Preparation method and application of rare earth ytterbium-holmium-dual-doped pyrochlore phase nanofiber

Abstract

The invention discloses a preparation method and application of a rare earth ytterbium-holmium-dual-doped pyrochlore phase nanofiber. The method comprises the steps that with dimethylformamide as a solvent, polyvinylpyrrolidone is added, a Taylor cone is formed through liquid drops under a static field, under the liquid surface tension and application force of an electric field, an electrospinningmethod is used for preparing a one-dimensional nano material, then through the processes of heat increase, heat preservation and cooling, organic matter is removed, and a cube pyrochlore phase one-dimensional nano material is prepared. The one-dimensional nanofiber has good dispersity in water and has good upconversion performance and a photo-thermal effect under irradiation of near-infrared light. The preparation method is simple, easy to implement and good in repeatability and can meet the batch production demand. The upconversion photo-thermal material base is an oxide, is good in chemicalstability, free of toxicity and low in price and is easily dispersed in water, and the demands of photo-thermal treatment and industrial production can be met. The preparation method is expected to play an important role in the field of treatment for serious 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+ ,Ho 3+ The technical field of compound one-dimensional nanomaterial preparation, specifically relates to a rare earth ytterbium holmium double-doped pyrochlore phase nanofiber preparation method and its application. Background technique

[0002] Malignant tumors have become a disease with a relatively high mortality rate in the world, seriously threatening people's health. With the advancement and development of science and technology, although there have been breakthroughs in the diagnosis and treatment of tumors, the early diagnosis techniques are low, and the treatment methods mainly include radiotherapy, chemotherapy and surgery. Its toxic side effect is big, brings great misery to patient's body and mind. Therefore, the majority of researchers are also actively exploring new means of cancer diagnosis and treatment.

[0003] Photothermal therapy is a new type of cancer treatmen...

Examples

preparation example Construction

[0033] A method for preparing rare earth ytterbium holmium double-doped pyrochlore phase nanofibers of the present invention comprises the following steps:

[0034] S1, DMF and acetic acid are mixed and stirred according to the mass ratio of 1:(0.2~0.8), to obtain solution A;

[0035] S2. In the process of continuous stirring, tetrabutyl titanate with a mass ratio of 1: (3-5) to solution A is added to solution A to obtain solution B;

[0036] S3, adding ytterbium nitrate and holmium nitrate with a mass ratio of 1: (3 to 18) in solution B to obtain solution C during continuous stirring, the mass ratio of solution B to the sum of ytterbium nitrate and holmium nitrate is (3.8 to 5.2 ):1;

[0037] S4, adding bismuth nitrate with a mass ratio of 1: (5.5 to 6.5) to solution C in the process of continuous stirring to obtain solution D;

[0038] S5. Add PVP with a mass fraction of 4-8% to the solution C and stir to prepare an electrospinning precursor solution;

[0039] S6. In the ...

Embodiment 1

[0049] DMF and acetic acid were mixed according to a mass ratio of 1:0.2, and a transparent solution was formed by magnetic stirring; then 0.9ml of tetrabutyl titanate was added and fully dissolved by stirring; 0.027g of holmium nitrate and 0.112g of ytterbium nitrate; after it is fully dissolved, add 1.018g of bismuth nitrate and fully stir to dissolve it, and finally add PVP with a mass fraction of 4%, and obtain an electrospinning precursor solution after magnetic stirring.

[0050] Under the conditions of control voltage of 15KV and flow rate of 3μl / 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 600°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ ,Ho 3+ nanomaterials.

[0051] figure 1 Given the obtained Bi 2 Ti 2 o 7 : Yb...

Embodiment 2

[0053] DMF and acetic acid were mixed according to a mass ratio of 1:0.4, and a transparent solution was formed by magnetic stirring; then 1.0ml of tetrabutyl titanate was added and fully dissolved by stirring; 0.019g of holmium nitrate and 0.12g of ytterbium nitrate; after it is fully dissolved, add 1.018g of bismuth nitrate and fully stir to dissolve it, and finally add PVP with a mass fraction of 5%, and obtain an electrospinning precursor solution after magnetic stirring.

