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In this study, the AlCoCrFeNiTi0.2 high-entropy alloy (HEA) was plasma nitrided to investigate the microstructure and mechanical properties of high-entropy nitrides formed in the surface layer of the bulk sample. XRD measurements revealed a BCC → FCC crystal structure transformation, with the σ phase disappearing and hexagonal aluminum nitride emerging. Further experimental studies on the nitrided samples, including SEM, EDS, and EBSD, uncovered element segregation into multiple FCC phases with similar lattice constants, such as the NaCl-type (AlCrCoFeNiTi0.2)N high-entropy nitride. These observations align with theoretical analysis based on KKR-CPA calculations. Additionally, plasma nitriding induced high surface porosity; however, micropillar compression testing combined with nanoindentation revealed localized areas with significant hardness. A substantial reduction in the coefficient of friction was also observed. These findings not only provide deeper insights into the nitriding process of complex alloys, like dual-phase HEAs, but also hold promise for further exploration in the manufacturing of super-hard surfaces with high-entropy nitrides, enhancing mechanical properties for applications in harsh environments.