Sonochemical Synthesis and Photocatalytic Properties of Metal Hydroxide and Carbonate (M:Mg, Ca, Sr or Ba) Nanoparticles

In this work Mg(OH)₂, Ca(OH)₂, CaCO₃, SrCO₃ and BaCO₃ nanoparticles were synthesized via a simple sonochemical reaction at room temperature. Nanoparticles were synthesized via a surfactant-free reaction solvent water. Nanostructures materials were characterized by scanning electron microscopy, X-ray diffraction and fourier transform infrared spectroscopy. The photocatalytic behavior of nanoparticles was evaluated using the degradation of a methyl orange aqueous solution under ultraviolet light irradiation. The results show that metal hydroxide and metal carbonate nanoparticles are promising materials with excellent performance in photocatalytic applications.     

Synthesis and Characterization of CeO2 Nanoparticles via Solution Combustion Method for Photocatalytic and Antibacterial Activity Studies

CeO₂ nanoparticles have been proven to be competent photocatalysts for environmental applications because of their strong redox ability, nontoxicity, long-term stability, and low cost. We have synthesized CeO₂ nanoparticles via solution combustion method using ceric ammonium nitrate as an oxidizer and ethylenediaminetetraacetic acid (EDTA) as fuel at 450 °C. These nanoparticles exhibit good photocatalytic degradation and antibacterial activity. The obtained product was characterized by various techniques. X-ray diffraction data confirms a cerianite structure: a cubic phase CeO₂ having crystallite size of 35 nm. The infrared spectrum shows a strong band below 700 cm⁻¹ due to the Ce−O−Ce stretching vibrations. The UV/Vis spectrum shows maximum absorption at 302 nm. The photoluminescence spectrum shows characteristic peaks of CeO₂ nanoparticles. Scanning electron microscopy (SEM) images clearly show the presence of a porous network with a lot of voids. From transmission electron microscopy (TEM) images, it is clear that the particles are almost spherical, and the average size of the nanoparticles is found to be 42 nm. CeO₂ nanoparticles exhibit photocatalytic activity against trypan blue at pH 10 in UV light, and the reaction follows pseudo first-order kinetics. Finally, CeO₂ nanoparticles also reduce Cr^VI to Cr^III and show antibacterial activity against Pseudomonas aeruginosa.     

Syntheses of MO2 (M=Si, Ce, Sn) nanoparticles by solid-state reactions at ambient temperature

Nano oxides (SiO₂, CeO₂, SnO₂) were successfully synthesized by solid-state reactions at ambient temperature. The nanoparticles were characterized by X-ray powder diffraction, TEM, BET, and TGA-DTA. The SiO₂ particles were also investigated using IR spectra. Effects of calcination on the nanoparticles were studied in this paper. The solid-state reaction technique is a convenient, inexpensive and an effective preparation method of monodisperse oxide nanoparticles in high yield. The mechanisms of the formation of nano materials by solid-state reactions at ambient temperature were primarily investigated.     

Facile Synthesis of Platinum–Cerium(IV) Oxide Hybrids Arched on Reduced Graphene Oxide Catalyst in Reverse Micelles with High Activity and Durability for Hydrolysis of Ammonia Borane

Highly dispersed Pt‐CeO₂ hybrids arched on reduced graphene oxide (Pt‐CeO₂/rGO) were facilely synthesized by a combination of the reverse micelle technique and a redox reaction without any additional reductant or surfactant. Under a N₂ atmosphere, the redox reaction between Ce³⁺ and Pt²⁺ occurs automatically in alkaline solution, which results in the formation of Pt‐CeO₂/rGO nanocomposites (NCs). The as‐synthesized Pt‐CeO₂/rGO NCs exhibit superior catalytic performance relative to that shown by the free Pt nanoparticles, Pt/rGO, Pt‐CeO₂ hybrid, and the physical mixture of Pt‐CeO₂ and rGO; furthermore, the nanocomposites show significantly better activity than the commercial Pt/C catalyst toward the hydrolysis of ammonia borane (NH₃BH₃) at room temperature. Moreover, the Pt‐CeO₂/rGO NCs have remarkable stability, and 92 % of their initial catalytic activity is preserved even after 10 runs. The excellent activity of the Pt‐CeO₂/rGO NCs can be attributed not only to the synergistic structure but also to the electronic effects of the Pt‐CeO₂/rGO NCs among Pt, CeO₂, and rGO.     

