Synthesis,characterization and photocatalytic performance of W,N, S-tri-doped TiO2 under visible light irradiation

W–S–N-tri-doped TiO₂ photocatalysts (WSNTiO₂) were prepared by a simple sol–gel method. Tungstic acid, sodium sulfate and urea were used as tungsten, sulfur and nitrogen sources, respectively. The morphology and microstructure characteristics of the photocatalysts were evidenced by means of XRD, BET, TEM, SEM and UV–vis DRS techniques. The XRD results show that the main crystal phase of samples is anatase. It was also found that the tri-doping of TiO₂ increases its BET specific surface area from 95 to 121 m²·g⁻¹. Besides, it was shown that tri-doping narrows the band gap of TiO₂ effectively, which has greatly improved the photocatalytic activity in the visible light region. The photocatalytic activity of tri-doped TiO₂ powders was compared to that of bi-doped ones through the degradation of Congo Red (CR) under visible irradiation. Thus, the prepared 0.5% W–N–S–TiO₂ heat treated at 450 °C showed the best photocatalytic activity compared to the prepared pure TiO₂, Degussa P25, and co-doped samples (WNTiO₂ and WSTiO₂). In particular, a Congo Red degradation rate of approximately 99% was reached after only 35 min of visible light irradiation in the presence of 0.5% of WNSTiO₂. Total organic carbon (TOC) removal of CR was up to 72% and confirmed its significant mineralization in the presence of 0.5% of WNSTiO₂ photocatalyst.     

Novel synthesis of high-surface-area ordered mesoporous TiO2 with anatase framework for photocatalytic applications

Ordered mesoporous TiO₂ materials with an anatase frameworks have been synthesized by using a cationic surfactant cetyltrimethylammonium bromide (C₁₆TMABr) as a structure-directing agent and soluble peroxytitanates as Ti precursor through a self-assembly between the positive charged surfactant S⁺ and the negatively charged inorganic framework I^? (S⁺I^? type). The low-angle X-ray diffraction (XRD) pattern of the as-prepared mesoporous TiO₂ materials indicates a hexagonal mesostructure. XRD and transmission electron microscopy results and nitrogen adsorption–desorption isotherms measurements indicate that the calcined mesoporous TiO₂ possesses an anatase crystalline framework having a maximum pore size of 6.9 nm and a maximum Brunauer–Emmett–Teller specific surface area of 284 m² g^?1. This ordered mesoporous anatase TiO₂ also demonstrates a high photocatalytic activity for degradation of methylene blue under ultraviolet irradiation.     

Doping level effect on visible-light irradiation W-doped TiO2–anatase photocatalysts for Congo red photodegradation

A series of W-modified TiO₂ (W–TiO₂) photocatalysts were synthesized by a simple sol–gel method. The new photocatalysts were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV–vis-diffuse reflectance spectroscopy (DRS), and Brunauer, Emmett and Teller (BET) surface area analyzer. The photoactivity of the W–TiO₂ photocatalysts was evaluated by the photocatalytic oxidation of Congo red (CR) dye. It was found that the average size of the prepared photocatalysts is 10 nm. Moreover, they have high surface areas (∼ 216 m² g⁻¹) and their light-absorption extends to the visible region compared to pure TiO₂. The effects of W-loading and of the calcination temperature of the prepared photocatalysts on their photocatalytic activity were also studied. The obtained results show that the W_0.5–TiO₂ photocatalyst calcined at 350 °C is much highly photoactive than non-doped or highly doped TiO₂. The enhanced photocatalytic activity of the weakly doped TiO₂ may be attributed to the increase in the charge separation efficiency and the presence of surface acidity on the W_0.5–TiO₂ photocatalyst.     

