3 ) 3 solution, 4.6ml of Y(NO 3 ) 3 solution, and were added to the sodium citrate solution, ultrasonic treatment for 30min. Weigh 0.10507g (0.5mmol) of the organic ligand trimesic acid and dissolve it in 40ml of N,N...

Embodiment 2

[0048] Effect of the amount of sodium citrate on crystal nucleation

[0049] (1) The preparation method is as follows:

[0050] 1) Weigh 0.08607g of erbium oxide, 0.08682g of thulium oxide, and 1.0161g of yttrium oxide and dissolve them in concentrated nitric acid respectively, heat and stir to form erbium nitrate, thulium nitrate, and yttrium nitrate solutions, and dilute to 45ml with deionized water respectively to prepare the concentration 0.01mol / L, 0.01mol / L, 0.2mol / L stock solutions of erbium nitrate, thulium nitrate, and yttrium nitrate.

[0051] 2) Weigh 0.08823g (0.3mmol), 0.11764g (0.4mmol), 0.14705g (0.5mmol) of sodium citrate dihydrate and mix them with 10ml of deionized water, and measure 6ml of Er(NO 3 ) 3 solution, 2ml of Tm(NO 3 ) 3 solution, 4.6ml of Y(NO 3 ) 3 solution, and were added to the sodium citrate solution, ultrasonic treatment for 30min. Weigh 0.10507g organic ligand trimesic acid and dissolve in 40ml of N,N-dimethylformamide (DMF) solution, ...

Embodiment 3

[0060] Influence of Doping Ratio of Rare Earth Ions on Luminescence Intensity

[0061] (1) The preparation method is as follows:

[0062] 1) Weigh 0.08607g of erbium oxide, 0.08682g of thulium oxide, and 1.0161g of yttrium oxide and dissolve them in concentrated nitric acid respectively, heat and stir to form erbium nitrate, thulium nitrate, and yttrium nitrate solutions, and dilute to 45ml with deionized water respectively to prepare the concentration 0.01mol / L, 0.01mol / L, 0.2mol / L stock solutions of erbium nitrate, thulium nitrate, and yttrium nitrate.

[0063] 2) Weigh 0.14705g (0.5mmol) of sodium citrate dihydrate and mix with 10ml of deionized water evenly. In order to verify Er 3+ 、Tm 3+ , Y 3+ The effect of the doping ratio of ions on the luminous intensity of MOFs materials, in this experiment Er 3+ 、Tm 3+ , Y 3+ The doping ratio of is selected as:

[0064] ①Er 3+ 、Tm 3+ , Y 3+ =5%, 2%, 93%, that is, measure 2.5ml of Er(NO 3 ) 3 solution, 1ml of Tm(NO 3 )...

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Abstract

The invention relates to an Er with blue light up-conversion 3+ / Tm 3+ ‑MOFs fluorescent material and its preparation method. Dissolve trimesic acid in DMF; add erbium nitrate, thulium nitrate, and yttrium nitrate into sodium citrate; mix the two solutions and place them in a hydrothermal kettle for hydrothermal reaction. In the rare earth MOFs material prepared by the present invention, sodium citrate as an "auxiliary group" can provide a large number of carboxyl groups, coordinate with trimesic acid ligands and rare earth ions, and inhibit individual The rapid growth of crystals inhibits the secondary nucleation process of crystals in the system. When near-infrared light is used as the excitation light source, sodium citrate as a matrix can effectively increase Er 3+ To Tm 3+ The energy transfer efficiency without doping Yb 3+ Under the circumstances, the MOFs material can still exhibit strong blue light emission, effectively avoiding the "autofluorescence" interference effect caused by ultraviolet excitation in biological detection.

Description

technical field [0001] The invention belongs to the field of material chemistry, and in particular relates to the use of sodium citrate as a substrate to prepare lanthanide metal-organic framework materials (MOFs-Y 1-x-y / Er x / Tm y ), its BET specific surface area is 119.02m 2 / g. It solves the problem of uneven growth rate of MOFs materials in the early stage, and effectively improves the Er 3+ To Tm 3+ Under the excitation of near-infrared light (980nm), the MOFs material exhibits strong blue light emission, which effectively avoids the "autofluorescence" interference effect caused by ultraviolet excitation in biological detection. Background technique [0002] Metal-Organic Frameworks (MOF) is a material with a porous structure. Because of its large BET specific surface area, it can effectively increase the contact range with the target and improve the detection sensitivity. The structural stability, adjustable pore size and other advantages have attracted great at...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C09K11/06
CPCC08G83/008C09K11/06C09K2211/182Y02P20/10
Inventor 刘雯赵铭钰王绩伟丁勇梅勇张璐黄峻霆杨涵
Owner LIAONING UNIVERSITY
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