TiO2@CdS core–shell nanorods films: Fabrication and dramatically enhanced photoelectrochemical properties

In this paper, we prepared TiO₂@CdS core–shell nanorods films electrodes using a simple and low-cost chemical bath deposition method. The core–shell nanorods films electrodes were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and UV–vis spectrometry techniques. After applying these TiO₂@CdS core–shell nanorods electrodes in photovoltaic cells, we found that the photocurrent was dramatically enhanced, comparing with those of bare TiO₂ nanorods and CdS films electrodes. Moreover, TiO₂@CdS core–shell nanorods film electrode showed better cell performance than CdS nanoparticles deposited TiO₂ nanoparticles (P25) film electrode. A photocurrent of 1.31 mA/cm², a fill factor of 0.43, an open circuit photovoltage of 0.44 V, and a conversion efficiency of 0.8% were obtained under an illumination of 32 mW/cm², when the CdS nanoparticles deposited on TiO₂ nanorods film for about 20 min. The maximum quantum efficiency of 5.0% was obtained at an incident wavelength of 500 nm. We believe that TiO₂@CdS core–shell heterostructured nanorods are excellent candidates for studying some fundamental aspects on charge separation and transfer in the fields of photovoltaic cells and photocatalysis.     

Fe-doped SnO2 transparent semi-conducting thin films deposited by spray pyrolysis technique: Thermoelectric and p-type conductivity properties

In this paper, we report structural, electrical, optical, and especially thermoelectrical characterization of iron (Fe) doped tin oxide films, which have been deposited by spray pyrolysis technique. The doping level has changed from 0 to 10 wt% in solution ([Fe]/[Sn] = 0–40 at% in solution). The thermoelectric response versus temperature difference has exhibited a nonlinear behavior, and the Seebeck coefficient has been calculated from its slope in temperature range of 300–500 K. The Hall effect and thermoelectric measurements have shown p-type conductivity in SnO₂:Fe films with [Fe]/[Sn] ≥ 7.8 at%. In doping levels lower than 7.8 at%, SnO₂:Fe films have been n-type with a negative thermoelectric coefficient. The Seebeck coefficient for SnO₂:Fe films with 7.8 at% doping level has been obtained to be as high as +1850 μV/K. The analysis of as-deposited samples with thicknesses ～350 nm by X-ray diffraction (XRD) and scanning electron microscopy (SEM) has shown polycrystalline structure with clear characteristic peak of SnO₂ cassiterite phase in all films. The optical transparency (T%) of SnO₂:Fe films in visible spectra decreases from 90% to 75% and electrical resistivity (ρ) increases from 1.2 × 10^?2 to 3 × 10³ Ω cm for Fe-doping in the range 0–40 at%.     

Electrochemical sensing of hydroxylamine by gold nanoparticles on single-walled carbon nanotube films

The arrays of gold nanoparticles (AuNPs) were fabricated on flexible and transparent single-walled carbon nanotube (SWCNT) films using the electrochemical deposition method, and the patterned nanotubes were then used as electrodes for hydroxylamine detection. The sizes and densities of the AuNPs could easily be controlled by varying the amount of charge deposited, and the gold-deposited area showed a homogeneous distribution on the exposed SWCNT film surface. X-ray diffraction analysis of the AuNPs shows a face-centered cubic structure that is dominated by the lowest energy {111} facets. The oxidation of the hydroxylamine on the AuNP-deposited SWCNT films depended strongly on the solution pH, and the maximum catalytic current was observed at a pH of 9.0. A linear electrical response was observed for concentrations ranging from 0.016 to 0.210 mM, and the detection limit and the sensitivity were 0.72 μM and 165.90 μAmM^?1 cm^?2, respectively. Moreover, the amperometric response in hydroxylamine showed a stable response for a long time (300 s), during which time it retained 94% of its initial value. In the long-term storage stability test, the current response to hydroxylamine decreased slightly, with only 17% leakage after 30 days.     

Direct electrodeposition of PbTe thin films on n-type silicon

High quality lead telluride thin films were directly deposited onto n-type silicon (1 0 0) substrates by electrodeposition at room temperature. The deposition mechanism was studied using cyclic voltammetry. The films were characterized by scanning electron microscopy, energy dispersive X-ray, X-ray diffraction, and Fourier transform infrared spectroscopy. The results indicated that the deposited PbTe films exhibited a polycrystalline rock salt structure and good optical properties with a direct band gap of 0.31 eV.     