CeO2 nanofibers-CdS nanostructures n–n junction with enhanced visible-light photocatalytic activity

In the present work, the n-cerium (IV) oxide (CeO₂)/n-cadmium sulfide (CdS) composite nanofibers were successfully synthesized via a facile electrospinning and hydrothermal synthesis strategy. The physicochemical properties of the synthesized composite nanofibers were investigated by using X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy Dispersive X-Ray Spectroscopy (EDS), diffuse Reflectance Spectroscopy (DRS), Fourier-transform infrared (FTIR), photoluminescence (PL), Brunauer–Emmett–Teller (BET) and Raman spectroscopy analysis. The activities of the CeO₂/CdS were evaluated through the photocatalytic degradation of Rose Bengal (RB) in an aqueous solution under blue LED light radiation. CeO₂/CdS composites exhibit higher photocurrent density in photocurrent response experiment and smaller charge-transfer resistance in electrochemical impedance spectroscopy (EIS). Overall, the results confirmed higher charge separation efficiency in CeO₂/CdS composites compared to pristine CeO₂ nanofibers, and CdS, which is related to intimately contact among the CeO₂, and CdS. The present work provides a new approach to construct n-n heterojunction photocatalysts based on electrospinning and a deeper insight for the photocatalytic degradation activity. In addition, possible degradation mechanism and pathways were proposed according to the identified intermediates.     

Controlled synthesis of monodisperse sub-100 nm hollow SnO2 nanospheres: a template- and surfactant-free solution-phase route, the growth mechanism, optical properties, and application as a photocatalyst

Controlled synthesis of low‐dimensional materials, such as nanoparticles, nanorods, and hollow nanospheres, is vitally important for achieving desired properties and fabricating functional devices. We report a systematic investigation of the growth of low‐dimensional sub‐100 nm SnO₂ hollow nanostructures by a mild template‐ and surfactant‐free hydrothermal route, aiming to achieve precise control of morphology and size. The starting materials are potassium stannate and urea in an ethylene glycol (EG)/H₂O system. We found the size of the SnO₂ hollow nanospheres can be controlled by simply adjusting the urea concentration. Investigation of the mechanism of formation of the SnO₂ hollow nanospheres revealed that reaction time, urea concentration, and reaction temperature make significant contributions to the growth of hollow nanospheres. On switching the solvent from EG/H₂O to H₂O or ethanol, the SnO₂ nanostructures changed from nanospheres to ultrafine nanorods and nanoparticles. On the basis of reaction parameter dependent experiments, oriented self‐assembly and subsequent evacuation through Ostwald ripening are proposed to explain the formation of hollow nanostructures. Their size‐dependent optical properties, including UV/Vis absorption spectra and room‐temperature fluorescence spectra, were also studied. Moreover, the studies on the photocatalytic property demonstrate that the fabricated hollow structures have slightly enhanced photocatalytic degradation activity for rhodamine B when exposed to mercury light irradiation compared to solid SnO₂ nanospheres under the same conditions. The synthesized tin oxide nanoparticles display high photocatalytic efficiency and have potential applications for cleaning polluted water in the textile industry.     

