Facile Preparation Method of TiO2/Activated Carbon for Photocatalytic Degradation of Methylene Blue.

The development of nanocomposite photocatalysts with high photocatalytic activity, cost-effectiveness, a simple preparation process, and scalability for practical applications is of great interest. In this study, nanocomposites of TiO2 Degussa P25 nanoparticles/activated carbon (TiO2/AC) were prepared at various mass ratios of (4:1), (3:2), (2:3), and (1:4) by a facile process involving manual mechanical pounding, ultrasonic-assisted mixing in an ethanol solution, paper filtration, and mild thermal annealing. The characterization methods included XRD, SEM-EDS, Raman, FTIR, XPS, and UV-Vis spectroscopies. The effects of TiO2/AC mass ratios on the structural, morphological, and photocatalytic properties were systematically studied in comparison with bare TiO2 and bare AC. TiO2 nanoparticles exhibited dominant anatase and minor rutile phases and a crystallite size of approximately 21 nm, while AC had XRD peaks of graphite and carbon and a crystallite size of 49 nm. The composites exhibited tight decoration of TiO2 nanoparticles on micron-/submicron AC particles, and uniform TiO2/AC composites were obtained, as evidenced by the uniform distribution of Ti, O, and C in an EDS mapping. Moreover, Raman spectra show the typical vibration modes of anatase TiO2 (e.g., E1g(1), B1g(1), Eg(3)) and carbon materials with D and G bands. The TiO2/AC with (4:1), (3:2), and (2:3) possessed higher reaction rate constants (k) in photocatalytic degradation of methylene blue (MB) than that of either TiO2 or AC. Among the investigated materials, TiO2/AC = 4:1 achieved the highest photocatalytic activity with a high k of 55.2 × 10-3 min-1 and an MB removal efficiency of 96.6% after 30 min of treatment under UV-Vis irradiation (120 mW/cm2). The enhanced photocatalytic activity for TiO2/AC is due to the synergistic effect of the high adsorption capability of AC and the high photocatalytic activity of TiO2. Furthermore, TiO2/AC promotes the separation of photoexcited electron/hole (e-/h+) pairs to reduce their recombination rate and thus enhance photocatalytic activity. The optimal TiO2/AC composite with a mass ratio of 4/1 is suggested for treating industrial or household wastewater with organic pollutants.

Effects of Oxygen Pressure on the Microstructures and Nanomechanical Properties of Samarium-Doped BiFeO3 Thin Films.

In this study, samarium (Sm-10at%)-doped BiFeO3 (SmBFO) thin films were grown on platinum-coated glass substrates using pulsed laser deposition (PLD) to unveil the correlation between the microstructures and nanomechanical properties of the films. The PLD-derived SmBFO thin films were prepared under various oxygen partial pressures (PO2) of 10, 30, and 50 mTorr at a substrate temperature of 600 °C. The scanning electron microscopy analyses revealed a surface morphology consisting of densely packed grains, although the size distribution varied with the PO2. X-ray diffraction results indicate that all SmBFO thin films are textured and preferentially oriented along the (110) crystallographic orientation. The crystallite sizes of the obtained SmBFO thin films calculated from the Scherrer and (Williamson-Hall) equations increased from 20 (33) nm to 25 (52) nm with increasing PO2. In addition, the nanomechanical properties (the hardness and Young's modulus) of the SmBFO thin films were measured by using nanoindentation. The relationship between the hardness and crystalline size of SmBFO thin films appears to closely follow the Hall-Petch equation. In addition, the PO2 dependence of the film microstructure, the crystallite size, the hardness, and Young's modulus of SmBFO thin films are discussed.

The Microstructures and Characteristics of NiO Films: Effects of Substrate Temperature.

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.

Influence of Post-Annealing on the Structural and Nanomechanical Properties of Co Thin Films.

The correlations between the microstructure and nanomechanical properties of a series of thermal annealed Co thin films were investigated. The Co thin films were deposited on glass substrates using a magnetron sputtering system at ambient conditions followed by subsequent annealing conducted at various temperatures ranging from 300 C to 800 C. The XRD results indicated that for annealing temperature in the ranged from 300 C to 500 C, the Co thin films were of single hexagonal close-packed (hcp) phase. Nevertheless, the coexistence of hcp-Co (002) and face-centered cubic (fcc-Co (111)) phases was evidently observed for films annealed at 600 C. Further increasing the annealing temperature to 700 C and 800 C, the films evidently turned into fcc-Co (111). Moreover, significant variations in the hardness and Young's modulus are observed by continuous stiffness nanoindentation measurement for films annealed at different temperatures. The correlations between structures and properties are discussed.

