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Method for preparing superfine zirconia powder

A technology of ultra-fine zirconia and zirconia powder, which is applied in the field of ceramic materials, can solve the problems of restricting production enterprises, and achieve the effect of uniform particle size and short aging time

Inactive Publication Date: 2011-05-04
LUMING SCI & TECH GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many types of dispersants, and the impracticality of ultrasonic technology relative to industrial production will restrict manufacturers

Method used

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  • Method for preparing superfine zirconia powder
  • Method for preparing superfine zirconia powder
  • Method for preparing superfine zirconia powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation method of ultrafine zirconia powder comprises the following steps:

[0025] (1) 16.27gZrOCl 2 ·8H 2 O was dissolved in 50ml of deionized water to make a 1mol / L zirconium oxychloride solution, and 100.32g of tetraethylammonium hydroxide (C8H20NOH 25%) was weighed; the two solutions were quickly stirred and mixed at a speed greater than 400 rpm Reaction, the temperature is controlled at 40°C, the pH is controlled between 11-12 by precision pH test paper, and the reaction is carried out for 10 minutes to prepare the zirconium hydroxide precursor;

[0026] (2) The precursor is filtered and washed with deionized water until the filtrate is detected to be free of Cl with silver nitrate solution - , to prepare zirconium hydroxide filter cake;

[0027] (3) Stir and disperse the obtained zirconium hydroxide filter cake in n-butanol, then heat it to 80°C under the condition of vacuum degree of 0.1 MPa, and recover the water-containing alcohol by vacuum azeotrop...

Embodiment 2

[0030] The steps of the preparation method of ultrafine zirconia powder are as described in Example 1, and the precipitating agent is adjusted to adopt 70.83g of tetramethylammonium hydroxide (25%); 16.21gZrOCl 2 ·8H 2 O was dissolved in 50ml of deionized water to make a 1mol / L zirconium oxychloride solution. The reaction temperature was controlled at 50°C; the pH was kept between 12-13, and the reaction was carried out for 15 minutes; the drying temperature was 80°C, and azeotropic distillation was carried out for 8 hours; the calcination temperature was controlled at Calcined at 600°C for 3h. Prepare ultrafine zirconia powder.

Embodiment 3

[0032] The steps of the preparation method of ultrafine zirconia powder are as described in Example 1, the concentration of zirconium oxychloride is adjusted, and 16.12gZrOCl 2 ·8H 2 O was dissolved in 62.5ml deionized water to make a 0.8mol / L zirconium oxychloride solution; the precipitation agent was tetramethylammonium hydroxide (25%), and 70.12g was weighed; the temperature was controlled at 50°C, and the pH was maintained at 12- Between 13 and 5 minutes of reaction; the alcohol used in the azeotropic distillation is n-pentanol, the drying temperature is 80°C, and the azeotropic distillation is carried out for 8 hours; calcined at 700°C for 2 hours; ultrafine zirconia powder is obtained.

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Abstract

The invention provides a method for preparing superfine zirconia powder, wherein the superfine zirconia powder is prepared by using quaternary ammonium base as a precipitator and adopting a special precipitation method. In the special precipitation method, two types of solutions are rapidly stirred and simultaneously added into a reaction kettle to react rapidly for nucleation without ageing, and the nucleuses are directly washed with water so as to achieve the purpose of controlling the growing of the nucleuses. The quaternary ammonium base is an alkaline substance which can be used for precipitating aqueous zirconia (zirconium hydroxide gel) from a zirconium salt solution, and is also a surfactant which can change interfacial tension so as to achieve a dispersion effect, therefore the addition of a dispersing agent is omitted and the cost is saved; and meanwhile, tetragonal-phase and cubic-phase zirconia powder can be prepared as required by controlling the addition of a yttrium-containing compound.

Description

technical field [0001] The invention relates to a method for preparing ultrafine zirconia powder, in particular to a method for preparing ultrafine zirconia powder by rapid precipitation using a special precipitant, which belongs to the field of ceramic materials. Background technique [0002] As a ceramic material, zirconia has excellent physical and chemical properties, such as high temperature resistance, wear resistance, corrosion resistance, its own acidity and alkalinity, redox property, and has the ability to respond to light, electricity, sound, The sensitive characteristics of gas and temperature make it widely used in high-tech fields such as electronic ceramics, functional ceramics and structural ceramics. In recent years, with the continuous development of the technology of preparing nano-zirconia, its use as a heterogeneous catalyst or adsorbent carrier has also received great attention. Zirconia mostly exists in the monoclinic phase at room temperature, and tr...

Claims

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Application Information

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IPC IPC(8): C04B35/626C04B35/48
Inventor 陈杨英邱孝鹏李明刘辉孙颖肖志国
Owner LUMING SCI & TECH GRP
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