This work shows an approach on the role of the gas mixture used in the pulsed DC plasma nitriding aiming to enhance the niobium cavitation erosion resistance through the formation of niobium nitride on the treated surfaces. For this purpose, nitriding was carried out at 1353 K (1080 °C) for 2 h, under a pressure of 1.2 kPa (9 Torr), and a 5 × 10
−6 Nm
3s
−1 (300 sccm) flow rate for three distinct gas mixtures, namely 30% N
2 + 50% H
2 + 20% Ar, 50% N
2 + 30% H
2 + 20% Ar, and 70% N
2 + 10% H
2 + 20% Ar. Surfaces were comparatively characterized before and after nitriding through scanning electron microscopy (SEM), X-ray diffractometry, 3D roughness, and nanoindentation hardness measurements. The cavitation erosion test was carried out in accordance with ASTM G32-09, obtaining the cumulative mass loss (CML) curve and the average (AER) and maximum (MER) erosion rate of the tested surfaces. Surfaces showed multiphase layers mainly constituted of ε-NbN and β-Nb
2N nitride phases, for the three distinct gas mixture conditions investigated. A CML of 25.0, 20.2, and 34.6 mg, and an AER of 1.56, 1.27, and 2.16 mg h
−1 was determined to the 960 min (16 h) cavitation erosion testing time, for NbN surfaces obtained at the 30% N
2, 50% N
2, and 70% N
2 gas mixture, respectively. In this case, the nominal incubation period (NIP) was 600, 650, 550 min, and the maximum erosion rate (MER) was 4.2, 3.4, and 5.1 mg h
−1, respectively. Finally, the enhancement of the cavitation erosion resistance, based on the NIP of the NbN surfaces, regarding the Nb substrates (with NIP of ≈100 min), was up ≈6 times, on average, thus significantly improving the cavitation erosion resistance of the niobium.
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