Hostname: page-component-76fb5796d-wq484 Total loading time: 0 Render date: 2024-04-26T08:09:03.063Z Has data issue: false hasContentIssue false

An Infrared Study of Metal Isopropoxide Precursors for SrTiO3*

Published online by Cambridge University Press:  15 February 2011

R. E. Riman
Affiliation:
Massachusetts Institute of Technology, Cambridge, MA
D. M. Haaland
Affiliation:
Sandia National Laboratories, Albuquerque, NM
C.J.M. Northrup Jr.
Affiliation:
Sandia National Laboratories, Albuquerque, NM
H. K. Bowen
Affiliation:
Massachusetts Institute of Technology, Cambridge, MA
A. Bleier
Affiliation:
Massachusetts Institute of Technology, Cambridge, MA; Presently at Oak Ridge National Laboratories
Get access

Abstract

A Sr/Ti bimetallic isopropoxide complex was synthesized by two methods. The complex served as a precursor to the production of homogeneous SrTiO3 powders via alkoxide hydrolysis. Infrared spectra were obtained for Sr(OPri)2, Ti(OPri)4, and the product of the syntheses. In addition, the IR spectra of the solutions of each of the alkoxides were followed as hydrolysis reactions proceeded. Detailed analysis of the spectral features support the existence of a 1:1 Sr/Ti bimetallic alkoxide. The new Sr/Ti compound exhibits characteristic absorption bands at (1017, 993, 972, 961 cm−1), (844, 838, 827 cm−1) and (620, 596, and 572 −1). A band at 819−1 might also be associated with the new Sr/Ti bimetallic alkoxide. The infrared spectra suggest that the isopropoxide ligands in the bimetallic alkoxide are in at least three separate local environments. This information offers insight into possible structures for the complex.

Type
Research Article
Copyright
Copyright © Materials Research Society 1984

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

Footnotes

*

A portion of this work was performed at Sandia National Laboratories supported by the U.S. Department of Energy under contract number DE–ACO4–76DP00789. The M.I.T. work is supported by an industry consortium.

References

REFERENCES

1. Riman, R. E., Ph.D. Thesis, in progress.Google Scholar
2. Barringer, E. and Bowen, H. K., “Formation, Packing and Sintering of Monodisperse TiO2 Powders,” J. Am. Ceram. Soc. Comm. 65 (12), C199201 (1982).Google Scholar
3. Smith II, J. S., Dolloff, R. T., and Mazdiyasni, K. S., “Preparation and Characterization of Alkoxy-Derived SrZrO3 and SrTiO3,” J. Am. Ceram. Soc. 53 (2) 9195 (1970).Google Scholar
4. Mazdiyasni, K. S., Dolloff, R. T., and Smith II, J. S., “Preparation of High-Purity Submicron Barium Titanate Powders,” J. Am. Ceram. Soc. 52 (10) 523526 (1969).Google Scholar
5. Turova, N. Ya. and Turevskaya, E. P., “Primary Hydrolysis Product of Titanium Ethylate” Koord. Khim. 3 (5) 679684 (1977).Google Scholar
6. Suwa, Y., Sugimoto, Y. and Naka, S., “Preparation of Compounds in BaO–TiO2 System by Coprecipitation from Alkoxides,” Funtai Oyobi Fummatsu Yakin 25 (5), 2023 (1978).Google Scholar
7. Turevskaya, E. P., Turova, N. Ya. and Novoselova, A. V., “Investigation of the Formation of Bimetallic Alkoxides Reaction of Barium Ethoxide and Titanium Ethoxide,” Dok. Akad. Navk SSSR 242 (4), 883886 (1978).Google Scholar
8. Bradley, D. C., Mehvotra, R. C. and Wardiaw, W., “Structural Chemistry of the Alkoxides, Part I. Amyloxides of Silicon, Titanium, and Zirconium,” J. Chem. Soc., London 2027–2032 (1952).Google Scholar
9. Zeiss, H. H. and Tsutsui, M., “The Carbon-Oxygen Absorption Band in the Infrared Spectra of Alcohols,” J. Am. Chem. Soc. 75, 897900 (1953).Google Scholar
10. Lutz, Von H. D., “IR-spektroskopische Untersuchungen an Mg(OC2H5)2, Ca(OC2H5)2, Sr(OC2H5)2 and Ba(OC2H5)2,” Z. Anorg. Alleg. Chem. 356, 132139 (1968).Google Scholar
11. Sheppard, N. and Simpson, D. M., “The Infra-Red and Raman Spectra of Hydrocarbons. Part II Paraffins.Google Scholar
12. Silverstein, R. M. and Bassler, C. C., Spectroscopic Identification of Organic Compounds, John Wiley and Sons, NY, Second Edition, 1967 p. 84.Google Scholar
13. Barraclough, C. G., Bradley, D. C., Lewis, J. and Thomas, I. M., “The Infrared Spectra of Some Metal Alkoxides, Trialkylsilyloxides and Related Silanols,” J. Chem. Soc., London 2601–2605 (1961).Google Scholar
14. Lynch, C. T., Mazdiyasni, K. S., Smith, J. S. and Crawford, W. J., “Infrared Spectra of Transition Metal Alkoxides,” Anal. Chem. 36 (12), pp. 23322337 (1964).Google Scholar
15. Seubold, F. H., “Anionic Conjugation: The Infrared Spectra of Sodium Alkoxides,” J. Org. Chem. 21, 156160 (1956).Google Scholar
16. Grigorev, A. I. and Turova, N. Ya., “The IR Absorption Spectra of Alcoholates of Berryllium, Magnesium and the Alkaline Earth Metals,” Akad. Nauk SSSR Proceedings Chem. Section 162. pp. 424427 (1965).Google Scholar
17. Bellamy, L. J., The Infrared Spectra of Complex Molecules, 1, J. Wiley & Sons, NY (1975).Google Scholar
18. Suetich, G. W. and Voge, A. A., “Crystal Molecule Structure of Tetraphenoxytitanium (IV) Monophenolate, Ti(OPh)4.HOPh,” Chem. Comm. 676–677 (1971).Google Scholar
19. Stoeckli-Evans, H., “Studies of Organometallic Compounds XVI, The Crystal Structure of Di-μ-ethoxy-bis (dibenzlethoxy-titanium (IV),” Hel. Chim. Acta 58 (2) 373377 (1975).Google Scholar