Characterization of nitride coatings on high density graphite deposited by magnetron sputtering

Cathode deposit consolidation operation after electrorefining of spent metallic fuels of fast breeder reactors involves melting of U and Pu at 1300 °C after distillation of occluded chloride salt and Cd, in graphite crucibles. Nitride coatings possessing high hardness, melting point and thermodynamic stability against reactive materials and molten LiCl–KCl salts have greater potential for coating the graphite crucibles. In the present study nanocrystalline TiN, ZrN and Ti–Si–N coatings were deposited on high density graphite disc and crucible samples by DC/RF magnetron sputtering. The coated samples were characterized by SEM, GIXRD and AFM. The results indicated that coatings with uniform thickness of 3 to 6 µm were deposited on high density graphite which adheres well to the substrate. The surface morphology of TiN, ZrN and Ti–Si–N coatings examined by SEM and AFM showed the presence of spherical nanoparticles of nitrides getting agglomerated into clusters. Characterisation of nitride coated crucibles was carried out before and after uranium melting by induction heating to simulate cathode processor crucible conditions. TiN and Ti–Si–N coating appears to offer better stability, ease of ingot release and coating adhesion. The paper highlights the results of the present investigation.