Electrochemical Synthesis of Crystalline Niobium Oxide

Features of creation of porous nanostructured oxides of transition materials on an example of niobium are considered. It has been experimentally shown that variation in anodizing modes makes it possible to obtain non-porous and porous amorphous anodic oxide films (AOF) and films of the crystalline type. It is determined that the process of AOF formation on niobium, as well as its structure and properties depend on such parameters as the type of electrolyte, anodizing voltage, activator concentration, the duration of the process. It is confirmed that the presence of an activator in the electrolyte is a necessary and decisive factor in the process of forming a nanostructured anode oxide layer. To obtain a nanostructured surface of niobium oxide, a necessary condition is the introduction of fluoride into the electrolyte, but also an important task is to determine the type of compound with which F– ions are introduced into the electrolyte. It has been experimentally determined that the optimal solution for the rapid growth of porous crystalline oxide is a solution consisting of a background electrolyte in the form of 1M H2SO4 with the addition of a fluoride ion activator in the form of 0.5M NaF. The increase in the activator accelerates the formation of the crystal structure on the surface of niobium. It is shown that higher voltage and longer anodizing time leads to an increase in the size of microcones and their number on the surface of niobium. Optimal for the formation of porous crystalline oxide is a voltage of 60 V in the electrolyte 1M H2SO4 + 0.5M NaF for 2 hours.