Method for preparing zirconium oxide micro powder

A technology of ultra-fine powder and zirconia, applied in the direction of zirconia, titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems of long heating time, inconsistent size of ultra-fine powder, energy consumption, etc., to improve efficiency and save inoculation the effect of time

Active Publication Date: 2006-06-21
河北恒博新材料科技股份有限公司
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  • Description
  • Claims
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Problems solved by technology

The consequence is that the crystallization of the particles is not perfect, and there are holes in the primary particles.
[0007] Hydrolysis method: Heating the zirconium oxychloride aqueous solution to a certain temperature to continuously volatilize hydrogen chloride. After the pH value rises to a certain level, the solution spontaneously nucleates to form a crystal core, and the prepared ultrafine powder is inconsistent in size. In addition, it is heated It takes a long time, usually takes 5-10 days, consumes a lot of energy, and the cost is high

Method used

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  • Method for preparing zirconium oxide micro powder

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Follow the steps below in order:

[0022] i) Prepare zirconium oxychloride into solution B with a concentration of 1.0M, dilute 14M ammonia water into solution A of 1.0M, and add solution A to solution B under constant stirring conditions to produce precipitation of zirconium hydroxide. Stop at PH=7.0, aging for 12 hours;

[0023] ii) Wash the precipitate fully with deionized water until no white precipitate can be detected with silver nitrate, and obtain precipitate C; dissolve zirconium oxychloride in deionized water to obtain solution D; add precipitate C to solution D, add water When the concentration of zirconium ions reaches 1.0M, heat to boiling under stirring conditions until all the precipitates are peptized;

[0024] iii) Centrifugal sedimentation to separate the unpeptized precipitate: put the sol into a closed container and settle for 1 hour on a centrifuge with a separation factor of 3600 to obtain Sol E;

[0025] iv) Heat sol E to boiling, continuously a...

Embodiment 2

[0028] Follow the steps below in order:

[0029] i) Prepare zirconium oxychloride and yttrium chloride mixed solution and prepare ammonia solution according to the following ratio: 322 grams of zirconium oxychloride and 43 grams of yttrium chloride solution that can be converted to 6.4 grams of yttrium oxide are mixed and prepared into a concentration of 1.0M For solution B, dilute 14M ammonia water into 1.0M solution A, add solution A to solution B under constant stirring conditions, and produce zirconium hydroxide precipitation, stop when pH=7.0, and age for 12 hours;

[0030] ii) Wash the precipitate fully with deionized water until no white precipitate can be detected with silver nitrate, and obtain precipitate C; dissolve 966 grams of zirconium oxychloride in deionized water to obtain solution D; add precipitate C to solution D , add water until the concentration of zirconium ions reaches 1.0M, and heat to boiling under stirring conditions until all the precipitates are p...

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Abstract

A method for preparing zirconium oxide superfine powder, characterized in that ammonia water and zirconium salt are reacted in a solution by co-precipitation, and the resulting precipitate is added to the zirconium oxychloride solution after being washed and filtered to make the precipitate produce Peptization, using the sol as the crystallization core, continuously and slowly adding zirconium oxychloride solution, heating to further hydrolyze the solution to produce precipitation, washing, calcining and grinding the hydrolyzate to prepare a uniform and uniform nano-zirconia super fine powder. The invention solves the problem of uncontrollable crystallization nucleation and growth process and uneven primary particle size in the prior art, and the prepared zirconia primary particle size is controllable, uniform, high in quality, low in preparation cost and high in efficiency. .

Description

technical field [0001] The invention relates to a method for preparing zirconia superfine powder. The powder prepared by the method has uniform particle distribution and compact structure, and is mainly used for preparing high-strength and high-density structural ceramics. Background technique [0002] Existing methods for preparing zirconia ultrafine powder include: uniform precipitation method, co-precipitation method, heating hydrolysis method, etc. [0003] Uniform precipitation method: Mix zirconium oxychloride and urea solution evenly, heat it above 70°C, urea will decompose, and the decomposition reaction equation is as follows: [0004] <chemistry num="001"> <chem file="200410064520_cml001.xml" / > < / chemistry> [0005] With the continuous decomposition of urea, the ammonia water produced will continuously increase the pH value of the solution. To a certain extent, the viscosity of the solution will suddenly increase, and precipitation will occur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02C01G23/047
Inventor 骆树立
Owner 河北恒博新材料科技股份有限公司
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