ZnO Nanofiber and Nanoparticle Synthesized Through Electrospinning and Their Photocatalytic Activity Under Visible Light

In this paper, we fabricate ZnO nanofibers and nanoparticles through electrospinning precursor solution zinc acetate(ZnAc)/cellulose acetate(CA) in mixed-solvent N , N -dimethylformamide/acetone. Depending on the posttreatment of precursor ZnAc/CA composite nanofibers, both ZnO nanofibers and nanoparticles were synthesized after calcination of precursor nanofibers. The morphology and crystal structure of the ZnO nanofiber and nanoparticle were characterized by scanning electron microscopy, transmission electron microscopy, atomic force microscopy, and X-ray diffraction. It was found that the mean diameter of the ZnO nanofiber and nanoparticle was ca. 78 and 30 nm, respectively. The photo-degradation of dye molecules such as Rhodamine B and acid fuchsin catalyzed by the ZnO nanofiber and nanoparticle was evaluated under the irradiation of visible light. Both morphological ZnO species showed strong photocatalytic activity. However, the ZnO nanofiber in the form of nanofibrous mats showed much higher efficiency than the nanoparticle although the latter has a smaller size than the former. The porous structure of ZnO nanofibrous mats is believed to improve the contacting surface areas between the catalyst and the dye molecules, while the aggregation of ZnO nanoparticle in the solution lowers the photocatalytic efficiency.     

Green Synthesis of ZnO Nanoparticles and Its Application in the Degradation of Some Dyes

A novel ZnO photocatalyst was synthesized by a green method using lemon juice and zinc acetate as precursors, and then the effect of sucrose addition on the initial precursors was investigated. The samples were characterized by field‐emission scanning electron microscopy, X‐ray diffraction, Fourier transform infrared, UV‐visible, and photoluminescence analysis. The result showed that the as‐obtained products with the mix of lemon juice (30 mL) and sucrose had a spherical morphology with the mean particle size of about 21.5 nm. The photocatalytic activity of this sample was tested for the degradation of methyl orange, methyl red and methylene blue solutions. The results also revealed the good photocatalytic activity for the degradation of these three organic dyes. Furthermore, as‐synthesized sample was used in decolorization processes and the treatment of textile dyes (reactive blue 21).     

Preparation of Pectin–ZnO Nanocomposite

Pectin–ZnO nanocomposite was prepared in the aqueous solution condition at room temperature. The Fourier transform infrared, X-ray diffraction, and transmission electron microscope (TEM) measurements confirmed the nanoscaled structure of pectin–ZnO composite. According to the TEM observation, the average composite granules size was about 150 nm and the embedded ZnO nanoparticles were uniform with an average diameter of 70 nm.     

针状ZnO的纳米纤维素诱导制备及光催化性能

以纳米纤维素（NCC）为形貌诱导剂,乙酸锌为反应前驱物,采用水热法合成针状ZnO。通过X射线衍射仪（XRD）、扫描电子显微镜（SEM）和能量色散X射线光谱仪（EDS）对ZnO的形貌、微观结构、结晶特性进行了表征,并探讨了其形成机理及光催化降解性能。结果表明水热条件下,NCC能诱导ZnO在其表面沉积和生长,可形成直径260nm、长度10μm的针状结构,诱导制备的针状ZnO室温下2h内对孔雀绿的紫外光降解效率为88.5%。针状ZnO在光催化剂等领域具有潜在应用价值。     

PREPARATION OF ZINC OXIDE NANOPARTICLE VIA UNIFORM PRECIPITATION METHOD AND ITS SURFACE MODIFICATION BY METHACRYLOXYPROPYLTRIMETHOXYSILANE

Zinc oxide nanoparticles were prepared by uniform precipitation using urea hydrolysis. The ZnO precursor was slowly deposited from aqueous solution. Anionic surfactant was added into solution to block ZnO crystal growth and its agglomeration. Then ZnO nanoparticles were synthesized by the calcination of the precursor at high temperature. Transmission electron microscope (TEM) observation and particle size analyzer demonstrated that the ZnO nanoparticle exhibited nearly spheric shape with 10-40 nm particle size. The surface of the ZnO nanoparticle was modified by methacryloxypropyltrimethoxysilane (MPS). FT-IR (Fourier transform-infrared spectrophotometry) and XPS (X-ray photoelectron spectrophotometry) revealed that MPS was grafted onto the zinc oxide nanoparticle. XRD (X-ray diffraction) showed that the ZnO nanoparticle was a hexagonal crystal with a perfect crystalline structure, and its crystalline morphology was not altered through surface modification. The activation index (AI) of the modified ZnO nanoparticle was measured. It was found that the surface of the ZnO nanoparticle was changed from hydrophilicity into hydrophobicity via surface modification, implying the enhancement of its compatibility with organic polymers. FE-SEM (field scanning electron microscopy) showed that the modified ZnO nanoparticles were homogeneously dispersed in PVC matrices. Consequently, ZnO nanoparticles were integrated with PVC matrices by the grafting organic molecule.     

