Synthesis of NiWO4 nano-particles in low-temperature molten salt medium

Nickel tungstate (NiWO₄) nano-particles were successfully synthesized at low temperatures by a molten salt method, and characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet visible spectra techniques (UV–vis), respectively. The effects of calcining temperature and salt quantity on the crystallization and development of NiWO₄ crystallites were studied. Experimental results showed that the well-crystallized NiWO₄ nano-particles with about 30 nm in diameter could be prepared at 270 °C with 6:1 mass ratio of the salt to NiWO₄ precursor. XRD analysis confirmed that the product was a pure monoclinic phase of NiWO₄ with wolframite structure. UV–vis spectrum revealed that NiWO₄ nano-particles had good light absorption properties in both ultraviolet and visible light region.     

SrMoO4 powders processed in microwave-hydrothermal: Synthesis, characterization and optical properties

In this work, we report on the synthesis of SrMoO₄powders by co-precipitation method and processed in a microwave-hydrothermal at 413 K for 5 h. These powders were analyzed by X-ray diffraction (XRD), Fourier transform Raman (FT-Raman), ultraviolet–visible (UV–vis) absorption spectroscopy and photoluminescence (PL). XRD analyses revealed that the SrMoO₄ powders are free of secondary phases and crystallize in a tetragonal structure. FT-Raman investigations showed the presence of Raman-active vibration modes correspondent for this molybdate. UV–vis technique was employed to determine the optical band gap of this material. SrMoO₄ powders exhibit an intense PL emission at room temperature with maximum peak at 540 nm (green region) when excited by 488 nm wavelength of an argon ion laser.     

Effect of TiO2 particle size on the photocatalytic reduction of CO2

Pure TiO₂ anatase particles with a crystallite diameters ranging from 4.5 to 29 nm were prepared by precipitation and sol–gel method, characterized by X-ray diffraction (XRD), BET surface area measurement, UV–vis and scanning electron microscopy (SEM) and tested in CO₂ photocatalytic reduction. Methane and methanol were the main reduction products. The optimum particle size corresponding to the highest yields of both products was 14 nm. The observed optimum particle size is a result of competing effects of specific surface area, charge–carrier dynamics and light absorption efficiency.     

Microstructure and optical properties of nanocrystalline Cu2O thin films prepared by electrodeposition

Cuprous oxide (Cu₂O) thin films were prepared by using electrodeposition technique at different applied potentials (−0.1, −0.3, −0.5, −0.7, and −0.9 V) and were annealed in vacuum at a temperature of 100°C for 1 h. Microstructure and optical properties of these films have been investigated by X-ray diffractometer (XRD), field-emission scanning electron microscope (SEM), UV-visible (vis) spectrophotometer, and fluorescence spectrophotometer. The morphology of these films varies obviously at different applied potentials. Analyses from these characterizations have confirmed that these films are composed of regular, well-faceted, polyhedral crystallites. UV–vis absorption spectra measurements have shown apparent shift in optical band gap from 1.69 to 2.03 eV as the applied potential becomes more cathodic. The emission of FL spectra at 603 nm may be assigned as the near band-edge emission.     

Photo-catalytic degradation of Rhodamine B on C-, S-, N-, and Fe-doped TiO2 under visible-light irradiation

C-, S-, N-, and Fe-doped TiO₂ photocatalysts were synthesized by a facile sol–gel method. The structure and properties of catalysts were characterized by N₂ desorption–adsorption, X-ray diffraction (XRD), UV–vis spectroscopy, and X-ray photoelectron spectroscopy (XPS). Results revealed that the surface area of the multi-doped TiO₂ was significantly increased and the crystallite size was smaller than the pure TiO₂ obtained by a similar route. Compared with TiO₂, the peak position in doped-TiO₂ XRD patterns was slightly shifted, which could be attributed to the distortion by the substitution of carbon, nitrogen, and sulfur dopants for some oxygen atoms and Fe³⁺ for Ti⁴⁺ in the lattice of TiO₂. These substitutions were confirmed by XPS. In addition, these dopants were responsible for narrowing the band gap of TiO₂ and shifting its optical response from ultraviolet (UV) to the visible-light region. The photocatalytic reactivities of these multi-doped TiO₂ catalysts were investigated by degrading Rhodamine B (RB) in aqueous solution under visible-light irradiation (λ > 420 nm). It was found out that the reactivity was significantly enhanced and the catalyst doped with nitrogen, carbon, sulfur, and 0.3 wt% iron had the highest photocatalytic activity.     

