Copper and Graphene activated ZnO nanopowders for enhanced photocatalytic and antibacterial activities

ZnO, ZnO:Cu and ZnO:Cu:Graphene nanopowders were synthesized via a facile wet chemical method. The XRD studies show that the synthesized samples have hexagonal wurtzite structure. It is found that graphene addition induces a decrease in crystallite size. UV–vis absorption spectra of the samples show sharp absorption edges around 380 nm. Photoluminescence studies reveal that the incorporation of copper and graphene in ZnO facilitates the efficient photo generated electron–hole pair separation. It is found that the ZnO:Cu and ZnO:Cu:Graphene nanopowder exhibit improved photocatalytic efficiency for the photodegradation of Methylene Blue (MB) under visible light irradiation. Moreover, improved antibacterial activity of ZnO:Cu:Graphene nanopowder against Escherichia coli and Staphylococcus aureus bacteria is observed.     

Ultrasound assisted synthesis of monoclinic structured spindle BiVO4 particles with hollow structure and its photocatalytic property

Bismuth vanadate (BiVO₄) spindle particles with monoclinic scheelite structure have been successfully synthesized via a facile sonochemical method. The as-prepared BiVO₄ photocatalyst exhibited a hollow interior structure constructed from the self-assembly of cone shape primary nanocrystals. A possible oriented attachment growth mechanism has been proposed based on the results of time-dependent experiments, which indicates the formation of spindle particles is mainly attributed to the phase transformation procedure induced by ultrasound irradiation. A series of morphology evolutions of BiVO₄ from compact microspheres, to hollow microspheres, and then to spindle particles have been arrested in the process of sonochemical treatment. Optical absorption experiments revealed the BiVO₄ spindle had strong absorption in the visible light region. A much higher photocatalytic activity of these spindle particles was found in comparison with the SSR-BiVO₄ material for degradation of rhodamine-B under visible light irradiation, which may be ascribed to its special single-crystalline nanostructure.     

Effect of Fe-doping on the structural,morphological and optical properties of ZnO nanoparticles synthesized by solution combustion process

The effect of Fe-doping on the structural, morphological and optical properties of ZnO nanoparticles synthesized by simple solution combustion process are reported. The powder XRD pattern indicates that the Fe-doped ZnO samples exhibit primary and secondary phases. The primary phase indicates the hexagonal wurtzite structure with the average crystalline size of around 25–50 nm and the secondary phase is associated with the face centered cubic structure of magnetite iron oxide. The elemental composition of pure and Fe-doped samples are evaluvated by EDX. The results of FE-SEM and HR-TEM cleary show that particles morphology have changed with respect to the incorporation of doping agent and particles are in aggregating nature. The vibrational properties of the synthesized ZnO nanoparticles are investigated by Raman scattering technique and it exhibits that the influence of Fe-doping significantly modify the lattice vibrational characteristics in ZnO sites. The optical properties of the Fe-doped ZnO nanoparticles are carried out by UV–vis absorption and PL spectra. The results of PL spectra show the near-band edge related emission as well as strong blue emissions in the Fe-doped ZnO nanoparticles.     

Sonochemical preparation and characterization of photochromic MoO3 nanoparticles

The effect of ultrasound irradiation on molybdenum trioxide has been investigated. Under ultrasonic irradiation, spherical-like MoO₃ nanoparticles were obtained, while bulk-like MoO₃ nanoparticles were prepared without ultrasonic irradiation. The changes in the physicochemical properties of MoO₃ have been investigated using techniques such as X-ray powder diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and ultraviolet and visible spectroscopy (UV-vis). The physicochemical changes of MoO₃ due to ultrasound irradiation have been attributed to the sonochemical cavity collapse onto the molybdenum trioxide particles. The ultrasonically prepared particles can also greatly improve the photochromism efficiency.      

