Thin layers of HfO2 grown on the (1 0 0)Si crystal surface using atomic layer deposition or metallo-organic chemical vapour deposition were analysed using x-ray photoelectron spectroscopy (XPS) of Hf 4f, Si 2p and O 1s electron states. The chemical indepth profiling was conducted by combining XPS with Ar+ ion sputtering. In addition to establishing the deposition-sensitive oxide structure, Ar+ ion sputtering was found to lead to the formation of a metallic Hf layer on the surface of the sample. The latter observation suggests HfO2 as a feasible candidate for not only insulating applications but, thanks to the high mass and electron density of the cation, also as a material suitable for the fabrication of nanometre-sized conductors by direct oxide decomposition.

HfO(2) thin films of different thicknesses and deposited by two methods (ALD and MOCVD) were studied. The microstructure of films was characterized by reflection spectroscopy, x-ray diffraction (XRD), and soft x-ray reflectometry. It was established that the HfO(2) film microstructure is closely dependent on film thickness. The 5 nm thick film synthesized by ALD shows an amorphous phase while the film prepared by MOCVD was inhomogeneous in depth and showed signs of crystalline structure. First results on the reconstruction of the depth distribution of chemical elements based on the analysis of reflectivity curves are discussed.

The paper shows the importance of soft X‐ray reflection spectroscopy as a non‐destructive in‐depth characterization tool for the middle atomic ordering in TiO2 thin films. The microstructure of TiO2 films synthesized by magnetron sputtering on Si(100) wafers was characterized by X‐ray reflection spectroscopy (XRS), X‐ray Diffraction (XRD) method and X‐ray reflectometry (XRR). Reflection spectra and calculated absorption spectra were analyzed in the vicinity of Ti L2,3 and O K absorption edges. It was established that the 70 nm TiO2 film is polycrystalline with an anatase structure and homogeneous in depth. The 10 nm TiO2 film is amorphous. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)