How can H content influence the tribological behaviour of W-containing DLC coatings

In this paper, the influence of the addition of W and H to pure DLC coatings on the structural, mechanical and tribological properties will be presented. The coatings were deposited by r.f. magnetron sputtering from a C target embedded with different numbers of W pellets. Working in non-reactive or reactive atmosphere allowed to deposit H-free or H-containing coatings, respectively, on steel and Si substrates. A Cr adhesion interlayer was interposed between the films and the substrate. Films with W content from 0 to 12 at.% and H incorporated up to a maximum value close to 40 at.% were deposited. All coatings had an amorphous structure, although vestiges of crystallinity could be detected in W-containing films. The addition of W led to a significant hardening of the DLC coating (from ～10 to 18 GPa); inversely, with H incorporation the hardness drop down to values even lower than that of pure DLC films. It was possible to establish a good correlation between the hardness and the residual stresses. In spite of decreasing friction and wear coefficients when alloying DLC with W, almost no difference was found among the W–DLC films whatever the W content was. A similar trend was achieved with the H addition. However, in this case a decrease in the friction coefficient was registered whereas the wear rate increased. The best performance concerning the friction was obtained for an H-containing coating (0.05) whereas, for the wear resistance, H-free W–DLC films were better performing (0.3 × 10^?16 m³ N^?1 m^?1).     

Si-doped carbon nanostructured films by pulsed laser deposition from a liquid target

Ablation of a silicone oil, Dow Corning's DC-705 with laser pulses of sub-ps duration in high vacuum is a novel approach to fabrication of Si-doped carbon nanocomposite films. Gently focused, temporally clean 700 fs pulses @ 248 nm of a hybrid dye/excimer laser system produce power densities of the order of 10¹¹–10¹² W cm^?2 on the target surface. The evolution of the chemical structure of film material is followed by comparing Fourier Transformed Infrared and X-ray Photoelectron spectra of films deposited at temperatures between room temperature and 250 °C. Despite the low thermal budget technique, in the spectrum of films deposited at room temperature the fingerprint of the silicone oil can clearly be identified. With increasing substrate temperature the contribution of the features characteristic of the oil gradually diminishes, but does not completely disappear even at 250 °C. This result is intriguing since the chance of oil droplets to survive in their original liquid form on the hot surface should be minimal. The results of the X-ray Photoelectron Spectroscopy suggest that the chemical structure of the film material resembles that of the oil. Both reflection mode optical microscopy and low magnification Scanning Electron Microscopy reveal that the films are inhomogeneous: areas of lateral dimensions ranging from a few to tens of micrometers, characterized by different contrasts can be identified. On the other hand, surface mapping by Scanning Electron and Atomic Force Microscopy unambiguously proves that all films possess a solid surface consisting of nanoparticles of less than 100 nm dimension, without the presence of any drop of oil. Possible explanations of the puzzling results can be that the films are polymers consisting mainly of the molecules of the target material, or composites of solid C:Si nanoparticles and oil residues.     

Hydrogen bubble dynamic template synthesis of porous gold for nonenzymatic electrochemical detection of glucose

Gold (Au) films with open interconnected macroporous walls and nanoparticles have been successfully sculptured using the hydrogen bubble dynamic template synthesis followed by a galvanic replacement reaction. Copper (Cu) films with open interconnected macroporous walls and nanoparticles were synthesized using the electrochemically generated hydrogen bubbles as a dynamic template. Then through a galvanic replacement reaction between the porous Cu sacrificial templates and KAu(CN)₂ in solution, the porous Cu films were converted to porous Au films with the similar morphologies. Additional electrochemical dealloying process was introduced to remove the remaining Cu from the porous Au films. X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), Energy-dispersive X-ray (EDX), X-ray diffraction (XRD) and electrochemical methods were adopted to characterize the porous Au films. The resulted porous Au films show excellent catalytic activity toward the electrooxidation of glucose. A nonenzymatic glucose sensor based on those Au film electrodes shows a linear range from 2 to 10 mM with a sensitivity of 11.8 μA cm⁻² mM⁻¹, and a detection limit of 5 μM.     

