Microwave-assisted solution synthesis and photocatalytic activity of Ag nanoparticles supported on ZnO nanostructure flowers

Ag nanoparticles supported on the surface of three-dimensional (3D) flower-like ZnO nanostructure were synthesized by a microwave-assisted solution method. The obtained products were characterized by X-ray diffraction analysis, field-emission scanning electron microscopy, Fourier-transform infrared spectroscopy, Raman spectrophotometry, X-ray photoelectron spectroscopy, and photoluminescence spectroscopy. The analytical results confirmed homogeneously distributed Ag nanoparticles supported on the surface of flower-like ZnO nanostructure. The photocatalytic effect of the heterostructure Ag/ZnO nanocomposites was investigated using photodegradation under ultraviolet (UV) light of methylene blue as model dye. The heterostructure Ag/ZnO nanocomposites exhibited much higher photocatalytic activity than pure ZnO flowers. The improved photocatalytic properties are attributed to formation of a Schottky barrier at the metal–semiconductor interface of the Ag/ZnO nanocomposites.     

纳米Ag/ZnO微波辅助合成与微波增强光催化罗丹明B

本文通过微波辅助、程序升温溶剂热以及煅烧等不同方法制备了系列纳米复合材料Ag/ZnO,并采用X-射线衍射(XRD)、紫外-可见漫反射吸收光谱(UV-Vis/DRS)、X射线光电子能谱(XPS)、氮气吸附-脱附测定以及扫描电子显微镜配合X-射线能量色散谱仪(SEM-EDS)等测试手段对上述合成材料的晶型结构、形貌及表面物理化学性质进行了表征。结果表明,合成过程中辅以微波后其纤锌矿晶型结构未发生明显变化。但同时,其光的吸收性质以及粒子尺寸、形貌以及颗粒分布等方面则有较大改变。其中,经微波辐射、程序升温溶剂热以及煅烧三步处理的样品(mcd-Ag/ZnO)更多呈现规则的六棱柱结构。在紫外光照射和微波辐射下,合成产物光催化降解罗丹明B的实验结果显示,经微波辅助合成的Ag/ZnO光催化活性较未经微波处理样品的活性有较大提高,且明显高于市售P25。同时,mcd-Ag/ZnO在微波辐射下的光催化活性也被有效增强。     

Microwave-assisted method for preparation of Sb-doped ZnO nanostructures and their photocatalytic activity

Nanostructures of Sb-doped ZnO with 0.00, 0.03, 0.06, 0.10 and 0.15 mol fractions of Sb⁺³ ions were prepared by a one-pot method in water under microwave irradiation for 5 min. Powder X-ray diffraction studies display that the nanostructures are excellently crystallized in the form of Wurtzite hexagonal crystalline phase and doping Sb⁺³ ions does not change structure of ZnO. Moreover, size of the nanostructures decreases with increasing mole fraction of Sb⁺³ ions. Scanning electron microscopy and transmission electron microscopy images show that morphology and size of the nanostructures are changing with mole fraction of the dopant. In Fourier transform infrared spectra, intensity of the characteristic peak corresponding to Sb–O bond gradually increases with mole fraction of Sb⁺³ ions. UV–vis diffuse reflectance spectra of the nanostructures are similar to each other and they have a maximum of about 357 nm. Photocatalytic activity of the nanostructures was investigated by degradation of methylene blue under UV irradiation. For the nanostructures with 0.10 mol fraction of Sb⁺³ ions, the degradation rate constant increases nearly two times relative to pure ZnO. In addition, influence of various operational parameters on the degradation activity was investigated and the results were discussed.     

Ultrasonic assisted synthesis of ZnO nanoflakes and photocatalytic activity evaluation for the degradation of methyl orange

In the present investigation, ZnO nanoflakes was prepared via sonochemical synthesis route. Effect of ultrasonic treatment time was studied based on structural, morphological and optical properties. X-ray diffraction (XRD) reveals the formation of wurtzite hexagonal crystalline structure of ZnO nanoflakes. Ultrasonic treatments affected the crystallite size and the density of dislocation, which is due to increased nucleation and growth rates of nanoflakes. The samples synthesized at 40–50 min ultrasonic treatment showed a strong absorption band at 605 and 650 (cm^?1) versus other treatments, which is an indication of 2D nanostructure (nanoflakes). FE-SEM analysis further confirms the formation of 2D nanostructures of the ZnO. The composition and purity was confirmed by the energy dispersive X-ray (EDX) analysis, which displays the occurrence of Zn and O elements in the sample. Photocatalytic activity (PCA) of ZnO nanoflakes was studied for methyl orange (MO) dye degradation under UV light exposure and up to 93.13 % dye degradation is achieved within 90 min. Effect of various parameters (dye concentration, mass of photocatalytic material) and kinetic study was also performed. Results revealed that the ultrasonic treatment affected the optical and photocatalytic properties of the of ZnO nanoflakes, which could be employed for the remediation of dyes in textile effluents.     

