Spectroscopic ellipsometry of Palladium thin films
Creators: name: Sullivan, Brian Thomas
Publisher: name: University of British Columbia
Year: 2010

description: Spectroscopic ellipsometry is a nondestructive, ambient surface analysis technique for studying surfaces, interfaces and thin films. To take advantage of this method an automatic spectroscopic ellipsometer was designed and constructed for the microstructural characterization of thin films. This high precision instrument is capable of measuring in real-time the optical properties of bulk or thin film materials over the visible-UV region (1.5 - 6.0 eV). The microstructure of thin films can be determined from an effective medium theory analysis of the spectroellipsometric data to investigate how the film morphology evolves with varying preparation conditions and to determine the optimum deposition parameters. In this thesis the pseudodielectric function of palladium films prepared by dc planar magnetron sputtering was measured while the substrate temperature, argon partial pressure and rf-induced substrate bias were varied independently during deposition. The film data are in excellent agreement with the effective medium theory of Sen, Scala, and Cohen, relevant for a random coated-particle microstructure where the grains are optically isolated from each other. With increasing substrate temperature, the Pd volume fraction in the bulk was found to decrease slightly, while the rms microroughness of the film surface increased in magnitude. At 190° C, the rms microroughness was 80 ± 3 Awith the Pd volume fraction in the bulk region falling slightly to 97 ± 1% relative to the film deposited at 22° C. For argon partial pressures below a transition pressure, Pt≃15 mTorr, the films consisted of densely packed grains, corresponding to the zone T in Thornton's structure zone model. Above this transition pressure, the films developed into a more voided columnar structure, characteristic of the zone 1 region. A microstructural analysis indicated a general trend towards increased porosity and microroughness of the films with higher argon pressures. The zone 1 region was best described optically by a random coated-particle microstructure and the electron microscopy confirmed that for thin films prepared at argon pressures higher than Pt, the grains became isolated by void boundaries. The optical data could not distinguish whether or not the films were 2- or 3-dimensionally isotropic. With increasing rf-induced substrate biasing, the Pd film microstructure was modified in a manner similar to that obtained by varying the substrate temperature alone. Significant resputtering of the Pd films occurred, varying from 2 to 11 A/sec for bias voltages of -550 V to -1375 V, respectively. The measured deposition rate while bias sputtering was significantly higher than that expected upon the measured resputtering rate and several mechanisms were proposed to account for the enhancement in the deposition rate. The films were best characterized by a 2-dimensional isotropy which was supported by the columnar nature of the films observed by electron microscopy. Finally, the dielectric function of the "best" palladium film is compared to optical constants of Pd previously reported in the literature for bulk and thin film specimens. While all the authors quote essentially the same values for the real part of the dielectric function, regardless of the preparation or measurement technique, the imaginary part differs up to a factor of two. Surface microroughness, bulk porosity and oxide layers are unable to account for the difference. A possible grain boundary scattering mechanism is suggested.