Preparation of nanocrystalline ZrO₂ by reverse precipitation method

Abstract

Nanocrystalline ZrO₂ particulates with different sizes were prepared by precipitation method using ethanol as dispersive and protective reagent. XRD patterns show that the synthesized ZrO₂ is monoclinic in structure with space group P21/a when calcination temperature is in the range of 400–1000°C. It is found that the smaller the particle, the bigger the crystal lattice distortion, the worse the crystal growth, and the lower the diffraction intensity. TEM images reveal that ZrO₂ particles are spherical in shape, and the particle size distribution is in, narrow range. The mean sizes of the particles increase with the increase of calcination temperatures. It is first to observe the streaks of different crystallographic planes. Thermogravimetric analysis indicates that the crystallization temperature of ZrO₂ is 461.32°C. Measurement of ZrO₂ relative density shows that the relative density of nanocrystalline ZrO₂ powders increases with the increasing of ZrO₂ particle sizes.

Keywords

zirconium / zirconium dioxide / nanoparticulate / precipitation method

References

[1] Henglein A. Small-particle Research: Physicochemical Properties of Extremely Small Colloidal metal and Semiconductor Particles. Chem. Rev., 1989, 89(8): 1861-1873.

[2] Dong X T, Liu Z R, Yang K S, Liu J H. Preparation and Properties of Rare Earth Hydroxides and Oxides Ultrafine Powders in Alcohol. Chin. Chem. Lett., 1995, 6(11): 1017-1020.

[3] Beecroft L L, Ober C K. Nanocomposite Materials for Optical Applications. Chem. Mater., 1997, 9(6): 1302-1317.

[4] Dong X T, Li M, Zhang W, Liu G X, Hong G Y. Preparation and Characterization of Nanocrystalline CeO₂ by Precipitation Method. J. of Rare Earths, 2002, 20(6): 583-586.

[5] Dong X T, Liu G X, Zhang W, Wang D Y, Li Y H, Liu J H, Li J L, Hong G Y. Nanocrystalline SnO₂ Synthesized by Means of Hydrothermal Precipitation. Rare Metal Mater. and Eng., 2000, 29(3): 197-199.

[6] Wang Y, Henon N. Nanometer-sized Semiconductor Clusters, Materials Synthesis, Quantum Size Effects and Photophysical Properties. J. Phys. Chem., 1991, 95(2): 525-532.

[7] Dong X T, Zhang L, Zhang W, Wang L P, Hong G Y. Preparation and Characterization of Nanometer-sized CeO₂/Polystyrene Hybrid Material. Acta Phys.-Chem. Sin., 2001, 17(8): 739-742.

[8] Dong X T, Liu G X, Sun J, Li J L, Liu J H, Hong G Y. Preparation and Properties of Nanocrystalline Yb₂O₃. Rare Metal Mater. and Eng., 2001, 30(1): 73-76.

[9] Dong X T, Sun J, Liu G X, Wang G H, Yan J H, He Y, Liu Z X, Hong G Y. Preparation and Characterization of Nanometer-sized CeO₂/PMMA Hybrid Material. Acta Chimica Sinica, 2003, 61(1): 122-125.

[10] Dong X T, Hong G Y, Yu D C, Yu D S. Synthesis and Properties of Cerium Oxide Nanometer Powders by Pyrolysis of Amorphous Citrate. J. Mater. Sci. & Technol., 1997, 13(2): 113-116.

[11] Dong X T, Qu X G, Hong G Y, Yu D C, Lu T H, Ni J Z. Preparation and Application in Electrochemistry of Nanocrystalline CeO₂. Chin. Sci. Bull., 1996, 41(16): 1396-1401.

[12] Dong X T, Liu G X, Sun J, Yan J H, Hong G Y. Preparation of CeO₂ Nanoparticles Hydrosol. Rare Metal Mater. and Eng., 2002, 31(3): 229-231.

[13] Fornasiero P, Balducci G, Di Monte R, Kaspar J, Sergo V, Gubitosa G, Ferrero A, Grazian M. Modification of the Redox Behavior of CeO₂ Induced by Structural Doping with ZrO₂. J. Catal., 1996, 164: 173-183.

[14] Zheng X H. Isothermal Transformation from Tetragonal (t) to Monoclinic (m) in ZrO₂ Ceramics. Materials Science and Engineering, 1999, 17(1): 75-79.

[15] Cheng K G, Wan J, Liang K M. Fabrication of ZrO₂ Toughened Glass-Ceramics. J. Chin. Ceram. Soc., 1998, 26(3): 365-368.

[16] Cheng H M, Wu L J, Ma T M, Zhao Z G, Qi L M. Hydrothermal Preparation of Nanosized Cubic ZrO₂ Powders. J. Mater. Sci. Lett., 1996, 15: 895-897.

[17] Xie Y Q. Preparation of Ultrafine Zirconium Dioxide Particles. Chin. J. Mater. Res., 2000, 14(Suppl.): 45-48.

[18] Li W, Wang H Z, Gao L, KGuo J. Sintering Behavior of ZrO₂ Powder Synthesized by Heating of Alcohol-Aqueous Salt Solution. J. Chin. Ceram. Soc., 2000, 28(1): 57-60.