PREPARATION OF ZINC OXIDE NANOPARTICLE VIA UNIFORM PRECIPITATION METHOD AND ITS SURFACE MODIFICATION BY METHACRYLOXYPROPYLTRIMETHOXYSILANE

Zinc oxide nanoparticles were prepared by uniform precipitation using urea hydrolysis. The ZnO precursor was slowly deposited from aqueous solution. Anionic surfactant was added into solution to block ZnO crystal growth and its agglomeration. Then ZnO nanoparticles were synthesized by the calcination of the precursor at high temperature. Transmission electron microscope (TEM) observation and particle size analyzer demonstrated that the ZnO nanoparticle exhibited nearly spheric shape with 10–40 nm particle size. The surface of the ZnO nanoparticle was modified by methacryloxypropyltrimethoxysilane (MPS). FT-IR (Fourier transform-infrared spectrophotometry) and XPS (X-ray photoelectron spectrophotometry) revealed that MPS was grafted onto the zinc oxide nanoparticle. XRD (X-ray diffraction) showed that the ZnO nanoparticle was a hexagonal crystal with a perfect crystalline structure, and its crystalline morphology was not altered through surface modification. The activation index (AI) of the modified ZnO nanoparticle was measured. It was found that the surface of the ZnO nanoparticle was changed from hydrophilicity into hydrophobicity via surface modification, implying the enhancement of its compatibility with organic polymers. FE-SEM (field scanning electron microscopy) showed that the modified ZnO nanoparticles were homogeneously dispersed in PVC matrices. Consequently, ZnO nanoparticles were integrated with PVC matrices by the grafting organic molecule.     

Vitis labruska skin extract assisted green synthesis of ZnO super structures for multifunctional applications

The formation of unique morphologies of zinc oxide (ZnO) super structured frameworks were reported via a simple and eco-friendly route employing Vitis labruska fruit Black Grape Skin (BGS) extract as a fuel. XRD, FTIR, UV–vis, PL, SEM and TEM studies are performed to analyse the formation and characterization of ZnO. XRD confirmed the crystalline nature of the material with hexagonal Wurtzite structure having average crystallite size of ~50 nm. FTIR spectrum shows a band at 532 cm⁻¹ due to the vibrational mode of Zn-O bending. The band gap of the ZnO was found to be 3.26 eV. SEM images confirm the formation of different morphologies like Mysore pak (a popular Indian dessert), canine teeth, hollow pyramids and gems were obtained by varying the weight of BGS. These superstructures were obtained due to the interaction of Zn²⁺ with BGS extract. TEM images clearly shows lattice spacing of 0.29 nm corresponding to the (002) plane of ZnO. Photoluminescence (PL) spectrum shows strong yellow light emission upon excitation at 320 nm due to the Zn-O defects. Synthesized ZnO nanoparticles (Nps) exhibited good photocatalytic activity for the degradation of Methylene blue (MB) dye. The photocatalytic activity was due to the production of OH˙ radicals during photo irradiation on ZnO Nps. ZnO Nps also exhibited superior antibacterial activity against Staphylococcus aureus and Escherichia coli bacteria. Further, ZnO Nps were also used in the development of novel electrochemical sensing platform towards the electrochemical detection of hydrazine as a model system at very low concentrations having a detection limit of 0.3 µM.     

Green Synthesis of Zinc Oxide Nanoparticles (ZnO NPs) for Effective Degradation of Dye,Polyethylene and Antibacterial Performance in Waste Water Treatment

At present, there is a vital need for river water purification by developing new approaches to eliminate bacterial biofilms, textile dyes, and Low-Density Polyethylene (LDPE) plastics that pose severe threats to human and environmental health. The current work put forward the construction of an eco-friendly green strategy to synthesize zinc oxide nanoparticles (ZnO NPs) using areca nut (Areca catechu) extract and their application to tackle the challenges in water purification. Prepared biogenic NPs were characterized by X-ray diffraction analysis (XRD), Fourier Transform Infra-Red (FT-IR), Energy Diffraction Spectroscopy (EDS), Scanning Electronic Microscopy (SEM), Transmission Electron Microscopy (TEM) analysis, confirmed the spherical shape in 20 nm and UV–vis spectroscopy. The characteristic absorption band exhibited at 326 nm confirmed the formation of ZnO NPs using UV–vis spectroscopy. Among all the tested bacterial pathogens, the E. coli at 50 µg/mL concentration showed the highest inhibition of biofilm activity, followed by the highest growth curve, cellular leakage, and potassium ion efflux. The ZnO NPs observed with photo-degradation of Rhodamine-B (Rh-B), Methylene Blue (MB), and Nigrosine dyes under sunlight irradiation at different time intervals. Finally, the photocatalytic activity of LDPE-ZnO NPs nanocomposite film showed the highest degradation under solar light irradiation were confirmed through photo-induced weight loss, SEM, FTIR, and MALDI-TOF analysis. This study demonstrates ZnO NPs exhibit efficacy against biofilm formation, degradation of photocatalytic textile dyes, and low-density LDPE film under solar light irradiation, which can be a step forward in water purification.