A study on solution deposited CuSCN thin films: Structural,electrochemical, optical properties

A cost-effective successive ionic layer adsorption and reaction (SILAR) method was used to deposit copper (I) thiocyanate (CuSCN) thin films on glass and steel substrates for this study. The deposited thin films were characterized for their structural, morphological, optical and electrochemical properties using X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–visible spectroscopy and VersaSTAT potentiostat. A direct band gap of 3.88 eV and 3.6 eV with film thickness of 0.7 μm and 0.9 μm was obtained at 20 and 30 deposition cycles respectively. The band gap, microstrain, dislocation density and crystal size were observed to be thickness dependent. The specific capacitance of the CuSCN thin film electrode at 20 mV/s was 760 F g⁻¹ for deposition 20 cycles and 729 F g⁻¹ for deposition 30 cycles.     

Effect of Hg2+doping and of the annealing temperature on the nanostructural properties of TiO2 thin films obtained by sol–gel method

This work is a study of Hg²⁺-doped TiO₂ thin films deposited on silicon substrates prepared by sol–gel method and treated at temperatures ranging between 600 to 1000 °C for 2 h. The structural and optical properties of thin films have been studied using different techniques. We analyzed the vibrations of the chemical bands by Fourier transform infrared (FTIR) spectroscopy and the optical properties by UV–Visible spectrophotometry (reflection mode) and photoluminescence (PL). The X-ray diffraction and Raman spectra of TiO₂ thin films confirmed the crystallization of the structure under the form of anatase, rutile, mercury titanate (HgTiO₃) as a function of the annealing temperature. The observation by scanning electron microscopy (SEM) showed the changing morphology, with respect to nanostructures, nanosheets, nanotubes, with the annealing temperature. The diameters of nanotubes ranged from 50 nm to 400 nm. The photoluminescence and reflectance spectra indicated that these structures should enhance photocatalytic activity.     

XRD and AFM studies of ZnS thin films produced by electrodeposition method

The structure and morphology of ZnS thin films were investigated. ZnS thin films have been grown on an indium tin oxide glass substrate by electrodeposition method using zinc chloride and sodium thiosulfate solutions at room temperature. The X-ray diffraction patterns confirm the presence of ZnS thin films. From the AFM images, grain size decreases as the cathodic potential becomes more negative (from ?1.1 to ?1.3 V) at various deposition periods. Comparison between all the samples reveals that the intensity of the peaks increased, indicating better crystalline phase for the films deposited at ?1.1 V. These films show homogeneous and uniform distribution according to AFM images. On the other hand, XRD analysis shows that the number of ZnS peaks increased as deposition time was increased from 15 to 30 min at ?1.1 V. The AFM images show thicker films to be formed at ?1.1 V indicating more favourable condition for the formation of ZnS thin films.     

MnO2 multilayer nanosheet clusters evolved from monolayer nanosheets and their predominant electrochemical properties

MnO₂ multilayer nanosheet clusters were prepared via electrochemical deposition route, which shows simpleness and high efficiency. The growth process of MnO₂ multilayer nanosheet clusters was investigated in this paper. The deposited MnO₂ films were characterized by XRD, SEM, TEM, and XPS. In addition, it was also electrochemically characterized by cyclic voltammetry in 1.0 M Na₂SO₄ electrolyte. The MnO₂ multilayer nanosheet clusters show a big specific capacitance, and it can be achieved about 521.5 F g^?1 at 5 mV s^?1. These materials also have a high electrochemical stability.     

Nanoplates and nanostars of β-PbO formed at the air/water interface

Nanoparticles with different shapes were prepared at the air/water interface via hydrolysis of Pb²⁺ ions under Langmuir films of poly(N-vinylcarbazole) (PVK) at 30–50 °C. It was found that round or irregular nanoparticles with the size of several to several tens of nanometers were formed when the PbCl₂ aqueous solution with the concentration of 1 × 10^?3 mol L^?1 was used as subphase, while single-crystalline quasi-hexagonal nanoplates, nanostars and dendrites with the size of several hundreds of nanometers were obtained when the subphase concentration was 1 × 10^?4 mol L^?1. Analysis on the selective-area electron diffraction (SAED) patterns revealed that the formed nanoparticles are β-PbO. The formation of the nanostructures should be attributed to the formation and dehydration of lead hydroxide, diffuse-limited growth and aggregation of nanoparticles at the air/water interface.     

