Method for preparing ytterbium-thulium-doped blue luminous pyrochlore-phase nanofiber and application of nanofiber

Abstract

The invention discloses a method for preparing a rare-earth ytterbium-thulium-doped blue luminous pyrochlore-phase nanofiber and application of the nanofiber. The method comprises the steps of addingpolyvinylpyrrolidone into dimethyl formamide, preparing a one-dimensional nanofiber material under the acting force of liquid surface tension and an electric field, and then removing organic matter residues in the processes of heating, heat preservation and cooling to prepare the cubic pyrochlore-phase one-dimensional nanofiber with high crystallinity. The obtained one-dimensional nanofiber achieves blue up-conversion luminescence perceivable for eyes and has high dispersibility in water and a great photothermal effect under the irradiation of near-infrared light. The preparation method is simple, feasible and high in repeatability and can meet the requirement of industrial batch production. An up-conversion photothermal material matrix is an oxide which is high in chemical stability and free of toxin and is easily dispersed in water, and the demands of photo-thermal therapy can be met. The prepared one-dimensional pure pyrochlore-phase nano material is expected to play an important role in the treatment field of major diseases such as cancers and tumors.

Description

technical field

[0001] The invention belongs to rare earth ternary Bi 2 Ti 2 o 7 : Yb 3+ ,Tm 3+ The technical field of compound one-dimensional nanomaterial preparation and up-conversion luminescence and photothermal therapy, specifically relates to a preparation method and application of ytterbium-thulium double-doped blue luminescent pyrochlore phase nanofibers. Background technique

[0002] Near-infrared conversion visible light up-conversion material is a new type of functional material that can convert invisible infrared light into visible light with naked eyes. Due to its unique physical and chemical properties, it has broad application prospects in the fields of three-dimensional displays, lasers, biological detection and anti-counterfeiting. If the up-conversion material is added to the ink or paint and applied to anti-counterfeiting, it can enhance the confidentiality of the product, which is called high-tech anti-counterfeiting technology. In addition, since ...

Examples

preparation example Construction

[0032] A preparation method and application of ytterbium-thulium double-doped blue luminescent pyrochlore phase nanofibers of the present invention, comprising the following steps:

[0033] S1, DMF and acetic acid are mixed and stirred according to the mass ratio of 1:(0.2~0.6), to obtain solution A;

[0034] S2. In the process of continuous stirring, tetrabutyl titanate with a mass ratio of 1: (4-4.5) to solution A is added to solution A to obtain solution B;

[0035] S3, adding ytterbium nitrate and thulium nitrate with a mass ratio of 1: (3 to 20) into solution B during continuous stirring to obtain solution C;

[0036] S4, adding bismuth nitrate with a mass ratio of 1: (20 to 30) to solution C during continuous stirring to obtain solution D;

[0037] S5, adding PVP with a mass fraction of 7-12% to the solution D and continuing to stir to form an electrospinning precursor solution;

[0038] S6. In the case of applying a high-voltage power supply of 18-22 kV, spray the pre...

Embodiment 1

[0048] Mix DMF and acetic acid at a mass ratio of 0.4:1, and form a transparent solution by magnetic stirring; then add 1 g of tetrabutyl titanate and dissolve it fully by stirring; add thulium nitrate and ytterbium nitrate, nitric acid The mass ratio of ytterbium and thulium nitrate is 3:1; after it is fully dissolved, add bismuth nitrate and fully stir to dissolve it. The mass ratio of bismuth nitrate to solution is 1:20, and finally add PVP with a mass fraction of 7%, and magnetically stir Then obtain the electrospinning precursor solution.

[0049] Under the conditions of a control voltage of 18KV and a flow rate of 3 μl / m, a large amount of nanomaterials appeared on the collector. After the electrospinning was completed, the nanomaterials on the collector were transferred to the muffle furnace and heated at 2°C / min. Raise the rate to 750°C for 1 hour to obtain pyrochlore phase Bi with high crystallinity 2 Ti 2 o 7 : Yb 3+ , Tm 3+ nanomaterials.

[0050] figure 1 Gi...

Embodiment 2

[0052] Mix DMF and acetic acid at a mass ratio of 0.4:1, and form a transparent solution by magnetic stirring; then add 1 g of tetrabutyl titanate and dissolve it fully by stirring; add thulium nitrate and ytterbium nitrate, nitric acid The mass ratio of ytterbium and thulium nitrate is 7:1; after it is fully dissolved, add bismuth nitrate and fully stir to dissolve it. The mass ratio of bismuth nitrate to solution is 1:25, and finally add PVP with a mass fraction of 9%, and magnetically stir Then obtain the electrospinning precursor solution.

