An easier method of preparation of mesoporous anatase TiO2 nanoparticles via ultrasonic irradiation

Mesoporous anatase TiO₂ nanopowder was synthesised by the sol–gel method using ultrasonic irradiation. This method is simple and faster for the synthesis of phase pure mesoporous anatase TiO₂ nanopowder. The product is characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron spectroscopy (TEM), thermo gravimetric analysis, Brunauer–Emmett–Teller (BET) surface area, UV–visible diffuse reflectance spectroscopy and Fourier transform infrared spectroscopy. Analysis of XRD patterns, SEM and TEM image shows that the average particles size is of 19.9 nm and has an anatase structure. The mesoporous nature was determined by the BET method using the Barrett–Joyner–Halenda (BJH) model.     

Preparation of N-methylaniline capped mesoporous TiO2 spheres by simple wet chemical method

Pure anatase mesoporous TiO₂ nanospheres were synthesized by simple wet chemical treatment and characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet–visible spectroscopy (UV–vis), Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (XRD). The results revealed that the surface morphology of the TiO₂ spheres could be controlled by adjusting the concentration of N-methylaniline and that the average diameter of the TiO₂ spheres was 600 nm. FTIR results confirmed the formation of N-methylaniline capped TiO₂ nanospheres.     

Combustion synthesized TiO2 for enhanced photocatalytic activity under the direct sunlight-optimization of titanylnitrate synthesis

Optimized synthesis of Ti-precursor ‘titanylnitrate’ for one step combustion synthesis of N- and C-doped TiO₂ catalysts were reported and characterized by using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), diffused reflectance UV–vis spectroscopy, N₂ adsorption and X-ray photoelectron spectroscopy (XPS). XRD confirmed the formation of TiO₂ anatase and nano-crystallite size which was further confirmed by TEM. UV-DRS confirmed the decrease in the band gap to less than 3.0 eV, which was assigned due to the presence of C and N in the framework of TiO₂ as confirmed by X-ray photoelectron spectroscopy. Degradation of methylene blue in aqueous solution under the direct sunlight was carried out and typical results indicated the better performance of the synthesized catalysts than Degussa P-25.     

Enhanced visible light activity and mechanism of TiO2 codoped with molybdenum and nitrogen

Mo-N-codoped TiO₂ was synthesized by using ammonium molybdate tetrahydrate and ammonia water as the sources of Mo and N, respectively. The resulting materials were characterized by X-ray diffraction (XRD), X-photoelectron spectroscopy (XPS) and UV–vis light diffuse reflection spectroscopy (DRS). Furthermore, the activity enhanced-mechanism was proposed. XRD results indicated that codoping favored the formation of anatase and improved the anatase crystallinity. XPS analysis revealed that N was incorporated into the lattice of TiO₂ through substituting lattice O and coexisted in the substitutional forms. Meanwhile, Mo was incorporated into the lattice of TiO₂ through substituting Ti and coexisted in the forms of Mo⁶⁺ and Mo⁵⁺. DRS showed that the light absorption in visible region was improved by co-doping, leading to a narrower band gap and higher visible activity for the degradation of phenol than that of others. The enhanced activity was attributed to the high anatase crystallinity, large amount of surface oxygen vacancies, intense light absorption and narrow band gap.     

An ionic liquid route to prepare mesoporous ZrO2–TiO2 nanocomposites and study on their photocatalytic activities

Mesostructured ZrO₂–TiO₂ nanoparticles with different ZrO₂ contents have been synthesized by an ionic liquid-assisted hydrothermal route. The prepared materials were characterized by means of X-ray diffraction (XRD), nitrogen adsorption–desorption, transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectra analysis (DRS) and NH₃-TPD technique. The obtained ZrO₂–TiO₂ materials exhibit large specific surface area and uniform pore sizes. Introduction of ZrO₂ species can effectively suppress phase transformation from anatase to rutile and promote thermal stability of ZrO₂–TiO₂ materials. The photocatalytic activity of the ZrO₂–TiO₂ sample is higher than that of the TiO₂ sample and commercially available Degussa P25. The high photocatalytic activity can be attributed to stronger adsorption in the ultraviolet region, higher specific area, smaller crystal size and increased surface OH groups.     

