Pyrolytic Ta205 films, in thicknesses up to 30,000.~, were produced by the TaCls-CO2-H2 reaction at 900~ These films were characterized by use of transmission electron microscopy, electron microprobe analysis, measurement of dielectric, and optical properties. It was found that the films were orthorhombic Ta205 (~-Ta205) with a fine grained structure. The films did not etch appreciably in hydrofluoric acid. Ellipsometric measurements indicated that the films had an index of refraction of 2.20 • 0.03 at 5461A. In addition, certain areas of the films exhibited slight optical absorption. The optical energy gap was found to be 4.20 eV. The dielectric constant and the loss tangent of the pyrolytic Ta205 films were measured over the temperature range 78~176 and the frequency interval 1-100 kHz and exhibited a surprisingly strong temperature dependence. These results and the electron microprobe results indicate the films are not stoichiometric.Tantalum pentoxide (Ta2Os) has played a very active role in electronic applications for over a decade. Ta205 has been used in thin film form long before the much studied thin film materials such as SIO2, SisN4, and A1203 came into positions of importance for applications such as integrated circuit (IC) passivation and insulated gate, field effect transistor gate dielectrics. It has been found for the latter materials that hightemperature (600~176 chemical vapor deposition (CVD) produced films with properties generally considered more desirable than those of films producd by other methods. In electronic applications Ta20~ is usually produced anodically, or sometimes thermally, but pyrolytic Ta205 has not been used, nor its properties investigated. This paper reports selected details on the preparation and properties of Ta205 films produced by CVD.
Film DepositionThe general subject of oxide film preparation by CVD has been well-treated by Powell et al. (1). Pyrolytic Ta205 has been produced by Peacock (2) through the reaction of Tat15 vapor, H2 gas, and CO2 gas at 900~ and by Wang et al. (3), through the reaction of tantalum alcoholate vapor, helium, and oxygen at 450~The properties of the films produced by the former reaction were not investigated, and those of the latter reaction were described as amorphous and annealable to polycrystalline ~-Ta205 fter 30 rain at 800~The reaction between TaCl5 vapor, H2, and C02 at 900~ was used to prepare the films for this study. The presumed over-all reaction is 900~ 2TaCI5 + 5H2 + 5CO2 -+ Ta205 + 6CO + 10HCIThe deposition apparatus, shown schematically in Fig. 1, is a modified version of the one reported by Tauber, Dumbri, and Caffrey (4) for the pyrolytic deposition of zirconium dioxide. The substrate rests on a molydenum susceptor, which is heated inductively at 480 kHz, The susceptor is rotated by a specially designed harmonic drive. The gases are carefully metered through Brooks rotometers and are carried through stainless steel lines to the deposition chamber. The TaC15 vapor is transferred to the chamber by passing hydrogen through a h...