[0053] Under the conditions of a control voltage of 20KV and a flow rate of 8μl / m, a large amount of nanomaterials appeared on the collector. After the electrospinning was completed, the nanomaterials on the collector were transferred to the muffle furnace and heated at 3°C / min. If the rate is increased to 800°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ , Tm 3+ n...

technical field

[0001] The invention belongs to rare earth ternary Bi 2 Ti 2 o 7 : Yb 3+ ,Tm 3+ The technical field of compound one-dimensional nanomaterial preparation and up-conversion luminescence and photothermal therapy, specifically relates to a preparation method and application of ytterbium-thulium double-doped blue luminescent pyrochlore phase nanofibers. Background technique

[0002] Near-infrared conversion visible light up-conversion material is a new type of functional material that can convert invisible infrared light into visible light with naked eyes. Due to its unique physical and chemical properties, it has broad application prospects in the fields of three-dimensional displays, lasers, biological detection and anti-counterfeiting. If the up-conversion material is added to the ink or paint and applied to anti-counterfeiting, it can enhance the confidentiality of the product, which is called high-tech anti-counterfeiting technology. In addition, since ...

Examples

preparation example Construction

[0032] A preparation method and application of ytterbium-thulium double-doped blue luminescent pyrochlore phase nanofibers of the present invention, comprising the following steps:

[0033] S1, DMF and acetic acid are mixed and stirred according to the mass ratio of 1:(0.2~0.6), to obtain solution A;

[0034] S2. In the process of continuous stirring, tetrabutyl titanate with a mass ratio of 1: (4-4.5) to solution A is added to solution A to obtain solution B;

[0035] S3, adding ytterbium nitrate and thulium nitrate with a mass ratio of 1: (3 to 20) into solution B during continuous stirring to obtain solution C;

[0036] S4, adding bismuth nitrate with a mass ratio of 1: (20 to 30) to solution C during continuous stirring to obtain solution D;

[0037] S5, adding PVP with a mass fraction of 7-12% to the solution D and continuing to stir to form an electrospinning precursor solution;

[0038] S6. In the case of applying a high-voltage power supply of 18-22 kV, spray the pre...

Embodiment 1

[0048] Mix DMF and acetic acid at a mass ratio of 0.4:1, and form a transparent solution by magnetic stirring; then add 1 g of tetrabutyl titanate and dissolve it fully by stirring; add thulium nitrate and ytterbium nitrate, nitric acid The mass ratio of ytterbium and thulium nitrate is 3:1; after it is fully dissolved, add bismuth nitrate and fully stir to dissolve it. The mass ratio of bismuth nitrate to solution is 1:20, and finally add PVP with a mass fraction of 7%, and magnetically stir Then obtain the electrospinning precursor solution.

[0049] Under the conditions of a control voltage of 18KV and a flow rate of 3 μl / m, a large amount of nanomaterials appeared on the collector. After the electrospinning was completed, the nanomaterials on the collector were transferred to the muffle furnace and heated at 2°C / min. Raise the rate to 750°C for 1 hour to obtain pyrochlore phase Bi with high crystallinity 2 Ti 2 o 7 : Yb 3+ , Tm 3+ nanomaterials.

[0050] figure 1 Gi...

Embodiment 2

[0052] Mix DMF and acetic acid at a mass ratio of 0.4:1, and form a transparent solution by magnetic stirring; then add 1 g of tetrabutyl titanate and dissolve it fully by stirring; add thulium nitrate and ytterbium nitrate, nitric acid The mass ratio of ytterbium and thulium nitrate is 7:1; after it is fully dissolved, add bismuth nitrate and fully stir to dissolve it. The mass ratio of bismuth nitrate to solution is 1:25, and finally add PVP with a mass fraction of 9%, and magnetically stir Then obtain the electrospinning precursor solution.

[0053] Under the conditions of a control voltage of 20KV and a flow rate of 8μl / m, a large amount of nanomaterials appeared on the collector. After the electrospinning was completed, the nanomaterials on the collector were transferred to the muffle furnace and heated at 3°C / min. If the rate is increased to 800°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ , Tm 3+ n...

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