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A kind of ultra-small size hexagonal phase nano-matrix material and preparation method thereof

A technology of nano-matrix and matrix material, applied in luminescent materials, nano-technology, nano-optics, etc., can solve the problem of large size of nano-materials, and achieve the effect of low luminous threshold and high luminous intensity

Active Publication Date: 2020-01-17
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a preparation method of an ultra-small size hexagonal phase nano-matrix material, aiming at improving the existing NaYbF 4 、NaLuF 4 Problems with Larger Sizes of Nanomaterials

Method used

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  • A kind of ultra-small size hexagonal phase nano-matrix material and preparation method thereof
  • A kind of ultra-small size hexagonal phase nano-matrix material and preparation method thereof
  • A kind of ultra-small size hexagonal phase nano-matrix material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] First prepare the rare earth salt, each composition and the mole percentage in the rare earth salt are 76% of rare earth lutetium chloride, 20% of rare earth ytterbium chloride, 2% of rare earth erbium chloride, and 2% of rare earth neodymium chloride. Put the rare earth salt, 15mL octadecene, and 6mL oleic acid in a 100mL three-necked flask to obtain a rare earth solution. Under the protection of argon, the rare earth solution was heated and stirred while heating. When the heating temperature reached 50°C, it was kept for 20 Minutes, then continue to heat when the temperature reaches 160 ° C for 30 minutes, then cool to room temperature to obtain the first solution.

[0044] Dissolve 2.5mmol sodium hydroxide in 8mL methanol solution to prepare a 0.31mol / L sodium source methanol solution, and dissolve 4mmol ammonium fluoride in 8mL methanol solution to prepare a 0.5mol / L ammonium fluoride methanol solution. The source methanol solution and the ammonium fluoride methanol...

Embodiment 2

[0047] First prepare the rare earth salt, each component in the rare earth salt and its mole percentage are 90% of rare earth ytterbium chloride, 1% of rare earth thulium chloride, and 9% of rare earth gadolinium chloride. 1. Place 6mL oleic acid in a 100mL three-necked flask to obtain a rare earth solution. Under the protection of argon, heat the rare earth solution and stir while heating. When the heating temperature reaches 70°C, keep it warm for 30 minutes, and then continue heating when the temperature When it reaches 160°C, keep it warm for 30 minutes and then cool to room temperature to obtain the first solution.

[0048] Dissolve 2.5mmol sodium hydroxide in 8mL methanol solution to prepare a 0.31mol / L sodium source methanol solution, and dissolve 4mmol ammonium fluoride in 8mL methanol solution to prepare a 0.5mol / L ammonium fluoride methanol solution. The source methanol solution and the ammonium fluoride methanol solution were successively added dropwise in the first...

Embodiment 3

[0051] First prepare the rare earth salt, each component in the rare earth salt and its mole percentage is 99.9% of rare earth ytterbium chloride (89.8% of rare earth ytterbium chloride is used as matrix material, 10% of rare earth ytterbium chloride is used as sensitizer) and rare earth Erbium chloride 0.1%, put the configured 1mmol rare earth salt, 18mL octadecene, and 3mL oleic acid into a 100mL three-necked flask to obtain a rare earth solution. Under the protection of argon, the rare earth solution is heated, and the Stir, keep warm for 30 minutes when the heating temperature reaches 55°C, then continue heating, keep warm for 30 minutes when the temperature reaches 160°C, then cool to room temperature to obtain the first solution.

[0052] Dissolve 2mmol sodium chloride in 6mL methanol solution to prepare a 0.33mol / L sodium source methanol solution, dissolve 6mmol ammonium fluoride in 10mL methanol solution to prepare a 0.6mol / L ammonium fluoride methanol solution, and dis...

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Abstract

The invention belongs to the technical field of upconversion luminescent nano materials, and provides a super-small-size hexagonal-phase nano matrix material and a preparation method thereof. The method comprises the following steps: respectively preparing a sodium source methanol solution and an ammonium fluoride methanol solution, sequentially adding the sodium source methanol solution and ammonium fluoride methanol solution into a rare-earth solution, and regulating the reactant mol concentration ratio and the reaction temperature and time to generate the super-small-size hexagonal-phase nano matrix material. The method is simple and easy to implement, and has high repetitiveness. The size variance ratio of nanoparticles prepared by multiple repeated experiments does not exceed 5%. The hexagonal-phase particle size of the prepared super-small-size hexagonal-phase nano matrix material can be regulated within the range of 8-20nm; and besides, the super-small-size hexagonal-phase nano matrix material has low upconversion luminescence threshold and high luminescent intensity. In addition, the heavy rare earth matrix material has high absorptive capacity for X-rays, is beneficial to developing multimode imaging, and can obtain more accurate disease information when being used for disease diagnosis.

Description

technical field [0001] The invention relates to the technical field of up-conversion luminescent nanomaterials, in particular to an ultra-small hexagonal phase nano-matrix material and a preparation method thereof. Background technique [0002] Up-conversion luminescent materials refer to materials that can absorb low-frequency photons and emit high-frequency photons. Up-conversion luminescent materials have very important application prospects in laser, communication, energy, medical, military, aerospace and people's daily life. In 2003, Chen Ruoyu of Soochow University and others proposed in Chinese patent (CN 1415693A) to prepare infrared dual-wavelength up-conversion marking materials for anti-counterfeiting marks such as bills, banknotes, and trademarks. In recent years, with the development of nanotechnology, the application of up-conversion fluorescent probes in the biological field has become a research hotspot worldwide, and a large number of scientific research an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/85C01F17/00B82Y20/00B82Y40/00
CPCB82Y20/00B82Y40/00C01F17/36C01P2002/72C01P2004/04C01P2004/64C09K11/7705
Inventor 翟雪松范柳燕王凯罗驹华贺盟杜建周张新疆
Owner YANCHENG INST OF TECH
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