The Indentation-Induced Pop-in Phenomenon and Fracture Behaviors of GaP(100) Single-Crystal.

The deformation behaviors and fracture features of GaP(100) single-crystal are investigated by using nano- and micro-scale indentation techniques. The hardness and Young's modulus were measured by nanoindentation using a Berkovich diamond indenter with continuous contact stiffness measurements (CSM) mode and the values obtained were 12.5 ± 1.2 GPa and 152.6 ± 12.8 GPa, respectively. In addition, the characteristic "pop-in" was observed in the loading portion of load-displacement curve, which was caused by the nucleation and/or propagation of dislocations. An energetic estimation methodology on the associated nanoindentation-induced dislocation numbers resulting from the pop-in events was discussed. Furthermore, the Vickers indentation induced fracture patterns of GaP(100) single-crystal were observed and analyzed using optical microscopy. The obtained fracture toughness KC of GaP(100) single-crystal was ~1.7 ± 0.1 MPa·m1/2, which is substantially higher than the KIC values of 0.8 MPa·m1/2 and 1.0 MPa·m1/2 previously reported for of single-crystal and polycrystalline GaP, respectively.

Nanomechanical and Material Properties of Fluorine-Doped Tin Oxide Thin Films Prepared by Ultrasonic Spray Pyrolysis: Effects of F-Doping.

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.

Localized Deformation and Fracture Behaviors in InP Single Crystals by Indentation.

The indentation-induced deformation mechanisms in InP(100) single crystals were investigated by using nanoindentation and cross-sectional transmission electron microscopy (XTEM) techniques. The results indicated that there were multiple "pop-in" events randomly distributed in the loading curves, which were conceived to arise primarily from the dislocation nucleation and propagation activities. An energetic estimation on the number of nanoindentation-induced dislocations associated with pop-in effects is discussed. Furthermore, the fracture patterns were performed by Vickers indentation. The fracture toughness and the fracture energy of InP(100) single crystals were calculated to be around 1.2 MPa·m1/2 and 14.1 J/m², respectively.

Nanoindentation of Bi2Se3 Thin Films.

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.

The High Temperature Tensile and Creep Behaviors of High Entropy Superalloy.

This article presents the high temperature tensile and creep behaviors of a novel high entropy alloy (HEA). The microstructure of this HEA resembles that of advanced superalloys with a high entropy FCC matrix and L12 ordered precipitates, so it is also named as "high entropy superalloy (HESA)". The tensile yield strengths of HESA surpass those of the reported HEAs from room temperature to elevated temperatures; furthermore, its creep resistance at 982 °C can be compared to those of some Ni-based superalloys. Analysis on experimental results indicate that HESA could be strengthened by the low stacking-fault energy of the matrix, high anti-phase boundary energy of the strengthening precipitate, and thermally stable microstructure. Positive misfit between FCC matrix and precipitate has yielded parallel raft microstructure during creep at 982 °C, and the creep curves of HESA were dominated by tertiary creep behavior. To the best of authors' knowledge, this article is the first to present the elevated temperature tensile creep study on full scale specimens of a high entropy alloy, and the potential of HESA for high temperature structural application is discussed.

Reduction of Photoluminescence Quenching by Deuteration of Ytterbium-Doped Amorphous Carbon-Based Photonic Materials.

In situ Yb-doped amorphous carbon thin films were grown on Si substrates at low temperatures (<200 °C) by a simple one-step RF-PEMOCVD system as a potential photonic material for direct integration with Si CMOS back end-of-line processing. Room temperature photoluminescence around 1 µm was observed via direct incorporation of optically active Yb3+ ions from the selected Yb(fod)3 metal-organic compound. The partially fluorinated Yb(fod)3 compound assists the suppression of photoluminescence quenching by substitution of C-H with C-F bonds. A four-fold enhancement of Yb photoluminescence was demonstrated via deuteration of the a-C host. The substrate temperature greatly influences the relative deposition rate of the plasma dissociated metal-organic species, and hence the concentration of the various elements. Yb and F incorporation are promoted at lower substrate temperatures, and suppressed at higher substrate temperatures. O concentration is slightly elevated at higher substrate temperatures. Photoluminescence was limited by the concentration of Yb within the film, the concentration of Yb ions in the +3 state, and the relative amount of quenching due to the various de-excitation pathways associated with the vibrational modes of the host a-C network. The observed wide full-width-at-half-maximum photoluminescence signal is a result of the variety of local bonding environments due to the a-C matrix, and the bonding of the Yb3+ ions to O and/or F ions as observed in the X-ray photoelectron spectroscopy analyses.

Erbium-Doped Amorphous Carbon-Based Thin Films: A Photonic Material Prepared by Low-Temperature RF-PEMOCVD.

