Scandium(III) Beta-Diketonate Derivatives As Precursors For Oxide Film Deposition By CVD

Complexes with acetylacetone Sc(acac)(3), dipivaloylmethane Sc(thd)(3), 2,2,6,6-tetramethyl-4-fluoro-3,5-heptanedione Sc(tfhd)(3), pivaloyltrifluoroacetone Sc(ptac)(3), trifluoroacetylacetone Sc(tfac)(3), and hexafluoroacetylacetone Sc(hfac)(3) were synthesized, purified and identified by elemental analysis, m.p., IR and NMR spectroscopy, and mass spectrometry. The thermal behaviour of the synthesized compounds in the solid state was investigated by the method of difference-scanning calorimetry in vacuum. As a result the thermodynamic characteristics of the melting processes were determined. The temperature dependences of saturated and unsaturated vapour pressure of complexes under study were measured by static method with membrane-gauge manometers. The average molecular weight of gas calculated from the experimental data on unsaturated vapours using ideal gas law was close to the molecular weight of monomer for all investigated compounds. Decomposition temperatures of compounds under study were defined as the temperature above that pressure changes became irreversible. The information about melting and decomposition processes were taken into account at measuring saturated vapour pressure of complexes. The row of volatility Sc(hfac)(3) > Sc(ptac)(3) > Sc(tfac)(3) > Sc(thd)(3) Sc(tfhd)(3) > Sc(acac)(3)) was determined from the p-T dependences obtained. Above information about thermal behaviour of complexes enabled one to use it as a guide for CVD experiments aimed at achieving oxide films with high optical properties. Precursor chosen for film deposition was Sc(thd)(3). The Sc2O3 film deposition conditions were following: the gas-carrier rate 1 l/h, He gas-reagent rate 10 l/h, total pressure 10 Torr, evaporator temperature 105-110 degrees C, substrate temperature 450-650 degrees C, substrate Si(100). Ellipsometry was applied to characterize the film thickness and refractive index. The morphology and the composition of the films were determined with XPS and SEM. (C) 2013 The Authors. Published by Elsevier B.V.