Synthesis of solar light driven nanorod-zinc oxide for degradation of rhodamine B,industrial effluent and contaminated river water

Surface water contamination by various dyes and pigments is a global problem caused by rapid industry, particularly textile/dyeing. Bangladesh's export-oriented textile sector has exploded in recent decades, polluting local waterways significantly. In this study, nano-ZnO were prepared using surfactant-assisted sol–gel, hydrothermal and thermal methods. SEM, XRD, reflectance spectrophotometer, EDS and adsorption tests were used to characterize the synthesized nano-ZnO. BET isotherms were used to determine the surface area, pore volume, and pore size of the as-prepared nano-ZnO. The mixed surfactant assisted-sol gel method produced nanorod-ZnO, whereas the hydrothermal and/or thermal methods yielded clusters of needles ZnO, as proven by SEM images. XRD data revealed that the synthesized nanorod-ZnO had a mainly wurtzite crystalline structure and their size was estimated using the Scherrer equation to be about 23.90 nm. EDS spectra confirmed the synthesis of pure nanorod-ZnO. Using a UV–visible reflectance spectrophotometer, the band gap energy of the as-prepared nanorod-ZnO was found to be 3.35 eV. According to BET isotherms, the BET and Langmuir surface areas were 4 and 5.4 m²/g, respectively. Prior to analyzing photodegradation, the RB was adsorbing in the presence of various doses of the nanorod-ZnO in the dark, but no adsorption was observed. The photocatalytic activities of the synthesized nano-ZnO were compared to TiO₂ (anatase) for the degradation of RB in an aqueous system under solar light, UV, fluorescence, and tungsten filament light irradiation. Nanorod-ZnO showed exceptional photocatalytic activity in degrading RB in an aqueous solution under solar light irradiation. The results suggest that 0.01 g/50 mL nanorod-ZnO with a solution pH of 7.8 is the best combination for complete degradation of 2.00 × 10^-5 M RB under solar light irradiation. When nano-ZnO was exposed to light, the inhibiting effect of ethanol and/or tert-butanol on the degradation of RB confirmed the formation of mostly hydroxyl free radicals. The synthesized nanorod-ZnO shown substantial photocatalytic activity in the removal of pollutants from industrial effluents and contaminated river water under solar light irradiation. A mechanism of excellent photocatalytic activity of the nanorod-ZnO is discussed.     

Thermal plasma synthesis of nanotitania and its characterization

Titanium dioxide (TiO₂) nanoparticles were prepared by the thermal plasma synthesis; which give a highly crystalline product. Their morphological studies are carried out by using techniques like SEM, EDAX, TEM and SEAD. Crystal size was calculated by XRD using Scherrer equation; which is observed at two current amperes; at 80 A size ranges between 25 and 30 nm and at 120 A size ranges between 30 and 42 nm. Composition analysis was done by TEM–EDAX, FTIR and Fast Fourier Transform techniques. The FTIR peaks clearly show that synthesized TiO₂ nanoparticles are in anatase phase; this phase is generally preferred because of its high photocatalytic activity, since it has a more negative conduction band edge potential (higher potential energy of photogenerated electrons), high specific area, nontoxic, photochemically stable and relatively in expensive.     

The Preparation of Dye Sensitized Solar Cell (DSSC) from TiO2 and Tamarillo Extract

Energy crisis is what being faced by every country today. Many efforts have been devoted to overcome the problems. One of several offered solutions is to develop solar cells (SCs) since solar energy is abundant and free to use. Especially in a tropical country like Indonesia, solar energy is available a whole year with quite high power 450 mWcm^-2. Several types of SCs, especially silicon-based, have been mass-produced and applied in our daily life. Silicon-based SC has high efficiency yet has high price. Dye Sensitized Solar Cell is an inexpensive type of SC. The natural ingredients could be utilized as dyes for DSSC. In this research, tamarillo extract was employed as the dye for TiO₂-based DSSC. TiO₂ powder was spin-coated on top of Fluorine- Doped Tin Oxide (FTO) conductive glass and calcined at 550 ̊C, 650 ̊C and 750 ̊C each for 60 and 120 min. Scanning ElectronMicroscope (SEM) and X-Ray Diffractometer (XRD) were used to characterize the morphology and structure of the material. Brunauer-Emmet-Teller (BET) analysis was utilized to measure the material active surface area. As the result, the sample calcined at 650 ̊C for 60 minutes showed the highest electrical performance of 542.5 mV and 0.356 mAcm^-2 which corresponded to an SC efficiency of 0.043%. This result was supported by the BET analysis showing the sample calcined at 650 ̊C for 60 min had the largest active surface area of 9.3 m²g^-1. A large active surface area enabled more dye and electrolyte to be stored inside the material so that photon adsorptions from solar energy became more effective and resulting in higher efficiency. Despite of the small efficiency, this work demonstrated the opportunities of tamarillo and TiO₂ to be applied as a DSSC.     

