Effect of carbon doping on WO3/TiO2 coupled oxide and its photocatalytic activity on diclofenac degradation

The improved photocatalyst carbon-doped WO₃/TiO₂ mixed oxide was synthesized in this study using the sol–gel method. The catalyst was thoroughly characterized by X-ray diffraction (XRD), diffuse reflectance UV–vis spectroscopy, N₂ adsorption desorption analysis, scanning electron microscopy coupled with energy dispersive X-ray analysis (SEM/EDX), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The photocatalytic efficiency of the prepared materials was evaluated with respect to the degradation of sodium diclofenac (DCF) in a batch reactor irradiated under simulated solar light. The progress of the degradation process of the drug was evaluated by high-performance liquid chromatography (HPLC), whereas mineralization was monitored by total organic carbon analysis (TOC) and ion chromatography (IC). The results of the photocatalytic evaluation indicated that the modified catalyst with tungsten and carbon (TWC) exhibited higher photocatalytic activity than TiO₂ (T) and WO₃/TiO₂ (TW) in the degradation and mineralization of diclofenac (TWC>TW>T). Complete degradation of diclofenac occurred at 250 kJ m⁻² of accumulated energy, whereas 82.4% mineralization at 400 kJ m⁻² was achieved using the photocatalytic system WO₃/TiO₂-C. The improvement in the photocatalytic activity was attributed to the synergistic effect between carbon and WO₃ incorporated into the TiO₂ structure.     

Synthesis of ruthenium complex and its application in dye-sensitized solar cells

An amphiphilic bipyridyl ligand, 4,4′-dicarboxy-octyl-2,2′-bipyridine, and its ruthenium(□) complex (termed as S8) were synthesized and characterized by UV/Vis, IR and NMR spectroscopy. The performance of this S8 complex as charge transfer photo-sensitizer in TiO₂-based dye-sensitized solar cells was studied under standard AM 1.5 sunlight and by using an electrolyte consisting of 0.70 M 1,2-dimethyl-3-propyl-imidazolium iodide, 0.10 M LiI, 40 mM iodine and 0.125 M 4-tert-butylpyridine in acetonitrile. Aliphatic chains linking to carboxylate groups of S8 act as an effective electron donor and carboxylate groups act as an effective electron withdrawing between the TiO₂ layer and the carboxylate linking TiO₂ layer leading to increasing of electron density at this interface, which is attributed to increasing efficiency of electron injection to the TiO₂ conduction band from the excited state of dye. The complex, S8, gave a photocurrent density of 13.02 mA/cm², 0.60 V open circuit voltage and 0.69 fill factor yielding 5.36% efficiency. The S8 dye with aliphatic chain improved conversion efficiency of the resulting DSSCs compared with a cell fabricated using the N3 dye.     

Sol–gel hydrothermal synthesis of bismuth–TiO2 nanocubes for dye-sensitized solar cell

Bismuth–TiO₂ nanocubes were synthesized via a facile sol–gel hydrothermal method with titanium tetraisopropoxide as the precursor. The influence of the bismuth on the size, morphology, crystallinity and optical behavior of TiO₂ nanocubes were investigated. The samples were characterized by X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), field emission scanning electron microscopy (FESEM) and UV–visible spectroscopy (UV–vis). Photovoltaic behavior of dye-sensitized solar cells (DSSCs) fabricated using Bi–TiO₂ nanocubes was studied. The DSSCs had an open-circuit voltage (V_oc) of 590 mV, a short-circuit current density (J_sc) of 7.71 mA/cm², and the conversion efficiency (η) of 2.11% under AM 1.5 illumination, a 77% increment as compared to pure TiO₂ nanocubes.     

Synthesis and characterisation of thin-film TiO2 dye-sensitised solar cell

A TiO₂ dye-sensitised solar cell (DSSC) is fabricated and characterised using: X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM), electron diffraction X-ray (EDX) analysis, UV–vis spectrometry and a current?voltage (I?V) test. Thicker anatase TiO₂ gives rise to better crystallinity and subsequently leads to better cell efficiency. Mesoporous TiO₂ with a suitable, average pore size results in higher conversion efficiency. Smaller particle sizes lead to higher dye uptake and increase short circuit current density, J_sc. Addition of scattering layer and/or dual TiCl₄ treatment for DSSCs having optimum thickness enhanced their performance. A DSSC having double TiO₂ layers (20 nm+50 nm) with dual TiCl₄ treatment achieved the highest conversion efficiency of 9.78%.     