Study on activities of vanadium (IV/V) doped TiO2(R) nanorods induced by UV and visible light

Vanadium (IV/V) doped rutile TiO₂ naonorods had been successfully synthesized through a single step hydrothermal method. The photocatalyst was characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), UV–vis diffusive reflectance spectroscopy (DRS) and X-ray photoelectron spectroscopy (XPS). The results showed that the doping of V ions had significant influence on the band gap energy and the surface state of TiO₂. The photo-activities of the new catalysts were investigated under ultraviolet (UV) and visible light. The UV-photocatalytic activity of the as-prepared catalysts was hardly influenced by doping V ions; while under visible light, the samples with 1 wt% and 0.1 wt% V exhibited enhanced activity to the oxidation of methylene blue (MB) and the reduction of Cr (VI), respectively.     

Phosphomolybdic acid-modified highly organized TiO2 nanotube arrays with rapid photochromic performance

TiO₂ nanotube arrays were prepared by means of an electrochemical anodization technique in an organic electrolyte solution doped with polyvinyl pyrrolidone (PVP) and were subsequently modified with phosphomolybdic acid (PMoA) to obtain PMoA/TiO₂ nanotube arrays. The microstructure and photochromic properties were investigated via X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet–visible spectroscopy (UV–vis), and X-ray photoelectron spectroscopy (XPS). The results indicated that the Keggin structure of PMoA and the nanotube structure of TiO₂ were not destroyed, and there was a strong degree of interaction between PMoA and TiO₂ at the biphasic interface with lattice interlacing during the compositing process. The XPS results further indicated that there was a change in the chemical microenvironment during the formation process of the composite, and a new charge transfer bridge was formed through the Mo-O-Ti bond. Under visible light irradiation, the colorless PMoA/TiO₂ nanotube array quickly turned blue and exhibited a photochromic response together with reversible photochromism in the presence of H₂O₂. After visible light irradiation for 60 s, the appearance of Mo⁵⁺ species in the XPS spectra indicated a photoreduction process in accordance with a photoinduced electron transfer mechanism.     

Preparation and characterization of Cu-doped TiO2 nanomaterials with anatase/rutile/brookite triphasic structure and their photocatalytic activity

Pure TiO₂ and Cu–doped TiO₂ containing different amounts of copper ions with anatase/rutile/brookite triphasic structure were successfully synthesized through a simple hydrothermal method. The obtained samples were characterized by X–ray diffraction (XRD), Raman spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), X–ray photoelectron spectroscopy (XPS), UV?vis diffuse reflectance spectroscopy (UV-DRS), photoluminescence spectroscopy (PL) and Brunauer–Emmett–Teller surface area analyze (BET). Both pure and Cu–doped TiO₂ show relatively high photocatalytic activity owing to their considerable surface areas. Moreover, the three–phase coexisting structure and the conversion between Cu²⁺ and Cu⁺ ions facilitate the separation of photogenerated electrons and holes, which is favorable for photocatalytic performance. 1%Cu–TiO₂ exhibits the highest photocatalytic activity and the degradation degree of rhodamine B (RhB) reaches 93.5% after 30 min, which is higher than that of monophasic/biphasic 1%Cu–TiO₂. ·O₂^? radical is the main active species, and h⁺ and ·OH species are subsidiary in the degradation process.

     

Visible light photoelectrocatalysis with salicylic acid-modified TiO2 nanotube array electrode for p-nitrophenol degradation

This research focused on immersion method synthesis of visible light active salicylic acid (SA)-modified TiO₂ nanotube array electrode and its photoelectrocatalytic (PEC) activity. The SA-modified TiO₂ nanotube array electrode was synthesized by immersing in SA solution with an anodized TiO₂ nanotube array electrode. Scanning electron microscope (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (IR), UV–vis diffuse reflectance spectrum (DRS), and Surface photovoltage (SPV) were used to characterize this electrode. It was found that SA-modified TiO₂ nanotube array electrode absorbed well into visible region and exhibited enhanced visible light PEC activity on the degradation of p-nitrophenol (PNP). The degradation efficiencies increased from 63 to 100% under UV light, and 79–100% under visible light (λ > 400 nm), compared with TiO₂ nanotube array electrode. The enhanced PEC activity of SA-modified TiO₂ nanotube array electrode was attributed to the amount of surface hydroxyl groups introduced by SA-modification and the extension of absorption wavelength range.     

