Abstract
Forced hydrolysis preparation of zirconia sols and powders by microwave heating of zirconium tetrachloride solutions at temperatures equal to 180 °C leads in a few minutes to monodispersed nanoscale zirconia particles. Synthesis was performed in a microwave reactor called the RAMO system. This microwave reactor was designed by the authors. This flash-synthesis process combines the advantages of forced hydrolysis (homogeneous precipitation) and microwave heating (very fast heating rates). The sols and powders were characterized by x-ray diffraction,photon correlation spectroscopy (PCS), small-angle x-ray scattering, and transmission electron microscopy. Sols are colloidally stable, which means that after 6 months no sedimentation is observed and the size distribution given by PCS measurements has not changed. For all synthesis conditions (with or without HCl, zirconium salt concentration, and synthesis time), zirconia polycrystalline particles were produced. According to the different analyses, these zirconia polycrystalline particles were constituted of aggregates of small primary clusters.
Similar content being viewed by others
References
J.Y.Dai, H.C. Ong, and R.P.H. Chang, J. Mater. Res. 14, 1329 (1999).
J.A. Belot, R.J. McNeely, A. Wang, C.J. Reedy, T.J. Marks, G.P.A. Yap, and A.L. Rheingold, J. Mater. Res. 14, 12 (1999).
J. Si, S.B. Desu, and CY. Tsai, J. Mater. Res. 9, 1721 (1994).
B.J. Gould, I.M. Povey, M.E. Pemble, and W.R. Flavell, J. Mater. Chem. 4, 1815 (1994).
E.T. Kim and S.G. Yoon, Thin Solid Films 227, 7 (1993).
A.S. Kao and G.L. Gorman, J. Appl. Phys. 67, 3826 (1990).
A.H. Heuer, J. Am. Ceram. Soc. 70, 689 (1987).
J.L. Shi, J. Mater. Res. 14, 1389 (1999).
R. Ramamoorthy, S. Ramasamy, and D. Sundararaman, J. Mater. Res. 14, 90 (1999).
E. Matijevic, Pure Appl. Chem. 60, 1479 (1988).
S.L. Chen, P. Dong, G.H. Yang, and J.J. Yang, Ind. Eng. Chem. Res. 35, 4487 (1996).
E. Matijevic, Acc. Chem. Res. 14, 22 (1981).
A. Clearfield, Inorg. Chem. 3, 146 (1964).
Y. Murase and E. Kato, J. Am. Ceram. Soc. 66, 196 (1983).
P.E.D. Morgan, J. Am. Ceram. Soc. 67, C204 (1984).
M.A. Blesa, A.J.G. Maroto, S.I. Passaggio, N.E. Figliolia, and G. Rigotti, J. Mater. Sci. 20, 4601 (1985).
M.Z.C. Hu, M.T. Harris, and C.H. Byers, J. Colloid Interface Sci. 198, 87 (1998).
P. Rigneau, K. Bellon, I. Zahreddine, and D. Stuerga, Eur. Phys. J. AP 7, 41 (1999).
P. Rigneau, K. Bellon, and D. Stuerga, in Second European Workshop on Microwave Processing of Materials (Second European Workshop on Microwave Processing of Materials Proceedings, Karlsruhe, Germany, 1997), (M. Willert-Porada, Karlsruhe, Germany), p. 101.
P. Rigneau, K. Bellon, and D. Stuerga, in Sixth International Conference on Microwave and High Frequency Heating (Sixth International Conference on Microwave and High Frequency Heating Proceedings, Fermo, Italy, 1997), (G. Breccia, Fermo, Italy), p. 465.
D. Daichuan, H. Pinjie, and D. Shushan, Mater. Res. Bull. 30, 531 (1995).
D. Daichuan, H. Pinjie, and D. Shushan, Mater. Res. Bull. 30, 537 (1995.)
Y.T. Moon, D.K. Kim, and C.H. Kim, J. Am. Ceram. Soc. 78, 1103 (1995).
R. Rodriguez-Clemente and J. Gomez-Morales, J. Cryst. Growth 169, 339 (1996).
Y. Ma, E. Vileno, S.L. Suib, and P.K. Dutta, Chem. Mater. 9, 3023 (1997).
S. Komarneni, Q.H. Li, and R. Roy, J. Mater. Chem. 4, 1903 (1994).
I. Girnus, M-M. Pohl, J. Richter-Mendau, M. Schneider, M. Noack D. Venzke, and J. Caro, Adv. Mater. 7, 711 (1995).
D. Stuerga and P. Gaillard, Tetrahedron 52, 5505 (1996).
K.J. Randle, Chem. Ind. 19, 74 (1980).
N. De Jaeger, H. Demeyere, R. Finsy, R. Sneyers, J. Vanderdeelen, P. Van Der Meeren, and M. Van Laethem, Part. Part. Syst. Charact. 8, 179 (1991).
R. Finsy andN. De Jaeger, Part. Part. Syst. Charact. 8, 187 (1991).
R. Finsy, N. De Jaeger, R. Sneyers, and E. Geladé, Part. Part. Syst. Charact. 9, 125 (1992).
A. Clearfield and PA. Vaughan, Acta Crystallogr. 9, 555 (1956).
T.C.W. Mak, Can. J. Chem. 46, 3491 (1968).
G.M. Muha and P.A. Vaughan, J. Chem. Phys. 33, 194 (1960).
M. Aberg, Acta Chem. Scand. B 31, 171 (1977).
E. Matijevic, Langmuir 2, 12 (1986).
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Bellon, K., Chaumont, D. & Stuerga, D. Flash synthesis of zirconia nanoparticles by microwave forced hydrolysis. Journal of Materials Research 16, 2619–2622 (2001). https://doi.org/10.1557/JMR.2001.0360
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/JMR.2001.0360