Nanostructured cobalt oxide ͑Co 3 O 4 ͒ electrodes were prepared by two different methods. The first one involved the synthesis of Co 3 O 4 nanoparticles through a nanocasting route using commercial silica gel as a sacrificial template, and in the second one, the Co 3 O 4 electrodes were prepared by thermal decomposition. The electrodes were characterized by different techniques, such as scanning electron microscopy, energy-dispersive X-ray analysis ͑EDX͒, X-ray diffraction ͑XRD͒, transmission electron microscopy, X-ray photoelectron spectroscopy ͑XPS͒, and cyclic voltammetry. EDX, XRD, and XPS show a characteristic spinel-type structure and a similar chemical composition for the two nanostructured cobalt oxides. However, the surface morphology is different. The electrochemical oxidation of cyanide and phenol in alkaline medium were used as test reactions. The electrocatalytic activity of the nanocrystalline Co 3 O 4 electrodes for cyanide and phenol oxidation turned out to be highly dependent on the electrode preparation method. Conductive transition-metal oxides ͑TMOs͒ form important and diverse materials that have attracted much attention in many fields of technological interest because of their outstanding electronic, optical, magnetic, and catalytic properties.1,2 Tetragonal rutilelike TMOs containing noble-metal cations have been successfully applied as anode coatings ͓commonly known as dimensionally stable anodes ͑DSAs͔͒ in a number of important electrolytic processes, such as oxygen and chlorine evolution and the electrochemical oxidation of biorefractory organic pollutants in wastewaters.3-9 However, spinel-type cobalt oxide-based coatings have emerged as a cheaper alternative to DSA electrodes in alkaline media because they possess long-term stability under anodic conditions, good electrical conductivity, and high electrocatalytic activity toward several reactions. 2,3,[10][11][12][13][14][15][16] In addition, these materials have found use in a host of solid-state applications, such as magnetic materials, electrochromic devices, Li-ion rechargeable batteries, etc.
17-21A substantial amount of information is now available on the crystallography, structural chemistry, thermal reactivity, and surface properties of both the precursors and thermally decomposed oxide materials. However, much less attention has been paid to the morphological-and size-controlled synthesis of nanoparticles, although it has been well documented that different electrical, optical, magnetic, and mechanical properties could be reached by reducing particle dimensions to the size of 1-100 nm. [22][23][24] In spite of the lesser attention, cobalt oxide nanoparticles have been prepared by sol-gel, 18,25 reduction/oxidation route, 26 homogeneous precipitation, 27 metallorganic chemical vapor deposition, 28,29 and nanocasting approaches. 30,31 It is well known that the behavior of nanophase materials strongly depends on the shapes and sizes of the particles, which are thus a key factor in their ultimate performance and applications.Diff...