Effect of swift heavy ion irradiation on the physical properties of CuIn(S0.4Se0.6)2 alloy thin films prepared by solution growth technique

Alloy thin films of CuIn(S_0.4Se_0.6)₂ material were deposited using the solution growth technique. The various deposition parameters such as pH of solution, time, concentration of ions and temperature have been optimized for the device grade thin films. The as-deposited films were annealed in a rapid thermal annealing (RTA) system at 450 °C in air for 5 min and subjected to high-energy Ag ion irradiations. Ag ion irradiation has been performed with an energy of 100 MeV at a fluency of 5×10¹² ions/cm² on the thin film. The changes in optical and electrical properties that occurred before and after post-deposition treatments in CuIn(S_0.4Se_0.6)₂ thin films were studied using X-ray diffraction (XRD) and AFM; increase in crystallinity was observed after annealing and irradiation. In addition, structural damages were observed in irradiated thin films. After annealing and irradiation, the surface roughness was seen to be increased. Decrease in resistivity was observed, which is consistent with the optical energy band gap. The results are explained by considering the high energy deposited due to the electronic energy loss upon irradiation, which modified the properties of the material.     

An activated carbon with high capacitance from carbonization of a resorcinol–formaldehyde resin

A polymeric activated carbon (PAC) was synthesized from the carbonization of a resorcinol–formaldehyde resin with KOH served as an activation agent. The nitrogen adsorption–desorption at 77 K, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the prepared PAC. Compared with the commercial activated carbon (Maxsorb: Kansai, Japan), PAC shows superior capacitive performance in terms of specific capacitance, power output and high energy density as electrode materials for supercapacitors. PAC presents a high specific capacitance of 500 F g^?1 in 6 mol l^?1 KOH electrolyte at a current density of 233 mA g^?1 which remained 302 F g^?1 even at a high current density of 4.6 A g^?1. The good electrochemical performance of the PAC was ascribed to well-developed micropores smaller than 1.5 nm, the presence of electrochemically oxygen functional groups and low equivalent series resistance.     

Effects of electron beam irradiation on the photoelectrochemical properties of TiO2 film for DSSCs

TiO₂ has been widely utilized for various industrial applications such as photochemical cells, photocatalysts, and electrochromic devices. The crystallinity and morphology of TiO₂ films play a significant role in determining the overall efficiency of dye-sensitized solar cells (DSSCs). In this study, the preparation of nanostructured TiO₂ films by electron beam irradiation and their characterization were investigated for the application of DSSCs. TiO₂ films were exposed to 20–100 kGy of electron beam irradiation using 1.14 MeV energy acceleration with a 7.46 mA beam current and 10 kGy/pass dose rates. These samples were characterized using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and X-ray photoelectron spectroscopy (XPS) analysis. After irradiation, each TiO₂ film was tested as a DSSC. At low doses of electron beam irradiation (20 kGy), the energy conversion efficiency of the film was approximately 4.0% under illumination of simulated sunlight with AM 1.5 G (100 mW/cm²). We found that electron beam irradiation resulted in surface modification of the TiO₂ films, which could explain the observed increase in the conversion efficiency in irradiated versus non-irradiated films.     

Highly selective solid-phase extraction of trace Pd(II) by murexide functionalized halloysite nanotubes

The originality on the high efficiency of murexide modified halloysite nanotubes as a new adsorbent of solid phase extraction has been reported to preconcentrate and separate Pd(II) in solution samples. The new adsorbent was confirmed by Fourier transformed infrared spectra, X-ray diffraction, scanning electron microscope, transmission electron microscope and N₂ adsorption–desorption isotherms. Effective preconcentration conditions of analyte were examined using column procedures prior to detection by inductively coupled plasma-optical emission spectrometry (ICP-OES). The effects of pH, the amount of adsorbent, the sample flow rate and volume, the elution condition and the interfering ions were optimized in detail. Under the optimized conditions, Pd(II) could be retained on the column at pH 1.0 and quantitatively eluted by 2.5 mL of 0.01 mol L^?1 HCl–3% thiourea solution at a flow rate of 2.0 mL min^?1. The analysis time was 5 min. An enrichment factor of 120 was accomplished. Common interfering ions did not interfere in both separation and determination. The maximum adsorption capacity of the adsorbent at optimum conditions was found to be 42.86 mg g^?1 for Pd(II).The detection limit (3σ) of the method was 0.29 ng mL^?1, and the relative standard deviation (RSD) was 3.1% (n = 11). The method was validated using certified reference material, and has been applied for the determination of trace Pd(II) in actual samples with satisfactory results.     