Facile hydrothermal synthesis and optical limiting properties of TiO2-reduced graphene oxide nanocomposites

TiO₂/reduced graphene oxide (RGO) nanocomposites Gx (RGO titania nanocomposite, x grams tetrabutyl titanate per 0.03 g RGO, x = 0.25, 0.50, 1.00) were prepared by a hydrothermal method: graphene oxide was reduced to RGO in a 2:1 water:ethanol mixture in the presence of varying quantities of tetrabutyl titanate, which deposited as TiO₂ on the RGO sheets. The nanocomposites were characterized by a combination of Fourier transform infrared spectroscopy, diffuse reflectance ultraviolet–visible spectroscopy, photoluminescence spectroscopy, Raman spectroscopy, X-ray powder diffraction, X-ray photoelectron spectroscopy and transmission electron microscopy studies. The nanocomposite G0.25 exhibits enhanced nonlinear optical properties compared to its individual components, which is ascribed to a combination of mechanisms. The role of defects and electron/energy transfer in the optical limiting performance of G0.25 was clarified with the help of Raman and photoluminescence spectroscopies. Intensity-dependent switching between reverse saturable absorption and saturable absorption behavior was observed with the G0.50 nanocomposite.     

Photovoltaic efficiency on dye-sensitized solar cells (DSSC) assembled using Ga-incorporated TiO2 materials

This study examined the photoelectric conversion efficiency of DSSC (dye-sensitized solar cell) when nanometer sized Ga (0.25, 0.50, and 1.00 mol%)–TiO₂ prepared using a hydrothermal method was employed as a working electrode material. The particle sizes observed in the transmission electron microscopy images were <20 nm in all samples. However, with increasing Ga concentration, the size increased and the shapes transformed to a stick form. The absorption band was slightly blue-shifted upon the incorporation of gallium ions, but the intensity of the photoluminescence (PL) curves of the Ga-incorporated TiO₂ was significantly smaller, with the smallest case being the 0.50 mol% Ga–TiO_2, which was related to recombination between the excited electrons and holes. When Ga–TiO₂ was applied in DSSC, the energy conversion efficiency was enhanced considerably compared to that using pure TiO₂; it was approximately 4.57% with the N3 dye under 100 mW/cm² of simulated sunlight. These results are in agreement with an electrostatic force microscopy (EFM) study showing that the electrons were transferred rapidly to the surface of Ga–TiO₂ film, compared with that on a pure TiO₂ film.     

Slurry explosive detonation synthesis and characterization of 10 nm TiO2

TiO₂ was prepared by detonating a slurry explosive made of Ti precursor, ammonium nitrate, cyclotrimethylenetrinitramine (RDX), and polystyrene (EPS). X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectrometry, Fourier transform infrared spectroscopy, and UV–vis diffuse reflection spectroscopy revealed that the sample was composed of mixed crystals of rutile and anatase TiO₂ with irregular spherical shapes and 10 nm particle size. The minimum energy gap of the sample was 2.9 eV. An ideal TiO₂ explosive was prepared from a precursor/ammonium nitrate/RDX ratio of 1:1:0.6 and 2 g of EPS as a density modifier.     

Synthesis and catalytic properties of novel POM@TiO2 composite materials

Donor–π-bridge–acceptor (D–π–A) type polyoxometalates (POMs) were self-assembled for the first time on the surface of titanium dioxide (TiO₂) nanoparticles through the layer-by-layer (LBL) method. The obtained composite materials POM@TiO₂ were characterized by Transmission electron microscopy (TEM), Fourier transform IR spectroscopy (FTIR), Raman spectrum and energy dispersive X-ray (EDX) spectroscopy. Catalytic properties of POM@TiO₂ were also investigated by treating organic pollutants (typically, removal of 40 mL 20 mg L^− 1 methylene blue (MB) by 10 mg POM@TiO₂ was up to 99.5% within 3 min under ambient conditions and the photodegradation efficiency was obviously higher than bare TiO₂ nanoparticles under irradiation).     

