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A rare earth cerium ion doped rare earth pyrosilicate small-sized nanocrystal and its preparation method and application

A technology of ion doping and pyrosilicate, applied in nanotechnology, nano-optics, nanotechnology, etc., can solve the problem of uncontrollable nanocrystal shape and size, different size of nanocrystal shape, uneven doping, etc. problem, to achieve the effect of batch preparation of size, uniform shape and uniform doping

Active Publication Date: 2021-01-22
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It has been reported that the synthesis of nano-fluorescent powder doped with Eu by combustion method 3+ the Y 2 Si 2 o 7 , but the nanocrystals are unevenly doped and severely agglomerated; although the sol-gel method can also obtain nanocrystals with smaller particles, the shape and size of the nanocrystals are uncontrollable, and after high-temperature sintering, the agglomeration phenomenon is very serious; in addition , the nanocrystals can also be obtained by hydrothermal self-assembly, but the obtained nanocrystals have different shapes and sizes, are not uniformly doped, and the phase purity after sintering is not high.

Method used

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  • A rare earth cerium ion doped rare earth pyrosilicate small-sized nanocrystal and its preparation method and application
  • A rare earth cerium ion doped rare earth pyrosilicate small-sized nanocrystal and its preparation method and application
  • A rare earth cerium ion doped rare earth pyrosilicate small-sized nanocrystal and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1 prepares Lu of 30~50nm 1.999 Si 2 o 7 :0.001Ce 3+ Nanocrystalline

[0041] (1) Preparation of 10-30nm template silica (SiO2 ): Measure 10mL deionized water, 1mL absolute ethanol, 0.125mL ammonia water (NH 3 ·H 2 O), and take by weighing 1.2g hexadecyltrimethylammonium bromide (C 16 h 33 (CH 3 ) 3 NBr, CTAB) in a beaker, set the oil bath temperature to 40°C, add 0.25mL orthosilicate ethyl (Si(OC) dropwise while stirring 2 h 5 ) 4 ), reacted for 2 hours, centrifuged, washed, and dried to obtain 10-30nm template SiO 2 ;

[0042] (2) Then weigh 0.0601g of prepared template SiO 2 , 4.5006g CTAB, measure 100mL deionized water, mix in a 250mL single-necked flask, and ultrasonically disperse for 1h;

[0043] (3) Weigh 1.5004g urea (CH 4 N 2 O), measure the prepared 9.995mL 0.1M lutetium nitrate (Lu(NO 3 ) 3 ) solution, 0.025mL 0.02M cerium nitrate (Ce(NO 3 ) 3 ) solution in the above-mentioned single-necked flask, and then put the single-necked ...

Embodiment 2

[0045] Embodiment 2 prepares Lu of 30~50nm 1.9 Si 2 o 7 :0.1Ce 3+ Nanocrystalline

[0046] (1) Preparation of 10-30nm template silica: Measure 10mL of deionized water, 1mL of absolute ethanol, 0.125mL of ammonia water, and weigh 1.2g of CTAB into a beaker, set the oil bath temperature to 40°C, and stir 0.25mL Si(OC 2 h 5 ) 4 , after 2 hours of reaction, centrifuge, wash, and dry to obtain 10-30nm template SiO 2 ;

[0047] (2) Then weigh 0.0601g of prepared template SiO 2 , 4.5006g CTAB, measure 100mL deionized water, mix in a 250mL single-necked flask, and ultrasonically disperse for 1h;

[0048] (3) Weigh 1.5004g CH 4 N 2 O, measure the prepared 9.5mL 0.1M Lu(NO 3 ) 3 solution, 2.5mL 0.02MCe(NO 3 ) 3 Put the solution in the above-mentioned single-necked flask, and then place the single-necked flask in an 85°C oil bath to react for 12 hours while stirring, after precipitation, centrifugation, and washing, put it in a drying oven at 75°C to dry to obtain the prec...

Embodiment 3

[0050] Embodiment 3 prepares Lu of 30~50nm 1.99 Si 2 o 7 :0.01Ce 3+ Nanocrystalline

[0051] (1) Preparation of 10-30nm template silica: measure 10mL deionized water, 1mL absolute ethanol, 0.125mL NH 3 ·H 2 O, and weighed 1.2g CTAB in a beaker, set the oil bath temperature to 40°C, and added 0.25mL Si(OC 2 h 5 ) 4 , after 2 hours of reaction, centrifuge, wash, and dry to obtain 10-30nm template SiO 2 ;

[0052] (2) Then weigh 0.0601g of prepared template SiO 2 , 4.5006g CTAB, measure 100mL deionized water, mix in a 250mL single-necked flask, and ultrasonically disperse for 1h;

[0053] (3) Weigh 1.5004g CH 4 N 2 O, measure the prepared 9.95mL 0.1M Lu(NO 3 ) 3 solution, 0.25mL0.02M Ce(NO 3 ) 3 Put the solution in the above-mentioned single-necked flask, and then place the single-necked flask in an 85°C oil bath to react for 12 hours while stirring, after precipitation, centrifugation, and washing, put it in a drying oven at 75°C to dry to obtain the precursor po...

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Abstract

The invention discloses a rare-earth cerium ion-doped rare-earth pyrosilicate small-sized nanocrystal, a preparation method and application thereof. The chemical composition expression of described small size nanocrystal is: RE 2‑x Si 2 o 7 :x Ce 3+ , RE is a rare earth ion in Lu and Gd, and the value range of x is 0.001<x<0.1. The preparation method of the nano crystal is prepared by combining silicon dioxide as a template and a silicon source at the same time with a solution containing rare earth ions and a solution containing cerium ions in combination with a co-precipitation method. The method can control the size of the nanocrystal by controlling the size of the silicon sphere, and has the advantages of simple process, low calcining temperature, short time, controllable size of the nanocrystal, batch preparation and the like. Moreover, the obtained nanocrystalline phase has high purity, high luminous efficiency, short decay time, and can effectively absorb high-energy rays. Tumors or cancer cells have good therapeutic effects and application prospects.

Description

technical field [0001] The invention belongs to the technical field of rare earth nano-luminescent materials, and more specifically relates to a rare earth cerium ion-doped rare earth pyrosilicate small-sized nanocrystal and a preparation method and application thereof. Background technique [0002] Today, there are many ways to treat tumors or cancer cells, including physical therapy, chemotherapy and radiation therapy. Among them, photodynamic therapy is a non-destructive treatment method based on organic molecules (such as photosensitizers), so it has been favored by the medical community. However, the excitation wavelength usually used in photodynamic therapy is in the visible light range, and the penetration depth to human tissue is only about 6mm, so that photodynamic therapy can only treat tumors on the surface of the human body (such as tumors on the surface of the skin), while deep tumor cells still cannot clear. However, high-energy rays (such as X-rays or γ-rays...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/79B82Y20/00B82Y30/00B82Y40/00A61K41/00A61P35/00
CPCA61K41/0057A61P35/00B82Y20/00B82Y30/00B82Y40/00C09K11/7774
Inventor 钟玖平谢刘静
Owner SUN YAT SEN UNIV
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