Low-energy (∼100 eV) ion irradiation during growth of TiN deposited by reactive magnetron sputtering: Effects of ion flux on film microstructure

Cross-sectional transmission electron microscopy (XTEM) has been used to investigate the effects of variations in the low-energy ion irradiation flux during the growth of reactively sputter-deposited TiN. The films were deposited on steel substrates with a negative bias of 100 V at 350 °C in mixed Ar–N2 discharges at a pressure of 5 Pa (37 mTorr). The ion-to-Ti arrival rate ratio Jion /JTi at the substrate was varied between 0.3 and 7.1 through the use of a variable external magnetic field. Films grown with Jion /JTi ≲2 had a columnar morphology with a highly underdense microstructure. Increasing Jion /JTi ≳4 was sufficient to cause the growth of dense films with a more equiaxed grain structure due to renucleation. Further increases in Jion /JTi ≳7 resulted in increased TiN grain size and local heteroepitaxy between TiN and the martensitic phase of the substrate.