The photo-catalytic activities of neodymium and fluorine doped TiO2 nanoparticles

A series of photo-catalysts were synthesized by neodymium and fluorine doped TiO₂, and their characteristics evaluated by X-ray diffraction (XRD), UV–vis diffuse reflectance spectra (UV–vis), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDS). Neodymium and fluorine doped TiO₂ has obvious absorption in the visible light and the absorption edge shifts toward red wavelength. In addition, compared with pure TiO₂, the doped catalyst has intense absorption at 528, 587, 750, 808, and 881 nm. The catalytic efficiency was tested by monitoring the photo-catalytic degradation of methylene blue (MB) in visible light and ultraviolet light. The results showed that the optimum doping content was Nd:F:TiO₂ = 0.5:5:100 (molar ratio) heat treated at 500 °C, and the reaction rates of MB degradation were estimated to be about 1.76 times and 1.45 times higher than undoped TiO₂ in ultraviolet light and visible light.     

Highly visible light responsive metal loaded N/TiO2 nanoparticles for photocatalytic conversion of CO2 into methane

Photocatalytic reduction of carbon dioxide (CO₂) into valuable hydrocarbon such as methane (CH₄) using water as reducing agent is a good strategy for environment and energy applications. In this study, a facile and simple sol-gel method was employed for the synthesis of metal (Cu and Ag) loaded nanosized N/TiO₂ photocatalyst. The prepared photocatalysts were characterized by X-ray diffraction, transmission electron microscopy, BET Surface area analyzer, X-ray photoelectron spectroscopy and UV–vis diffuses reflectance spectroscopy. The photocatalytic conversion of CO₂ into methane was carried out under visible light irradiation (λ≥420 nm) by prepared photocatalysts in order to evaluate the photocatalytic efficiency. The results demonstrate that Ag loaded N/TiO₂ showed enhanced photocatalytic performance for methane production from CO₂ compared to other Cu–N/TiO₂, N/TiO₂ and TiO₂ photocatalysts. The improvement in the photocatalytic activity could be attributed to high specific surface area, extended visible light absorption and suppressed recombination of electron – hole pair due to synergistic effects of silver and nitrogen in the Ag–N/TiO₂ photocatalyst. This study demonstrates that Ag–N/TiO₂ is a promising photocatalytic material for photocatalytic reduction of CO₂ into hydrocarbons under visible light irradiation.     

Template-assisted hydrothermal synthesis and photocatalytic activity of novel TiO2 hollow nanostructures

TiO₂ hollow nanostructures were successfully synthesized by a controlled hydrothermal precipitation reaction using Resorcinol–Formaldehyde resin spheres as templates in aqueous solution, and then removal of the RF resins spheres by calcination in air at 450 °C for 4 h. The obtained TiO₂ hollow spheres were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, N₂ adsorption–desorption analysis, and UV–visible diffuse reflectance spectroscopy. The photocatalytic activity of the as-prepared samples was evaluated by photocatalytic decolorization of rhodamine B aqueous solution at ambient temperature under UV illumination. The results indicated TiO₂ hollow nanostructures exhibit the excellent photocatalytic activity probably due to the unique hollow micro-architectures.     

Simple fabrication of thermally stable apertured N-doped TiO2 microtubes as a highly efficient photocatalyst under visible light irradiation

Apertured N-doped TiO₂ microtubes have been fabricated by simple hydrolysis of titania tetrachloride using ammonia without any external templates. The morphology and microstucture characteristics of apertured N-doped TiO₂ microtubes were characterized by means of the specific surface area (BET), transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transformed infrared (FT-IR), UV–visible diffuse reflectance spectra (DRS) and X-ray powder diffraction (XRD). The unique morphology of microtubes and mesoporous microstructure were maintained after a heat treatment at 723 K for 3 h, exhibiting significantly thermal stability. The catalysts exhibited high ultraviolet and visible light photocatalytic activity in degrading phenol and methyl orange.     

Improved activity of a graphene–TiO2 hybrid electrode in an electrochemical supercapacitor

We present a simple and fast approach for the synthesis of a graphene–TiO₂ hybrid nanostructure using a microwave-assisted technique. The microstructure, composition, and morphology were characterized by X-ray diffraction, Fourier-transform infrared spectroscopy, Raman microscopy, X-ray photoelectron spectroscopy, and field-emission scanning electron microscopy. The electrochemical properties were evaluated using cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge–discharge tests. Structural analysis revealed a homogeneous distribution of nanosized TiO₂ particles on graphene nanosheets. The material exhibited a high specific capacitance of 165 F g⁻¹ at a scan rate of 5 mV s⁻¹ in 1 M Na₂SO₄ electrolyte solution. Theenhanced supercapacitance property of these materials could be ascribed to the increased conductivity of TiO₂ and better utilization of graphene. Moreover, the material exhibited long-term cycle stability, retaining ∼90% specific capacitance after 5000 cycles, which suggests that it has potential as an electrode material for high-performance electrochemical supercapacitors.     

