Prepn process of fluoride and nano composite fluoride particle

A nanoparticle and fluoride technology, applied in the preparation of fluoride, calcium/strontium/barium fluoride, calcium/strontium/barium halide, etc., can solve problems such as difficulty in achieving uniform distribution of nanoparticles

Inactive Publication Date: 2004-10-06
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is difficult to achieve uniform distribution of nanoparticles

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 10g of cetyltrimethylammonium bromide (CTAB) and 40g of 2-octanol to two beakers of I and II respectively, at this time CTAB:2-octanol=1:4, stir for 1 hour ;

[0012] Take 0.0015mol (0.3921g) Ba(NO 3 ) 2 and 0.003mol (0.206g) LiNO 3 , dissolved in 5.50mL water, dubbed A solution; take 0.01mol (0.3704g) NH 4 Dissolve F in 5.50mL of water to prepare B solution.

[0013] Slowly drop A solution into I beaker, slowly drop B solution into II beaker, after stirring for 2 hours, combine I and II solutions, react at room temperature (20°C) for 5min, and the water content is 10.6% (w / w) ), then centrifuged at 4000 rpm for 15 min, washed 5 times with absolute ethanol (8 mL each time), centrifuged again for 10 min, and the precipitate was dried under an infrared lamp to obtain a white powder. XRD identified it as cubic perovskite structure BaLiF3, the average particle size of the product was about 75nm calculated by Scherrer's formula and observed by scanning electron micr...

Embodiment 2

[0015] Add 10g of cetyltrimethylammonium bromide (CTAB) and 40g of 2-octanol to two beakers of I and II respectively, at this time CTAB:2-octanol=1:4, stir for 1 hour ;

[0016] Take 0.0015mol (0.3921g) Ba(NO 3 ) 2 and 0.003mol (0.206g) LiNO 3 , dissolved in 5.50mL water, dubbed A solution; take 0.01mol (0.3704g) NH 4 Dissolve F in 5.50mL of water to prepare B solution.

[0017] Slowly drop the A solution into the I beaker, slowly drop the B solution into the II beaker, after stirring for 2 hours, combine the I and II solutions, and react at room temperature (20°C) for 15 minutes, and the water content is 10.6% (w / w) ), then centrifuged at 4000 rpm for 20 min, washed 5 times with absolute ethanol (8 mL each time), centrifuged again for 10 min, and the precipitate was dried under an infrared lamp to obtain a white powder. XRD identified as cubic perovskite structure BaLiF 3 , Scherrer formula calculation and scanning electron microscope observation, the average particle s...

Embodiment 3

[0019] Add 7g of cetyltrimethylammonium bromide (CTAB) and 42g of 2-octanol to the two beakers of I and II respectively, at this time CTAB:2-octanol=1:6, stir for 1 hour ;

[0020] Take 0.0020mol (0.5228g) Ba(NO 3 ) 2 and 0.0025mol (0.1704g) LiNO 3 , dissolved in 5.50mL water, dubbed A solution; take 0.01mol (0.3704g) NH 4 Dissolve F in 5.50mL of water to prepare B solution.

[0021] Slowly drop A solution into I beaker, slowly drop B solution into II beaker, after stirring for 2 hours, combine I and II solutions, react at room temperature (20°C) for 10min, and the water content is 10.6% (w / w) ), then centrifuged at 4000 rpm for 15 min, washed 5 times with absolute ethanol (8 mL each time), centrifuged again for 5 min, and the precipitate was dried under an infrared lamp to obtain a white powder. XRD identified as cubic perovskite structure BaLiF 3 , Scherrer formula calculation and scanning electron microscope observation product average particle size of about 90nm.

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Abstract

By means of reverse micelle process, nanometer LiBaF3, BaF2, SrF2, CaF2 and BaF2:Ce particles are prepared in a cetyl trimethyl ammonium bromide-2-octanol-water microemulsion system. In the system, the ratio between cetyl trimethyl ammonium bromide and 2-octanol is 1 to 4-6, water content is 9.04-14.2 wt%. The material weight ratio between M(NO3)2 and NH4F is 1 to 1.5-2.5, where M is Ca, Sr and Ba; and that among Ba(NO3), LiNo3 and NH4F is 1 to 1-2 to 1-4. The reaction time at room temperature is 5-15 min. The process of the present invention can prepare nano particle with homogeneously distributed size smaller than 100 nm.

Description

technical field [0001] The present invention relates to the preparation method of fluoride and composite fluoride nanoparticles, in particular to nano fluoride MF 2 (M=Ca, Sr, Ba) and nanocomposite fluoride LiBaF 3 method of preparation. Background technique [0002] Transition metal or rare earth ion-doped fluoride and composite fluoride nanocomposite films, because of their advantages in structure and characteristics, will show a new prospect in the field of optical communication as laser amplification materials. The key to material preparation is the synthesis of nanoparticles. In 2000, C.M.Bender of Cornell University in the United States reported the synthesis of neodymium-doped barium fluoride BaF by the reverse micellar method on the 12th issue of "Chemistry of Materials", page 1969-1976. 2 :Nd 3+ Nanoparticle technology. In a certain doping concentration range, a nanoparticle product with a particle diameter of nearly 100nm is obtained. However, this method is ...

Claims

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Application Information

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IPC IPC(8): C01B9/08C01F11/22
Inventor 华瑞年石春山
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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