Process for prepairng granularity controllable nm-class zirconium oxide

A technology of nano-zirconia and particle size, which is applied in zirconia and other directions, can solve problems such as easy leakage, serious particle agglomeration, and uneven particle size distribution

Inactive Publication Date: 2002-02-06
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The transmission electron microscope results of the product show that the particles are agglomerated seriously, and the particle size distribution is uneven
In addition, this method requires the use of a large amount of gaseous ammonia, which is easy to leak and has high toxicity.

Method used

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  • Process for prepairng granularity controllable nm-class zirconium oxide
  • Process for prepairng granularity controllable nm-class zirconium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, choose TritonX-100, n-hexanol, and cyclohexane as the surfactant, co-surfactant, and oil phase, and mix 0.8 mol / l zirconium nitrate solution and 15 mol / l zirconium nitrate solution in the ratio of the following water phase and organic phase, respectively. 1 aqueous ammonia was added to the organic mixed solution to prepare two microemulsions, so that the volume ratio of each component was water: TritonX-100: n-hexanol: cyclohexane = 1: 2.1: 2.7: 15. Then, at 25° C., the two obtained microemulsions were mixed together under vigorous stirring, and the stirring was continued for 1 hour. The lower layer liquid in the liquid phase system was centrifuged at 9000 rpm for 30 minutes. After washing several times with methanol, water and acetone, the obtained solid was dried and calcined at 450°C, and its specific surface area was measured to be 74.3m 2 / g, the corresponding average particle size is 13.6nm.

Embodiment 2

[0020] In Example 1, the reaction temperature was controlled to be 50°C. After the obtained sample was treated in the same way, its specific surface area was measured to be 85.6m 2 / g, the corresponding average particle size is 11.8nm.

Embodiment 3

[0022] In Example 1, the reaction temperature was controlled to be 63°C. After the obtained sample was treated in the same way, its specific surface area was measured to be 53.7m 2 / g, the corresponding average particle size is 18.8nm.

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Abstract

A process for preparing nm-class zirconium oxide with controllable size (less than 30 nm) includes preparing two portions of microsuspension containing non-ionic surfactant, n-hexanol, cyclohexane and zirconium salt solution or amminia water, mixing, hydrolysis reaction, centrifuging or filtering, washing with alclohol and water several times, drying and calcining. It features that its size can be controlled by controlling the content of zirconium solution or ammonia water, the ratio of water to surfactant and reaction temp.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of size-controllable nanometer zirconia. Background technique [0002] Nano zirconia can be used as chemical sensors and high-performance ceramics. In recent years, the use of zirconia as a heterogeneous catalyst or adsorbent support has also received great attention. The preparation method of nano zirconia usually has precipitation method (Stichert W, Schuth F, J.Catal., 1998,174:242), sol-gel method (Ward D A, Ko E I, J.Catal.1995,157:321 ), hydrothermal synthesis (Tani E, Yoshimura M, Somiya S, J.Am.Ceram.Soc.1983, 66(1): 11), and cracking of organic compounds (Chraska T, King A H, Berndt C C, Mater. Sci. Eng. A, 2000, 286: 169) etc. In general, the liquid phase method is easy to operate, but often easily causes particle agglomeration. [0003] H. J. Stezel and W. Hess (Chinese patent application number: 97111560, publication nu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02
Inventor 黎维彬杨絮飞
Owner TSINGHUA UNIV
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