Effect of polymer concentration,needle diameter and annealing temperature on TiO2-PVP composite nanofibers synthesized by electrospinning technique

In this study, TiO₂-PVP nanofibers were successfully synthesized on an aluminium collector by using cost-effective electrospinning technique. The nanofibers were prepared at different polymer concentrations, needle diameters and annealing temperatures and properties were studied by various characterizations. The structural properties were studied by X-ray diffraction (XRD) and Raman spectroscopy techniques. Surface morphology and elemental analysis of the samples were investigated by scanning electron microscopy (SEM) attached with energy dispersive spectroscopy (EDS). The optical properties were carried out by UV–Visible absorption spectroscopy (UV–Vis). By varying the polymer concentration and needle diameter, the effect of viscosity and surface tension on the formation of TiO₂-PVP nanofibers was clearly observed by SEM micro images. EDS spectrum shows effective composition of pure TiO₂ nanofibers. XRD peaks observed at temperatures 500 °C, 700 °C and 900 °C confirmed the anatase, mixed and rutile phases of TiO₂ nanofibers respectively. Raman studies also confirmed these phases of TiO₂ nanofibers. The optical band-gap values calculated using Kubelka-Munk function lies in the range of 3.02–3.22 eV.     

Preparation of graphene film decorated TiO2 nano-tube array photoelectrode and its enhanced visible light photocatalytic mechanism

Graphene film decorated TiO₂ nano-tube array (GF/TiO₂ NTA) photoelectrodes were prepared through anodization, followed by electrodeposition strategy. Morphologies and structures of the resulting GF/TiO₂ NTA samples were characterized by scanning electrons microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and Raman spectroscopy. In addition, the optical and photoelectrochemical properties were investigated through UV–visible light diffuse reflection spectroscopy, photocurrent response and Mott–Schottky analysis. Furthermore, the photodecomposition performances were investigated through yield of hydroxyl radicals and photocatalytic (PC) degradation of methyl blue (MB) under visible light irradiation. It was found that GF/TiO₂ NTA photoelectrode exhibited intense light absorption both in UV light and visible region, higher transient photoinduced current of 0.107 mA cm⁻² and charge carrier concentration of 0.84 × 10¹⁹ cm⁻³, as well as effective PC performance of 65.9% for the degradation of MB. Furthermore, contribution of several reactive species to the PC efficiency of GF/TiO₂ NTA photoelectrode was distinguished. Moreover, the enhanced visible light PC mechanism was proposed and confirmed in detail.     

Hydrothermal preparation of Ag-TiO2 nanostructures with exposed {001}/{101} facets for enhancing visible light photocatalytic activity

Nano-composite materials of Ag nanoparticles dispersed TiO₂ nanocubes with exposed {001}/{101} crystal faces were fabricated mainly via a flexible one-step method of hydrothermal treatment with different content of Ag from 1 up to 3 mol%. Prepared photocatalysts were characterized by X-ray diffraction, scanning electron microscope, transmission electron microscopy, UV–vis absorption spectroscopy, X-ray photoelectron spectroscopy and Raman spectroscopy. These analysis was carried out for understanding the contribution of different content of silver for enhancing the photocatalytic activity of TiO₂ nanocubes. Prepared silver nanoparticles had small particle size and grafted to the {101} crystal face of TiO₂ with the role of template control agent and linking agent. The photocatalytic performance of Ag-TiO₂ nanocubes were researched via Rhodamine B dye removal under visible light irradiation ( ≧420 nm). Ag-TiO₂ composite materials with the content of 2 mol% Ag showed the best photocatalytic activity for degradation of Rhodamine B, which was five times more than bare TiO₂ and associated with the localized surface plasmon resonance (LSPR) propelled effect. The mechanism by which silver enhanced the photocatalytic activity of TiO₂ was also demonstrated.     

