Defects in nanocrystalline Nb films: Effect of sputtering temperature

Thin niobium (Nb) films (thickness 350-400 nm) were prepared on (1 0 0)Si substrate in a UHV chamber using the cathode beam sputtering. The sputtering temperature T_s was varied from 40 up to 500 °C and the influence of the sputtering temperature on the microstructure of thin Nb films was investigated. Defect studies of the thin Nb films sputtered at various temperatures were performed by slow positron implantation spectroscopy (SPIS) with measurement of the Doppler broadening of the annihilation line. SPIS was combined with transmission electron microscopy (TEM) and X-ray diffraction (XRD). We have found that the films sputtered at T_s = 40 °C exhibit elongated, column-like nanocrystalline grains. No significant increase of grain size with T_s (up to 500 °C) was observed by TEM. The thin Nb films sputtered at T_s = 40 °C contain a high density of defects. It is demonstrated by shortened positron diffusion length and a high value of the S parameter for Nb layer compared to the well-annealed (defect-free) bulk Nb reference sample. A drastic decrease of defect density was found in the films sputtered at T_s ≥ 300 °C. It is reflected by a significant increase of the positron diffusion length and a decrease of the S parameter for the Nb layer. The defect density in the Nb layer is, however, still substantially higher than in the well-annealed reference bulk Nb sample. Moreover, there is a layer at the interface between the Nb film and the substrate with very high density of defects comparable to that in the films sputtered at T_s < 300 °C. All the Nb films studied exhibit a strong (1 1 0) texture. The films sputtered at T_s < 300 °C are characterized by a compressive macroscopic in-plane stress due to lattice mismatch between the film and the substrate. Relaxation of the in-plane stress was observed in the films sputtered at T_s ≥ 300 °C. The width of the XRD profiles of the films sputtered at T_s ≥ 300 °C is significantly smaller compared to the films sputtered at lower temperatures. This is most probably due to a lower defect density which results in reduced microstrains in the films sputtered at higher temperatures.