The integration of photonic materials into CMOS processing involves the use of new materials. A simple one-step metal-organic radio frequency plasma enhanced chemical vapor deposition system (RF-PEMOCVD) was deployed to grow erbium-doped amorphous carbon thin films (a-C:(Er)) on Si substrates at low temperatures (<200 °C). A partially fluorinated metal-organic compound, tris(6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5- octanedionate) Erbium(+III) or abbreviated Er(fod)3, was incorporated in situ into a-C based host. Six-fold enhancement of Er room-temperature photoluminescence at 1.54 µm was demonstrated by deuteration of the a-C host. Furthermore, the effect of RF power and substrate temperature on the photoluminescence of a-C:D(Er) films was investigated and analyzed in terms of the film structure. Photoluminescence signal increases with increasing RF power, which is the result of an increase in [O]/[Er] ratio and the respective erbium-oxygen coordination number. Moreover, photoluminescence intensity decreases with increasing substrate temperature, which is attributed to an increased desorption rate or a lower sticking coefficient of the fluorinated fragments during film growth and hence [Er] decreases. In addition, it is observed that Er concentration quenching begins at ~2.2 at% and continues to increase until 5.5 at% in the studied a-C:D(Er) matrix. This technique provides the capability of doping Er in a vertically uniform profile.

Structural and nanomechanical properties of BiFeO3 thin films deposited by radio frequency magnetron sputtering.

The nanomechanical properties of BiFeO3 (BFO) thin films are subjected to nanoindentation evaluation. BFO thin films are grown on the Pt/Ti/SiO2/Si substrates by using radio frequency magnetron sputtering with various deposition temperatures. The structure was analyzed by X-ray diffraction, and the results confirmed the presence of BFO phases. Atomic force microscopy revealed that the average film surface roughness increased with increasing of the deposition temperature. A Berkovich nanoindenter operated with the continuous contact stiffness measurement option indicated that the hardness decreases from 10.6 to 6.8 GPa for films deposited at 350°C and 450°C, respectively. In contrast, Young's modulus for the former is 170.8 GPa as compared to a value of 131.4 GPa for the latter. The relationship between the hardness and film grain size appears to follow closely with the Hall-Petch equation.

Dislocation Energetics and Pop-Ins in AlN Thin Films by Berkovich Nanoindentation.

Nanoindentation-induced multiple pop-ins were observed in the load-displacement curves when the mechanical responses of AlN films grown on c-plane sapphire substrates were investigated by using Berkovich indenters. No evidence of phase transformation is revealed by cross-sectional transmission electron microscopy (XTEM) and selected area diffraction (SAD) analyses. Instead XTEM observations suggest that these "instabilities" resulted from the sudden nucleation of dislocations propagating along the slip systems lying on the {0001} basal planes and the pyramidal planes commonly observed in hexagonal compound semiconductors. Based on this scenario, an energetic estimation of dislocation nucleation is made.

Mechanical Properties of Cu2O Thin Films by Nanoindentation.

In this study, the structural and nanomechanical properties of Cu2O thin films are investigated by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM) and nanoindentation techniques. The Cu2O thin films are deposited on the glass substrates with the various growth temperatures of 150, 250 and 350 °C by using radio frequency magnetron sputtering. The XRD results show that Cu2O thin films are predominant (111)-oriented, indicating a well ordered microstructure. In addition, the hardness and Young's modulus of Cu2O thin films are measured by using a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. Results indicated that the hardness and Young's modulus of Cu2O thin films decreased as the growth temperature increased from 150 to 350 °C. Furthermore, the relationship between the hardness and films grain size appears to closely follow the Hall-Petch equation.

Fabrication of cone-shaped CNF/SiC-coated Si-nanocone composite structures and their excellent field emission performance.

Novel cone-shaped carbon nanofiber (CNF)/silicon carbide (SiC)-coated Si-nanocone (Si-NC) composite structures with excellent field emission (FE) performance have been fabricated by a simple microwave plasma chemical vapour deposition process. Transmission electron microscopy analyses reveal that the newly developed cone-shaped composite structures are composed of bamboo-like herringbone CNFs grown vertically on the tips of conical SiC layers with a flat-top Si cone embedded underneath. For this CNF/SiC-coated Si-NC composite array, a ultra-low threshold field of 0.32 V µm(-1) (at 10 mA cm(-2)), a large emission current density of 668 mA cm(-2) at 1.05 V µm(-1), and a field enhancement factor as high as ~48,349 are obtained. In addition, the FE lifetime test performed at a large emission current density of 200 mA cm(-2) under an applied field of 1 V µm(-1) shows no discernible decay during a period of over 260 minutes. We deduce that this superior FE performance can be attributed to the specific bamboo-like herringbone CNFs with numerous open graphitic edges and a faceted top end, and the conical base SiC/Si structures with sufficient adhesion to the substrate surface. Such a novel structure with promising emission characteristics makes it a potential material for electron field emitters.

