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Method for preparting Nano powder of zirconia

A technology of nano-zirconia and zirconium oxychloride, which is applied in the direction of zirconia, nanostructure manufacturing, nanotechnology, etc., can solve the problems of complex preparation equipment, and achieve the effects of overcoming uneven precipitation, uniform particle size, and high purity

Inactive Publication Date: 2007-02-21
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this increases the yield and shortens the preparation time, it ultimately comes at the cost of more complex preparation equipment

Method used

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  • Method for preparting Nano powder of zirconia
  • Method for preparting Nano powder of zirconia
  • Method for preparting Nano powder of zirconia

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Nano-ZrO 2 Preparation of:

[0036] First, prepare ZrOCl with a concentration of 0.2mol / L with deionized water 2 solution and ammonium tartrate at a concentration of 0.1 mol / L. In order to avoid the occurrence of uneven precipitation, strictly follow the order of addition. Measure 30ml of ZrOCl 2 solution, 60ml ammonium tartrate solution and 1ml polyethylene glycol, stir well. Add 4 times Zr 4+ Ion molar mass precipitant concentrated ammonia water (content 25-28%), stirred at room temperature for 20 minutes to obtain a transparent and clear solution. Then add 8ml hydrogen peroxide (30% content) while stirring, after a few minutes, the solution slowly becomes turbid from transparent, continue to stir for 30 minutes, stand at room temperature for 4h, and finally obtain milky white gel precipitation. Centrifuge at a speed of 4000r / min, and rinse repeatedly with deionized water until the clear liquid no longer contains chloride ions (use 0.1M AgNO 3 solution test), a...

Embodiment 2

[0047] Nano-ZrO 2 Preparation of:

[0048] The preparation method of the precursor is basically the same as in Example 1, and the precursor is placed in a muffle furnace and roasted at 400, 500 and 700°C for 2 hours respectively.

[0049] Characterization method:

[0050] Phase analysis of materials with Regaku D / max X-ray diffractometer (CuKα line)

[0051] result:

[0052] please see image 3 . image 3 , ZrO 2 XRD spectrum of ultrafine powder (400, 500 and 700℃ / 2h) image 3 It is the XRD analysis result of ultrafine powder after heat treatment at different temperatures for 2 hours. It can be seen from the figure that the main crystal phase of the powder calcined at 400°C is tetragonal zirconia, and no monoclinic phase appears. The XRD of the powder after holding at 500 and 700℃ for 2 hours showed that the monoclinic phase appeared in addition to tetragonal zirconia as the main crystal phase. Ammonia water is selected as the precipitating agent, and the zirconium hy...

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Abstract

This invention relates to a method for preparing zirconium oxide nanopowder. The method adds a masking agent before mixing the raw material solution and the precipitating agent, and the masking agent can form a stable complex with Zr4+ ions in the raw materials so that they do not react with the precipitating agent. After the solutions are mixed with evenly, the Zr4+ ions are released by adding a demasking agent, thus ensuring one-time explosive nucleation. The reaction is easily controlled by adding masking-demasking agents. The oversaturation degree is controlled within an appropriate range by controlling the addition speed and quantity of the demasking agent, so that the crystal nucleation and growth processes can be divided and high-purity nanoparticles with even distribution can be obtained. Besides, the method operates at room temperature under normal pressure, thus has such advantages as even precipitation, low cost, simple equipment and short preparation period.

Description

technical field [0001] The invention relates to a preparation method of nano zirconia powder, which belongs to the technical field of preparation of high-temperature structural materials. Background technique [0002] Zirconium dioxide is widely used and researched in high-temperature structural materials, high-temperature optical components, oxygen-sensitive components, fuel cells, etc. . In recent years, ZrO 2 The application in the field of catalysis has attracted much attention. Its surface has dual-functional properties of weak acid and weak base, which can be used as both catalyst and catalyst carrier. ZrO 2 Ultrafine particles also have the characteristics of high specific surface area and good stability. Its special surface structure and properties show good application prospects. In the preparation process, in order to make the powder have good sintering performance and microstructure, it is required to use ZrO 2 The powder components are evenly distributed, th...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82B3/00
Inventor 吴音司文捷
Owner TSINGHUA UNIV
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