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A preparation method of monodisperse rare earth doped lanthanum phosphate fluorescent quantum dots

A technology of rare earth doping and lanthanum phosphate, applied in the field of preparation of rare earth doped lanthanum phosphate fluorescent quantum dots, to achieve good fluorescence characteristics and biocompatibility

Inactive Publication Date: 2011-12-14
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the high-temperature pyrolysis method has been reported to be applied to the preparation of nanomaterials. However, the preparation of monodisperse rare earth phosphate nanocrystals with controllable particle size by the high-temperature pyrolysis method assisted by oleic acid and oleylamine composite surfactant has not been seen to report

Method used

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  • A preparation method of monodisperse rare earth doped lanthanum phosphate fluorescent quantum dots
  • A preparation method of monodisperse rare earth doped lanthanum phosphate fluorescent quantum dots
  • A preparation method of monodisperse rare earth doped lanthanum phosphate fluorescent quantum dots

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Embodiment 1

[0024] According to the process flow, 1mmol LaCl 3 Add 10ml 1-octadecene solvent, stir magnetically and add 1.8ml oleic acid and 1.8ml oleylamine, then add 1mmol Na 3 PO 4 . Then the temperature was raised to 110°C, heat treated for 1 hour, then heated to 240°C, heat treated for 3 hours, and finally cooled to room temperature naturally. Add 20ml of acetone and 20ml of ethanol to the mixture to precipitate the product, centrifuge to obtain the product, and finally dissolve it with n-hexane. The transmission electron microscope pictures of the final product are as follows: figure 2 The results show that the nanocrystals are spherical, uniform in size, good in dispersion, and the particle size is 3.5nm.

Embodiment 2

[0026] 1mmol LaCl 3 and 1 mmol Na 3 PO 4 And the corresponding amount of 0.3ml oleic acid and 0.3ml oleylamine were mixed, and vacuum treatment at 40°C for 30 minutes to remove excess water, then the mixture was added to the solution after natural cooling in Example 1, and then directly heated to 240°C, heat treatment 3 hours, and finally cooled to room temperature naturally. The post-processing is the same as the method of Example 1. TEM of the final product as image 3 The results show that the nanocrystals are spherical, uniform in size, good in dispersion, and the particle size is 5.0nm. Figure 7 It is a high-resolution transmission electron microscope picture of the product, and lattice fringes can be observed, indicating that the product crystallizes well. Figure 8 (a) XRD pattern shows that the product is a pure monoclinic phase. Figure 9 The energy spectrum of the product shows that the ratio of La atoms and P atoms is close to that of the chemical formula.

Embodiment 3

[0028] 1.5mmol LaCl 3 and 1.5 mmol Na 3 PO 4 And the corresponding amount of 0.5ml oleic acid and 0.5ml oleylamine were mixed, and vacuum treatment at 40°C for 30 minutes to remove excess water, then the mixture was added to the solution after natural cooling in Example 1, and then directly heated to 240°C, heat treatment 3 hours, and finally cooled to room temperature naturally. The post-processing is the same as the method of Example 1. TEM of the final product as Figure 4 The results show that the nanocrystals are spherical, uniform in size, good in dispersion, and the particle size is 5.8nm.

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Abstract

The invention relates to a method for preparing monodisperse rare earth-doped lanthanum phosphate fluorescent quantum dots. The method for preparing oleic acid and oleylamine as a composite surfactant to assist thermal cracking provided by the invention has the following characteristics: simple steps , short time consumption and low cost; the prepared rare earth phosphate nanocrystals have good dispersion, uniform morphology, and can be synthesized with controllable particle size. The rare earth lanthanum phosphate with good dispersion and controllable particle size and doped luminescent rare earth lanthanum phosphate nanocrystals prepared by the method can be applied in the fields of biological fluorescence detection, multicolor fluorescence detection, fluorescent labeling, tracking and the like.

Description

technical field [0001] The invention relates to a method for preparing rare earth-doped lanthanum phosphate fluorescent quantum dots with monodispersity and controllable particle size, and belongs to the technical field of inorganic materials and material preparation. Background technique [0002] Rare earth phosphates are a class of excellent luminescent materials, suitable for environments with high-density excitation and high-energy quantum excitation. For example (La, Ce, Tb)PO 4 : M (M=Eu, Y, Sr, Mg) is an excellent green and blue luminescent material, which is one of the luminescent materials with the highest luminous efficiency, and its thermal stability and vacuum ultraviolet radiation maintenance rate are better than other luminescent materials Material. With the development of high-density excitation and high-energy quantum excitation luminescent materials, the research on rare earth orthophosphate luminescent materials has attracted more and more attention. [...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/26C09K11/81C30B29/14C30B7/14
Inventor 步文博李静波施剑林
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI