In the present study, the concentration series of MgAl₂O₄:Ce³⁺ ceramics have been fabricated by the Spark Plasma Sintering (SPS) method. Cerium-doping concentration was varied within a range of 0.1–5 wt.%. The prepared ceramics have been tested using the various experimental techniques: X-ray diffraction (XRD), scanning electron microscopy, as well as optical and cathodoluminescence spectroscopy. According to XRD, all synthesized samples are biphasic with structural impurities. The cerium ion concentration effect on the cathodoluminescent characteristics of MgAl₂O₄:Ce³⁺ ceramics has been studied in terms of emission intensity and decay time. Before annealing the concentration, quenching is observed. The optimal doping Ce³⁺ concentration was determined to be 5 wt.% after temperature annealing at 1300 °C. The successfully prepared spinel ceramics could be potentially applying for high-energy electrons detection.