Abstract
Two lead titanium oxyalkoxides with composition Pb2Ti4O2(O2CCH3)2(OC2H5)14 and Pb2Ti2O2(O2CCH3)2(OCH(CH3)2)8 have been isolated and characterised by elemental analysis, IR, 207Pb NMR and molecular weight measurements. X-ray structural analysis of the 1:2 complex confirmed the presence of two Pb2Ti2O units which are linked by a common Pb···Pb edge and are held together by alkoxide and acetate bridges. The acetate groups have migrated from the Pb to the Ti centres during the reaction. Hydrolysis of the 1:1 Pb/Ti complex produced clear gels providing the H2O/complex ratio was less than 4. Heat treatment of the gel results in loss of residual organics below 400°C. The XRD pattern indicates the presence of the pyrochlore and perovskite phases after heating at 500°C but the sample is poorly crystalline. Complete conversion to the perovskite phase of lead titanate occurs on heating to 600°C for 1 hour. Thin films of lead titanate were deposited by dip-coating a solution of this complex in isopropanol. Analyses of the films, carried out using electron microprobe, Scanning Auger Spectroscopy and Rutherford Backscattering, indicated that they were of excellent quality, crystalline after heating at 600°C and with relatively sharp substrate-coating interface.
Similar content being viewed by others
References
Klein, L.C., “Sol-Gel Technology for Thin Fibres, Films, Preforms, Electronics and Specialty Shapes,” (Noyes, Parkridge, 1988).
Hubert-Pfalzgraf, L.G., New J. Chem. 11, 663 (1987).
Livage, J., Henry, M., and Sanchez, C., Prog. Solid St. Chem. 18, 259 (1988).
Brinker, C.J. and Ulrich, D.R., in “Transformation of Organometallics into Common and Exotic Materials” Ed. R.M. Laine, (Marinus Nijhoff, Dordrecht, 1988).
Hench, L.L. and West, J.K., Chem. Rev. 90, 33 (1990).
Caulton, K.G. and Hubert-Pfalzgraf, L.G., Chem. Rev., 90, 969 (1990).
Bradley, D.C., Chem. Rev., 89, 1317 (1989).
Spiccia, L. and West, B.O., J. Austral. Ceram. Soc., in press.
Gurkovich, S.R. and Blum, J.B., in “Ultrastructure Processing of Ceramics Glasses and Composites” eds. Hench, L.L., Ulrich, D.R., (Wiley and Sons, New York, 1984), p. 152.
Blum, J.B. and Gurkovich, S.R., J. Mater. Sci. 20, 4479 (1985).
Gurkovich, S.R. and Blum, J.B., Ferroelectrics 62, 189 (1985).
Lee, M.-H., Park, Y.-H., and Yang, C.-K., J. Am. Ceram. Soc. 70, C35 (1987).
Budd, K.D. and Payne, D.A., Inst. Phys. Conf. Ser. 103, 13 (1989).
Schwartz, R.W., Lakeman, C.D.E., and Payne, D.A., “Better Ceramics Through Chemistry,” Mater. Res. Soc. Proc. 180, 335 (1990).
Aoki, S.I., Choi, S.C., Payne, D.A., and Yanagida, H., “Better Ceramics Through Chemistry,” Mater. Res. Soc. Proc. 180, 485 (1990).
Janusson, H., Millar, C.E., and Milne, S.J., “Better Ceramics Through Chemistry,” Mater. Res. Soc. Proc. 180, 421 (1990).
Aegerter, M.A., Charbouillot, Y., Mohallem, N., and De Godoy, L.H., “Ultrastructure Processing of Advanced Materials,” Eds. Uhlmann, D.R., Ulrich, D.R., (Wiley and Sons, New York, 1992), p. 613.
Papiernik, R., Hubert-Pfalzgraf, L.G., and Chaput, F., J. Non-Cryst. Solids, 147 & 148, 36 (1992).
Dekleva, T.W., Hayes, J.M., Cross, L.E., and Geoffroy, G.L., J. Am. Ceram. Soc., 71, C280 (1988).
Ramamurthi, S.D. and Payne, D.A., “Better Ceramics Through Chemistry,” Mater. Res. Soc. Proc. 180, 79 (1990).
Papiernik, R., Hubert-Pfalzgraf, L.G., Daran, J.-C., and Jeannin, Y., J. Chem. Soc. Chem. Commun. 695 (1990).
Papiernik, R., Hubert-Pfalzgraf, L.G., and Massiani, M.-C., Inorg. Chim. Acta, 165, 1 (1989).
Papiernik, R., Hubert-Pfalzgraf, L.G., and Massiani, M.-C., Polyhedron, 10, 1657 (1991).
Full details of the structure of (1) will be published at a later stage.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Bates, J., Zhang, Q., Spiccia, L. et al. Heterometallic lead-titanium oxyalkoxide precursors to lead titanate thin films. J Sol-Gel Sci Technol 2, 29–34 (1994). https://doi.org/10.1007/BF00486209
Issue Date:
DOI: https://doi.org/10.1007/BF00486209