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Method for preparing rare earth doped lanthanum fluoride luminous hollow nano powder by using multi-element solvothermal method

A technology of rare earth doping and hollow nano, which is applied in chemical instruments and methods, nanotechnology, nano optics, etc. It can solve the problems of few research and application reports and difficult preparation, and achieve uniform grain size distribution and good dispersion , the effect of high degree of crystallization

Inactive Publication Date: 2011-06-15
SHANGHAI TRANSCOM ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis of hollow structure lanthanum fluoride nanopowders with good luminescent properties is relatively difficult to prepare, and there are few reports on research and application.

Method used

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  • Method for preparing rare earth doped lanthanum fluoride luminous hollow nano powder by using multi-element solvothermal method
  • Method for preparing rare earth doped lanthanum fluoride luminous hollow nano powder by using multi-element solvothermal method
  • Method for preparing rare earth doped lanthanum fluoride luminous hollow nano powder by using multi-element solvothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Analytical balance weighs 6.19gLa 2 o 3 and 0.18gTb 4 o 7 , under strong magnetic stirring, carefully add an appropriate amount of concentrated nitric acid, keep warm at 60°C until completely dissolved, put the rare earth nitrate solution in an oven at 80°C, evaporate to dryness, add a mixture of deionized water, ethylene glycol, and oleic acid Solvent, formulated as La 3+ ,Tb 3+ Namely [Re 3+ ]=0.02mol / L solution. Under magnetic stirring, 240 ml (1.2 times excess) of ammonium fluoride solution with a concentration of 0.06 mol / L was added dropwise into the above solution, and the titration rate was controlled at 60 drops / min. After the titration is complete, add an appropriate amount of ammonia water dropwise to the prepared suspension to adjust the pH to 10. The solvothermal precursor suspension was quickly transferred to a polytetrafluoroethylene tank with a volume filling rate of 60%, and N was introduced into the polytetrafluoroethylene tank. 2 And quickly ...

Embodiment 2

[0019] Analytical balance weighs 6.19gLa 2 o 3 ,0.35gEu 2 o 3 , under strong magnetic stirring, carefully add an appropriate amount of concentrated nitric acid, keep warm at 60°C until completely dissolved, put the rare earth nitrate solution in an oven at 80°C, evaporate to dryness, add a mixture of deionized water, ethylene glycol, and oleic acid Solvent, formulated as La 3+ , Eu 3+ Namely [Re 3+ ]=0.02mol / L solution. Under magnetic stirring, 240 ml of ammonium fluoride solution with a concentration of 0.06 mol / L was added dropwise into the above solution, and the titration rate was controlled at 60 drops / min. After the titration is complete, add an appropriate amount of ammonia water dropwise to the prepared suspension to adjust the pH to 10. The solvothermal precursor suspension was quickly transferred to a polytetrafluoroethylene tank with a volume filling rate of 60%, and N was introduced into the polytetrafluoroethylene tank. 2 And quickly seal it and put it in...

Embodiment 3

[0021] Analytical balance weighs 5.86gLa 2 o 3 ,0.67gNd 2 o 3 , under strong magnetic stirring, carefully add to an appropriate amount of concentrated nitric acid, keep warm at 60°C until the oxide is completely dissolved, put the rare earth nitrate solution in an oven at 80°C and evaporate to dryness, then add deionized water, ethylene glycol, and oleic acid A mixed solvent, prepared as La 3+ ,Nd 3+ Namely [Re 3+ ]=0.02mol / L solution. Under magnetic stirring, 240 ml of ammonium fluoride solution with a concentration of 0.06 mol / L was added dropwise into the above solution, and the titration rate was controlled at 60 drops / min. After the titration is complete, add an appropriate amount of ammonia water dropwise to the prepared suspension to adjust the pH to 10. The solvothermal precursor suspension was quickly transferred to a 125ml polytetrafluoroethylene tank with a volume filling rate of 60%, and N was introduced into the polytetrafluoroethylene tank. 2 And quickly ...

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Abstract

The invention provides a method for preparing rare earth doped lanthanum fluoride luminous hollow nano powder by using a multi-element solvothermal method, belonging to the technical field of rare earth ion doped luminous nano powder preparation technology. The method is characterized by comprising the following steps: through preparing multi-element type solution of rare earth aurum nitrate, preparing a mixed polar solvent of deionized water, glycol and oleic acid at a mole ratio of 1:3:1; dissolving the rare earth oxides in nitric acid so as to obtain a nitrate mixture, wherein the rare earth oxides such as lanthana and any of teribium oxide or neodymium oxide are weighed according to the stoichiometry rate of a chemical molecular formula La(1-x)RExF3, and x is equal to 0.01-0.1; and adding the multi-element polar solvent in the nitrate mixture, and dropwise adding ammonium fluoride in the nitrate mixture, so as to obtain precursor turbid liquid, subsequently putting the precursor turbid liquid in a high pressure kettle for solvothermal treatment reaction, thus lanthanum fluoride luminous hollow nano powder is generated through a dissolution-recrystallization process of precursor rare earth fluoride. A test indicates that the powder has good fluorescent characteristic spectrum.

Description

technical field [0001] The invention relates to a method for preparing rare earth-doped lanthanum fluoride luminescent hollow nano-powder by a multi-element solvothermal method, and belongs to the technical field of rare-earth ion-doped luminescent nano-powder preparation technology. Background technique [0002] Lanthanum fluoride (LaF 3 ) is a good fast ion conductor with high ionic conductivity and ultra-high heat capacity at 1000K high temperature. It is widely used in luminescence, optoelectronics, biomarkers, catalysis and other fields. At the same time, the lower phonon energy of lanthanum fluoride (~350 cm -1 ) determines that it is an ideal host material doped with a variety of rare earth ions, which can achieve the characteristic luminescence of different ions. Since the 1960s, researchers began to pay attention to the spectral properties of rare earth-doped lanthanum fluoride crystals. In 1980, D. J. Ehrlich of the Massachusetts Institute of Technology firs...

Claims

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Application Information

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IPC IPC(8): C09K11/85B82Y20/00
Inventor 任玉英施鹰郭婧叶茂松马佳贤
Owner SHANGHAI TRANSCOM ELECTRONICS TECH
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