Two-Step Plasma Electrolytic Oxidation of Advanced High-Strength Steel in Aluminate and Silicate Solutions

This work aims to clarify whether the individual advantages of the two commonly used silicate- and aluminate-based electrolytes for the plasma electrolytic oxidation (PEO) of steel can be combined in a two-step process. The first PEO step was carried out in an aluminate–phosphate electrolyte with pulsed voltage and anodic amplitudes between 150 V and 200 V. The second PEO step was carried out at an increased anodic voltage amplitude of 400 V in a silicate–phosphate electrolyte. As a reference, PEO was conducted in a single step in the same silicate–phosphate electrolyte at an increased anodic voltage amplitude of up to 400 V. The microstructural layer analysis was carried out using SEM and EDX analyses, Raman spectroscopy and XRD analysis. Heterogeneous layers containing iron oxide and iron phosphate form in the silicate–phosphate electrolyte at anodic voltage amplitudes up to 300 V by electrochemical reactions. Further increasing the anodic voltage amplitude up to 400 V results in heterogeneous layers, too. PEO in the aluminate–phosphate electrolyte at 150 V causes the formation of thin, amorphous layers mainly consisting of aluminum and iron oxides. At 200 V amplitude, a PEO layer with pronounced open porosity is formed, which primarily consists of the crystalline phases corundum and hercynite. During subsequent PEO in the silicate–phosphate electrolyte, the previously formed layers were replaced by a macroscopically homogeneous layer that is mostly nanocrystalline and may contain amorphous iron(-aluminum) phosphates and oxides as well as silicon oxide. It can be concluded that the two-step PEO process is suitable for the production of more homogeneous PEO layers.