Synthesis, characterization and optical properties of Mg(OH)2 micro-/nanostructure and its conversion to MgO

Magnesium hydroxide (Mg(OH)₂) micro- and nanostructures have been synthesized by a single step hydrothermal route. Surface morphology analysis reveals the formation of micro- and nanostructures with varying shape and size at different synthesis conditions. Structural investigations by X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirm that the synthesized material is Mg(OH)₂ with hexagonal crystal structure. An optical band gap of 5.7 eV is determined for Mg(OH)₂ nanodisks from the UV–vis absorption spectrum. A broad emission band with maximum intensity at around 400 nm is observed in the photoluminescence (PL) spectra of Mg(OH)₂ nanodisks at room temperature depicting the violet emission, which can be attributed to the ionized oxygen vacancies in the material. Furthermore, Mg(OH)₂ has been converted to MgO by calcination at 450 °C. Optical studies of the MgO nanodisks have shown an optical band gap of 3.43 eV and a broadband PL emission in the UV region. Mg(OH)₂ and MgO nanostructures with wide-band gap and short-wavelength luminescence emission can serve as a better luminescent material for photonic applications.     

Microwave hydrothermal synthesis and optical properties of flower-like Bi2MoO6 crystallites

Flower-like Bi₂MoO₆ crystallites were successfully synthesized by the microwave hydrothermal process using Bi(NO₃)₃·5H₂O and Na₂MoO₄·2H₂O as source materials and adding hexamethylene tetramine (HMT) as a template. X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM) were used to characterize the products. Ultraviolet–visible (UV–vis) spectroscopy was employed to study the optical properties of Bi₂MoO₆. Results show that the product morphology is flower-like on adding the template. These flower-like Bi₂MoO₆ crystallites are a self-assembly of many thin nanoplates. HMT plays an important role in the formation of the flower-like morphology. UV–vis absorption spectra of all the Bi₂MoO₆ samples show strong photoabsorption properties from the ultraviolet region to the visible-light region with wavelength shorter than 500 nm. The band gap of flower-like Bi₂MoO₆ crystallites displays a slight red-shift compared with the Bi₂MoO₆ plate-like structures.     

Simple fabrication and photocatalytic activity of S-doped TiO2 under low power LED visible light irradiation

A series of S-doped TiO₂ with visible-light photocatalytic activity were prepared by a simple hydrolysis method using titanium tetrachloride (TiCl₄) and sodium sulfate (Na₂SO₄) as precursors. The photocatalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), UV–vis diffuse reflectance spectrophotometer (UV–Vis DRS), and X-ray photoelectron spectroscopy (XPS). With the doping of S, photocatalysts with small crystal size, high content of anatase phase were obtained. The result showed that S-doped TiO₂ demonstrate considerably high photoactivity under low power visible LED light irradiation, while undoped TiO₂ and the Degussa P25 have nearly no activity at all. The possible mechanism of S-doped for the visible-light activity was discussed.     

Morphology and Photoluminescence of HfO2 Obtained by Microwave-Hydrothermal

In this letter, we report on the obtention of hafnium oxide (HfO₂) nanostructures by the microwave-hydrothermal method. These nanostructures were analyzed by X-ray diffraction (XRD), field-emission gum scanning electron microscopy (FEG-SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDXS), ultraviolet–visible (UV–vis) spectroscopy, and photoluminescence (PL) measurements. XRD patterns confirmed that this material crystallizes in a monoclinic structure. FEG-SEM and TEM micrographs indicated that the rice-like morphologies were formed due to an increase in the effective collisions between the nanoparticles during the MH processing. The EDXS spectrum was used to verify the chemical compositional of this oxide. UV–vis spectrum revealed that this material have an indirect optical band gap. When excited with 488 nm wavelength at room temperature, the HfO₂ nanostructures exhibited only one broad PL band with a maximum at around 548 nm (green emission).     

