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X-ray photoemission spectroscopy measurements of the Co3O4 films after growth and after annealing were carried out to assess the film stoichiometry. The XPS spectra were obtained using the Mg K¦Á line () of a double anode X-ray source and a double pass cylinder mirror analyzer (PHI 15-255G) set at a pass energy of 25 eV (energy resolution of about 0.8 eV). High resolution XPS spectra of the O 1s and Co 2p lines of the as-grown and annealed films are shown in Fig. 4. Corrections to the data include a five-point adjacent smoothing, satellite correction and correction of energy shifts due to charging (aligned with respect to the Co 2p peaks, using the energy assignments given in [32] and [33]). One observation is that the Co 2p spectra for both samples are identical, showing that no significant changes in stoichiometry or in the ionic state of the Co cations occur as a consequence of annealing. A second observation is that the Co 2p spectra are characteristic of a Co3O4 ionic environment [32] and [33] J. Haber and L. Ungier, J. Electr. Spectrosc. Relat. Phenom. 12 (1977), p. 305. Abstract | View Record in Scopus | Cited By in Scopus (27)[33], with strongly suppressed shake-up peaks compared to those of CoO [21], [30], [32], [33], [34], [35], [36] and [37]. The O 1s photoemission line is also similar before and after annealing, although some variation in the shape of the O 1s line is observed. This could be related, in some instances, to the effect of the O-plasma cleaning procedure (at room temperature) before XPS spectra collection: given the surface sensitivity of XPS, small variations in the amount of surface adsorbed O may lead to slight variations in the O 1s line; in fact, the additional peak observed at higher binding energies has been attributed to adsorbed oxygen [32], [38], [39], [40], [41], [42], [20] and [37], although surface hydroxylation, which also yields a similar peak [33] and [37], cannot be ruled out. From Surface Science Volume 603, Issue 2, 15 January 2009, Pages 291-297 |
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