Facile preparation of large aspect ratio ellipsoidal anatase TiO2 nanoparticles and their application to dye-sensitized solar cell

A simple one-step heat-treatment of peroxotitanate complex aqueous solution at around 100 °C was resulted in the formation of ellipsoidal anatase TiO₂ nanoparticles having a high aspect ratio with no branches. The length of these ellipsoidal TiO₂ falls in the range of 200–350 nm, depending on mole ratio of Ti⁴⁺/H₂O₂. Dye-sensitized solar cell based on these ellipsoidal nanocrystalline TiO₂ as photoanode was fabricated and characterized.     

Photocatalytic activity of nitrogen and copper doped TiO2 nanoparticles prepared by microwave-assisted sol-gel process

Cu and N-doped TiO₂ photocatalysts were synthesized from titanium (IV) isopropoxide via a microwave-assisted sol-gel method. The synthesized materials were characterized by X-ray diffraction, UV-vis diffuse reflectance, photoluminescence (PL) spectroscopy, SEM, TEM, FT-IR, Raman spectroscopy, photocurrent measurement technique, and nitrogen adsorption–desorption isotherms. Raman spectra and XRD showed an anatase phase structure. The SEM and TEM images revealed the formation of an almost spheroid mono disperse TiO₂ with particle sizes in the range of 9-17 nm. Analysis of N₂ isotherm measurements showed that all investigated TiO₂ samples have mesoporous structures with high surface areas. The optical absorption edge for the doped TiO₂ was significantly shifted to the visible light region. The photocurrent and photocatalytic activity of pure and doped TiO₂ were evaluated with the degradation of methyl orange (MO) and methylene blue (MB) solution under both UV and visible light illumination. The doped TiO₂ nanoparticles exhibit higher catalytic activity under each of visible light and UV irradiation in contrast to pure TiO₂. The photocatalytic activity and photocurrent ability of TiO₂ have been enhanced by doping of the titania in the following order: (Cu, N) - codoped TiO₂ > N-doped TiO₂ > Cu-doped TiO₂ > TiO₂. COD result for (Cu, N)-codoped TiO₂ reveals ∼92% mineralization of the MO dye on six h of visible light irradiation.     

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.     

The improved photocatalytic properties of P-type NiO loaded porous TiO2 sheets prepared via freeze tape-casting

For the interest of the practical application, porous TiO₂ sheets were prepared by a novel freeze tape-casting method, in order to improve the photocatalytic activities of these TiO₂ sheets, p-type NiO was loaded by chemical solution deposition. The samples were characterized by a series of physical means, including XRD, SEM, EDS, XPS, ICP-OES, and UV-vis spectroscopy. The photocatalytic activities of the samples were evaluated by the degradation of methyl orange solution. The results showed that the photocatalytic activity of the TiO₂ sheet was greatly enhanced by the NiO loading, and the photocatalytic efficiency increased with increasing the NiO loading, the extraordinary performance for the NiO-loaded sample with 0.1 M precursor dipped was related to its unique morphology. The sample annealed at 600 °C showed the better photocatalytic activity than the sample annealed at 400 °C and 800 °C. The improvement of the photocatalytic activity was attributed to the formation of p–n junctures at the interface of the NiO/TiO₂, which facilitates the photoinduced electron/hole pairs' separation by the inner electric field, thus leading to the higher photocatalytic activities for the NiO-loaded TiO₂ sheets.     

X-ray induced photocatalysis on TiO2 and TiO2 nanotubes: Degradation of organics and drug release

The photocatalytic activity of titanium dioxide under X-ray radiation is of great interest for biomedical applications. In the present work we explore the use of compact TiO₂ layers and TiO₂ nanotubes for X-ray induced photocatalysis, in particular the degradation of organics and monolayer chain scission for drug release. The radiation was done with a conventional X-ray source and doses up to 50 × 10^?3 J/kg. The results show the feasibility of X-ray catalysis on TiO₂ and X-ray induced monolayer chain scission by the release of surface attached Zn–porphyrin molecules. Furthermore, a higher efficiency for anatase films and nanotubes is obtained than for amorphous morphologies.     

