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The problem of the optimization of properties for biocompatible coatings as functional materials requires in-depth understanding of the coating formation processes; this allows for precise manufacturing of new generation implantable devices. Plasma electrolytic oxidation (PEO) opens the possibility for the design of biomimetic surfaces for better biocompatibility of titanium materials. The pulsed bipolar PEO process of cp-Ti under voltage control was investigated using joint analysis of the surface characterization and by in situ methods of impedance spectroscopy and optical emission spectroscopy. Scanning electron microscopy, X-ray diffractometry, coating thickness, and roughness measurements were used to characterize the surface morphology evolution during the treatment for 5 min. In situ impedance spectroscopy facilitated the evaluation of the PEO process frequency response and proposed the underlying equivalent circuit where parameters were correlated with the coating layer properties. In situ optical emission spectroscopy helped to analyze the spectral line evolutions for the substrate material and electrolyte species and to justify a method to estimate the coating thickness via the relation of the spectral line intensities. As a result, the optimal treatment time was established as 2 min; this provides a 9-11 µm thick PEO coating with Ra 1 µm, 3-5% porosity, and containing 75% of anatase. The methods for in-situ spectral diagnostics of the coating thickness and roughness were justified so that the treatment time can be corrected online when the coating achieves the required properties.