Nanoindentation of GaSe thin films.

The structural and nanomechanical properties of GaSe thin films were investigated by means of X-ray diffraction (XRD) and nanoindentation techniques. The GaSe thin films were deposited on Si(111) substrates by pulsed laser deposition. XRD patterns reveal only the pure (000 l)-oriented reflections originating from the hexagonal GaSe phase and no trace of any impurity or additional phases. Nanoindentation results exhibit discontinuities (so-called multiple 'pop-in' events) in the loading segments of the load-displacement curves, and the continuous stiffness measurements indicate that the hardness and Young's modulus of the hexagonal GaSe films are 1.8 ± 0.2 and 65.8 ± 5.6 GPa, respectively.

Deep-UV sensors based on SAW oscillators using low-temperature-grown AlN films on sapphires.

High-quality epitaxial AlN films were deposited on sapphire substrates at low growth temperature using a helicon sputtering system. SAW filters fabricated on the AlN films exhibited excellent characteristics, with center frequency of 354.2 MHz, which corresponds to a phase velocity of 5667 m/s. An oscillator fabricated using AlN-based SAW devices is presented and applied to deep-UV light detection. A frequency downshift of about 43 KHz was observed when the surface of SAW device was illuminated by a UV source with dominant wavelength of around 200 nm. The results indicate the feasibility of developing remote sensors for deep-UV measurement using AlN-based SAW oscillators.

Nanogrids and Beehive-Like Nanostructures Formed by Plasma Etching the Self-Organized SiGe Islands.

A lithography-free method for fabricating the nanogrids and quasi-beehive nanostructures on Si substrates is developed. It combines sequential treatments of thermal annealing with reactive ion etching (RIE) on SiGe thin films grown on (100)-Si substrates. The SiGe thin films deposited by ultrahigh vacuum chemical vapor deposition form self-assembled nanoislands via the strain-induced surface roughening (Asaro-Tiller-Grinfeld instability) during thermal annealing, which, in turn, serve as patterned sacrifice regions for subsequent RIE process carried out for fabricating nanogrids and beehive-like nanostructures on Si substrates. The scanning electron microscopy and atomic force microscopy observations confirmed that the resultant pattern of the obtained structures can be manipulated by tuning the treatment conditions, suggesting an interesting alternative route of producing self-organized nanostructures.

Enhanced visible photoluminescence from ultrathin ZnO films grown on Si-nanowires by atomic layer deposition.

Bright room temperature visible emission is obtained in heterostructures consisting of approximately 3.5 nm thick ZnO ultrathin films grown on Si-nanowires produced by means of self-masking dry etching in hydrogen-containing plasma. The ZnO films were deposited on Si-nanowires by using atomic layer deposition (ALD) under an ambient temperature of 25 degrees C. The orders of magnitude enhancement in the intensity of the room temperature photoluminescence peaked around 560 nm in the present ZnO/Si-nanowire heterostructures is presumably due to the high aspect (surface/volume) ratio inherent to the Si-nanowires, which has, in turn, allowed considerably more ZnO material to be grown on the template and led to markedly more efficient visible emission. Moreover, the ordered nanowire structure also features an extremely low reflectance (approximately 0.15%) at 325 nm, which may further enhance the efficiency of emission by effectively trapping the excitation light.

Berkovich Nanoindentation on AlN Thin Films.

Berkovich nanoindentation-induced mechanical deformation mechanisms of AlN thin films have been investigated by using atomic force microscopy (AFM) and cross-sectional transmission electron microscopy (XTEM) techniques. AlN thin films are deposited on the metal-organic chemical-vapor deposition (MOCVD) derived Si-doped (2 × 1017 cm-3) GaN template by using the helicon sputtering system. The XTEM samples were prepared by means of focused ion beam (FIB) milling to accurately position the cross-section of the nanoindented area. The hardness and Young's modulus of AlN thin films were measured by a Berkovich nanoindenter operated with the continuous contact stiffness measurements (CSM) option. The obtained values of the hardness and Young's modulus are 22 and 332 GPa, respectively. The XTEM images taken in the vicinity regions just underneath the indenter tip revealed that the multiple "pop-ins" observed in the load-displacement curve during loading are due primarily to the activities of dislocation nucleation and propagation. The absence of discontinuities in the unloading segments of load-displacement curve suggests that no pressure-induced phase transition was involved. Results obtained in this study may also have technological implications for estimating possible mechanical damages induced by the fabrication processes of making the AlN-based devices.