Photoinduced hydrophilic and photocatalytic response of hydrothermally grown TiO2 nanostructured thin films

It is demonstrated that nanostructured titanium (IV) oxide (TiO₂) films can be deposited on glass substrates at 95 °C using hydrothermal growth, their properties being greatly affected by the substrate materials. Anatase TiO₂ films grown on ITO for deposition period of 50 h were observed to exhibit a very efficient, reversible light-induced transition to super-hydrophilicity, reaching a nearly zero contact angle. Enhanced photocatalytic activity (65%) was found for the rutile TiO₂ samples grown on microscope glass, possibly due to their higher roughness with respect to anatase grown on ITO. The effect of the substrate material used is discussed in terms of the TiO₂ phase and morphology control, for the best photoinduced hydrophilic and photocatalytic performance of the samples.     

Synthesis and studies on photochromic properties of vanadium doped TiO2 nanoparticles

Pure and (0.5–3 at%) vanadium doped TiO₂ nanoparticles have been synthesized by wet chemical method. The as synthesized materials have been characterized by using XRD, atomic force microscope (AFM), Raman, EPR and UV–vis spectroscopy techniques. From XRD studies, both pure as well as vanadium doped TiO₂ have been found to show pure anatase phase. The value of lattice constant c is smaller in doped TiO₂ as compared to undoped and has been found to decrease with increase in vanadium concentration. AFM studies show formation of spherical particles with particle size ～23 nm in all the samples. Photochromic behavior of these materials has been studied by making their films in alkyd resin. Vanadium doped TiO₂ films show reversible change in color from beige-yellow to brownish violet on exposure to UV light. The mechanism of coloration and bleaching process has been discussed.     

Preparation of TiO2 nanocrystallites by hydrolyzing with gaseous water and their photocatalytic activity

TiO₂ nanocrystallites were prepared from precursors tetra-n-butyl titanate (Ti(OC₄H₉)₄) and titanium tetrachloride (TiCl₄). The precursors were hydrolyzed by gaseous water in autoclave, and then calcined at predetermined testing temperatures. The samples were characterized by X-ray diffraction (XRD), thermogravimetry–differential thermal analysis (TG–DTA), field emission scanning electron microscopy (FE-SEM), Fourier transform infrared spectra (FT-IR), and UV–vis diffuse reflectance spectra (DRS). The photocatalytic activities of the samples were evaluated by the photobleaching of methylene blue (MB) in aqueous solution and the photocatalytic oxidation of propylene in gas phase at ambient temperature. The results showed that the anatase phase nanocrystalline TiO₂ could be obtained at relatively low temperatures (for precursor Ti(OC₄H₉)₄ at 110 °C and for TiCl₄ at 140 °C, respectively), and that the as prepared samples exhibited high photocatalytic activities to photobleach MB in aqueous solution. As the calcination temperatures increasing, the decolor ratio of MB increased and reached the maximum value of nearly 100% at 600 °C, and then decreased. The photobleaching of MB by all samples followed the pseudo-first-order kinetics with respect to MB concentration. The photodecomposition amount of propylene by TiO₂ nanocrystallites calcined at 600 °C from precursor of Ti(OC₄H₉)₄ is 21.6%, which is approaching to that by Degussa P25 TiO₂ (24.9%).     

Effects of NH 4 + and Cl− on the preparation of nanocrystalline TiO2 by hydrothermal method