Photocatalytic degradation and mineralization of dye pollutants from wastewater under visible light using synthetic CuO-VO2/TiO2 nanotubes/nanosheets

CuO-VO₂/TiO₂ as a new nanocomposite was synthesized through hydrothermal method and identified by various spectroscopic techniques including X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray analysis (EDX), UV–visible, differential reflectance spectroscopy (DRS), and Mott–Schottky. The presence of nanotubes/nanosheets in the synthesized nanocomposite was confirmed by HR-TEM. The anatase and rutile crystalline forms of TiO₂ were detected by Raman spectroscopy and X-ray diffraction (XRD). XPS analysis confirmed the presence of CuO and VO₂ in the nanocomposite. The surface area and the band-gap energy of the nanocomposite were determined via N₂ adsorption–desorption analysis and DRS. The presence of a p–n junction between TiO₂ (n-type) and CuO/VO₂ (p-type) was confirmed by the Mott–Schottky analysis. The photocatalytic activity of the nanocomposite against methylene blue (MB), methyl orange (MO), and cango red (CR) was studied under visible-light irradiation. The times of degradation for the decomposition of the dyes were 10–25 min. The rate constants of degradation for MB, MO, and CR were calculated as 0.34, 0.090, and 0.155 min^?1, respectively. The catalyst was recovered four times. In addition, the mineralization of the dyes was investigated by chemical oxygen demand (COD). The reaction was performed in the presence of different radical scavengers, and the ·OH was found to be the predominantly active species in the photodegradation of the dyes.

     

Green synthesis of zinc oxide nanoparticles using tomato (Lycopersicon esculentum) extract and its photovoltaic application

With an increasing awareness of green and clean energy, zinc oxide-based solar cells were found to be suitable candidates for cost-effective and environmentally friendly energy conversion devices. In this paper, we have reported the green synthesis of zinc oxide nanoparticles (ZnONPs) by thermal method and under microwave irradiation using the aqueous extract of tomatoes as non-toxic and ecofriendly reducing material. The synthesised ZnONPs were characterised by UV–visible spectroscopy (UV–vis), infra-red spectroscopy, particle size analyser, scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction study (XRD). A series of ZnO nanocomposites with titanium dioxide nanoparticles (TiO₂) and graphene oxide (GO) were prepared for photovoltaic application. Structural and morphological studies of these nanocomposites were carried out using UV–vis, SEM, XRD and AFM. The current–voltage measurements of the nanocomposites demonstrated enhanced power conversion efficiency of 6.18% in case of ZnO/GO/ TiO₂ nanocomposite.     

Fabrication and characterization of nano TiO2 thin films at low temperature

Anatase TiO₂ thin films were successfully prepared on glass slide substrates via a sol–gel method from refluxed sol (RS) containing anatase TiO₂ crystals at low temperature of 100 °C. The influences of various refluxing time on crystallinity, morphology and size of the RS sol and dried TiO₂ films particles were discussed. These samples were characterized by infrared absorption spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission-scanning electron microscopy (FE-SEM) and UV–vis absorption spectroscopy (UV–vis). The photocatalytic activities of the TiO₂ thin films were assessed by the degradation of methyl orange in aqueous solution. The results indicated that titania films thus obtained were transparent and their maximal light transmittance exceeded 80% under visible light region. The TiO₂ thin films prepared from RS-6 sol showed the highest photocatalytic activity, when the calcination temperature is higher than 300 °C. The degradation of methyl orange of RS-6 thin films reached 99% after irradiated for 120 min, the results suggested that the TiO₂ thin films prepared from RS sol exhibited high photoactivities.     