CO2-enhanced dehydrogenation of ethane over sonochemically synthesized Cr/clinoptilolite-ZrO2 nanocatalyst: Effects of ultrasound irradiation and ZrO2 loading on catalytic activity and stability

CO₂-enhanced oxidative dehydrogenation of ethane was investigated over sonochemically synthesized Cr/clinoptilolite-ZrO₂ nanocatalyst with the aim of assessing the effect of composite support and ultrasonic irradiation on the nanocatalyst reactivity and stability. To this aim, ZrO₂ promoted clinoptilolite supports varying in zirconia content (0, 25, 50 wt%) were synthesized by hydrothermally precipitation method and impregnated with chromium nitrate under ultrasound irradiation. The samples were characterized by XRD, FESEM, EDX, TEM, ICP, BET, FTIR, TPR-H₂ and TPD-NH₃ techniques. The characterization results indicated that ultrasound irradiation could not only reduce the formation of Cr₂O₃ and decrease submicron particle size of chromium oxide to nanometer scale, but also promote the distribution of metallic particles and strengthen the chromium-support interaction. As a result, utilizing ultrasound irradiation in the synthesis of Cr/Clinoptilolite helped to maintain a high and stable catalytic activity. These features were more prominent in the presence of zirconia. It was found that the metal oxide nanoparticles with about 4–8 nm are dispersed uniformly on the surface of composite support containing 25 wt% ZrO₂ (CLT-Z25). Moreover, the addition of ZrO₂ resulted in the formation of new strong acid sites and a significant modification in the reducibility of chromium species, which alongside homogenous and small Cr nanoparticles account for the superior catalytic performance of ZrO₂ containing samples. However, excessive loading of ZrO₂ (50 wt%) severely covered the surface of clinoptilolite, afforded the aggregations of metallic particles and thereupon, weakened the contact between clinoptilolite and ZrO₂, which together with more acid strength seriously resulted in the deactivation of catalyst. In spite of superior initial activity of ZrO₂-rich sample among the catalysts tested, ultrasonic synthesized Cr/CLT-Z25 nanocatalyst showed the best catalytic performance after 5 h-catalytic reaction.     

Photocatalytic,sonocatalytic and sonophotocatalytic degradation of Rhodamine B using ZnO/CNTs composites photocatalysts

A series of ZnO nanoparticles decorated on multi-walled carbon nanotubes (ZnO/CNTs composites) was synthesized using a facile sol method. The intrinsic characteristics of as-prepared nanocomposites were studied using a variety of techniques including powder X-ray diffraction (XRD), high resolution transmission electron microscope (HR-TEM), transmission electron microscope (TEM), scanning electron microscope (SEM) with energy dispersive X-ray analysis (EDX), Brunauer Emmett Teller (BET) surface area analyzer and X-ray photoelectron spectroscopy (XPS). Optical properties studied using UV–Vis diffuse reflectance spectroscopy confirmed that the absorbance of ZnO increased in the visible-light region with the incorporation of CNTs. In this study, degradation of Rhodamine B (RhB) as a dye pollutant was investigated in the presence of pristine ZnO nanoparticles and ZnO/CNTs composites using photocatalysis and sonocatalysis systems separately and simultaneously. The adsorption was found to be an essential factor in the degradation of the dye. The linear transform of the Langmuir isotherm curve was further used to determine the characteristic parameters for ZnO and ZCC-5 samples which were: maximum absorbable dye quantity and adsorption equilibrium constant. The natural sunlight and low power ultrasound were used as an irradiation source. The experimental kinetic data followed the pseudo-first order model in photocatalytic, sonocatalytic and sonophotocatalytic processes but the rate constant of sonophotocatalysis is higher than the sum of it at photocatalysis and sonocatalysis process. The sonophotocatalysis was always faster than the respective individual processes due to the more formation of reactive radicals as well as the increase of the active surface area of ZnO/CNTs photocatalyst. Chemical oxygen demand (COD) of textile wastewater was measured at regular intervals to evaluate the mineralization of wastewater.     

Ultraviolet-assisted synthesis of hourglass-like ZnO microstructure through an ultrasonic and microwave combined technology

Well-defined hexagonal hourglass-like ZnO microstructures have been synthesized by using simultaneous ultrasound and microwave irradiation methods with the assistance of ultraviolet as well as double sonication (at 25 and 40 kHz). The structure and morphology of as-prepared samples were characterized by X-ray diffraction, scanning electron microscopy and photoluminescence spectrum. The results show the synergistic effect of ultrasound and microwave on the formation of ZnO microstructures. Meanwhile, the possible growth mechanism was proposed to elucidate the formation of hexagonal hourglass-like ZnO microstructures.     

