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Method for preparing powder of zirconium oxide in high purity

A nano-zirconia and zirconium oxychloride technology, applied in zirconia, nanostructure manufacturing, nanotechnology and other directions, can solve the problems of affecting the purity of nano-zirconia, cumbersome cleaning steps, complicated preparation process, etc. The effect of high quality and simple preparation process

Inactive Publication Date: 2009-06-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantages of these methods are: (1) complex equipment, complicated preparation process, long time consumption, high energy consumption and high cost; (2) using ammonia as precipitant, or introducing other complex organic reagents such as urea etc. in the process (Chinese patent CN151902), can cause ammonia pollution in the preparation process; (3) the strong alkali cation (Na + , K + ) (Chinese patent CN116875) is difficult to clean, making the cleaning steps cumbersome and may affect the purity of nano-zirconia

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] ●With a concentration of 0.75mol / L ZrOCl 2 ·8H 2 The O solution is used as the mother liquor, the pH is adjusted to about 4 with HCl, and 1% PEG8000 is added as a surfactant;

[0029] ●Reconstitute H with a concentration of 0.4mol / L 2 C 2 O 4 ·2H 2 O solution, slowly with ZrOCl in the process of constant stirring 2 ·8H 2 The amount of O and other substances in H 2 C 2 O 4 ·2H 2 The O solution is dropped into the mother liquor to obtain a transparent sol;

[0030] ●Stirring and aging for 0.5 hours, continue to add dropwise ZrOCl in the above mother liquor 2 ·8H 2 The above-mentioned H with an O mole content of 3% to 5% 2 C 2 O 4 ·2H 2 O, gradually transform the sol into a transparent gel, and then coagulate into a milky white opaque suspension;

[0031] ●Centrifugation to get precipitated ZrOC 2 O 4 ·2H 2 O, wash with deionized water for 3 times, ultrasonically disperse in anhydrous ethanol, dry in a mortar on an electric furnace at 200°C, and continuously grind the precipit...

Embodiment 2

[0035]With reference to the preparation steps of Example 1, the difference is: the concentration of the mother liquor of zirconium oxychloride is 0.5 mol / L, the concentration of oxalic acid is 0.4 mol / L, and the concentration of excessive oxalic acid is 5%, which is obvious during the drying process of the electric furnace. Agglomeration phenomenon, after burning, the average particle size is about 0.2 microns calculated.

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Abstract

This invention discloses a method for preparing high-purity ZrO2 nanopowder. The method utilizes ZrOCl2.8H2O as the precipitant, and adopts sol-gel method to prepare high-purity ZrO2 nanopowder. The method has such advantages as simple apparatus and process, low energy consumption, and high efficiency. The product purity is higher than 99.9%, and the particle sizes are distributed within 10-30 nm.

Description

Technical field [0001] The invention relates to a preparation method of high-purity nano-zirconia material, in particular to the preparation of high-purity nano-zirconia by sol-gel method using zirconium oxychloride as a raw material. Background technique [0002] Zirconia has excellent physical and chemical stability, and has the characteristics of a solid electrolyte at high temperatures. At the same time, due to the particularity of its molecular structure, it has a certain catalytic effect. Therefore, it is used in material modification, sensitive element modification, sensor preparation, and Fuel cells have a wide range of uses. The zirconia micropowder has the characteristics of high specific surface area and good stability, which makes it show good application prospects. At present, the preparation methods of nano-zirconia mainly include gas-phase method and liquid-phase method. The gas-phase method uses zirconium chloride or zirconium alkoxide as raw materials and undergo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82B3/00
Inventor 王敏李竹赟
Owner ZHEJIANG UNIV
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