Chapter 3
Experimental Methods
A variety of experimental methods have been used throughout the project and in
this chapter a description of these will be given. The overall focus of the thesis is
on metal oxide catalysts prepared by sputter deposition. As sample preparation
technique sputter deposition has certain advantages and disadvantages which
will be explained herein. In terms of sample characterization, emphasis has been
put on combining the electrochemical properties with information of oxide phase
determination, valency and stability. The methods of choice have been X-ray
Photoelectron Spectroscopy, X-ray Diraction, X-ray Absorption Spectroscopy,
Inductively Coupled Plasma - Mass Spectrometry and Electrochemical Quartz
Crystal Microbalance measurements.
3.1 Sample Preparation
As mentioned above, the samples tested for this thesis have been prepared by
sputter deposition and given the large amount of time spent optimizing this
technique a comprehensive introduction is justied.
3.1.1 Sputter Deposition
Sputtering is a vacuum technique utilizing bombardment of a target surface
with energetic particles widely used for surface cleaning, etching, surface layer
analysis and deposition. The energetic particles are typically charged Argon
ions, which are created with a plasma source. When sputtering is used for