Formation of crack-free nanoporous tin oxide layers via simple one-step anodic oxidation in NaOH at low applied voltages

A simple anodic oxidation of metallic tin in fluoride-free alkaline electrolyte at low potentials was proposed as a new and effective strategy for fabrication of crack-free nanoporous tin oxide layers. A low-purity Sn foil (98.8%) was used as a starting material, and a series of anodizations were performed in 1 M NaOH at different conditions such as anodizing potential, and duration of the process. It was proved for the first time that nanostructured tin oxides with ultra-small nanochannels having diameters of <15 nm can be synthesized by simple anodization of metallic tin at a potential of 2 V in 1 M NaOH electrolyte. Increasing anodizing potential to 3 and 4 V allowed for formation of tin oxide layers with much larger pores (40-50 nm in diameter) which were still free from internal cracks and transversal pores. Applying such low potentials significantly reduces the oxide growth rate and suppresses vigorous oxygen evolution at the anode. As a result mechanical deterioration of the oxide structure is prevented while strongly alkaline electrolyte is responsible for formation of the porous layer with completely open pores even at such low potentials. On the contrary, when anodization was carried out at potentials of 5 and 6 V, much faster formation of anodic layer, accompanied by vigorous oxygen gas formation, was observed. In consequence, as grown oxide layers exhibited typical cracked or even stacked internal structure. Finally, we demonstrated for the first time that nanoporous tin oxide layers with segments of different channel sizes can be successfully obtained by simple altering potential during anodization.