Preparation of upper conversion fluorescent nano particle

A technology of fluorescent nanoparticles and acid salts, which is applied in the field of materials, can solve the problems of increased particle size of nanoparticles and unfavorable biomolecular labeling applications, and achieve the effects of controllable crystal form, less demanding synthesis conditions, and high yield

Inactive Publication Date: 2009-08-05
NORTHEASTERN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, obtaining nanoparticles with high luminous intensity requires more severe solvothermal conditions (for example: higher reaction temperature and longer reaction time), and under these conditions, it is easy to cause the anisotropic growth of nanoparticles to form nanorods or Nanowires, which increase the particle size of nanoparticles, which is not conducive to biomolecular labeling applications

Method used

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  • Preparation of upper conversion fluorescent nano particle
  • Preparation of upper conversion fluorescent nano particle
  • Preparation of upper conversion fluorescent nano particle

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Weigh 1.1291g (5mmol) of yttrium oxide, add concentrated nitric acid solution to it and heat to dissolve the yttrium oxide, and volatilize the remaining concentrated nitric acid to obtain rare earth nitrate powder. Dissolve the powder with 20 mL of ethanol to obtain an ethanol solution of yttrium nitrate.

[0046] Yttrium nitrate ethanol solution, 8.5344g (30mmol) stearic acid and 40mL ethanol are placed in a three-necked flask, reflux reaction under stirring conditions, the reaction temperature is 78 ° C, and the stirring speed is 300rpm, and the reaction is until the stearic acid is completely dissolved. Sodium hydroxide solution was slowly added dropwise to the reaction mixture until the pH of the reaction system rose to 7, and the stirring and reflux reaction was continued for 40 min. The reacted material was filtered under reduced pressure and washed twice with water, and dried to remove water to obtain the yttrium precursor.

[0047] Weigh 1.9704g (5mmol) of ytte...

Embodiment 2

[0052] The preparation method of yttrium precursor is with embodiment 1; The preparation method of ytterbium precursor is with embodiment 1; After the fatty acid was dissolved, sodium hydroxide was added to control the pH value of the solution to 6, and the reflux stirring was continued for 30 min.

[0053] Add 0.2100g (5mmol) sodium fluoride and 4mL oleic acid (surfactant), 0.78mmol yttrium-containing precursor, 0.20mmol ytterbium-containing precursor, 0.02mmol erbium-containing precursor in the mixed solvent of 10mL water and 15mL ethanol, Stir under ultrasonic conditions to form a homogeneous mixture without massive solids; the frequency of ultrasonic waves is 40-100kHz.

[0054] Transfer 4 batches of the mixture prepared by the above method to a hydrothermal synthesis reactor, set the reaction temperature at 100°C, 150°C and 200°C respectively, and react at constant temperature for 8h and 24h under closed conditions. Each batch of materials after the reaction finishes pre...

Embodiment 3

[0061] Palmitic acid was used instead of stearic acid in an amount of 7.6929 g (3.0 mmol); the yttrium precursor, the ytterbium precursor and the erbium precursor were prepared according to the method described in Example 1. And prepare NaY by the method described in Example 1 0.78 f 4 :Yb 0.20 , Er 0.02 Nanoparticles, the difference is that the reaction temperature in water and the reactor is 200°C, and the reaction time is 24h, to obtain NaY 0.78 f 4 :Yb 0.20 , Er 0.02 Up-conversion fluorescent nanoparticle 6# product.

[0062] Myristic acid was used instead of stearic acid in an amount of 6.8514 g (30 mmol); the method described in Example 1 was used to prepare yttrium precursor, ytterbium precursor and erbium precursor. And prepare NaY by the method described in Example 1 0.78 f 4 :Yb 0.20 , Er 0.02 Nanoparticles, the difference is that the reaction temperature in water and the reactor is 100°C, and the reaction time is 24h, to obtain NaY 0.78 f 4 :Yb 0.20 , ...

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Abstract

A preparation method of up-conversion phosphor nanometer particles belongs to the technical field of materials and comprises the following steps: (1) dissolving rare-earth inorganic acid salt powder by ethanol to obtain rare-earth inorganic acid salt ethanol solution; (2) adding long-chain fatty acid, performing the reflux reaction under the mixing condition, and preparing a long-chain fatty acid precursor of rare-earth; (3) adding one of an erbium precursor, a thulium precursor and a holmium precursor as well as a yttrium precursor and a ytterbium precursor into a water-ethanol mixing system, adding and uniformly mixing sodium fluoride and surface active agent, and heating and reacting for 2-24h under the obturating condition; (4) adding organic solvent after lowering the temperature, centrifugalizing, and drying or naturally withering after washing white precipitate. The preparation method has simpler process, easy synthesis condition, good repetitiveness, low cost and higher productive rate.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a preparation method of up-conversion fluorescent nanoparticles. Background technique [0002] Up-conversion fluorescent materials are a class of materials that can emit short-wavelength light when excited by long-wavelength light. Due to its unique luminescent properties, this material has important applications in solid-state lasers, sensors, solar cells, three-dimensional presentations and other fields. In recent years, the use of nanoscale upconversion fluorescent materials as fluorescent labeling probes for biomolecules has received extensive attention. At present, there have been related reports on the quantitative detection of DNA and biotin molecules by using up-conversion fluorescent nanoparticles. Compared with traditional fluorescent markers (such as organic dyes and quantum dots), upconversion fluorescent materials have the advantages of low toxicity, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/85
Inventor 王猛徐淑坤张祎昕侯微巫显龙刘金玲密丛丛
Owner NORTHEASTERN UNIV
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