Effect of negative substrate bias on HWCVD deposited nanocrystalline silicon (nc-Si) films

The influence of the negative substrate bias on the interfacial and microstructural characteristics of nanocrystalline silicon (nc-Si) thin films was deposited by hot wire chemical vapor deposition (HWCVD). Structural characterization of nc-Si films was performed by small angle X-ray diffraction (SAXRD), Raman spectroscopy, X-ray reflectivity (XRR) and field emission scanning electron microscopy (FESEM). Crystalline fraction and crystallite size increases from 61.31 to 74.13% and 13.3 to 21.6 nm, respectively, with an increasing negative bias from 0 to ?200 V. Furthermore, the deposition rate of nc-Si films increases from 25 to 68 nm/min by increase of negative substrate bias from 0 to ?200 V.     

Electrodeposition of PtCo alloy nanoparticles on inclusion complex film of functionalized cyclodextrin–ionic liquid and their application in glucose sensing

Platinum–cobalt (PtCo) alloy nanoparticles (NPs) are successfully fabricated by ultrasonic-electrodeposition method, using an inclusion complex (IC) film of functionalized cyclodextrin (CD)–ionic liquid (IL) as support. The morphology and composition of the PtCo alloy NPs are characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction, respectively. It is found that they are well-dispersed on the CD–IL surface and exhibit many unique features. The resulting modified glassy carbon electrode shows excellent catalytic activity for glucose oxidation. Under the physiological condition, the oxidation current of glucose is linear to its concentration up to 20 mM with sensitivity of 13.7 μA mM^?1 cm^?2. In addition, the interference from the oxidation of ascorbic acid and uric acid could be effectively avoided. Therefore, it is promising as a nonenzymatic glucose sensor.     

Preparation and photocatalytic activity of Cu-deposited TiO2 film with high transparency

Cu-deposited TiO₂ films were prepared by photoreduction of Cu(II) in the presence of sodium formate. With the initial Cu(II) concentrations more than 100 mg L^?1, induction periods were observed before the transmittance decreased. Scanning electron microscopy indicated that Cu particles of 2.6 ± 0.5 μm were deposited isolatedly with much open space in the induction periods. The films prepared by changing the irradiation time within the induction periods showed a higher photocatalytic activity than a pure TiO₂ for the degradation of methylene blue under the reaction condition without purging air.     

Physicochemical studies on cross-linked thorium(IV)–alginate complex especially the electrical conductivity and chemical equilibrium related to the coordination geometry

The electrical conductivity of cross-linked thorium(IV)–alginate complex in the form of circular disc has been investigated as a function of temperature. The Arrhenius plot of log σ vs. 1/T showed a simple parabolic shape at the early stages, followed by a sharply increase in o values with raising the temperature at the final stages. This behaviour was interpreted by the formation of free-radicals at the initial stages, followed by the degradation of the complex at elevated temperatures to give rise to thorium oxide product. The heterogeneous chemical equilibrium for exchange of Th⁴⁺ counter ions in the complex by H⁺ ions has been investigated by titrimetric and complexometric techniques. The thermodynamic equilibrium constant was found to be 26 ± 0.25 dm⁹ mol^?3 at 25 °C. The X-ray diffraction pattern indicated that thorium(IV)–alginate complex is amorphous in nature. Infrared absorption spectra indicated that Th⁴⁺ is chelated to alginate macromolecular chains and displayed υ_s OCO^? and υ_as OCO^? in the ranges of 1419 and 1635 cm^?1, respectively. A geometrical structure for chelation of thorium(IV) to the functional groups of alginate macromolecule is suggested and discussed in terms of complex stability.