Growth and optical properties of cerium dioxide nanocrystallites prepared by coprecipitation routes

Nanosized cerium dioxide (CeO₂) powders have been synthesized using coprecipitation methods and cerium nitrate hexahydrate (Ce(NO₃)₃·6H₂O) as the starting material. The growth and optical properties of nanosized CeO₂ powders were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), nano-beam electron diffraction (NBED), high resolution TEM (HRTEM), and ultraviolet–visible (UV–vis) absorption spectrophotometry. The XRD result shows that the dried CeO₂ precursor powders (both before and after calcination at various temperatures and times) contained a single crystalline phase of CeO₂. In the dried precursor powders, the crystallites of CeO₂ measured 10.4 nm and 66.8 nm before and after calcination at 1273 K for 240 min, respectively. The indirect band gap energy (_Ei$E_i$) of CeO₂ decreased from 3.03 eV to 2.68 eV as the crystallite size increased from 10.4 nm to 66.8 nm, whereas the direct band gap energy (_Ed$E_d$) of CeO₂ also decreased from 3.79 eV to 3.38 eV.     

Incorporation of tin in different types of pores in SBA-15: Synthesis, characterization and catalytic activity

Mesoporous Sn-SBA-15 has been synthesized by three different methods such as conventional hydrothermal route, using cocatalyst NH₄F and in the presence of organosilane precursor. All the materials are thoroughly characterized by powder X-ray diffraction (XRD), SEM, TEM, N₂ sorption and surface area measurements, diffuse-reflectance UV–visible and FTIR spectroscopy, TG–DTA and elemental analysis through ICP. Nitrogen adsorption data, XRD patterns, and TEM observations suggests that the textural properties are retained during the isomorphous substitution of silicon by tin. ICP chemical analysis indicates that tin can be substituted in the range of Si/Sn = 69–162. UV–visible spectra of samples synthesized by the cocatalytic approach exhibit unique absorption band at 213 nm characteristics of tin atom substituted in the smaller pores (2–3 nm) located inside the walls of mesopores. Further, an additional band at 224 nm can be assigned to Sn atoms located in the distorted tetrahedral position along the primary mesopores. In contrary, only one absorption band centered at 224 nm is observed for all the samples synthesized by conventional hydrothermal as well as in the presence of organosilane precursor. ¹⁹F NMR spectra confirmed (no signal) the absence of occluded F⁻ ions in the samples made with NH₄F. Observed high catalytic activity in Baeyer–Villiger oxidation and Meerwin–Pondorf–Verly reduction under the liquid-phase conditions suggest the incorporation of a portion of tin in the smaller pores for the Sn-SBA-15 materials synthesized through cocatalyst method.     

TiO2 photoactivity in vis and UV light: The influence of calcination temperature and surface properties

A series of TiO₂ photocatalysts were obtained using several calcination temperatures ranging from 350 to 750 °C. The photocatalysts’ characteristics by X-ray diffraction, UV–vis and FTIR diffuse reflectance spectroscopies, X-ray photoelectron spectroscopy, BET and BJH methods showed that sample active in vis region had anatase structure, about 200 m²/g specific surface area, absorbed light for λ > 400 nm and contained 10.1 at.% of C–C species. The photocatalytic activity of the catalysts was estimated by measuring the decomposition rate of phenol in 0.21 mM aqueous solution in visible and ultraviolet light. The experimental data clearly indicate correlation between the absorption intensity of irradiation by obtained powders and their photocatalytic performance in phenol degradation. An increase in absorbance over the entire vis region and the highest photocatalytic activity for phenol degradation in visible light (λ > 400 nm) occurred for photocatalyst calcinated at 350 °C. Photocatalyst processed at 450 °C had the best activity in UV light (250 < λ < 400 nm).     

