Preparation method of large-specific-area stable nano zirconium oxide powder

A technology of nano zirconia and large specific surface area, which is applied in the preparation of stable nano zirconia powder and the preparation of stable nano zirconia powder with large specific surface area, which can solve the problem that sulfide ions cannot be removed, powder particle size is small, specific surface area Large and other problems, to achieve the effect of less agglomeration, control of the reaction process, and large specific surface area

Active Publication Date: 2014-06-11
陈兴生
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The powder prepared by the invention has high purity, which solves the problem that sulfur ions cannot be removed in the preparation by the sulfuric acid method, and reduces the pollution of ammonia water to the atmosphere in the conventional precipitation method; the prepared powder has a small particle size (2 / g), the particle size distribution is uniform, and there is no agglomeration (or less agglomeration)

Method used

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  • Preparation method of large-specific-area stable nano zirconium oxide powder
  • Preparation method of large-specific-area stable nano zirconium oxide powder
  • Preparation method of large-specific-area stable nano zirconium oxide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Prepare 850g of zirconium oxychloride, 116.71g of yttrium chloride, 13.31g of toughening agent aluminum chloride and 5800ml of deionized water to make an acidic solution with a concentration of 6%, heat it to 65°C under stirring conditions, completely dissolve and mix well;

[0024] 2. Prepare 630g of sodium hydroxide into a 5% alkaline solution, add the solution formulated in step 1 dropwise into the alkaline solution at a constant speed, adjust the pH value to 9.46, and make the two salts co-precipitate to obtain a solution with crystal water. Zirconia was stabilized with yttrium oxide and precipitated for 3 hours to obtain a hydrogel.

[0025] 3. Add a dispersant and an alkali removal agent to the gel prepared in step 2 for beating and filtering, and then wash the Zr(OH) with deionized water 4 AgNO for hydrogel 3 Check until no Cl is detected - . The dispersant is PEG20000, the addition amount is 0.05% of the weight of the slurry, the alkali removal agent is o...

Embodiment 2

[0028] 1. Prepare 240.63g of zirconium oxychloride, 35.74g of yttrium chloride and 4300ml of deionized water to make an acidic solution with a concentration of 6%, heat it to 65°C under stirring conditions, completely dissolve and mix thoroughly;

[0029] 2. Prepare 697g of potassium hydroxide into a 13% alkaline solution, add the prepared acidic solution dropwise into the alkaline solution at a constant speed, adjust the pH value to 9.42, and cause the two salts to co-precipitate to obtain an oxidation solution with crystal water. Yttrium-stabilized zirconia was precipitated for 3 hours to obtain a hydrogel.

[0030] 3. Add a dispersant and an alkali-removing agent to the hydrogel prepared in step 2 for beating and filtering, and then wash the Zr(OH) with deionized water 4 AgNO for hydrogel 3 Check until no Cl is detected -. The dispersant is PEG4000, and the addition amount is 0.03% of the weight of the slurry, and the alkali removal agent is oxalic acid, and the addition...

Embodiment 3

[0033] 1. Prepare 1000g of zirconium oxychloride, 250g of yttrium nitrate and 7400ml of deionized water to make an acidic solution with a concentration of 6%, heat it to 70°C under stirring conditions, completely dissolve and mix thoroughly;

[0034] 2. Prepare 804g of sodium hydroxide into an alkaline solution, add the prepared acidic solution dropwise to the alkaline solution at a constant speed, adjust the pH value to 9.53, and make the two salts co-precipitate to obtain a stable yttrium oxide with crystal water. Zirconia, precipitation for 4h, to obtain a gel.

[0035] 3. Add a dispersant and an alkali-removing agent to the hydrogel for beating and filtration. The dispersant is PEG2000, and the amount added is 3% of the weight of the slurry; the alkali-removing agent is citric acid, and the amount added is 4% of the weight of the slurry;

[0036] 4. Add isoamyl alcohol to the filtered filter cake and stir for 30 minutes. The volume ratio of filter cake to alcohol is 1:3. ...

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Abstract

The invention relates to a preparation method of large-specific-area stable nano zirconium oxide powder, which is characterized by comprising the following steps: (1) preparing zirconium salt raw material, stabilizer and toughener into a zirconium salt solution, dropwisely adding the zirconium salt solution into an alkali solution together with dispersing agent to carry out gelatination, thereby obtaining a zirconium hydroxide hydrogel; and (2) adding dispersing agent and alkali remover, pulping, filtering, washing, carrying out azeotropic distillation, drying and calcining to obtain stable nano zirconium oxide powder. Water molecules in the gel are removed by azeotropic distillation in an azeotropic mode, so that the OH- group between the surfaces on adjacent particles is substituted by the Zr-O-Zr chemical bond, so that no hard aggregation is formed in the subsequent drying and calcining process. Since common chloride ions and sulfur ions in the liquid-phase method do not exist in the reaction product, the product is easy to clean, and has the advantages of loose powder, less aggregation, high reaction activity, large specific area and high heat stability.

Description

technical field [0001] The present invention relates to a method for preparing stable nano zirconia powder, more precisely relates to a method for preparing stable nano zirconia powder with large specific surface area, which belongs to ZrO 2 powder field. Background technique [0002] As we all know, zirconia is an inorganic non-metallic material with high melting point, high boiling point, small thermal conductivity, large thermal expansion coefficient, good wear resistance and excellent corrosion resistance. Nano zirconia powder and its prepared ceramics have been used in solid electrolyte fuel cells, ceramic internal combustion engines, semiconductor oxygen sensitive components, optical fiber ceramic connectors, catalyst carriers, lubricating oil additives, thermal barrier coating materials, bioceramics, etc. The progress of these applications puts forward various new requirements for nano zirconia powder. Since nano-zirconia ceramics and coatings are solidified by nano...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C01G25/02B82Y30/00
Inventor王云生陶冶
Owner陈兴生