Niobium treated by Plasma Electrolytic Oxidation with calcium and phosphorus electrolytes

Niobium plates were electrochemically treated by Plasma Electrolytic Oxidation (PEO) with electrolytes containing phosphorous and/or calcium. Three different electrolyte and experimental parameters were used forming three different surfaces. Film morphology, thickness, and chemical composition were analyzed by scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS). A profilometer and the sessile drop technique measured the average surfaces roughness (Ra) and contact angles respectively. X-ray diffraction technique (XRD) analyzed the oxide crystallinity, and scratch tests evaluated the film adhesion. All oxidized surfaces presented pores, without observed cracks. Comparing the different experimental conditions, films obtained with phosphoric acid (P100) show superficial pores, phosphorus incorporation, high hydrophilicity, non-crystalline oxide formation, and good scratch resistance. Films treated with calcium acetate electrolyte (Ca100), compared to P100 exhibit smaller size pores and film thickness, smaller hydrophilicity, and lower scratch resistance. They also demonstrated higher oxide crystallinity, calcium incorporation, and pores interconnections. When the PEO was executed with a blended electrolyte containing calcium acetate and phosphoric acid (Ca50P50) the formed films presented the highest thickness, high phosphorus incorporation, and the lowest contact angle compared with other films. In addition, the pores size, the scratch resistance, calcium incorporation, and oxide crystallinity present intermediate values compared to P100 and Ca100 films. Film crystallinity seems to be influenced by calcium incorporation, whereas, hydrophilicity is phosphorus amount dependent. The pores amount and their interconnections reduced the scratch resistance. Surface features obtained in this work are largely mentioned as positive characteristics for osseointegration processes.