Synthesis and characterization of (Î²-diketonate) zirconium alkoxides for low temperature chemical vapor deposition of lead zirconium titanium thin films
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From the above reasoning, it was decided to prepare a zirconium di-(2,2,6,6 tetramethyl-3,5 heptadione) di-tert-butoxide compound. The compound was characterized and subjected to a variety of volatility studies. Thermogravimetric analysis provided evidence that the compound was volatile enough to be used in thin film synthesis. Initial attempts at film deposition, however, resulted in no film growth. Changing deposition parameters also resulted in no film growth. Visual inspection of the residue left after the deposition trials gave the first indication that the compound had undergone some change. Analysis of the material left in the reactor suggested the formation of a zirconium cluster compound. Further decomposition studies also resulted in the formation of the same zirconium cluster compound.
Attempts to make the compound more stable at deposition temperatures centered on changing the alkoxide. Tri-tert-butyl alcohol(tritox) was prepared, however, the synthesis of the tritox - Î²-diketonate zirconium complex was unsuccessful. Other changes involved using pivalic acid to replace the alkoxide. Reactions with pivalic acid and zirconium di-(2,2,6,6 tetramethyl-3,5 heptadione) di-tert-butoxide resulted in the decomposition of the starting material.
Other Î²-diketonate complexes were also investigated. Compounds synthesized from 2.4 pentadione(Acac), I-benzoyl acetone(Bzac) and dibenzoyl methane(Dbzm) could not be purified in order to subject them to chemical vapor deposition. A zirconium complex with two different Î² diketonate ligands was also synthesized. The complex was not investigated as a precursor for chemical vapor deposition because the isomers of the complex could not be separated.
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