High-flux low-energy (≂20 eV) N+2 ion irradiation during TiN deposition by reactive magnetron sputtering: Effects on microstructure and preferred orientation

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Abstract
The effects of the incident ion/metal flux ratio (1≤Ji /JTi≤15), with the N+2 ion energy Ei constant at ≂20 eV (≂10 eV per incident accelerated N), on the microstructure, texture, and stoichiometry of polycrystalline TiN films grown by ultrahigh‐vacuum reactive‐magnetron sputtering have been investigated. The layers were deposited in pure N2 discharges on thermally oxidized Si(001) substrates at 350 °C. All films were slightly overstoichiometric with a N/Ti ratio of 1.02±0.03 and a lattice constant of 0.4240±0.0005 nm, equal to that of unstrained bulk TiN. Films deposited with Ji/JTi=1 initially exhibit a mixed texture—predominately (111), (002), and (022)—with competitive columnar growth which slowly evolves into a pure (111) texture containing a network of both inter‐ and intracolumn porosity with an average column size of ≂50 nm at t=1.6 μm. In contrast, films grown with Ji/JTi≥5 do not exhibit competitive growth. While still columnar, the layers are dense with an essentially complete (002) preferred orientation and an average column size of ≂55 nm from the earliest observable stages. The normalized x‐ray diffraction (002) intensity ratio in thick layers increased from ≂0 to 1 as Ji/JTi was varied from 1 to ≥5. Both 111 and 001 interplanar spacings remained constant as a function of film thickness for all Ji/JTi. Thus, contrary to previous models, strain is not the dominant factor in controlling the development of preferred orientation in these films. Moreover, once film texture is fully evolved—whether it be (002) or (111)—during deposition, changing Ji/JTi has little effect as preferred orientation becomes controlled by pseudomorphic forces. Film porosity, however, can be abruptly and reversibly switched by increasing or decreasing Ji/JTi.