Magnetic and Thermal Properties of Novel Poly(ether-amide)/Fe3O4 Nanocomposite Containing Phosphine Oxide Group

New poly(ether-amide) nanocomposite containing phosphine oxide was prepared via solution polymerization process from synthesized poly(ether-amide) and Fe₃O₄ nanoparticles in a solution of N,N-dimethylformamide. Uniform monodisperse Fe₃O₄ nanoparticles were synthesized at room temperature via a facile sonochemical reaction. Poly(ether-amide) (PEA) as the polymer matrix was synthesized from reaction of 1,4-(4-carboxy phenoxy)butane (1) and bis(3-amino phenyl)phenyl phosphine oxide (2) via a direct polycondensation reaction. Nanoparticle and nanocomposite were characterized using X-ray diffraction, scanning electron microscopy, transmission electron microscopy and Fourier transform infrared. The effect of the presence of Fe₃O₄ nanoparticles on the thermal properties of PEA was studied using thermogravimetric analysis in nitrogen atmospheres. The magnetic properties of the sample were also investigated using an alternating gradient force magnetometer. We found that the Fe₃O₄ nanoparticles exhibit a ferromagnetic behaviour with a saturation magnetization of 59 emu/g and a coercivity of 104 Oe at room temperature. The coercivity of PEA/Fe₃O₄ nanocomposites is found to be 126 Oe, higher than 104 Oe which is obtained for Fe₃O₄.     

AgBr@TiO<Subscript>2</Subscript>/GO ternary composites with enhanced photocatalytic activity for oxidation of benzyl alcohol to benzaldehyde

AgBr@TiO₂/GO (graphene oxide) ternary composite photocatalyst was synthesized by fabricating core–shell-structured AgBr@TiO₂ and anchoring it onto the surface of GO. The obtained samples were characterized by transmission electron microscopy, X-ray diffraction analysis, X-ray photoelectron spectroscopy, ultraviolet–visible (UV–Vis) diffuse reflectance spectrum, and photoluminescence (PL) spectroscopy. It was found that the AgBr nanoparticles were prone to aggregation while the core–shell-structured AgBr@TiO₂ possessed excellent dispersity. PL analysis revealed that the ternary-structured AgBr@TiO₂/GO could effectively promote the separation rate of electron–hole pairs. Photocatalytic oxidation of benzyl alcohol to benzaldehyde under visible-light irradiation was selected as probe reaction to evaluate the photocatalytic activity of the different samples. It was found that the AgBr@TiO₂/GO ternary composite exhibited evidently improved photocatalytic activity compared with AgBr, AgBr@TiO₂, and AgBr/GO. On the basis of the experiment results, the photocatalytic oxidation mechanism of benzyl alcohol over AgBr@TiO₂/GO is tentatively discussed.     

Preparation and photocatalytic activity of cuprous oxides

Cuprous oxide (Cu₂O) nanoparticles and microcubes have been successfully fabricated by reduce of CuSO₄ using ascorbic acid at room temperature. The as-synthesized products were easily separation and purification, because there were no template or surfactant has been introduced. All of the samples were characterized by X-ray powder diffractometer (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectrometer (FTIR) and ultraviolet and visible light spectrometer (UV–vis). The microscale Cu₂O samples exhibited a high catalytic activity on photodegradation of methyl orange by visible light. It was found that Cu₂O microcubes have higher photocatalytic activity and the photocatalytic degradation ratio of methyl orange reached to 98.1%.     

Enhanced photocatalytic activity of cobalt-doped CeO2 nanorods

In this paper, CeO₂ and cobalt-doped CeO₂ nanorods synthesized by surfactant free co-precipitation method. The microstructures of the synthesized products were characterized by XRD, FESEM and TEM. The structural properties of the grown nanorods have been investigated using electron diffraction and X-ray diffraction. High resolution transmission electron microscopy studies show the polycrystalline nature of the Co-doped cerium oxide nanorods with a length of about 300?nm and a diameter of about 10?nm were produced. The X-ray Photoelectron spectrum confirms the presence of cobalt in cerium oxide nanorods. From BET, the specific surface area of the CeO₂ (Co-doped) nanostructures (131 m²?g^??) is found to be significantly higher than that of pure CeO₂ (52 m²?g^??). The Co-doped cerium nanorods exhibit an excellent photocatalytic performance in rapidly degrading azodyes acid orange 7 (AO7) in aqueous solution under UV illumination.     

