Abstract
Molybdenum-containing films electrochemically deposited from an aqueous solution of 12-molybdphosphate (PMo12O40)3− (denoted as PMo12) have been characterized by x-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR), and electron spin resonance (ESR) techniques. XPS and FTIR data indicate that electrolysis of PMo12 leads to the formation of Mo–O–Mo linkage by condensation of the polyanions accompanied by decomposition of the phosphate moiety. The ESR spectrum of the deposited film exhibits an asymmetric signal with g ∼1.92, indicative of pentavalent molybdenum (d1). The feature of this signal is close to that for a MoV ion in the amorphous MoO3 phase, but not in the PMo12 framework. It is therefore suggested that the deposited film no longer has the Keggin structure PMo12, but consists of a continuous structure containing molybdenum oxide.
Similar content being viewed by others
References
D.E. Katsoulis, Chem. Rev. 98, 359 (1998).
E. Itabashi, Bull. Chem. Soc. Jpn. 60, 1333 (1987).
M.T. Pope, in Heteropoly and Isopoly Oxometalates (Springer-Verlag, Berlin, Germany 1983).
M. Sadakane and E. Steckhan, Chem. Rev. 98, 219 (1998).
K. Reybier, J-P. Malugani, S. Fantini, M. Herlem, and B. Fahys, J. Electrochem. Soc. 149, E96 (2002).
B. Keita, L. Nadjo, and R. Contant, J. Electroanal. Chem. 443, 168 (1998).
B. Keita, E. Abdeljali, F.G. Sophie, L. Nadjo, R. Contant, and C. Haut, J. Solid State Electrochem. 3, 446 (1999).
G.D. Wilcox, D.R. Gabe, and M.E. Warwick, Corros. Sci. 28, 577 (1988).
S. Dong and B. Wang, J. Electroanal. Chem. 370, 141 (1990).
A. Guerfi, R.W. Paynter, and Le H. Dao, J. Electrochem. Soc. 142, 3457 (1995).
M. Nakayama, C. Matsushima, and K. Ogura, J. Electroanal. Chem. 536, 47 (2002).
I.G. Casella and M. Gatta, Anal. Chem. 72, 2969 (2000).
C. Rocchiccioli-Deltcheff, R. Thouvenot, and R. Franck, Spectrochim. Acta A 32, 578 (1976).
O.K. Srivastava and E.A. Secco, Can. J. Chem. 45, 585 (1967).
S.K. Deb and J.A. Chopoorian, J. Appl. Phys. 37, 4818 (1966).
R. Fricke and G. Ohlman, J. Chem. Soc., Faraday Trans. 1 82, 263 (1986).
A. Balas, J. Kliava, and J. Purans, J. Phys. C, Solid State Phys. 13, L437 (1980).
J.C. Vedrine, in Characterization of Heterogeneous Catalysts, edited by F. Delannay (Dekker, New York, 1984), p. 161.
S. Peulon and D. Lincot, Adv. Mater. 8, 166 (1996).
U. Opara Krašovec, A. Šurca Vuk, and B. Orel, Electrochim. Acta 46, 1921 (2001).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Nakayama, M., Ii, T. & Ogura, K. Spectrosopic and paramagnetic properties of molybdenum oxyhydroxide films electrochemically formed from the Keggin-type (PMo12O40)3− complex. Journal of Materials Research 18, 2509–2514 (2003). https://doi.org/10.1557/JMR.2003.0349
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/JMR.2003.0349