The influence of the substrate temperature on the structural, surface morphological, optical and nanomechanical properties of NiO films deposited on glass substrates using radio-frequency magnetron sputtering was examined by X-ray diffraction (XRD), atomic force microscopy (AFM), UV-Visible spectroscopy and nanoindentation, respectively. The results indicate that the substrate temperature exhibits significant influences on both the grain texturing orientation and surface morphology of the films. Namely, the dominant crystallographic orientation of the films switches from (111) to (200) accompanied by progressively roughening of the surface when the substrate temperature is increased from 300 °C to 500 °C. The average transmittance of the NiO films was also found to vary in the range of 60–85% in the visible wavelength region, depending on the substrate temperature and wavelength. In addition, the optical band gap calculated from the Tauc plot showed an increasing trend from 3.18 eV to 3.56 eV with increasing substrate temperature. Both the hardness and Young’s modulus of NiO films were obtained by means of the nanoindentation continuous contact stiffness measurements mode. Moreover, the contact angle between the water droplet and film surface also indicated an intimate correlation between the surface energy, hence the wettability, of the film and substrate temperature.
The evolution of iron local vibrational mode (Fe LVM) and phase transitions in n-type iron-doped indium phosphide (InP:Fe) were investigated at ambient temperature. In-situ angle-dispersive X-ray diffraction measurements revealed that InP:Fe starts to transform from zinc-blende (ZB) to rock-salt (RS) structure around 8.2(2) GPa and completes around 16.0(2) GPa. The Raman shift of both transverse and longitudinal optical modes increases monotonically with increasing pressure, while their intensities become indiscernible at 11.6(2) GPa, suggesting that the pressure-induced phase transition is accompanied by significant metallization. In contrast, originally absent at ambient pressure, the Raman shift of Fe LVM appears at ∼420 cm−1 near 1.2 GPa and exhibits a dome shape behavior with increasing pressure, reaching a maximum value of ∼440 cm−1 around 5 GPa, with an apparent kink occurring around the ZB-RS transition pressure of ∼8.5(2) GPa. The Fe K-edge X-ray absorption near edge structure (XANES) confirmed the tetrahedral site occupation of Fe3+ with a crystal field splitting parameter Δt = 38 kJ·mole−1. Our calculations indicate that the energy parameters governing the phase transition are Δt = 0.49 and Δo = 1.10 kJ·mole−1, respectively, both are much smaller than Δt = 38 kJ·mole−1 at ambient.
Hydrostatically pressurized studies using diamond anvil cells on the structural phase transition of the free-standing screw-dislocation-driven (SDD) GaSe thin film synthesized by molecular beam epitaxy have been demonstrated via in-situ angle-dispersive synchrotron X-ray diffraction and Raman spectroscopy. The early pressure-driven hexagonal-to-rock salt transition at approximately ~ 20 GPa as well as the outstandingly structural-phase memory after depressurization in the SDD-GaSe film was recognized, attributed to the screw dislocation-assisted mechanism. Note that, the reversible pressure-induced structural transition was not evidenced from the GaSe bulk, which has a layer-by-layer stacking structure. In addition, a remarkable 1.7 times higher in bulk modulus of the SDD-GaSe film in comparison to bulk counterpart was observed, which was mainly contributed by its four times higher in the incompressibility along c-axis. This is well-correlated to the slower shifting slopes of out-of-plane phonon-vibration modes in the SDD-GaSe film, especially at low-pressure range (< 5 GPa). As a final point, we recommend that the intense density of screw dislocation cores in the SDD-GaSe lattice structure plays a crucial role in these novel phenomena.
The correlations among microstructure, surface morphology, hardness, and elastic modulus of Bi2Te3 thin films deposited on c-plane sapphire substrates by pulsed laser deposition are investigated. X-ray diffraction (XRD) and transmission electron microscopy are used to characterize the microstructures of the Bi2Te3 thin films. The XRD analyses revealed that the Bi2Te3 thin films were highly (00l)-oriented and exhibited progressively improved crystallinity when the substrate temperature (TS) increased. The hardness and elastic modulus of the Bi2Te3 thin films determined by nanoindentation operated with the continuous contact stiffness measurement (CSM) mode are both substantially larger than those reported for bulk samples, albeit both decrease monotonically with increasing crystallite size and follow the Hall—Petch relation closely. Moreover, the Berkovich nanoindentation-induced crack exhibited trans-granular cracking behaviors for all films investigated. The fracture toughness was significantly higher for films deposited at the lower TS; meanwhile, the fracture energy was almost the same when the crystallite size was suppressed, which indicated a prominent role of grain boundary in governing the deformation characteristics of the present Bi2Te3 films.