Microwave-Assisted Hydrothermal Preparation, Characterization and Photocatalytic Properties of a Chrysanthemum-Shaped ZnWO4 Photocatalyst

A novel chrysanthemum-shaped monocline ZnWO₄ photocatalyst was synthesized by microwave-assisted hydrothermal method with Na₂WO₄·2H₂O and Zn(NO₃)₂·6H₂O as raw materials at different reaction temperatures. The prepared ZnWO₄ photocatalysts were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy, Photoluminescence spectrum (PL) and UV–Vis absorption spectrum (UV–Vis). The photocatalytic property of the prepared chrysanthemum-shaped monocline ZnWO₄ photocatalyst was evaluated by the degradation of Rhodamine B (RhB) in aqueous solution. The effects of reaction temperature on the photocatalytic degradation efficiency of RhB were investigated. The results indicated that the chrysanthemum-shaped monocline ZnWO₄ photocatalyst is prepared by foliated powders with the sizes of about 30 nm and 500 nm respectively at 160 and 220 °C. The PL relative intensity of prepared ZnWO₄ photocatalyst is apparently intensifying with increasing temperature. The photocatalytic property decreases with the increasing recombination probability of the excited electrons and holes. The chrysanthemum-shaped monocline ZnWO₄ photocatalyst prepared at 160 °C possesses the best photocatalytic property, and the degradation efficiency of RhB at 180 min UV-light irradiation is achieved 75 %. The ZnWO₄ has good reusability property on degradation of RhB and the degradation rate is still higher than 65 % after three cycles.     

Optimization and detailed stability study on Pb doped ceria nanocubes for enhanced photodegradation of several anionic and cationic organic pollutants

A series of Pb doped CeO₂ nanocubes with seven different Pb loadings (2–12 mol%) were synthesized via modified hydrothermal technique. The prepared samples were characterized by XRD, XPS, FT-IR, TGA, SEM, HR-TEM, EDS and UV–Vis DRS analysis. According to XRD analysis, the crystalline structure of synthesized pure CeO₂ and Pb-doped CeO₂ samples are cubic structure. The ceria nanocubes showed an increase in amount of oxygen vacancies with increasing the dopant concentrations. When the doping level of Pb is 6 mol%, the optical band gap of Pb-CeO₂ is smaller than that of pure CeO₂ nanocubes. The HR-TEM results confirms the cubic structure of 6% Pb-CeO₂ with average crystallite size of about 15 nm. The photocatalytic ability of Pb-CeO₂ catalysts were studied by degrading several anionic and cationic organic pollutants like methylene blue (MB), methylene orange (MO), methylene red (MR), rhodamine B (RhB), reactive blue 160 (RB160), salicylic acid (SA), coumarin and phenol. The 6% Pb-CeO₂ nanocubes shows better photocatalytic performance against anionic dyes especially for MB. To find the optimum condition for better photocatalytic performance of 6% Pb-CeO₂ nanocubes, the photocatalytic process was conducted in different initial reaction conditions like reaction temperature, catalytic dosage, dye concentration and pH of the reaction solution. The stability and recyclability of 6% Pb-CeO₂ photocatalyst was studied by XRD, FT-IR and EDS analysis after 5 cycles of MB degradation. The hydroxyl radical estimation and trapping experiments were conducted to observe the photocatalytic mechanism process in 6% Pb-CeO₂ nanocubes. The perfect doping concentration for better organic pollutant degradation by Pb-CeO₂ is found to be 6 mol% of Pb.     