Preparation and characterisation of mixed matrix Al2O3- and TiO2-based ceramic membranes prepared using polymeric synthesis route

Al₂O₃- and TiO₂-based ceramic membranes prepared using polymeric synthesis route were characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR) and gas permeability tests. The influence of the final calcination temperature and the systematic investigation of the properties of the membranes are provided. The calcination temperature affected morphological, structural and chemical properties, as well as the gas permeability of the ceramic membranes. XRD analysis revealed rhombohedral and tetragonal structures of Al₂O₃ and TiO₂-based ceramic, respectively, prepared at calcination temperatures of 1100 and 1200 °C. The TiO₂-based ceramic matrix calcined at temperatures of 1100 and 1200 °C exhibited a well-defined crystalline microstructure with the grains increasing in size as a function of temperature. FTIR analysis revealed that phosphorus additives in orthoclase clay tend to form phosphonate groups during the calcination process. The decomposition of organic source was not fulfilled as tested at calcination temperatures of 1000, 1100 and 1200 °C.     

Polyimide/nano-TiO2 hybrid films having benzoxazole pendent groups: In situ sol–gel preparation and evaluation of properties

Polyimide/titania (PI/TiO₂) nanocomposite films have been successfully fabricated through the in situ formation of TiO₂ within a PI matrix via sol–gel method. Poly(amic acid) (PAA), which is the precursor of PI, was successfully synthesized by mixing pyromellitic dianhydride (PMDA), with equimolar amount of a diamine monomer having a pendent benzoxazole unit and two flexible ether linkages in N,N-dimethylformamide (DMF) solvent. Tetraethyl orthotitanate [Ti(OEt)₄] and acetylacetone were then added to the resulted PAA. After imidization at high temperature, PI/TiO₂ hybrid films were formed. The structure and morphology of the hybrid nanocomposites with different titania contents (0 wt%, 5 wt%, 10 wt%, and 15 wt%) were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, and transmission electron microscopy. The results indicate that the TiO₂ nanoparticles were homogeneously dispersed in the hybrid films. The thermogravimetric analysis of nanocomposites confirms the improvement in the thermal stability with the increase in the percentage of titania nanoparticle. Transmission electron microscopy showed that the nanoparticles with an average diameter of 25–40 nm were dispersed in the polymer matrix.     

Influence of Ge and GeO2 on the microstructure and varistor properties of TiO2–Ta2O5–CaCO3 ceramics

This study investigated the effect of elemental crystal Ge or/and GeO₂ doping on the microstructure and varistor properties of TiO₂–Ta₂O₅–CaCO₃ varistor ceramics, which were prepared via the traditional ball milling–molding–sintering process. X-ray diffraction, scanning electron microscopy, scanning transmission electron microscopy-energy dispersive X-ray spectroscopy, scanning electron microscopy-energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy demonstrated that co-doping with Ge and GeO₂ changed the microstructure of TiO₂–Ta₂O₅–CaCO₃ ceramics, thereby increasing the nonlinear coefficient and decreasing the breakdown voltage. The optimum doping concentrations of Ta₂O₅, CaCO₃, Ge, and GeO₂ exhibited the highest nonlinear coefficient (α=14.6), a lower breakdown voltage (E_B=18.7 V mm⁻¹), the least leakage current (J_L=10.5 μA cm⁻²), and the highest grain boundary barrier (Φ_B=1.05 eV). In addition, Ge and GeO₂ function as sintering aids, which reduce the sintering temperature because of their low melting points.     

Chemical synthesis of TiO2 nanoparticles and their inclusion in Ni–P electroless coatings

The work addresses the preparation of Ni3P3TiO₂ nanocomposite coatings on mild steel substrate by the electroless technique. Nanosized TiO₂ particles were first synthesized by the precipitation method and then were codeposited (4 g/l) into the Ni3P matrix using alkaline hypophosphite reduced EL bath. The surface morphology, particle size, elemental composition and phase analysis of as-synthesized TiO₂ nanoparticles and the coatings were characterized by field emission scanning electron microscopy (FESEM), energy-dispersive analysis of X-ray (EDAX) and X-ray diffraction (XRD). Coatings with 20 µm thickness were heat treated at 400 °C for 1 h in argon atmosphere. The morphology, microhardness, wear resistance and friction coefficient characteristics (ball on disc) of electroless Ni3P3TiO₂ nanocomposite coatings were determined and compared with Ni3P coatings. The results show that as-synthesized TiO₂ nanoparticles are spherical in shape with a size of about12 nm. After heat treatment, the microhardness and wear resistance of the coatings are improved significantly. Superior microhardness and wear resistance are observed for Ni3P3TiO₂ nanocomposite coatings over Ni3P coatings.