Synergistic effect of efficient adsorption g-C3N4/ZnO composite for photocatalytic property

Novel g-C₃N₄/ZnO composite photocatalyst was synthesized from an oxygen-containing precursor by direct thermal decomposition urea in air without any other templates assistance. Different percentages of g-C₃N₄ were hybridized with ZnO via the monolayer-dispersed method. The prepared g-C₃N₄/ZnO composites were characterized by XRD, SEM, UV–vis diffuse reflectance spectra (DRS), FT-IR, TEM and XPS. The composites showed much higher efficiency for degradation of Rhodamine B (RhB) than ZnO under UV and visible light irradiation. Especially, the photocatalytic efficiency was the highest under UV light irradiation when the percentage of g-C₃N₄ was 6%. The improved photocatalytic activity may be due to synergistic effect of photon acquisition and direct contact between organic dyestuff and photocatalyst. Then, effective separation of photogenerated electron–hole pairs at the interface of g-C₃N₄ is an important factor for improvement of photocatalytic activity. This work indicates that g-C₃N₄ hybrid semiconductors photocatalyst is a promising material in pollutants degradation.     

Preparation of nano-sized platinum metal catalyst using photo-assisted deposition method on mesoporous silica including single-site photocatalyst

Pt particles in a uniform dispersion were successfully synthesized on single-site photocatalyst (Ti-containing mesoporous silica (Ti-HMS)) under UV-light irradiation by a photo-assisted deposition (PAD) method. Using an aqueous solution of H₂PtCl₆ as a precursor, the nano-sized Pt metal particles were deposited directly on the photo-excited tetrahedrally coordinated titanium oxide moieties within the framework of mesoporous silica (PAD-Pt/Ti-HMS). The Pt catalysts were characterized by means of XRD, Pt L_III-edge XAFS, CO adsorption, and TEM analysis. It was demonstrated that Pt particles had mean diameter of 4 nm in a narrow size distribution. Meanwhile, Pt particles loaded by a conventional impregnation method (imp-Pt/Ti-HMS) showed a wide size distribution ranging from 2 to 30 nm. The PAD-Pt/Ti-HMS catalyst was more active in the CO oxidation than the conventional impregnated imp-Pt/Ti-HMS catalyst. It is suggested that the PAD method using single-site photocatalyst is a useful and unique technique to prepare fine and uniform Pt nanoparticles.     

Electrophoreted Zn-TiO2-ZnO nanocomposite coating films for photocatalytic degradation of 2-chlorophenol

TiO₂-ZnO nano-powders with different TiO₂/ZnO ratios have been synthesized by hydrothermal method. Nanocomposite coating films consisting of TiO₂-ZnO and Zn with thickness of 20 μm have been electrophoreted on steel plates by rapid plating from a ZnO-based alkaline bath. X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis were used to investigate the structure, the size distribution, and the composition of prepared nano-powders and plated materials. The effect of the operating parameters such as powder contents, pH and current density on the electrophoresis process has been investigated and optimum conditions of coating process were determined. Corrosion properties of plated samples have been studied by salt spray test. The catalytic activity of the prepared nanocomposite Zn-TiO₂-ZnO films for the photocatalytic degradation of 2-chlorophenol (2-CP) was measured.     

Enhanced photoluminescence of ZnO-SiO2 nanocomposite particles and the analyses of structure and composition

Stable blue-green photoluminescent ZnO-SiO₂ nanocomposite particles exhibiting quantum efficiency as high as 34.8% under excitation at 360 nm were prepared using a spray-drying process from a feed solution that contained both luminescent ZnO nanoparticles synthesized by a sol-gel method and commercially-available SiO₂ nanoparticles. The effects of silica nanoparticle size and SiO₂-to-ZnO concentration ratio on the PL properties of the composite particles were investigated. The internal structure and chemical composition were investigated in detail using elemental mapping, which revealed that ZnO nanoparticles were well-dispersed within silica nanoparticle matrix. At a LiOH concentration of 0.23 M, the predicted ZnO crystallite diameter before and after spray drying was approximately constant at 3.3 and 3.6 nm, respectively. This result indicates that ZnO particle growth was inhibited and therefore the PL property of ZnO nanoparticles was stably preserved in the composite.     