Preparation, characterization and visible-light-driven photocatalytic activity of Fe-doped titania nanorods and first-principles study for electronic structures

Fe-doped TiO₂ (Fe-TiO₂) nanorods were prepared by an impregnating-calcination method using the hydrothermally prepared titanate nanotubes as precursors and Fe(NO₃)₃ as dopant. The as-prepared samples were characterized by scanning electron microscope, transmission electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy, N₂ adsorption–desorption isotherms and UV–vis spectroscopy. The photocatalytic activity was evaluated by the photocatalytic oxidation of acetone in air under visible-light irradiation. The results show that Fe-doping greatly enhance the visible-light photocatalytic activity of mesoporous TiO₂ nanorods, and when the atomic ratio of Fe/Ti (R_Fe) is in the range of 0.1–1.0%, the photocatalytic activity of the samples is higher than that of Degussa P25 and pure TiO₂ nanorods. At R_Fe = 0.5%, the photocatalytic activity of Fe-TiO₂ nanorods exceeds that of Degussa P25 by a factor of more than two times. This is ascribed to the fact that the one-dimensional nanostructure can enhance the transfer and transport of charge carrier, the Fe-doping induces the shift of the absorption edge into the visible-light range with the narrowing of the band gap and reduces the recombination of photo-generated electrons and holes. Furthermore, the first-principle density functional theory (DFT) calculation further confirms the red shift of absorption edges and the narrowing of band gap of Fe-TiO₂ nanorods.     

Aerosol-assisted flow synthesis of B-doped, Ni-doped and B–Ni-codoped TiO2 solid and hollow microspheres for photocatalytic removal of NO

In this study, highly effective B-doped, Ni-doped and B–Ni-codoped TiO₂ microspheres photocatalysts were directly synthesized via an aerosol-assisted flow synthesis method. The resulting samples were characterized by XRD, SEM, TEM, UV–vis diffuse reflectance spectroscopy, nitrogen adsorption and XPS. The characterizations revealed hollow microspherical structure of the B-doped and B–Ni-codoped TiO₂ photocatalysts, while the Ni-doped and undoped TiO₂ products consisted of solid microspheres. It was found that the boron dopant was partially embedded into the interstitial TiO₂ structure, existing in the form of Ti–O–B structure. The band gap was enlarged after the boron doping. However, both Ni-doped and B–Ni-codoped TiO₂ samples showed obvious red shift in their absorption edges because of the Ni doping. The photocatalytic activities of these samples were evaluated on the photocatalytic removal of NO under simulated solar light irradiation. All the aerosol-assisted flow synthesized samples had much higher photocatalytic activities than P25 and the doped TiO₂ microspheres exhibited enhanced photocatalytic activity than the undoped counterparts. More interestingly, the B–Ni-codoped TiO₂ photocatalyst possessed superior photocatalytic activity to the as-prepared single doped TiO₂ products. The enhanced photocatalytic activity was explained and the formation mechanisms of hollow and solid microspheres were also proposed on the basis of characterizations. We think this general method may be easily scaled up for industrial production of highly active microspherical photocatalysts for efficient NO removal under simulated solar light irradiation.     

Photocatalytic behaviour of Bi2MO6 polymetalates for rhodamine B degradation

Bi₂MO₆ (M = W or Mo) have been successfully synthesized using the citrate complex method. The samples were characterized by X-ray diffraction, Brunauer–Emmet–Teller surface area and UV–vis spectroscopy. The solids crystallized in the orthorhombic Aurivillius-type structure and display optimum light absorption properties to be used as photocatalysts. The photoactivity power of the samples was investigated systematically using the rhodamine B degradation under different irradiation wavelengths. The behaviour of the solids and the photodegradation mechanism was studied as a function of the irradiation light (UV or visible) employed. Direct solar light was also employed as irradiation source showing that this type of structures could drive to a plausible strategy for developing finest photocatalyst to degrade wastewaters by using solar light.     

Photocatalytic O2 evolution under visible light irradiation on BiVO4 in aqueous AgNO3 solution

BiVO₄ with a 2.3 eV band gap showed an activity for O₂ evolution from aqueous solutions containing Ag⁺ as an electron scavenger under visible light irradiation (λ > 520 nm). The quantum yield was 0.5% at 450 nm. This revised version was published online in July 2006 with corrections to the Cover Date.     

