An investigation of cobalt oxide based nanocrystalline thin films by secondary ion mass spectrometry (SIMS) is presented. The coatings, whose composition ranged between CoO and Co 3 O 4 , were synthesized by chemical vapor deposition (CVD) on indium tin oxide (ITO) substrates, using cobalt(II) b-diketonate as precursor. The SIMS analysis revealed a satisfactory precursor conversion into the oxides and allowed distinction of regions in the films at different compositions. Filmsubstrate intermixing phenomena were evidenced and studied as a function of deposition temperature, film thickness and composition. Copyright # 2001 John Wiley & Sons, Ltd.Oxide-based materials show a broad spectrum of characteristics ranging from insulating to metallic, through optical, catalytic and superconducting properties 1 and, in this widespread context, nanocrystalline oxide based thin films have attracted a markedly growing interest in recent years. Nanocrystalline materials are usually defined as polycrystalline solids with particle diameters or grain sizes ranging from sub-nanometers up to 100 nm. As the crystal size decreases, there is a continuous transition from bulk to molecular properties with a number of effects being attributed to quantum confinement or more generally to restricted geometry. 2 These size effects are undoubtedly of outstanding importance in the fields of catalysis, gas sensors and semiconductor devices, whose functional properties are affected by various features, i.e. composition, grain size distribution, grain-grain and grain-substrate mutual interactions. and to obtain the necessary basis for thin films engineering, many techniques have to be used to attain a deeper insight into the structure-properties relations. With this aim, an extensive study has been devoted to the characterization of CoO-and Co 3 O 4 -based films obtained by chemical vapor deposition (CVD) from a Co(II) b-diketonate, Co(dpm) 2 (Hdpm = 2,2-6,6-tetramethyl-3,5-heptanedione) by means of XRD (X-ray diffraction), optical absorption, XPS (X-ray photoelectron spectroscopy), XE-AES (X-ray excited auger electron spectroscopy) and AFM (atomic force microscopy).
9,10In this work, a SIMS investigation is described, which enabled us (i) to verify the conversion degree of the organometallic precursor under the adopted conditions; (ii) to establish the composition and homogeneity of mixed deposits; (iii) to investigate the influence of the substrate material and the preparation conditions on the composition and thickness of the interface regions; and (iv) to detect eventual impurities due to film-substrate intermixing phenomena or to an unclean decomposition pattern of the employed precursor. SIMS, in fact, is a powerful and versatile analytical tool, as often demonstrated in the characterization of several oxide thin films.
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EXPERIMENTAL
Film preparationNanocrystalline cobalt oxide thin films were deposited in a cold-wall low-pressure custom-built CVD reactor using O 2 as the carrier gas as well as the oxidizing agent. The ITO substrate (indiu...