Microwave-assisted synthesis of BiOBr/graphene nanocomposites and their enhanced photocatalytic activity

BiOBr/graphene nanocomposites were synthesized by a green single-step microwave strategy and characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy. The photocatalytic activity of the as-prepared BiOBr nanoplates and BiOBr/graphene nanocomposites for the photodegeneration of organic dyes in aqueous solution under visible light irradiation was investigated. The results show that BiOBr/graphene nanocomposites have a higher photocatalytic activity than bare BiOBr nanoplates.     

微波辅助离子热合成具有高光催化活性的BiOBr片层微米立方体

微波辅助离子热合成技术因其加热和反应速度快、反应时间短、产物选择性高、环保、节能等优点, 而广泛应用于纳米棒、纳米线和中空纳米微球等各种形貌功能材料的合成. BiOBr 光催化剂具有毒性低、光生空穴氧化能力强、光降解活性高等优点, 在光催化降解污染物方面研究非常广泛. 虽然各种形貌的 BiOBr 光催化剂可以通过传统的溶剂热法合成,但仍然需要开发绿色和高效节能的合成方法, 来设计新型结构和高光催化降解活性的 BiOBr 光催化剂. 本文首次报道了由微波辅助离子热自组装的方法合成新型结构的 BiOBr 微米立方体. 该 BiOBr 由规则的多层纳米片组成, 其通过在 Br-端表面上选择性吸附离子液体形成, 随后形成氢键的π-π堆叠. 结果显示 BiOBr 是由厚度小于 50 nm 的纳米片组装成为 4 μm 左右的纳米立方块. 其中 Bi:Br:O 摩尔比为 1:1:1, 表明生成纯化学计量比的 BiOBr, 且具有高结晶度的纯四方相. 我们通过添加不同的表面活性剂, 进一步确认氢键-co-π-π叠层在 BiOBr 片层立方块形成中的重要性.将 BiOBr 片层立方块研磨粉碎后其 BET 表面积为从 2.30 急剧增至 17.3 m2/g, 但其降解 RhB 活性却大幅度下降. 由于纳米片层的层间反射和散射, 有效地提升了 BiOBr 的可见光吸收, 光学带隙由 2.66 窄化为 2.56 eV, 因而具有高的可见光光降解活性和优异的稳定性及矿化能力. 光催化降解 180 min 后, 罗丹明 B 的转化率约为 99.57%, 而有机碳去除率高达12.24%; 对于磨碎的 BiOBr 罗丹明 B 的转化率和有机碳去除率分别为 68.68% 和 8.62%. 光催化反应前后的 BiOBr 中, Bi3+离子的 XPS 峰位置没有明显的变化, 进一步表明 BiOBr 光催化剂具有较高的稳定性. 这种具有高活性、优异的稳定性以及高矿化能力的 BiOBr, 在实际应用光催化降解染料废水和清洁能源方面显示出很好的潜力. 此外, 通过光催化反应过程中不同捕获剂的添加确定了光降解的主要活性物种. 当加入硝酸银溶液的时候, 由于光生电子快速被 Ag+离子捕获, 光降解活性明显下降. 活性物种的捕获实验表明, 光生电子为主要的活性物种.     

Hydrothermal synthesis and photocatalytic activity of highly dispersed ZnO powders

The micromorphology of highly dispersed ZnO powders formed from Zn(OH)₂ gels under hydrothermal conditions is studied by powder X-ray diffraction, X-ray diffraction analysis, and low-temperature nitrogen adsorption. The parameters of hydrothermal synthesis (heating rate, treatment duration, and temperature) are found to effect the microstructural characteristics of the products. The photocatalytic activity of the synthesized zinc oxide samples in the model reaction of Methyl Orange photodegradation is studied. The synthesis parameters for preparing ZnO powders with high photocatalytic activity are determined.     

