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Method for synthesizing rare-earth oxide sulfate nano-grain by high-molecular gel network template

A technology of rare earth sulfur oxide and polymer gel, which is applied in the field of material science, can solve the problems of high cost and complicated process of microemulsion, and achieve the effect of low cost, high phase purity and good dispersion

Inactive Publication Date: 2009-03-11
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of this method is more complicated, and the cost of microemulsion is higher

Method used

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  • Method for synthesizing rare-earth oxide sulfate nano-grain by high-molecular gel network template
  • Method for synthesizing rare-earth oxide sulfate nano-grain by high-molecular gel network template
  • Method for synthesizing rare-earth oxide sulfate nano-grain by high-molecular gel network template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 0.2M La(NO 3 ) 3 and Tb(NO 3 ) 3 The solution is mixed according to the molar ratio La:Tb=95:5, and 0.5M ammonium sulfate [(La+Tb):SO is added 4 2- =2:1 molar ratio)] and polymer reticulating agent (gelatin 15wt%) were vigorously stirred and mixed evenly, and a translucent sol was formed at 80°C. The sol was allowed to stand at room temperature, and then placed in a refrigerator at 4°C to form a gel. Cut the gel into 1cm cubes, soak in 4mol / l ammonia water, wash with cold water after 24 hours, and dry under vacuum at 110°C for 3 hours. Heating the dry gel at 500°C in air in a tube furnace and keeping it warm for 2 hours, and then reducing it in a hydrogen atmosphere at 650, 700, 750 and 800°C for 1 hour to obtain rare earth sulfur oxide nanoparticles. Gained nanoparticle is carried out test and analysis result is as follows:

[0035] Xerogel TG-DTA curve figure 2 It can be seen that gelatin has a high decomposition temperature (482°C) and a narrow temperature r...

Embodiment 2

[0045] 0.3M La(NO 3 ) 3 and Pr(NO 3 ) 3 The solution is mixed according to the molar ratio La:Pr=98:2, and 1.0M ammonium sulfate [(La+Pr):SO is added 4 2- =2:1 molar ratio)] and the polymer network agent (gelatin 10wt%) were vigorously stirred and mixed evenly, and a translucent sol was formed at 85°C. The sol was allowed to stand at room temperature, and then placed in a refrigerator at 4°C to form a gel. Cut the gel into 2cm cubes, soak in 8mol / l ammonia water, wash with cold water after 24 hours, and dry in vacuum at 110°C for 4 hours. Heating the dry gel at 500°C in air in a tube furnace and keeping it warm for 2 hours, and then reducing it in a hydrogen atmosphere at 750°C for 1 hour to obtain La 2 o 2 S:2mol%Pr 3+ nanoparticles, spectra such as Figure 7 .

Embodiment 3

[0047] 0.2M La(NO 3 ) 3 and Eu(NO 3 ) 3 The solution is mixed according to the molar ratio La:Eu=98:2, and 1.0M ammonium sulfate [(La+Pr):SO is added 4 2- =2:1 molar ratio)] and the polymer network agent (gelatin 15wt%) were vigorously stirred and mixed evenly, and a translucent sol was formed at 70°C. The sol was allowed to stand at room temperature, and then placed in a refrigerator at 4°C to form a gel. Cut the gel into 1cm cubes, soak in 8mol / l ammonia water, wash with cold water after 24 hours, and dry in vacuum at 110°C for 4 hours. Heat the dry gel at 500°C in air in a tube furnace and keep it warm for 2 hours, then hydrogen + nitrogen at 750°C (volume ratio H 2 :N 2 =2:1) ​​Reduction in atmosphere for 1 hour to get La 2 o 2 S:2mol%Eu 3+ nanoparticles, spectra such as Figure 8 .

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Abstract

A method for synthesizing rare-earth sulfur oxide nano-grain by polymer gel grid template is carried out by taking rare-earth nitrate as raw material, taking sulfate as vulcanizing agent, taking polymer grid as template, preparing mixed solution of rare-earth nitrate and sulfate, adding polymer grid agent into mixed solution, heating while agitating to form into semi-transparent sol, laying aside to room temperature, putting it into refrigerator to form into gel at 0-8 degree, cutting into small pieces, immersing it into ammonia water for 24 hrs, washing by cold water, vacuum drying at 110 degree, putting dry gel into tube furnace, heating, keeping temperature to obtain solid powder, and reducing in tube hydrogen furnace for 1-2 hrs to obtain final product. It's cheap, has better purity and dispersion, it can control precursor size and appearance and have low synthetic temperature.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to a method for synthesizing rare earth sulfur oxide nanoparticles with a polymer gel grid template. Background technique [0002] Rare earth sulfur oxides (Re 2 o 2 S, Re=Y, La and Gd) crystals are hexagonal, and the space group is (P-3ml). Re 2 o 2 S has a wide band gap (4.6-4.8eV), and has very high light absorption and energy transmission efficiency as a luminous matrix, and is an important class of optical functional materials. Re 2 o 2 Various rare earth doped sulfur oxides (Re 2 o 2 S:Ln) high-performance luminescent materials have been widely used in color TV picture tubes, flat panel imaging [including electroluminescence (EL), field emission (FED) and plasma imaging (PDP)] and other fields. It was recently reported that Re 2 o 2 S:Ln will be used in ultraviolet excitation light-emitting diodes, which can solve the problem of poor color repro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 孙旭东刘志刚连景宝李晓东修稚萌霍地李强
Owner NORTHEASTERN UNIV LIAONING
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