ZnO@GQDs核壳结构量子点的制备及性能研究

采用原位聚合法制备了以ZnO量子点为核、石墨烯量子点（GQDs）为壳的ZnO@ GQDs核壳结构量子点。通过TEM和HR-TEM对量子点进行形貌和结构的分析表征。结果表明,合成的ZnO@ GQDs核壳结构量子点为球形,粒径为～7 nm,且尺寸均匀。PL光谱研究表明,新型量子点的发射峰位于369 nm,发光峰窄、强度高;相对于ZnO的本征发射峰,GQDs的引入使得ZnO@GQDs核壳量子点的荧光发射峰出现蓝移、强度变高,从而使复合量子点的荧光具有较纯的色度和较高的强度,说明GQDs的引入具有协同优化效应。该量子点有望应用于LED显示器件。     

Facile photo-ultrasonic assisted synthesis of flower-like Pt/N-MoS2 microsphere as an efficient sonophotocatalyst for nitrogen fixation

Semiconductor photocatalytic technology is a sustainable and less energy consuming one for nitrogen (N₂) reduction to produce ammonia (NH₃). In this study, flower-like hierarchical N doped MoS₂ (N-MoS₂) microsphere was synthesized as a photocatalyst by one-step solvothermal method, which was assembled by numerous interleaving nanosheets petals with thin thickness. Besides, Pt nanoparticles were loaded on the surface of N-MoS₂ via photo-ultrasonic reduction method. The as-prepared Pt/N-MoS₂ photocatalyst exhibited higher N₂ fixation ability than that over pure MoS₂ and N-MoS₂, which can be attributed to that the N doping narrows the band gap, and the Schottky barrier due to the existence of Pt nanoparticles improves the charge transfer and carrier separation. The reduction of N₂ with ultrasonic irradiation was also investigated under visible light irradiation to evaluate the sonophotocatalytic activity of the Pt/N-MoS₂ microsphere. The results showed that the N₂ reduction rate of sonophotocatalysis (133.8 µmol/g_(cat)h) was higher than that of sonocatalysis and photocatalysis, which can be ascribed to the synergistic effect of ultrasound and visible light irradiation. The effects of catalyst dosage, ultrasonic power and ultrasonic pulse on the photocatalytic efficiency were also studied. Meanwhile, a possible mechanism for improved sonophotocatalytic performance was also proposed.     

Free surface entrainment of oxide particles and their role in ultrasonic treatment performance of aluminum alloys

Although the ultrasonic treatment of molten aluminum has been studied for long period, there is still much to be revealed for this process. Many studies have focused on the investigation of acoustic cavitation and streaming under the horn tip and their effects on the treatment efficiency. However, to the best of our knowledge, no attempt has been done to explain phenomena occurring near or on the melt free surface. Thus, the goal of this study is to investigate phenomena occurring at the free surface during ultrasound irradiation and clarify their possible influence on the ultrasound treatment performance. The results of high temperature and water model experiments reveal that ultrasound irradiation significantly promotes the formation of alumina particles on the melt free surface around sonotrode, and part of these particles can be entrained into aluminum melts. Furthermore, TEM observation results suggested that the entrained alumina inclusions can serve as nucleation sites for the primary Al₃Zr compounds. Most importantly, the oxidation and entrainment of particles from free surface are likely to be controllable by the immersion depth of sonotrode into molten aluminum.     

Insight into the synthesis procedure of Fe3+/TiO2-based photocatalyst applied in the selective photo-oxidation of benzyl alcohol under sun-imitating lamp

Fe³⁺/TiO₂/zeolite Y photocatalyst synthesized by using sonophotodeposition method was compared with photocatalysts prepared by simple photodeposition and sonodeposition methods in order to clarify the role of light irradiation and ultrasounds while they are used simultaneously. To gain an insight into the mechanism of this method a detailed characterization of the photocatalysts was carried out by means of the following techniques: UV–vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, Mössbauer measurements and photocatalytic test reaction. Basing on the results from these techniques the chemical role of light and mainly mechanical role of ultrasound were observed. The selective photocatalytic oxidation of benzyl alcohol into benzaldehyde in liquid phase was a test reaction verifying the utility of the prepared materials. The best photocatalytic efficiency in this reaction was performed by photocatalyst synthesized using compilation of ultrasound energy with photoexcitation.     