Synthesis,characterisation, and effect of pH on degradation of dyes of copper-doped TiO2

Copper-doped TiO₂ nanoparticles were synthesised using an ultrasonic-assisted sol–gel method with various doping concentrations from 0 to 2.5 at.%. The samples were characterised by X-ray diffraction, UV–vis diffuse reflectance spectroscopy (UV–vis), transmission electron microscopy (TEM), Brunauer–Emmett–Teller surface area determination, and zeta potential. The presence of copper in TiO₂ crystal structure was revealed by UV–vis spectra, and the TEM analysis showed that particles are mainly spherical around the size range of 15–20 nm. In addition, doping copper into TiO₂ lattice caused a decrease in the surface area due to the aggregation of nanoparticles and a shift of isoelectric point towards lower pH when the dopant concentration increased. The photocatalytic reactivity of these materials was evaluated by the degradation of methylene blue and methyl orange under the UV light. The effect of the initial solution pH on the adsorption capacity and the photocatalytic behaviour of the Cu-doped TiO₂ in the decolourisation of these dyes were also studied.     

Synthesis and characterization of N-doped TiO2/ZrO2 visible light photocatalysts

Zirconia and nitrogen-doped TiO₂ powder was synthesized using a polymer complex solution method for the preparation of an enhanced visible light photocatalyst. The produced catalysts were characterized via the Brunauer, Emmett, and Teller method (BET), X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, and UV–Vis spectrophotometry analyses. The N-doped TiO₂/ZrO₂ photocatalyst showed a high specific surface area and small crystal sizes. The XPS spectra of the N-doped TiO₂/ZrO₂ sample indicated that nitrogen was doped into the TiO₂ lattice and enhanced the photocatalytic activity. The UV–Vis absorption spectra of the N-doped TiO₂/ZrO₂ sample noticeably shifted to the visible light region compared to that of the TiO₂. The photocatalytic activities of the prepared catalysts were evaluated for the decomposition of gaseous NO_x under UV and visible light irradiations. The photocatalytic activities of N-doped TiO₂/ZrO₂ were much greater than those of commercial Degussa P25 in both the UV and visible light regions. The high photocatalytic activity can be attributed to stronger absorption in the visible light region, a greater specific surface area, smaller crystal sizes, more surface OH groups, and to the effect of N-doping, which resulted in a lower band gap energy.     

One-pot low-temperature synthesis of BiOX/TiO2 hierarchical composites of adsorption coupled with photocatalysis for quick degradation of colored and colorless organic pollutants

BiOX/TiO₂ (X = Cl, Br, and I) hierarchical composites with superior photoelectrochemical performances were successfully synthesized by one-pot low-temperature solvothermal process without any structure-directing agents. The dual functions of adsorption coupled with photocatalysis based on BiOX/TiO₂ were fully exhibited in terms of the quick degradation of colored and colorless organic pollutants (OPs). The as-prepared composites were characterized by field-emitting scanning electron microscope (FESEM), X-ray power diffraction (XRD) analysis, transmission electron microscope (TEM), N₂ adsorption/desorption, UV–vis diffuse reflectance spectra (DRS), photoluminescence spectra (PL), photocurrent measurements (PC), and electrochemical impedance spectroscopy (EIS), respectively. As-prepared BiOX/TiO₂ composites exhibited outstanding photoelectrochemical activities. Especially, the considerably enhanced adsorption and photocatalytic efficiencies were observed in the optimized BiOCl/TiO₂ composites compared to their counterparts. The improvement of adsorption and photocatalytic performances should be ascribed to the presence of columbite TiO₂-II in anatase, which would not only improve the ability of absorbing visible light and the charge separation efficiency, but also to effectively tailor the particle size, surface area and the exposed active facet of composites.     

Characterization and photoactivity of TiO2 sols prepared with triethylamine

Using triethylamine as a surface protective agent, a transparent and pale yellowish TiO₂ sol had been prepared at 90 °C. This method was very different from the traditional methods, which produced titanium dioxide nanoparticles with anatase crystalline structure either at high acid condition or high temperature. X-ray diffraction (XRD) and transmission electron spectroscopy (TEM) demonstrated that the as-prepared TiO₂ sol nanoparticles with anatase crystalline structure were uniformly distributed, and the average size was 3 nm. X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectra showed that triethylamine was adsorbed on TiO₂ sol particles surface. FTIR spectroscopy noted that TiO₂ sol particles had the similar spectra with Degussa P25. Photoactivity of the as-prepared TiO₂ sol was studied by investigating the photodegradation of methyl violet in hydrosol reaction system under visible light irradiation.     