Biosynthesis of cerium oxide nanoparticles and its cytotoxicity survey against colon cancer cell line

Nanoparticles of cerium oxide (CeO₂-NPs), as a metal oxide of rare earth, have found an important role in improving technologies such as polishing, the degradation of harmful industrial dyes and even the treatment of some diseases. Therefore, the development of quick and inexpensive production methods for CeO₂-NPs is sought by researchers. In the present study, we report the biosynthesis of CeO₂-NPs using aqueous extract of Salvadora persica. Synthesized nanoparticles were investigated through powder X-ray diffraction (PXRD), ultraviolet–visible (UV–vis), Fourier transform infrared, transmission electron microscope (TEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray and Raman techniques. The UV–vis result shows an absorption peak at 325 nm, which confirms the formation of CeO₂-NPs. The band-gap of synthesized nanoparticles (4.1 eV) is higher than in its bulk state. PXRD and Raman show a crystalline fluorite cubic structure for synthesized nanoparticles. The morphology of synthesized nanoparticles shows a uniform and almost spherical shape via TEM and FESEM images. The particles size was estimated in the range of 10–15 nm. Cytotoxic activity of synthesized nanoparticles was determined through 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay against a colon (HT-29) cancer cell line. The results did not show any significant cytotoxic effect for synthesized samples even for concentration higher than 800 μg/mL. Hence, CeO₂-NPs were synthesized using a natural source; the procedure was rapid with good productivity and biosynthesized nanoparticles were non-toxic.     

Preparation and characterization of TiO2 sols and their UV-cured hybrid thin films on plastic substrates

In this research, TiO₂ sols were synthesized via a sol?Cgel reaction at room temperature followed by heating under reflux. Hybrid thin films were prepared using the TiO₂ sols and dipentaerythritol hexacrylate on poly(methyl methacrylate) substrates via spin coating followed by UV-curing. The images of transmission electron microscopy (TEM) and results of dynamic light scattering (DSL) showed that some originally synthesized TiO₂ nanoparticles aggregated while many small-sized (~5?nm) TiO₂ nanoparticles still existed after reflux heating. The synthesized TiO₂ sols showed poor photocatalytic ability, which might avoid degradation of organic moieties in the hybrids. The refractive indices of the hybrid thin films were increased from 1.66 to 1.82 while the water contact angles on the thin films were increased from 70.2° to 87.7° with the increment of TiO₂ content. Increasing the heating time of the TiO₂ sol resulted in an increase in the refractive index and contact angle.     

Green Synthesis of CeO2 Nanoparticles from the Abelmoschus esculentus Extract: Evaluation of Antioxidant,Anticancer, Antibacterial,and Wound-Healing Activities

Metal oxide nanoparticles synthesized by the biological method represent the most recent research in nanotechnology. This study reports the rapid and ecofriendly approach for the synthesis of CeO₂ nanoparticles mediated using the Abelmoschus esculentus extract. The medicinal plant extract acts as both a reducing and stabilizing agent. The characterization of CeO₂ NPs was performed by scanning electron microscopy (SEM), X-ray diffraction (XRD), ultraviolet-visible spectroscopy (UV-Vis), and Fourier transform infrared spectroscopy (FTIR). The in vitro cytotoxicity of green synthesized CeO₂ was assessed against cervical cancerous cells (HeLa). The exposure of CeO₂ to HeLa cells at 10–125 µg/mL caused a loss in cellular viability against cervical cancerous cells in a dose-dependent manner. The antibacterial activity of the CeO₂ was assessed against S. aureus and K. pneumonia. A significant improvement in wound-healing progression was observed when cerium oxide nanoparticles were incorporated into the chitosan hydrogel membrane as a wound dressing.     

Low cost, surfactant-less, one pot synthesis of Cu2O nano-octahedra at room temperature

Cu₂O octahedra were successfully synthesized via a novel wet-chemical method using d-glucose and hydrazine as reducing agent at room temperature without the presence of any other surfactant. Presence of d-glucose was important for the stabilization of the evolved copper octahedra and also for facilitating the reduction of the Cu(II) ions. The existence of glucose moieties on the surface as capping agent was confirmed by the FT-IR spectra while there was presence of excess oxygen atoms on the surface leading to the formation of a thin CuO layer at the octahedra surface, as confirmed by the XPS study, probably promoted by the capping glucose. Effect of NaOH concentration on the reaction and the formation of octahedra was also studied. The formation mechanism of obtained Cu₂O octahedra has been discussed. These octahedra were then studied for their photocatalytic properties in degradation of organic dyes, rhodamine B and methyl orange.     

