Hostname: page-component-8448b6f56d-t5pn6 Total loading time: 0 Render date: 2024-04-18T23:45:31.392Z Has data issue: false hasContentIssue false
  • English
  • Français

Synthesis and Decomposition of a Novel Carboxylate Precursor to Indium Oxide

Published online by Cambridge University Press:  15 February 2011

Aloysius F. Hepp ,
Maria T. Andras ,
Stan A. Duraj ,
Eric B. Clark ,
David G. Hehemann ,
Daniel A. Scheiman  and
Phillip E. Fanwick
Aloysius F. Hepp
Affiliation:
NASA Lewis Research Center, Photovoltaic Branch, M.S. 302-1, Cleveland, OH 44135
Maria T. Andras
Affiliation:
Department of Chemistry, Cleveland State University, Cleveland, OH, 44115
Stan A. Duraj
Affiliation:
Department of Chemistry, Cleveland State University, Cleveland, OH, 44115
Eric B. Clark
Affiliation:
NASA Lewis Research Center, Photovoltaic Branch, M.S. 302-1, Cleveland, OH 44135
David G. Hehemann
Affiliation:
School of Technology, Kent State University, Kent, OH 44242
Daniel A. Scheiman
Affiliation:
Sverdrup Technology, Inc., 2001 Aerospace Parkway, Brook Park, OH 44142
Phillip E. Fanwick
Affiliation:
Department of Chemistry, Purdue University, West Lafayette, IN 47907
Get access

Abstract

Reaction of metallic indium with benzoyl peroxide in 4-methylpyridine (4-Mepy) at 25 °C produces an eight-coordinate mononuclear indium(III) benzoate, In(η2-O2CC6H5)3(4- Mepy)2 4H2O (I), in yields of up to 60%. The indium(III) benzoate was fully characterized by elemental analysis, spectroscopy, and X-ray crystallography; (I) exists in the crystalline state as discrete eight-coordinate molecules; the coordination sphere around the central indium atom is best described as pseudo-square pyramidal. Thermogravimetric analysis of (I) and X-ray diffraction powder studies on the resulting pyrolysate demonstrate that this new benzoate is an inorganic precursor to indium oxide. Decomposition of (I) occurs first by loss of 4-methylpyridine ligands (100°-200°C), then loss of benzoates with formation of In2O3 at 450°C. We discuss both use of carboxylates as precursors and our approach to their preparation.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 335: Symposium Y – Metal-Organic Chemical Vapor Deposition of Electronic Ceramics , 1993 , 227
Copyright
Copyright © Materials Research Society 1994

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.)

References

1. Weinberg, I., Solar Cells 29, 225 (1990).CrossRefGoogle Scholar
2. van de Ven, J., Binsma, J.J.M., and de WIld, N.M.A., J. Appl. Phys. 67, 7568 (1990).CrossRefGoogle Scholar
3. Andras, M.T., Duraj, S.A., Hepp, A.F., Fanwick, P.E., and Bodnar, M.M., J. Am. Chem. Soc. 114, 786 (1992).CrossRefGoogle Scholar
4. Mehrotra, R.C. and Bohra, R., Metal Carboxylates; (Academic Press, London, 1983) pp. 121–129, 178-181.Google Scholar
5. Tuck, D.G., in Comprehensive Organometallic Chemistry; Vol.1, edited by Wilkinson, G., F.G.A., Stone, Abel, E.W., (Pergamon Press, New York, 1982) pg.719. Google Scholar
6. Lindel, V.W. and Huber, F.Z., Anorg. AlIg. Chem. 408, 167 (1974).CrossRefGoogle Scholar
7. Hausen, H.D., J. Organometal. Chem. 39, C37 (1972).CrossRefGoogle Scholar
8. Einstein, F.W.B., Gilbert, M.M., and Tuck, D.G., J. Chem. Soc., Dalton Trans., 248 (1973).Google Scholar
9. Habeeb, J.J. and Tuck, D.G., Can. J. Chem. 52, 3950 (1974).CrossRefGoogle Scholar
10. Nomura, R., Fujii, S., Kanaya, K., and Matsuda, H., Polyhedron 9, 361 (1990).CrossRefGoogle Scholar
11. Khan, M.A., Peppe, C., and Tuck, D.G., Acta Cryst. C39, 1339 (1983).Google Scholar
12. Andras, M.T., Hepp, A.F., Duraj, S.A., Clark, E.B., Scheiman, D.A., Hehemann, D.G., and Fanwick, P.E., Inorg. Chem. 32, 4150 (1993).CrossRefGoogle Scholar
13. Habeeb, J.J. and Tuck, D.G., J. Chem. Soc., Dalton Trans., 243 (1973).Google Scholar
14. For example, In(O 2CMe) 3L where L is a bidentate N, N′-donor molecule, i.e., 2,2′ bipyridine or 1,10-phenanthroline; see Preut, V.H. and Huber, F.Z., Anorg. Allg. Chem. 450, 120 (1979).Google Scholar
15. Kumar, R., Mabrouk, H.E., and Tuck, D.G., J. Chem. Soc., Dalton Trans., 1045 (1988).Google Scholar
16. The diffraction pattern was matched with In2O3 in the JCPDS International Center for Diffraction Data 1989. Powder Diffraction File No. 6-0416.Google Scholar
17. Chemical analysis showed total C, H, and N content below detection limit.Google Scholar
18. Handbook of Chemistry and Physics, edited by Weast, R.C., 55th ed. (Chemical Rubber Company Press, Cleveland, OH, 1974) pg. B–96.Google Scholar