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Rare earth-doped fluoride lanthanum potassium nano fluorescent marking material and preparation method thereof

A technology of fluorescent labeling and nano-fluorescence, applied in luminescent materials, chemical instruments and methods, fluorescence/phosphorescence, etc., to achieve good application potential, simple preparation process, and easy control of synthesis conditions

Active Publication Date: 2012-09-19
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Problems solved by technology

Recently, Yan Chunhua's research group reported the synthesis of oil-soluble potassium fluoride lanthanide matrix nanocrystals, and Nagarajan's research group reported Eu 3+ and Er 3+ Synthesis of Doped Agglomerated Potassium Fluoride Lanthanide Nanocrystals (References: Yan Chunhua et al., Optically active uniform potassium and lithium rare earth fluoride nanocrystals derived from metal trifluroacetate precursors, Dalton Transactions, 8574-8581 (2009); Neetu Tyagi et al., KLaF 4 :Er 3+ an efficient upconversion phosphor, Optical Materials 33, 42-47(2010)), but there is no report on the synthesis of monodisperse water-soluble rare earth doped potassium fluoride lanthanum nanofluorescence labeling materials

Method used

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  • Rare earth-doped fluoride lanthanum potassium nano fluorescent marking material and preparation method thereof
  • Rare earth-doped fluoride lanthanum potassium nano fluorescent marking material and preparation method thereof
  • Rare earth-doped fluoride lanthanum potassium nano fluorescent marking material and preparation method thereof

Examples

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example 1

[0024] Example 1: KLaF 4 : Preparation of 0.05Ce / 0.05Tb nanocrystals, first weigh 0.1730g CF 3 COOK, 0.4788g La (CF 3 COO) 3 , 0.0266g Ce (CF 3 COO) 3 and 0.0266g Tb (CF 3 COO) 3 into a three-hole flask, and then add 8 mL of oleic acid, 10 mL of oleylamine and 2 mL of octadecene solvent. Then pass in N 2 The temperature was raised to 100 °C for 10 min under the same conditions, so that the solid reactant was dissolved until transparent, and then heated to 320 °C for 1 h. After cooling to room temperature, add 20 mL of ethanol for precipitation, centrifuge and wash to obtain oil-soluble KLaF 4: 0.05Ce / 0.05Tb nanocrystals. Disperse the nanocrystals in 20 mL of cyclohexane, add 15 mL of a dichloromethane solution in which 20 mg of nitrous tetrafluoroborate is dissolved, mix and react for 1 h, and then centrifuge to re-disperse the obtained precipitate in dimethylformamide, add 0.1 After 1 h of stirring reaction and exchange of g phosphoethanolamine, the precipitate was ...

example 2

[0025] Example 2: KLaF 4 :0.01Nd 3+ Preparation of nanocrystals, first weigh 0.1730g CF 3 COOK, 0.5267g La (CF 3 COO) 3 , 0.0054g Nd(CF 3 COO) 3 into a three-hole flask, and then add 9 mL of oleic acid, 9 mL of oleylamine and 2 mL of octadecene solvent. Then pass in N 2 The temperature was raised to 120 °C for 10 min under the same conditions, so that the solid reactant was dissolved until transparent, and then heated to 330 °C and reacted for 1.5 h. After cooling to room temperature, add 20 mL of acetone for precipitation, centrifuge and wash to obtain oil-soluble KLaF 4 :0.01Nd 3+ Nanocrystalline. Disperse the nanocrystals in 30 mL of cyclohexane, add 30 mL of a dichloromethane solution in which 30 mg of nitrous tetrafluoroborate is dissolved, mix and react for 1 h, and then centrifuge to re-disperse the obtained precipitate in dimethylformamide, add 0.2 After 1 h of stirring reaction and exchange of g phosphoethanolamine, the precipitate was obtained by centrifuga...

example 3

[0026] Example 3: KLaF 4 : Preparation of 0.02Er / 0.18Yb nanoparticles, first weigh 0.1730g CF 3 COOK, 0.4256g La (CF 3 COO) 3 , 0.0112g Er(CF 3 COO) 3 and 0.1019g Yb (CF 3 COO) 3 into a three-hole flask, and then add 10 mL of oleic acid, 8 mL of oleylamine and 2 mL of octadecene solvent. Then pass in N 2 The temperature was raised to 130 °C for 10 min under the same conditions, so that the solid reactant was dissolved until transparent, and then heated to 340 °C for 0.5 h. After cooling to room temperature, add 20 mL of acetone for precipitation, centrifuge and wash to obtain oil-soluble KLaF 4 : 0.02Er / 0.18Yb nanocrystals. Disperse the nanocrystals in 10 mL of cyclohexane, add 10 mL of a dichloromethane solution dissolved in 10 mg of nitrous tetrafluoroborate, mix and react for 0.5 h, and then centrifuge to re-disperse the obtained precipitate in dimethylformamide. After 0.05g of phosphoethanolamine was stirred and exchanged for 0.5h, the precipitate was obtained by...

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Abstract

The invention provides a rare earth-doped fluoride lanthanum potassium nano fluorescent marking material and a preparation method thereof. The preparation method comprises the following steps: firstly, carrying out high temperature cracking on in mixed solvent of oleic acid, oleyl amine and octadecylene to synthesize oil-soluble rare earth-doped fluoride lanthanum potassium nanocrystalline; and secondly, displacing the oleic acid on the surface of the nanocrystalline by using phosphate ethanol to enable the oleic acid to be converted into water-soluble nanocrystalline, wherein the size of the oil-soluble rare earth-doped fluoride lanthanum potassium nanocrystalline is about 10 nm; and the hydrated particle size of the improved water-soluble nanocrystalline is about 20 nm. The rare earth-doped fluoride lanthanum potassium nano fluorescent marking material obtained by synthesizing can be connected with a biological molecule by using an amino group on the surface of the rare earth-doped fluoride lanthanum potassium nano fluorescent marking material; and the application of the rare earth-doped fluoride lanthanum potassium nano fluorescent marking material in the fluorescent marking such as biological detection or biological imaging through rare earth ion doped light emitting can be realized.

Description

technical field [0001] The invention relates to a method for synthesizing rare earth doped inorganic nano fluorescent materials, in particular to a method for synthesizing a water-soluble surface aminated rare earth doped potassium fluoride lanthanide nano fluorescent labeling material by a two-step method. Background technique [0002] After years of development, rare earth-doped nanomaterials have made great progress in synthesis methods, spectral theory, etc., and have broad applications in green lighting sources, nano-optical devices, flat-panel displays and other fields. Only in recent years has it received much attention. Compared with quantum dots and organic fluorescent dyes, rare earth-doped nanocrystals have the advantages of narrow-band emission, long lifetime (subtle to millisecond level), high stability, and low toxicity, which make rare-earth-doped nanomaterials suitable for biological applications. prospect. In rare earth doped nanocrystals, since inorganic ...

Claims

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Application Information

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IPC IPC(8): C09K11/85G01N21/64
Inventor 陈学元刘睿涂大涛刘永升朱浩淼
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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