A single thin MnCr2O4 spinel layer was synthesized on a Ni-25Cr-1.5Mn alloy by a fine control of oxygen partial pressure using the Rhines pack method, a technique allowing a fine control of the oxygen partial pressure by an appropriate buffering powder mixture. The spinel was characterized using X-Ray Diffraction, Raman spectroscopy and photoelectrochemistry. The cubic spinel MnCr2O4 was formed under the oxygen partial pressure close to 5 x 10–21 atm. at 1050°C controlled by the buffering Ni-25Cr/Cr2O3 powder mixture. Raman MnCr2O4 spectrum is characterized by 5 vibrational modes whereas photoelectrochemical characterization revealed the MnCr2O4 band gap measurement at 3.7 eV with a n-type conductivity.