Facile synthesis of ZnO nanoparticles for the photocatalytic degradation of methylene blue

Journal of Sol-Gel Science and Technology - ZnO nanoparticle photocatalysts with a grain size range of 20–100?nm were prepared via a simple sol–gel method and characterized by...     

Microwave-assisted hydrothermal synthesis of cube-like Ag-Ag2MoO4 with visible-light photocatalytic activity

Cube-like Ag-Ag₂MoO₄ composite has been successfully prepared in the presence of PVP (polyvinylpyrrolidone) via a facile microwave-assisted hydrothermal process. Studies of its photocatalytic performance in the decomposition of RhB indicate that the cube-like Ag-Ag₂MoO₄ composite exhibits good catalytic activities under visible-light irradiation. The face that Ag promotes the absorption of visible light may be attributed to the surface plasmon resonance. Further XRD characterization after recycle photocatalytic tests confirms that partial Ag⁺ ions in Ag₂MoO₄ have been reduced to metallic Ag. Reaction temperature, reaction time and the amount of PVP have also been studied and found to play crucial roles in the formation of the cube-like microstructures.     

One-step synthesis of novel flower-like Sn-doped ZnO architectures with enhanced photocatalytic activity

A facile hydrothermal method to synthesize flower-like Sn-doped ZnO (FLSn-ZnO) nanostructures is described. The obtained hierarchical architectures of FLSn-ZnO are found to be assembled with abundant regular-shaped nanosheets and nanoparticles. A possible formation mechanism is proposed on the base of a series of control experiments. The tests show that FLSn-ZnO architectures exhibit higher photocatalytic activity in the degrading Rhodamine B and tetracycline aqueous solution than pure ZnO under UV-light irradiation. And photocurrent response and photoluminescence of ZnO and FLSn-ZnO demonstrates that in photocatalytic performance, the latter is higher.     

Microwave-assisted synthesis of the Fe2O3/g-C3N4 nanocomposites with enhanced photocatalytic activity for degradation of methylene blue

The preparation and photocatalytic performance of the Fe₂O₃/g-C₃N₄ nanocomposites with different weight percentage of iron was investigated in this study. Samples were successfully synthesized using melamine and ferric nitrate as the precursors via the green and facile microwave-assisted method. The physicochemical and structural properties of the Fe₂O₃-doped g-C₃N₄ were characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), the Brunauer–Emmett–Teller (BET) method, transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and ultraviolet–visible spectroscopy (UV–Vis). The photocatalytic activity of the Fe₂O₃/g-C₃N₄ catalysts was evaluated by the degradation of methylene blue (MB) at room temperature under visible light irradiation. As expected, the as-synthesized samples exhibited considerable improvement in the photodegradation of MB. The Fe₂O₃/g-C₃N₄ (1.0 wt%) nanocomposite had superior photocatalytic activity, with almost 70% degradation efficiency within 90 min of irradiation. The enhanced performance was ascribed to the separation and migration of the photoinduced electron–hole pairs and taking part of the charge carriers in the chemical redox reactions at the surface of the photocatalyst. In this work, the effect of Fe weight percentage on the degradation potential was also studied, and the photocatalytic mechanism was proposed with the main reactive species •OH.     

Combustion synthesis of calcium doped ZnO nanoparticles for the photocatalytic degradation of methylene blue dye

ZnO nanoparticles are one of the prominent photocatalysts for environmental applications due to its high redox ability, nontoxic and higher stability. This report explains the synthesis of ZnO nanoparticles by a simple solution combustion method using zinc nitrate hexahydrate as an oxidizing agent and incense stick powder as fuel at 400 °C. Several techniques were adopted for the characterization of the obtained product. X-ray diffraction (XRD) pattern shows that a lower concentration of fuel gives pure ZnO and a higher concentration of fuel results in calcium doped ZnO with a cubic phase having a crystallite size of 32–28 nm. UV–vis spectrum shows that as the fuel concentration increases, band gap decreases and reaches to 3.33 eV for 3 g of fuel. Spongy networks with many pores wereobserved in the scanning electron microscope (SEM) and transmission electron microscope (TEM) images showed the average particle size of Ca doped ZnO NPs is about 20 nm. Pure and Ca doped ZnO nanoparticles were examined for photocatalytic degradation of methylene blue (MB) dye under UV light irradiation. The results prove that Ca doped ZnO nanoparticles show good photocatalytic activity.     