Sonocatalytic removal of naproxen by synthesized zinc oxide nanoparticles on montmorillonite

ZnO/MMT nanocomposite as sonocatalyst was prepared by immobilizing synthesized ZnO on the montmorillonite surface. The characteristics of as-prepared nanocomposite were studied by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD) techniques. The synthesized samples were used as a catalyst for sonocatalytic degradation of naproxen. ZnO/MMT catalyst in the presence of ultrasound irradiation was more effective compared to pure ZnO nanoparticles and MMT particles in the sonocatalysis of naproxen. The effect of different operational parameters on the sonocatalytic degradation of naproxen including initial drug concentration, sonocatalyst dosage, solution pH, ultrasonic power and the presence of organic and inorganic scavengers were evaluated. It was found that the presence of the scavengers suppressed the sonocatalytic degradation efficiency. The reusability of the nanocomposite was examined in several consecutive runs, and the degradation efficiency decreased only 2% after 5 repeated runs. The main intermediates of naproxen degradation were determined by gas chromatography–mass spectrometry (GC–Mass).     

A Z-scheme CuO–ZnO–ZnS–CuS quaternary nanocomposite for solar-light-driven photocatalytic performance

A quaternary CuO–CuS–ZnO–ZnS nanocomposite was successfully synthesized via a facile microwave irradiation based on the preprepared ZnS and CuO nanoparticles. CuO–CuS–ZnO–ZnS nanocomposite was a porous photocatalyst, providing excellent adsorption performance. It was sensitive to both ultraviolet and visible light, moreover, the photoelectrochemical measurements confirmed that there was a high separation rate and low recombination rate of photo-generated charge carriers in the nanocomposite, endowing excellent photocatalytic activity in the sunlight. Under the simulated solar light irradiation, the removal efficiency of rhodamine B (RhB) pollutant (30 mg/L) over CuO–CuS–ZnO–ZnS nanocomposite was 33.98 and 2.90 times of pristine CuO and ZnS, respectively. The outstandingt photocatalytic performance was attributed to Z-scheme charge transfer path.     

Synthesis, characterizations, photocatalytic and sensing studies of ZnO nanocapsules

ZnO nanocapsules have been synthesized hydrothermally. The structural and morophological properties were investigated using X-ray powder diffraction (XRD), field emission scanning electron microscopy (FESEM), FTIR, Raman, EDS and UV-vis absorption spectroscopy. For the first time chemical sensing properties of the synthesized ZnO nanocapsules have been investigated by I-V technique, where chloroform is used as a target compound. The chloroform sensors show good sensitivity (0.478 μA cm⁻² mM⁻¹), lower detection limit (6.67 μM), and large linear dynamic range (LDR, 12.0 μM-12.0 mM) with good linearity (R, 0.8523) in short response time. Additionally, photocatalytic activity of the prepared capsule shaped ZnO photocatalyst was evaluated by the degradation of acridine orange. Prepared ZnO nanocapsules posses high photocatalytic activity when compared with TiO₂-UV100.     

Properties of ZnO thin films grown on Si substrates by photo-assisted MOCVD

ZnO thin films were grown on (1 0 0) p-Si substrates by Photo-assisted Metal Organic Chemical Vapor Deposition (PA-MOCVD) using diethylzinc (DEZn) and O₂ as source materials and tungsten-halogen lamp as a light source. The effects of tungsten-halogen lamp irradiation on the surface morphology, structural and optical properties of the deposited ZnO films have been investigated by means of atomic force microscope (AFM), X-ray diffraction and photoluminescence (PL) spectra measurements. Compared with the samples without irradiation, the several characteristics of ZnO films with irradiation are improved, including an improvement in the crystallinity of c-axis orientation, an increase in the grain size and an improvement in optical quality of ZnO films. These results indicated that light irradiation played an important role in the growth of ZnO films by PA-MOCVD.     

Luminescence from ZnO/MgO nanoparticle structures prepared by solution techniques

The optical and structural properties of mixed ZnO/MgO particles prepared by solution techniques are investigated by the cathodoluminescence and electron microscopy techniques. The samples annealed at 400–1000 °C show well crystalline wurtzite structure of the ZnO (MgZnO) particles with the size in range of 10–100 nm. Annealing at high temperatures (>700 °C) leads to Mg diffusion in ZnO and Mg_xZn_1−xO alloy formation. The blue shifts of the near-band-edge emission as a result of the alloy band gap widening and quantum confinement effect for the small size particles are demonstrated.