Synthesis of metallic mixed 3R and 2H Nb_{1+: X} S₂nanoflakes by chemical vapor deposition

In this work, we report the synthesis and characterization of mixed phase Nb1+xS2 nanoflakes prepared by chemical vapor deposition. The as-grown samples show a high density of flakes (thickness ∼50 nm) that form a continuous film. Raman and X-ray diffraction data show that the samples consist of both 2H and 3R phases, with the 2H phase containing a high concentration of Nb interstitials. These Nb interstitials sit in between the NbS2 layers to form Nb1+xS2. Cross-sectional Energy Dispersive Spectroscopy analysis with transmission electron microscopy suggests that the 2H Nb1+xS2 region is found in thinner flakes, while 3R NbS2 is observed in thicker regions of the films. The evolution of the phase from 2H Nb1+xS2 to 3R NbS2 may be attributed to the change of the growth environment from Nb-rich at the start of the growth to sulfur-rich at the latter stage. It was also found that the incorporation of Nb interstitials is highly dependent on the temperature of the NbCl5 precursor and the position of the substrate in the furnace. Samples grown at high NbCl5 temperature and with substrate located closer to the NbCl5 source show higher incorporation of Nb interstitials. Electrical measurements show linear I-V characteristics, indicating the metallic nature of the Nb1+xS2 film with relatively low resistivity of 4.1 × 10-3 Ω cm.