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Volatility and Thermal Stability of Lead bis-Heptafluorodimethyloctadione [Pb(fod)2] and Lead bis-Tetramethylheptadione [Pb(thd)2]

Published online by Cambridge University Press:  25 February 2011

May Nyman  and
Seshu B. Desu
May Nyman
Affiliation:
Department of Materials Engineering, Virginia Polytechnic Institute and State University, Blacksburg, VA 24061
Seshu B. Desu
Affiliation:
Department of Materials Engineering, Virginia Polytechnic Institute and State University, Blacksburg, VA 24061
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Abstract

Lead bis-heptafluorodimethyloctadione, or Pb(fod)2 and lead bis-tetramethylbeptadione, or Pb(thd)2 are useful precursors for MOCVD of PbO, a component of PZT ferroelectrics. The two compounds differ only by substituents on their respective ligands, and properties such as volatility and thermal stability differ as a function of the substituents. The volatilities and thermal stabilities of Pb(fod)2 and Pb(thd)2 were examined and compared, in order to further determine usefulness as precursors for MOCVD. Pb(fod)2 and Pb(thd)2 were synthesized and purified via a procedure developed in our laboratory, and purity was confirmed by several techniques. Isothermal and dynamic thermogravimetric analysis experiments were carried out. Regions of thermal stability and thermal instability were identified as a function of heating time and temperature. The region of instability was further examined by heating experiments and chemical ionization mass spectrometry. It was proposed that vaporization of the monomeric form of Pb(fod)2 and Pb(thd)2 controls the rate of weight loss observed in the region of thermal stability, and oligomerization controls the observed rate of weight loss in the region of thermal instability. Heat of vaporization was calculated to be 75 KJ/mol for Pb(fod)2 and 86 KJ/mol for Pb(thd)2.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 243: Symposium G – Ferroelectric Thin Films II , 1991 , 381
Copyright
Copyright © Materials Research Society 1992

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