Nanocrystalline TiO₂ powders with different morphologies and grain sizes were successfully synthesized by the hydrothermal method. Different concentrations of hydrochloric acid (HCl), ammonium chloride (NH₄Cl), ammonium sulfate [(NH₄)₂SO₄], and ammonium carbonate [(NH₄)₂CO₃] were used as additives in the hydrothermal process to investigate the effect of the concentration of ammonium (NH ₄ ⁺ ) and chloride ions (Cl^?) on the phase compositions, morphologies, and grain sizes of the prepared TiO₂. The as-synthesized samples were characterized by X-ray diffraction (XRD), transmission electron microscopy, Brunauer–Emmett–Teller analysis, and UV–Vis spectra. XRD results show that the as-synthesized powders are composed of anatase or a mixture of anatase and brookite. The grain size of the synthesized nano-TiO₂ powder ranged from 5.0 to 11.3 nm, and the related BET specific surface area varied from 127.5 to 191.0 m²/g. The photocatalytic activities of the prepared TiO₂ powders were evaluated by degradation of methylene blue (MB) in aqueous solution under UV light irradiation, and the results show that the photocatalytic performance of TiO₂ powders synthesized with additives is improved compared with that of TiO₂ prepared without any additives.     

Simultaneous growth of rutile TiO2 as 1D/3D nanorod/nanoflower on FTO in one-step process enhances electrochemical response of photoanode in DSSC

Simultaneous growth of 1D/3D-nanorod/nanoflower like structures of TiO₂ on fluorine doped tin oxide (FTO) glass substrates has been achieved in one-step hydrothermal process. X-ray diffraction (XRD) pattern confirms the formation of rutile phase whereas enhanced light scattering in 1D/3D nanorod/nanoflower TiO₂ photoanode was observed at longer wavelengths of 600–750 nm. Dye sensitized solar cell (DSSC) prepared with 1D/3D-nanorod/nanoflower structures had about 90% increases in efficiency as compared to 1D nanorod like structure. Thus, simultaneous assembly of TiO₂ as 1D/3D-nanorod/nanoflower like structure without significant change in their surface oxidation states (Ti^3 + and Ti^4 +) had better capabilities for light harvesting and efficient electron transportation for improving electrochemical responses of photo-electrode in DSSC to achieve higher sensitivity.     

Fabrication and electrochemical performance of nickel ferrite nanoparticles as anode material in lithium ion batteries

Nano-sized nickel ferrite (NiFe₂O₄) was prepared by hydrothermal method at low temperature. The crystalline phase, morphology and specific surface area (BET) of the resultant samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and nitrogen physical adsorption, respectively. The particle sizes of the resulting NiFe₂O₄ samples were in the range of 5–15 nm. The electrochemical performance of NiFe₂O₄ nanoparticles as the anodic material in lithium ion batteries was tested. It was found that the first discharge capacity of the anode made from NiFe₂O₄ nanoparticles could reach a very high value of 1314 mAh g⁻¹, while the discharge capacity decreased to 790.8 mAh g⁻¹ and 709.0 mAh g⁻¹ at a current density of 0.2 mA cm⁻² after 2 and 3 cycles, respectively. The BET surface area is up to 111.4 m² g⁻¹. The reaction mechanism between lithium and nickel ferrite was also discussed based on the results of cycle voltammetry (CV) experiments.     

The effect of silver doping on photocatalytic properties of titania multilayer membranes

In this investigation an Ag doped titania multilayer membrane is successfully fabricated via the sol–gel processing method. The doped membrane is characterized via X-ray Diffraction and N₂-sorption techniques and the photocatalytic properties of the membrane are investigated via methyl orange degradation. The properties included high surface area (101 m²/g), small pore size (3.1 nm), and active anatase crystal phase. The prepared titania membrane has a high photocatalytic activity and decomposes methyl orange by 50% after 9 h of UV irradiation. The prepared membrane can be applied in the development of efficient photocatalytic systems for the treatment of water. Due to the high photoactivity of the prepared titania membrane, this study reveals the possibility of combining two processes for removal of organic pollutants: the photocatalytic process and the membrane separation process. In the combining process the lifetime of the membrane increases and the quality of water is enhanced.     

Fibriform polyaniline/nano-TiO2 composite as an electrode material for aqueous redox supercapacitors

Fibriform polyaniline/nano-TiO₂ composite is prepared by one-step in situ oxidation polymerization of aniline in the presence of nano-TiO₂ particles, which contains 80% conducting polyaniline by mass, with a conductivity of 2.45 S/cm at 25 °C. Its maximum specific capacitance is 330 F g^?1 at a constant current density of 1.5 A g^?1, and can be subjected to charge/discharge over 10,000 cycles in the voltage range of 0.05–0.55 V.     

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.