Hydrangea-like ZnO nanospheres on Al substrates via hydrothermal synthesis for photocatalytic activity

Hydrangea-like ZnO nanospheres were fabricated on Al substrates via a facile hydrothermal method with only one step. Scanning electron microscopy, energy-dispersive spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and photoluminescence were used to investigate their morphology, component, structure, and optical properties. The hierarchical nanospheres are fabricated by 2D nanosheets with the shape of 3D sphere. By adjusting the reaction time, the formation process was monitored. The photocatalytic activity of ZnO nanospheres was also investigated for their dye degradation, and they exhibit good photocatalytic ability to congo red, with the degradation rate of 98.4%. Besides, they have universal catalysis effect on methyl orange.     

ZnO nanopowders and their excellent solar light/UV photocatalytic activity on degradation of dye in wastewater

Low-cost and scalable preparation,high photocatalytic activity,and convenient recycle of Zn O nanopowders(NPs)would determine their practical application in purifying wastewater.In this contribution,ZnO NPs were scalably synthesized via the simple reaction of Zn powder with H_2O vapor in autoclave.The structural,morphological and optical properties of the samples were systematically characterized by X-ray diffraction,scanning electron microscopy,Fourier transform infrared spectra,transmission electron microscopy,Micro-Raman,photoluminescence,and ultraviolet-visible spectroscopy.The as-prepared Zn O NPs are composed of nanoparticles with 100–150 nm in diameter,and have a small Brunauer-Emmett-Teller surface area of 6.85 m~2/g.The formation of Zn O nanoparticles is relative to the peeling of H_2 release.Furthermore,the product has big strain-stress leading to the red-shift in the band gap of product,and shows a strong green emission centered at 515 nm revealing enough atomic defects in Zn O NPs.As a comparison with P25,the obtained dust gray Zn O NPs have a strong absorbance in the region of 200–700 nm,suggesting the wide wave-band utilization in sunlight.Based on the traits above,the Zn O NPs show excellent photocatalytic activity on the degradation of rhodamine B(Rh-B)under solar light irradiation,close to that under UV irradiation.Importantly,the Zn O NPs could be well recycled in water due to the quick sedimentation in themselves in solution.The low-cost and scalable preparation,high photocatalytic activity,and convenient recycle of Zn O NPs endow themselves with promising application in purifying wastewater.     

Parameters affecting carbofuran photocatalytic degradation in water using ZnO nanoparticles

Carbofuran photodegradation in water using zinc oxide nanoparticles as a catalyst was examined as well as some parameters influencing its percentage degradation rate such as zinc oxide load, initial concentration of carbofuran, the temperature of the reaction, the initial pH of the solution, and doping of zinc oxide nanoparticles with 5% (w:w) silver. Zinc oxide and Ag-doped zinc oxide nanoparticles were produced using solvothermal and photoreduction methods, respectively, and silver doping effects on the structural, optical, and photocatalytic properties of zinc oxide nanoparticles were investigated using XRD, UV-VIS spectrophotometer, TEM, SEM, SEM/EDX, and FTIR. The average diameter of the synthesized samples was 26.6, 30.55 nm for undoped zinc oxide and Ag-doped zinc oxide, respectively. Zinc oxide doping with silver did not change the shape of the zinc oxide crystal, but decreased the reflection in the visible region, as well as the energy of the bandgap, and increased the zinc oxide photocatalytic activity.     

Synthesis of ZnO nanoparticles and its application in photocatalytic degradation of LABS by the trial-and-error and Taguchi methods

In the work ZnO nanoparticles were prepared by sol-gel method. The catalyst was characterized by X-ray powder diffractometer (XRD), scanning electron microscopy (SEM). The photocatalytic oxidation of anionic surfactant in detergent industries was studied using ZnO nanoparticles with diameter size 20 nm as catalyst on irradiation with UV light. Analysis of kinetic showed that the amount of surfactant photocatalytic degradation can be fitted with pseudo-first-order model and studied photochemical elimination of Linear alkyl benzene sulfonates by the trial-and-error and Taguchi methods. Our experimental design consisted of testing five factors, i.e. dosage of K₂S₂O₈, concentration of surfactant, amount of ZnO, irradiation time, and initial pH. The results showed that photocatalytic degradation of linear alkyl benzene sulfonates was strongly influenced by these parameters.     