Preparation,characterization and photocatalytic activity of TiO2 codoped with yttrium and nitrogen

Nanocrystalline photocatalysts of TiO₂ codoped with yttrium and nitrogen were prepared by the sol–gel method and investigated by X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), the Brunauer–Emmett–Teller (BET) surface area measurement, X-ray photoelectron spectroscopy (XPS) and ultraviolet–visible diffuse reflectance spectroscopy (UV–vis DRS), respectively. Slight red-shifts of the Raman peak at 144 cm^?1 were observed in the doped samples after the incorporation of Y³⁺ and N^3? into the lattice of TiO₂. The N doping caused the improvement of visible light absorption because of the formation of the N 2p states isolated above the valence band maximum of TiO₂. Whereas, the absorption property of the pure or N doped TiO₂ was depressed after the introduction of Y. The photocatalytic activities of the samples were evaluated by monitoring the degradation of methylene blue (MB) solution. The codoped sample with N and 0.05 at.% Y exhibited an enhanced photocatalytic efficiency. It is suggested that the charge trapping due to the Y doping and the visible light response due to the N doping are responsible for the enhanced photocatalytic performance in this sample. However, the photocatalytic activity of the codoped TiO₂ was suppressed step by step as the Y doping level increased, which could be attributed to the formation of photogenerated charge carriers recombination centers at the Y substituting sites.     

Synthesis and photocatalytic properties of TiO2 nanostructures

TiO₂ particles, rods, flowers and sheets were prepared by hydrothermal method via adjusting the temperature, the pressure and the concentration of TiCl₄. The as-prepared TiO₂ powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV–vis diffuse reflectance spectra and N₂ adsorption–desorption measurements. It was found that pressure is the most important factor influencing the morphology of TiO₂. The photocatalytic activity of the products was evaluated by the photodegradation of aqueous brilliant red X-3B solution under UV light. Among the as-prepared nanostructures, the flower-like TiO₂ exhibited the highest photocatalytic activity.     

Visible-light absorption and photocatalytic activity of Cr-doped TiO2 nanocrystal films

Chromium doped titanium dioxide (TiO₂) nanocrystal films with various doping concentration have been successfully prepared by a sol–gel dip-coating process. These films have been characterized by XRD, XPS, AFM, and UV–vis absorption spectroscopy. It is found that Cr doping can effectively reduce the transition temperature of anatase to rutile phase as well as the grain size. The absorption edges of TiO₂ thin films shift towards longer wavelengths (i.e. red shifted) from 375 nm to about 800 nm with increasing Cr concentration, which greatly enhances TiO₂ nano-materials on the absorption of solar spectrum. The appearance of UV–vis absorption features in the visible region can be ascribed to the newly formed energy levels such as Cr 2p level and oxygen vacancy state between the valence and the conduction bands in the TiO₂ band structure. The enhancement of the photocatalytic properties is observed for Cr-doped TiO₂ thin film.     

Sonochemical preparation of TiO2 nanoparticles in the ionic liquid 1-(3-hydroxypropyl)-3-methylimidazolium-bis(trifluoromethylsulfonyl)amide

Spherical shaped anatase nanoparticles (ø 5 nm) have been synthesized in the ionic liquid 1-(3-hydroxypropyl)-3-methylimidazolium-bis(trifluoromethanesulfonyl)amide from titanium tetraisopropoxide by ultrasound assisted synthesis under ambient conditions. XRD, EDX, TEM, XPS, Raman, UV–vis, PL and BET measurements have been employed for characterization of the nanostructure of as-prepared TiO₂. XRD and Raman measurements both show that the obtained material is crystalline with anatase structure. The morphology of TiO₂ nanoparticles was characterized by transmission electron microscopy (TEM). The bandgap of the TiO₂ nanocrystals estimated from XRD and UV–vis measurements is about 3.3 eV. The surface area of a typical sample is 177 m² g⁻¹. The synthesized anatase nanocrystals show good photocatalytic activity in the degradation of methylorange.