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Rare earth oxyfluoride nanomaterial and its preparation method and application

A technology of oxyfluoride and nanomaterials, applied in the field of rare earth oxyfluoride nanomaterials and its preparation, can solve the problems of heterogeneous phases, narrow variable range, and easy occurrence of fluoride, etc., and the conditions are easy to control, uniform and repeatable Good performance and good repeatability

Active Publication Date: 2018-02-02
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method needs to control the fluorination and fluorine oxidation process of rare earth ions by finely adjusting the solvent ratio and reaction temperature, that is, the variable range of the reaction conditions is very narrow, and the fluoride heterophase is easy to appear in the synthetic product.
[0005] In addition, the previous research involving rare earth oxyfluoride materials mainly focused on the study of luminescence properties, and new application fields have yet to be developed.

Method used

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  • Rare earth oxyfluoride nanomaterial and its preparation method and application
  • Rare earth oxyfluoride nanomaterial and its preparation method and application
  • Rare earth oxyfluoride nanomaterial and its preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Preparation of Rare Earth Oxyfluoride Nanomaterials by High Temperature Solvothermal Decomposition Using Rare Earth Trifluoroacetate and Ammonium Acetate as Precursors:

[0063] (1) Preparation of oil-soluble LaOF: 5% Eu nanocrystals

[0064] Weigh 0.5054 g of lanthanum trifluoroacetate, 0.0273 g of europium trifluoroacetate, and 0.1156 g of ammonium acetate into a three-hole flask at room temperature, and add 5 mL of oleic acid, 9 mL of oleylamine and 2 mL of octadecene as solvents. Heated under an inert atmosphere until the above-mentioned trifluoroacetate and ammonium acetate were dissolved, then continued to heat up to 310°C, reacted for 2 hours, cooled naturally to room temperature, precipitated and washed to obtain oil-soluble LaOF:5%Eu nanocrystals.

[0065] From figure 1 In a), it can be seen that the oil-soluble nanocrystal has good crystallinity, and its diffraction peak position and relative intensity are consistent with the PDF standard card of LaOF (JCPDS ...

Embodiment 2

[0094] Based on dissolution-enhanced time-resolved fluorescent immunoassay method, using Lu 6 o 5 f 8 :Eu Nanoprobes for Prostate Specific Antigen Detection

[0095] 1) Preparation of oil-soluble Lu 6 o 5 f 8 :40% Eu Nanocrystalline

[0096] Weigh 0.3408g lutetium trifluoroacetate, 0.2180g europium trifluoroacetate, and 0.0812g ammonium acetate into a three-hole flask at room temperature, add 5mL oleic acid and 9mL oleylamine as solvents; After dissolving with ammonium acetate, continue to heat up to 320°C, react for 2 hours, cool to room temperature naturally, precipitate and wash to obtain oil-soluble Lu 6 o 5 f 8 : 40% Eu nanocrystals.

[0097] Among them, the oil-soluble Lu 6 o 5 f 8 : The powder diffraction pattern and transmission electron microscope image of 40% Eu nanocrystals are shown in Figure 6 a) and Figure 6 b) as shown.

[0098] 2) Preparation of water-soluble Lu 6 o 5 f 8 :40% Eu Nanocrystalline

[0099] Weigh 30 mg of the oil-soluble Lu pr...

Embodiment 3

[0114] Lu 6 o 5 f 8 : Application performance test of Yb / Er nanocrystals

[0115] (1) Preparation of oil-soluble Lu 6 o 5 f 8 :20%Yb / 2%Er nanocrystalline

[0116] Weigh 0.4431g of lutetium trifluoroacetate, 0.1132g of ytterbium trifluoroacetate, 0.0112g of erbium trifluoroacetate, and 0.0812g of ammonium acetate into a three-hole flask at room temperature, add 5mL of oleic acid and 9mL of oleylamine as solvents; heat to After dissolving the above trifluoroacetic acid salt and ammonium acetate, continue to heat up to 320°C, react for 2 hours, cool to room temperature naturally, precipitate and wash to obtain oil-soluble Lu 6 o 5 f 8 : 20%Yb / 2%Er nanocrystals.

[0117] Figure 8 a) and 8b) for Lu 6 o 5 f 8 : Powder diffraction pattern and transmission electron microscope pattern of 20%Yb / 2%Er nanocrystals.

[0118] Such as Figure 9 As shown, under the excitation of 980nm near-infrared light, the material exhibits typical green (520-570nm) and red (640-670nm) up-c...

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Abstract

The invention relates to a rare-earth oxyfiuoride nanometer material, and a preparation method and application thereof. According to the method, rare-earth trifluoroacetic acid salts and ammonium acetate are used as precursors; in addition, a high-temperature solvent thermolysis method is used, so that the oil-soluble rare-earth oxyfiuoride nanometer material is obtained. The synthesis conditions are easy to control; the repeatability is good; the prepared nanometer material is in a particle shape; the dispersibility, the uniformity and the repeatability of the particle are good. The prepared rare-earth oxyfiuoride nanometer material is an ideal substrate material capable of being applied to the field of biological detection and biological imaging.

Description

technical field [0001] The invention belongs to the technical field of nano-biological materials, and in particular relates to a rare-earth oxyfluoride nano-material and its preparation method and application. Background technique [0002] In recent years, rare earth-doped inorganic luminescent materials have received widespread attention. These materials have shown great application value in three-dimensional display, anti-counterfeiting technology, solid-state lasers, optical storage, solar cells, etc., the most notable of which is the recent rise of Application of rare earth doped inorganic nanomaterials in fluorescent biomarkers. Compared with traditional fluorescent labeling materials (such as fluorescent dyes and quantum dots), rare earth-doped inorganic nanomaterials have comprehensive advantages such as high thermal stability, long fluorescence lifetime, low toxicity, and tunable fluorescence emission wavelength. A generation of fluorescent biomarkers. [0003] Flu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/86C01F17/00B82Y30/00
CPCB82Y30/00C01F17/00C01P2002/72C01P2004/03C01P2004/04C01P2004/61C01P2006/60C09K11/7728C09K11/777C09K11/7788
Inventor 陈学元徐金涂大涛郑伟卢珊
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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