Formation and properties of hydrophobic CeO2 nanoparticles

Uniform hydrophobic cerium oxide (CeO₂) nanoparticles in a cubic structure with an average size of 4.6 nm were obtained by a novel oil-water interface method in the presence of 0.40 M NaOH. Effects of reactants concentration, oxidation reaction temperature, and the type of surfactants on the final products were investigated. The products were characterized by X-ray diffraction, transmission electron microscopy, UV-visible spectroscopy, room-temperature photoluminescence spectroscopy and contact angle measurements. The products exhibited high luminescence and strong hydrophobicity. The data suggest that Ce(OH) _x ^4?x (x < 4) is a precursor complex for the formation of CeO₂ nanoparticles in liquid phase and its concentration controls the size of CeO₂ particles. The adsorption of the surfactant influences the formation of the hydrophobic particles of CeO₂ by the oil-water interface method.     

Nitrogen‐doped graphene‐cerium oxide (NG‐CeO2) photocatalyst for the photodegradation of methylene blue in waste water

This study shows a facile approach for the preparation of CeO₂ nanoparticles decorated with porous nitrogen‐doped graphene (NG) nanosheets for effective photocatalytic degradation of methylene blue (MB). NG nanosheets were first synthesized using a hydrothermal method and then nitrogen‐doped graphene‐cerium oxide (NG‐CeO₂) was prepared through mixing of cerium nitrate with different concentrations of NG under ultrasonication followed by hydrothermal treatment. The synthesized nanocomposites were characterized using X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE‐SEM). The photocatalytic activity of the synthesized nanocomposites was analyzed against MB dye. Results showed that the nanocomposites of NG‐CeO₂ have an average particle size of 20 nm. The as‐prepared NG‐CeO₂ nanocomposites exhibited outstanding photocatalytic activity for dye degradation under visible light irradiation, which could be attributed to synergistic effects between the NG nanosheets and CeO₂. The quantum of photodegradation increases with the increase of the NG content in the nanocomposites.     

Synthesis,characterization and photocatalytic properties of CaNb2O6 with ellipsoid-like plate morphology

Ellipsoid-like two-dimensional (2D) plates of calcium niobate (CaNb₂O₆) were synthesized via the hydrothermal route without any surfactants or templates by controlling the reaction conditions, viz. the pH value, reaction time and temperature. The prepared powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), fluorescence spectroscopy, and diffuse reflectance UV–vis spectroscopy. It was found that the plates were consisted of uniaxially aligned nanorods and can absorb UV light with wavelengths of less than 340 nm. Compared with the powder of the same material prepared by the solid-state reaction method, the ellipsoid-like 2D plates exhibited a much lower room temperature luminescence intensity and higher photocatalytic activity for the degradation of Rhodamine B dye solution under UV light irradiation. The enhanced photocatalytic activity of the plates was assigned to their higher optical absorption capability, higher diffusion rate of charge carriers and higher surface area resulting from their reduced dimensionality.     

Synthesis, characterization of TiO2 nanotubes-supported MS (TiO2NTs@MS, M=Cd, Zn) and their photocatalytic activity

TiO₂ nanotubes-supported MS (TiO₂NTs@MS, M=Cd, Zn) are synthesized by a simple wet chemical method at room temperature. The products are characterized with transmission electron microscopy (TEM), X-ray diffraction (XRD), UV-vis absorption spectrum and photoluminescence (PL) spectrum. Their optical and morphological properties indicate the interaction between the TiO₂ nanotube and MS nanoparticle. The photocatalytic activities of the TiO₂NTs@MS are evaluated upon the oxidation of methyl orange under UV light illumination. The results reveal that the photocatalytic efficiency of the nanocomposites strongly depends on the specific interaction between MS and support.