Abstract
PbTiO3 film and powder materials have been obtained from a sol prepared at room temperature by mixing lead(II) acetate trihydrate (LAT) and tetraisopropylorthotitanate (TPOT) in methoxyethanol. The sol-gel process was studied by means of207Pb nuclear magnetic resonance and infrared spectroscopy, differential thermal analysis and X-ray diffraction measurements. This investigation shows that an interaction between LAT and TPOT occurs immediately on mixing in solution and, as a result of the interaction, the lead and titanium compounds are indistinctly linked togetherthrough bidentate acetate bridging. This linkage remains unchanged during solution reactions and gelation, Pb-O-Ti bonding being absent at this stage. Pb-O-Ti bonding in the sol-gel materials is believed to be first formed between 200 and 350 °C during the decomposition of the OAc group of LAT and its removal from the gel. The gel retains its amorphous state on heating at 370 °C for 1 h. An unidentified primary crystal phase appears after heating the gel at 400 °C for 1 h, and it is transformed into perovskite PbTiO3 crystals at 500 °C and higher temperatures.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
K. D. Budd, S. K. Dey andD. A. Payne, in “Better ceramics through chemistry II”, edited by C. J. Brinker, D. E. Clark, and D. R. Ulrich (Materials Research Society Proceedings 73, Pittsburgh, PA, 1986) pp. 711–716.
H. Jansson, C. E. Millar andS. J. Milne, in “Better ceramics through chemistry IV”, edited by B. J. J. Zelinski, C. Jeffrey Brinker, D. E. Clark and D. R. Ulrich (Materials Research Society Proceedings 180, Pittsburgh, PA, 1990) p. 421.
J. Marillet andD. Bourret,J. Non-Cryst, Solids 147/148 (1992) 266.
H. Dislich, in “Sol-gel technology for thin films”, edited by L. C. Klein (Noyes, Park Ridge, NJ, 1988) p. 50–79.
J. B. Blum andS. R. Gurkovich,J. Mater. Sci. 22 (1987) 2655.
S. D. Ramamurthi andA. D. Payne, in “Better ceramics through chemistry IV”, edited by B. J. J. Zelinski, C. Jeffrey Brinker, D. E. Clark and D. R. Ulrich (Materials Research Society Proceedings 180, Pittsburgh, PA, 1990) p. 79.
R. K. Harris andB. E. Mann, “NMR and the periodical table” (Academic Press, London, New York, San Francisco, 1978).
K. Nakamoto, “Infrared and raman spectra of inorganic and coordination compounds”, 3rd Edn (Wiley, New York, 1978).
K. H. Von Thiele andM. Panse,Z. Anorg. Allg. Chem. 441 (1978) 23.
T. W. Dekleva, J. M. Hayes, L. E. Cross andG. L. Geoffroy,J. Am. Ceram. Soc. 71 (1988) C280.
S. R. Gurkovich andJ. B. Blum, in “Ultra structure processing of ceramics, glasses and composites”, edited by L. L. Hench and D. R. Ulrich (Wiley, New York, 1984) p. 152.
S. Doeuff, M. Henry, C. Sanchez andJ. Livage,J. Non-Cryst. Solids 89 (1987) 206.
B. E. Yoldas, in “Ultra structure processing of ceramics, glasses and composites”, edited by L. L. Hench and D. R. Ulrich (Wiley, New York, 1984) p. 65.
K. A. Mauritz andC. K. Jones,J. Appl. Polym. Sci. 40 (1990) 1401.
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Lan, L., Montenero, A., Gnappi, G. et al. PbTiO3 sol-gel process studied by207Pb-NMR, IR, DTA and XRD. J Mater Sci 30, 3137–3141 (1995). https://doi.org/10.1007/BF01209228
Received:
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF01209228