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Preparation method of zirconium oxide nanometer powder

A technology of nano-powder and zirconia, applied in the direction of zirconia, which can solve the problems of low activity, pollution of the environment, and impurities in products, and achieve the effect of easy conditions, high activity, and uniform particle size

Inactive Publication Date: 2014-02-12
SHENYANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 3. The use of organic reagents will pollute the environment and cause impurities to remain in the product
[0006] 4. The prepared powder is crystal particles with low activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A preparation method of zirconia nanopowder is:

[0019] 1. Put 100 grams of solid zirconium oxychloride into a container, add 1000 milliliters of deionized water, and stir for about 5 minutes until completely dissolved to obtain a zirconium oxychloride solution.

[0020] 2. Place the container holding the zirconium oxychloride solution in a refrigerator to freeze into a frozen product of the zirconium oxychloride solution.

[0021] 3. Turn on the lyophilizer, and place the above-mentioned frozen material in the freeze-drying box of the lyophilizer. The shelf temperature in the freeze-drying box is kept at -5°C, and the vacuum pump is turned on, and the cold trap and the freeze-drying box of the freeze-drying machine are vacuumed to 10-30 Pa, so that all the water molecules in the frozen material are sublimated. Raise the temperature of the shelf to 90°C and continue to vacuumize, so that all the water molecules combined in the zirconium oxychloride are resolved and vo...

Embodiment 2

[0024] A preparation method of zirconia nanopowder is:

[0025] 1. Put 10 kg of ammonium zirconium carbonate into a container, add 50 liters of deionized water, and stir for about 10 minutes until completely dissolved to obtain an ammonium zirconium carbonate solution.

[0026] 2. Put the container containing the ammonium zirconium carbonate solution on the shelf in the freeze drying box of the freeze dryer, turn on the freeze dryer, cool the shelf to -10°C, and completely freeze the ammonium zirconium carbonate solution into a freezer. things.

[0027] 3. Keep the above-mentioned frozen matter in the freeze-drying box of the freeze-drying machine, and evacuate the cold trap and the freeze-drying box of the freeze-drying machine to 10-30 Pa, so that all the water molecules in the frozen thing are sublimated. Raise the temperature of the shelf to 20°C and continue to vacuumize, so that all the water molecules bound in the ammonium zirconium carbonate are resolved and volatiliz...

Embodiment 3

[0030] A preparation method of zirconia nanopowder is:

[0031] 1. Put 0.5 kg of zirconium acetate into a container, add 2 liters of deionized water, and stir for about 10 minutes until completely dissolved to obtain a zirconium acetate solution.

[0032] 2. Put the container containing the zirconium acetate solution on the shelf in the freeze-drying box of the freeze-drying machine, turn on the freeze-drying machine, cool the cold trap of the freeze-drying machine to -40°C, and set the temperature for the freeze-drying box and the freezer. Vacuum the trap to freeze the zirconium acetate solution into a frozen substance by vacuum evaporation.

[0033] 3. Keep the above-mentioned frozen matter in the freeze-drying box of the freeze-drying machine, and continue to vacuumize the cold trap and the freeze-drying box of the freeze-drying machine to 10-20 Pa, so that all the water molecules in the frozen thing are sublimated. Raise the shelf temperature of the lyophilizer to 20°C an...

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PUM

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Abstract

The invention discloses a preparation method of zirconium oxide nanometer powder, which is characterized by comprising the following steps of 1, preparing a precursor solution; 2, freezing the precursor solution into a congelation; 3, refrigerating the congelation and drying in vaccum; and 4, calcining precursor powder in vacuum so that the precursor powder is decomposed and converted into zirconium oxide nanometer powder. The process is simple in course and convenient to operate, reaction conditions are easy to control and realize, and the zirconium oxide nanometer powder can be industrially produced. A precursor is prepared in a water solution, any organic solvent is not used, an environment is not polluted, and the prepared zirconium oxide nanometer powder is pure in chemical components, uniform in grain diameter, free of hard agglomerate and high in activity and is amorphous nanometer powder.

Description

technical field [0001] The invention relates to the technical field of preparation of nanometer powder materials, in particular to a method for preparing zirconia nanometer powder materials by adopting freeze vacuum drying technology. Background technique [0002] Due to the special physical and chemical properties of zirconia nanopowders, zirconia nanopowders have broad application prospects in functional ceramics, new catalysts, sensors, lubricants, fuel cells, etc. Therefore, the method for preparing zirconia nanopowder has become the focus of people's research. At present, chemical liquid phase methods are mainly used to prepare zirconia nanopowder, such as precipitation method, microemulsion method, gel method, hydrolysis method and so on. These methods are generally in the liquid phase, by controlling the chemical reaction conditions, including temperature, pressure, stirring speed, pH value range, the speed of adding chemical reagents and the order of dropping, etc.,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02
Inventor 刘军彭润玲李洪仁
Owner SHENYANG UNIV
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