[0054] Under the conditions of control voltage of 15KV and flow rate of 7μl / 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 650°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ ,Ho 3+ nanomaterials.

[0055] figure 2 Given that the laser with a wavelength o...

technical field

[0001] The invention belongs to rare earth ternary Bi 2 Ti 2 o 7 :Yb 3+ ,Ho 3+ The technical field of compound one-dimensional nanomaterial preparation, specifically relates to a rare earth ytterbium holmium double-doped pyrochlore phase nanofiber preparation method and its application. Background technique

[0002] Malignant tumors have become a disease with a relatively high mortality rate in the world, seriously threatening people's health. With the advancement and development of science and technology, although there have been breakthroughs in the diagnosis and treatment of tumors, the early diagnosis techniques are low, and the treatment methods mainly include radiotherapy, chemotherapy and surgery. Its toxic side effect is big, brings great misery to patient's body and mind. Therefore, the majority of researchers are also actively exploring new means of cancer diagnosis and treatment.

[0003] Photothermal therapy is a new type of cancer treatmen...

Examples

preparation example Construction

[0033] A method for preparing rare earth ytterbium holmium double-doped pyrochlore phase nanofibers of the present invention comprises the following steps:

[0034] S1, DMF and acetic acid are mixed and stirred according to the mass ratio of 1:(0.2~0.8), to obtain solution A;

[0035] S2. In the process of continuous stirring, tetrabutyl titanate with a mass ratio of 1: (3-5) to solution A is added to solution A to obtain solution B;

[0036] S3, adding ytterbium nitrate and holmium nitrate with a mass ratio of 1: (3 to 18) in solution B to obtain solution C during continuous stirring, the mass ratio of solution B to the sum of ytterbium nitrate and holmium nitrate is (3.8 to 5.2 ):1;

[0037] S4, adding bismuth nitrate with a mass ratio of 1: (5.5 to 6.5) to solution C in the process of continuous stirring to obtain solution D;

[0038] S5. Add PVP with a mass fraction of 4-8% to the solution C and stir to prepare an electrospinning precursor solution;

[0039] S6. In the ...

Embodiment 1

[0049] DMF and acetic acid were mixed according to a mass ratio of 1:0.2, and a transparent solution was formed by magnetic stirring; then 0.9ml of tetrabutyl titanate was added and fully dissolved by stirring; 0.027g of holmium nitrate and 0.112g of ytterbium nitrate; after it is fully dissolved, add 1.018g of bismuth nitrate and fully stir to dissolve it, and finally add PVP with a mass fraction of 4%, and obtain an electrospinning precursor solution after magnetic stirring.

[0050] Under the conditions of control voltage of 15KV and flow rate of 3μl / 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 600°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ ,Ho 3+ nanomaterials.

[0051] figure 1 Given the obtained Bi 2 Ti 2 o 7 : Yb...

Embodiment 2

[0053] DMF and acetic acid were mixed according to a mass ratio of 1:0.4, and a transparent solution was formed by magnetic stirring; then 1.0ml of tetrabutyl titanate was added and fully dissolved by stirring; 0.019g of holmium nitrate and 0.12g of ytterbium nitrate; after it is fully dissolved, add 1.018g of bismuth nitrate and fully stir to dissolve it, and finally add PVP with a mass fraction of 5%, and obtain an electrospinning precursor solution after magnetic stirring.

[0054] Under the conditions of control voltage of 15KV and flow rate of 7μl / 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 650°C for 2 hours, the pyrochlore phase Bi with high crystallization performance can be obtained. 2 Ti 2 o 7 : Yb 3+ ,Ho 3+ nanomaterials.

[0055] figure 2 Given that the laser with a wavelength o...

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