Microwave-assisted rapid photocatalytic degradation of malachite green in TiO2 suspensions: mechanism and pathways

Microwave-assisted photocatalytic (MPC) degradation of malachite green (MG) in aqueous TiO2 suspensions was investigated. A 20 mg/L sample of MG was rapidly and completely decomposed in 3 min with the corresponding TOC removal efficiency of about 85%. To gain insight into the degradation mechanism, both GC-MS and LC-ESI-MS/MS techniques were employed to identify the major intermediates of MG degradation, including N-demethylation intermediates [(p-dimethylaminophenyl)(p-methylaminophenyl)phenylmethylium (DM-PM), (p-methylaminophenyl)(p-methylaminophenyl)phenylmethylium (MM-PM), (p-methylaminophenyl)(p-aminophenyl)phenylmethylium (M-PM)]; a decomposition compound of the conjugated structure (4-dimethylaminobenzophenone (DLBP)); products resulting from the adduct reaction of hydroxyl radical; products of benzene removal; and other open-ring intermediates such as phenol, terephthalic acid, adipic acid, benzoic acid, etc. The possible degradation mechanism of MG included five processes: the N-demethylation process, adduct products of the hydroxyl radical, the breakdown of chromophores such as destruction of the conjugated structure intermediate, removal of benzene, and an open-ring reaction. To the best of our knowledge, it is the first time the whole MG photodegradation processes have been reported.     

High-yield synthesis of pure ZnO nanoparticles by one-step solid-state reaction approach for enhanced photocatalytic activity

Zinc oxide (ZnO) nanostructures were synthesized via a one-step solid-state reaction approach in ammonia (NH₃) gas environment with different temperature ramp rates. The so-formed nanostructures were characterized using X-ray diffraction (XRD) for phase identification, where the typical wurtzite hexagonal structure was observed. Scanning electron microscopy (SEM) confirmed the particle size to be in the range 45–50 nm, the same as calculated by the XRD pattern for the ramp rate of 10 °C/min. Energy dispersive X-ray (EDX) spectroscopy and X-ray photoelectron spectroscopy (XPS) confirmed the chemical purity of the samples. The photoluminescence (PL) spectrum indicated multiple near-band-edge emissions and energy-band emissions. Then, these ZnO nanomaterials were used for the degradation of crystal violet (CV) dye under UV light irradiation. The CV solution was completely degraded in 2 hr. The initial photocatalyst and dye amounts of 0.2 g/100 ml and 0.5 mg/L, respectively, were found to be the optimum values for maximum degradation efficiency. The ZnO-based photocatalyst was stable up to three cycles of reuse. These results indicate that the high surface area and porosity of the nanomaterials are responsible for the high efficiency, which was confirmed by specific surface area analysis.     

Facile synthesis of polyoxometalate-thionine composite via direct precipitation method and its photocatalytic activity for degradation of rhodamine B under visible light

(TH)(3)PW(12) (TH=thionine, PW(12)=PW(12)O(40)(3-)) composite was prepared by direct precipitation of TH and PW(12). The (TH)(3)PW(12) was characterized via UV-vis spectrum, FT-IR, SEM, and BET surface area. PW(12) was intact during the precipitation process. The composite has a bar-like shape and relatively large surface area (Langmuir surface of (TH)(3)PW(12) was 31.59 m(2)g(-1), BET surface was 20.26 m(2)g(-1)). Using the material as the photocatalyst, rhodamine B (RhB) was efficiently bleached and mineralized under visible light irradiation (λ>420 nm). The kinetics of the photodecomposition follow the first-order reaction. The (TH)(3)PW(12) catalyst can be easily separated from the reaction system and has good stability for reuse.     

Aspect-ratio-dependent photoinduced antimicrobial and photocatalytic organic pollutant degradation efficiency of ZnO nanorods

The photo-antimicrobial and photocatalytic performance of ZnO nanorods as a function of aspect ratio are presented. The antibacterial activity of the synthesized ZnO nanorod samples against Gram-negative and Gram-positive bacteria (Staphylococcus aureus and Escherichia coli, respectively) was determined by shake flask method with respect to time. ZnO nanorods with high aspect ratio showed superior antimicrobial and photocatalytic activity. These results are supported by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, ultraviolet–visible (UV–Vis) spectroscopy, photoluminescence, and Brunauer–Emmett–Teller (BET) studies. Degradation of methylene blue dye as model organic pollutant was used to assess their photocatalytic activity. Pseudo-first-order rate kinetics was used to calculate the photocatalytic reaction rate constant. The mechanisms for both antimicrobial and photocatalytic activity are elucidated.