Preparation of polyaniline-modified TiO2 nanoparticles and their photocatalytic activity under visible light illumination

Titanium dioxide nanoparticles were modified by polyaniline (PANI) using ‘in situ’ chemical oxidative polymerization method in hydrochloric acid solutions. Powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared spectra (FT-IR), X-ray photoelectron spectroscopy spectrum (XPS) and UV–vis spectra were carried out to characterize the composites with different PANI contents. The photocatalytic degradation of phenol was chosen as a model reaction to evaluate the photocatalytic activities of the modified catalysts. Results show that TiO₂ nanoparticles are deposited by PANI to mitigate TiO₂ particles agglomeration. The modification does not alter the crystalline structure of the TiO₂ nanoparticles according to the X-ray diffraction patterns. UV–vis spectra reveal that PANI-modified TiO₂ composites show stronger absorption than neat TiO₂ under the whole range of visible light. The resulting PANI-modified TiO₂ composites exhibit significantly higher photocatalytic activity than that of neat TiO₂ on degradation of phenol aqueous solution under visible light irradiation (λ ≥ 400 nm). An optimum of the synergetic effect is found for an initial molar ratio of aniline to TiO₂ equal to 1/100.     

Synthesis and photocatalytic behavior of BiVO4 with decahedral structure

Decahedral BiVO₄ was successfully synthesized with Tween-80 as a template by the microwave hydrothermal method. The effects of hydrothermal temperature and Tween-80 on crystal phase and morphology of the obtained BiVO₄ were investigated. The crystal phase and morphology were characterized by X-ray diffraction, field emission scanning electron microscopy and UV–vis diffuse reflectance spectroscopy. The results indicated that the as-prepared decahedral BiVO₄ was monoclinic. The photocatalytic behavior for methylene blue (MB) degradation was enhanced with the assistance of an appropriate amount of hydrogen peroxide (H₂O₂) under visible light irradiation. The photocatalytic tests indicated that the photocatalytic efficiency of decahedral BiVO₄ synthesized at 180 °C was 63.5%. However, BiVO₄ sample synthesized at 160 °C showed the highest photocatalytic degradation rate, up to 81.6%, due to its small size and crystal defects.     

Synthesis,microstructure and optical characterization of zirconium oxide nanostructures

Zirconium oxide (ZrO₂) nanostructures were synthesized by hydrothermal route. Surface morphology analysis depicts the formation of the nanobars and hexagonal-shaped nanodiscs at different synthesis conditions. The structural analysis confirms that the as-synthesized ZrO₂ product is of pure monoclinic phase (m-ZrO₂) with crystallite size of about 25 nm. The product consists of monodispersed nanoparticles of uniform composition, high purity, and crystallinity. The Raman spectra are quantitatively analyzed and the observed peaks are attributed to various vibration modes of the m-ZrO₂. The UV–vis absorption spectrum showed a strong absorption peak at about 292 nm and the estimated optical band gap was around 3.57 eV. Photoluminescence (PL) spectrum of ZrO₂ nanostructure showed a strong and broad emission peak at around 410 nm at room temperature, which can be attributed to the ionized oxygen vacancy in the material.     

Synthesis and characterization of polythiophene/titanium dioxide composites

Polythiophene/titanium dioxide (PT/TiO₂) composites were prepared by the in situ chemical oxidative polymerization method. The resulting PT/TiO₂ composites were characterized by Fourier transform infrared (FT-IR) spectroscopy, ultraviolet–visible (UV–Vis) diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and field emission scanning electron microscopy (SEM). UV–Vis diffuse reflectance spectra measurements show that the PT/TiO₂ composites can adsorb light of wavelengths ranging from 200 nm to 800 nm. The PT/TiO₂ composites showed good adsorption properties and were more efficient in removing dye from solution than pure PT and pure TiO₂. The PT/TiO₂ composites exhibited photocatalytic activities to some extent under UV light illumination.