Nitrogen-doped TiO2 nanotube arrays (N-TNAs) were successfully fabricated by a simple thermal annealing process in ambient N2 gas at 450 °C for 3 h. TNAs with modified morphologies were prepared by a two-step anodization using an aqueous NH4F/ethylene glycol solution. The N-doping concentration (0–9.47 at %) can be varied by controlling N2 gas flow rates between 0 and 500 cc/min during the annealing process. Photocatalytic performance of as-prepared TNAs and N-TNAs was studied by monitoring the methylene blue degradation under visible light (λ ≥ 400 nm) illumination at 120 mW·cm−2. N-TNAs exhibited appreciably enhanced photocatalytic activity as compared to TNAs. The reaction rate constant for N-TNAs (9.47 at % N) reached 0.26 h−1, which was a 125% improvement over that of TNAs (0.115 h−1). The significant enhanced photocatalytic activity of N-TNAs over TNAs is attributed to the synergistic effects of (1) a reduced band gap associated with the introduction of N-doping states to serve as carrier reservoir, and (2) a reduced electron‒hole recombination rate.
Fluorine-doped tin oxide (FTO) thin films were deposited on glass substrates using ultrasonic spray pyrolysis (USP) at a fixed substrate temperature of 400 °C and various Fluorine/Tin (F/Sn) atomic ratios of 0, 0.1, 0.5, and 1.0. Effects of F/Sn atomic ratios on structural-morphological, compositional, electrical, optical, and nanomechanical properties of the FTO thin films were systematically studied. The FTO films exhibited a tetragonal structure with preferred orientations of (110), (200), and (211), and polycrystalline morphology with spear-like or coconut shell-like particles on the surfaces. The presence of F-doping was confirmed by XPS results with clear F1s peaks, and F-concentration was determined to be 0.7% for F/Sn = 0.1 and 5.1% for F/Sn = 0.5. Moreover, the resistivity of FTO films reduced remarkably from 4.1 mΩcm at F/Sn = 0 to 0.7 mΩcm at F/Sn = 1, primarily due to the corresponding increase of carrier concentration from 2 × 1020 cm−3 to 1.2 × 1021 cm−3. The average optical transmittance of the films prepared at F/Sn of 0–0.5 was over 90%, and it decreased to 84.4% for the film prepared at F/Sn = 1. The hardness (H) and Young’s modulus (E) of the FTO films increased when the F/Sn ratios increased from 0 to 0.5, reaching maximum values of H = 12.3 ± 0.4 GPa, E = 131.7 ± 8.0 GPa at F/Sn = 0.5. Meanwhile, the H and E reduced considerably when the F/Sn ratio further increased to 1.0, following the inverse Hall-Petch effect approximately, suggesting that the grain boundary effect played a primary role in manipulating the nanomechanical properties of the FTO films. Furthermore, favorable mechanical properties with large H/Ef and H 3 / E f 2 ratios were found for the FTO film prepared at F/Sn = 0.5, which possessed high crystallinity, large grain size, and compact morphology.
The nanomechanical properties and nanoindentation responses of bismuth selenide (Bi2Se3) thin films are investigated in this study. The Bi2Se3 thin films are deposited on c-plane sapphire substrates using pulsed laser deposition. The microstructural properties of Bi2Se3 thin films are analyzed by means of X-ray diffraction (XRD). The XRD results indicated that Bi2Se3 thin films are exhibited the hexagonal crystal structure with a c-axis preferred growth orientation. Nanoindentation results showed the multiple “pop-ins” displayed in the loading segments of the load-displacement curves, suggesting that the deformation mechanisms in the hexagonal-structured Bi2Se3 films might have been governed by the nucleation and propagation of dislocations. Further, an energetic estimation of nanoindentation-induced dislocation associated with the observed pop-in effects was made using the classical dislocation theory.
In the present study, the structural, morphological, compositional, nanomechanical, and surface wetting properties of Bi2Se3 thin films prepared using a stoichiometric Bi2Se3 target and a Se-rich Bi2Se5 target are investigated. The Bi2Se3 films were grown on InP(111) substrates by using pulsed laser deposition. X-ray diffraction results revealed that all the as-grown thin films exhibited were highly c-axis-oriented Bi2Se3 phase with slight shift in diffraction angles, presumably due to slight stoichiometry changes. The energy dispersive X-ray spectroscopy analyses indicated that the Se-rich target gives rise to a nearly stoichiometric Bi2Se3 films, while the stoichiometric target only resulted in Se-deficient and Bi-rich films. Atomic force microscopy images showed that the films’ surfaces mainly consist of triangular pyramids with step-and-terrace structures with average roughness, Ra, being ~2.41 nm and ~1.65 nm for films grown with Bi2Se3 and Bi2Se5 targets, respectively. The hardness (Young’s modulus) of the Bi2Se3 thin films grown from the Bi2Se3 and Bi2Se5 targets were 5.4 GPa (110.2 GPa) and 10.3 GPa (186.5 GPa), respectively. The contact angle measurements of water droplets gave the results that the contact angle (surface energy) of the Bi2Se3 films obtained from the Bi2Se3 and Bi2Se5 targets were 80° (21.4 mJ/m2) and 110° (11.9 mJ/m2), respectively.
In this study, TiO2 nanowires on TiO2 nanotubes arrays (TNWs/TNAs) and Au-decorated TNWs/TNAs nanostructures are designed and fabricated as a new type of photoanode for photoelectrochemical (PEC) water splitting. The TNWs/TNAs were fabricated on Ti folds by anodization using an aqueous NH4F/ethylene glycol solution, while Au nanoparticles (NPs) and Au nanorods (NRs) were synthesized by Turkevich methods. We studied the crystal structure, morphology, and PEC activity of four types of nanomaterial photoanodes, including TNWs/TNAs, Au NPs- TNWs/TNAs, Au NRs-TNWs/TNAs, and Au NPs-NRs-TNWs/TNAs. The TiO2 and Au-TiO2 samples exhibited pure anatase phase of TiO2 with (0 0 4), (1 0 1), and (1 0 5) preferred orientations, while Au-TiO2 presented a tiny XRD peak of Au (111) due to a small Au decorated content of 0.7 ± 0.2 at.%. In addition, the samples obtained a well-defined and uniformed structure of TNAs/TNWs; Au NPs (size of 19.0 ± 1.9 nm) and Au NRs (width of 14.8 ± 1.3 nm and length of 99.8 ± 15.1 nm) were primarily deposited on TNWs top layer; sharp Au/TiO2 interfaces were observed from HRTEM images. The photocurrent density (J) of the photoanode nanomaterials was in the range of 0.24–0.4 mA/cm2. Specifically, Au NPs-NRs- decorated TNWs/TNAs attained the highest J value of 0.4 mA/cm2 because the decoration of Au NPs and Au NRs mixture onto TNWs/TNAs improved the light harvesting capability and the light absorption in the visible-infrared region, enhanced photogenerated carriers’ density, and increased electrons’ injection efficiency via the localized surface plasmon resonance (LSPR) effect occurring at the Au nanostructures. Furthermore, amongst the investigated nanophotocatalysts, the Au NPs-NRs TNWs/TNAs exhibited the highest photocatalytic activity in the degradation of methylene blue with a high reaction rate constant of 0.7 ± 0.07 h−1, which was 2.5 times higher than that of the pristine TNWs/TNAs.
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