The growth of titanium dioxide nanotubes (TiO2) via anodization process depends on the controlling parameters such as applied potential, anodization time, and electrolyte composition. In the present work, the Taguchi method was applied to evaluate statistically the influence of the anodization parameters on the morphology of anodized TiO2 films. Mixture of ethylene-glycol and glycerol was used as an electrolyte and the settings of the experimental design were parameterized on the basis of four important anodization factors consisting of chemical pretreatment, amount of fluoride, water content and applied potential. Samples were characterized by XRD and FEG-SEM. Based on 4 variables at 3 different settings, full factorial plan requires 34 = 81 tests. In this work the experiment was designed on the basis of an L9 (34) orthogonal array (4 variables, 3 levels, 9 tests). The optimum conditions were found on the basis of smaller-is-better and larger-is-better analyses. The signal-to-noise ratio was employed to find optimal process parameters levels and to analyze the influence of these parameters on the tubular length, internal and external diameters and formation of nanograss on the film surface. Hence, it is clearly shown that the performance of TiO2 nanotubes can be evaluated by the Taguchi method.

The evolution of TiO2 nanotubular morphology, synthesized in a mixture of fluorinated ethylene glycol and glycerol electrolyte, was studied as a function of the anodization time. The samples were characterized by FEG-SEM, XRD, XPS, UV-Vis and EIS. The formation of single-or double-walled TiO2 nanotube structure can be efficiently controlled by the anodization time. For anodization times less than 30 minutes, a compact oxide layer is formed, followed by double-walled nanotube formation up to 120 minutes and single-walled nanotubes up to 240 minutes. XPS analyses show that the samples obtained with short anodization time have a high carbon content and oxygenated surface species compared to the longer-time anodized sample; however, binding energy peaks for Ti 2p remained invariant. The performances of TiO2 nanotubular photoelectrodes were evaluated in photoelectrochemical water splitting where TiO2 nanotubes anodized for 120 minutes presented the best performance that was related to their optimal morphology and charge transportation.

La anodización de acero inoxidable ferrítico ha sido utilizada con fines decorativos, para obtener una capa de barrera. El electrólito más comúnmente utilizado para este proceso es el INCO (5M H2SO4 + 2,5M CrO3). Con adición de glicerina induce la formación de estructuras porosas ordenadas, pues la glicerina reduce la conductividad del electrólito. Se anodizaron muestras de acero inoxidable ferrítico, en electrólito de 2M H2SO4 con la adición de glicerina en diferentes concentraciones, sin adición de óxido de cromo. Se observa que la adición de glicerina en un 90 v/v % promovió la reducción de la conductividad del electrólito, lo que ocasionó un aumento del potencial de anodización. Los resultados muestran que la adición de glicerina al electrólito redujo la disolución del óxido en la solución electrolítica y promovió la formación de un óxido con una estructura porosa ordenada.

Anodizing of ferritic stainless steel has been used for decoration purposes to obtain a barrier effect. The most commonly used electrolyte for this process is INCO (5M H2SO4 + 2,5M CrO3). INCO electrolyte with glycerin addition induces the formation of ordered porous structures, because glycerin reduces the electrolyte conductivity. Ferritic stainless steel was anodized in electrolyte composed by 2M H2SO4 with glycerin addition in different concentrations, without chromium oxide addition. It was observed that the addition of 90 v/v% glycerin promoted a reduction in the electrolyte conductivity, which caused an increase in the anodizing potential. The glycerin addition to the electrolyte diminished the oxide dissolution in the electrolytic solution, promoting the formation of an oxide with an ordered porous structure.