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Aluminum-containing zirconia hollow microspheres and preparation method thereof

A technology of hollow microspheres and zirconia, which is applied in the direction of zirconia, can solve the problems of limited use and poor high temperature resistance of zirconia hollow microspheres, and achieve the effects of low temperature resistance, good dispersion and low raw material cost

Active Publication Date: 2020-07-14
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The heat insulation materials prepared by these two processes have good heat insulation performance, but because the zirconia hollow microspheres used have poor high temperature resistance, usually lower than 1200°C, which limits their use in higher temperature environments

Method used

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  • Aluminum-containing zirconia hollow microspheres and preparation method thereof
  • Aluminum-containing zirconia hollow microspheres and preparation method thereof
  • Aluminum-containing zirconia hollow microspheres and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The preparation method of aluminum-containing zirconia hollow microspheres is as follows:

[0024] Add 0.008mol of aluminum nitrate, 0.016mol of zirconium oxychloride, and 0.032mol of urea into 200ml of absolute ethanol, and slowly add 50ml of concentrated hydrochloric acid (concentration of hydrogen ions in concentrated hydrochloric acid is 12mol / L) during the stirring process. Stir magnetically in a water bath until a clear solution is obtained. The prepared clear solution was poured into a stainless steel reactor lined with polytetrafluoroethylene, sealed and heated in an oven at 160°C for 12h. After the reaction was completed and naturally cooled, the precipitate produced by the reaction was filtered out, washed three times with absolute ethanol, and placed in an oven at 60° C. for 24 hours until completely dried. The powder obtained after drying was calcined at 1000° C. for 2 hours to obtain aluminum-containing zirconia hollow microspheres, and a part of the alumi...

Embodiment 2

[0026] The preparation method of aluminum-containing zirconia hollow microspheres is as follows:

[0027] Add 0.004mol of aluminum nitrate, 0.016mol of zirconium oxychloride, and 0.032mol of urea into 200ml of absolute ethanol, and slowly add 50ml of concentrated hydrochloric acid (concentration of hydrogen ions in concentrated hydrochloric acid is 12mol / L) during the stirring process. Stir magnetically in a water bath until a clear solution is obtained. The prepared clear solution was poured into a stainless steel reactor lined with polytetrafluoroethylene, sealed and heated in an oven at 160°C for 12h. After the reaction is completed and cooled naturally, the precipitate produced by the reaction is filtered out, washed three times with absolute ethanol, and placed in an oven at 60°C for 24 hours to completely dry; the powder obtained after drying is calcined at 1000°C for 2 hours to obtain an aluminum-containing Zirconia hollow microspheres, and a part of aluminum-containin...

Embodiment 3

[0029] The preparation method of aluminum-containing zirconia hollow microspheres is as follows:

[0030] Add 0.002mol of aluminum nitrate, 0.016mol of zirconium oxychloride, and 0.032mol of urea into 200ml of absolute ethanol, and slowly add 50ml of concentrated hydrochloric acid (the concentration of hydrogen ions in the concentrated hydrochloric acid is 12mol / L) during the stirring process. Stir magnetically in a water bath until a clear solution is obtained. The prepared clear solution was poured into a stainless steel reactor lined with polytetrafluoroethylene, sealed and heated in an oven at 160°C for 12h. After the reaction is completed and cooled naturally, the precipitate produced by the reaction is filtered out, washed three times with absolute ethanol, and placed in an oven at 60°C for 24 hours to completely dry; the powder obtained after drying is calcined at 1000°C for 2 hours to obtain an aluminum-containing Zirconia hollow microspheres, and a part of aluminum-c...

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Abstract

The invention discloses an aluminum-containing zirconia hollow microsphere. The aluminum-containing zirconia hollow microsphere comprises an aluminum element and a zirconium element in a molar ratio of (1-4):8, and the diameter of the aluminum-containing zirconia hollow microsphere is 0.1 to 10 mu m. The invention also discloses a method for preparing the aluminum-containing zirconia hollow microsphere, comprising the following steps: uniformly mixing an aluminum precursor, a zirconium precursor, urea and strong acid in ethanol to form a clear solution; placing the clear solution in a closed reaction kettle, performing solvothermal reaction at 160 to 200 DEG C for 6 to 18 hours, cooling, collecting white precipitates in the product, and performing washing and drying; calcining at 800 to 1000 DEG C for 1 to 4 hours. In the invention, the aluminum element is introduced into the zirconia hollow microsphere to effectively reduce the diffusion rate of zirconia at high temperature, so that the hollow microsphere is kept stable above 1300 DEG C or more; the introduction process of the aluminum element is simple, the raw material cost is low, and the prepared aluminum-containing zirconia hollow microsphere has stable structure and good dispersibility.

Description

technical field [0001] The invention belongs to the field of heat insulating materials, and in particular relates to an aluminum-containing zirconia hollow microsphere and a preparation method thereof. Background technique [0002] Zirconia hollow spheres have broad application prospects in the field of heat insulation due to their low density, high specific surface area, low thermal conductivity, good chemical stability and good heat resistance. Zirconia hollow spheres are mostly used in the field of heat insulation as raw materials for the preparation of thermal barrier coatings or bulk porous ceramics, and the prepared heat insulation materials show excellent heat insulation performance. [0003] The particle size and temperature resistance of zirconia hollow spheres seriously affect the heat insulation performance of the final product. Generally, when the porosity of the thermal barrier coating or the bulk porous ceramic is constant, the smaller the diameter of the zirc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02
CPCC01G25/02C01P2002/80C01P2004/03C01P2004/34C01P2004/61C01P2004/62
Inventor 刘玉付郭启王会一
Owner SOUTHEAST UNIV
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