     

Preparation of Zinc Oxide Nanofibers by Electrospinning

Ultra-thin fibers of zinc oxide (ZnO) were prepared by sol–gel processing and the electrospinning technique using poly(vinyl acetate) and zinc acetate as precursors. The fibers were characterized by thermogravimetric analysis, scanning electron microscopy, Fourier-transfer infrared, and X-ray diffraction, respectively. The results showed that the diameter of the precursor fibers increased with increasing zinc acetate content, and the size of the inorganic ZnO nanofibers decreased obviously as the calcining time increased.     

Application of impregnation combustion method for fabrication of nanostructure CuO/ZnO composite oxide: XRD,FESEM, DRS and FTIR study

Nanostructured CuO/ZnO composite oxide was prepared by a novel impregnation combustion method using copper nitrate and zinc oxide tetrapod. The X-ray diffraction patterns revealed that CuO/ZnO composite oxide was formed. The effects of different impregnation combustion parameters on the properties of composite were studied by field-emission scanning electron microscope (FESEM), powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR) and UV–vis diffuse reflectance spectrum (DRS). The synthesis of ZnO–CuO nanocomposites through impregnation of a zinc oxide tetrapod with copper nitrate aqueous sodium carbonate solutions is reported. During thermal treatment the samples evolve toward the formation of nanocrystalline ZnO particles (zincite phase) dispersed onto tenorite, CuO annealed at 450 °C. XRD patterns of the precursors calcined at 450 °C showed the formation of the zincite–tenorite phases. Field emission scanning electron microscopy (FESEM) exhibited loosely agglomerated hexagonal particles with uniform morphology having a size around 50 nm.     

Sn-containing layered double hydroxides as precursors for nano-sized ZnO/SnO2 photocatalysts

Sn⁴⁺-containing LDH was prepared using the co-precipitation method at constant pH, and characterized using X-ray diffraction, UV–vis diffuse reflectance spectroscopy and TG/DTG methods. The obtained product was further exposed to different thermal treatments in order to obtain nano-sized coupled ZnO/SnO₂ systems with enhanced photocatalytic performances than the ones obtained by mixing the two semiconductor oxides. The formation of a well-defined ZnO/SnO₂ system and the crystallite size, fully investigated using XRD, micro-Raman scattering and UV–vis DR techniques, were found to be influenced by the nature of the precursors and the calcination temperature. The photocatalytic activity of the ZnO/SnO₂ systems, evaluated for the photodegradation of methyl orange (MO) dye, was studied as a function of the initial pH, catalyst loading and the calcination temperature. The metal dispersion supplied by layered structures proved to be an advantage when preparing coupled ZnO/SnO₂ systems, the photocatalytic activity being 2.3 times higher comparing with the physical mixtures performances. The maximum photocatalytic activity of the coupled ZnO/SnO₂ system having a layered precursor was observed when using neutral pH, at a catalyst loading of 1 g/L calcined at 600 °C for 4 h.     

低温固相法制备纳米氧化锌及其在脱硫中的应用

以乙酸锌和草酸为原料,采用低温固相法制备了纳米氧化锌,考察了表面活性剂和焙烧温度对氧化锌晶粒的影响,采用XRD、TG-DTA、IR和TEM等技术进行表征。以不同晶粒的氧化锌为锌源,采用等体积浸渍法制备一系列NiO/ZnO吸附荆;以噻吩/正庚烷为模型化合物,在固定床微反装置考察氧化锌晶粒对吸附剂脱硫性能的影响。结果表明,表面活性剂以十二烷基硫酸钠效果最好,合适的焙烧温度为400℃;制备的氧化锌呈球形,为六方晶系纤锌矿结构,具有较好的分散性,平均粒径约15 nm。活性评价表明,NiO/ZnO吸附剂对噻吩类硫化物具有较高的活性。可以实现超深度脱硫;氧化锌晶粒越小,相应NiO/ZnO吸附剂的脱硫活性越高;脱硫前后吸附剂的XRD谱图对比表明,脱硫过程中S以ZnS的形式固定在吸附剂上。     

Structure and Photoluminescent Properties of ZnO Encapsulated in Mesoporous Silica SBA-15 Fabricated by Two-Solvent Strategy

The two-solvent method was employed to prepare ZnO encapsulated in mesoporous silica (ZnO/SBA-15). The prepared ZnO/SBA-15 samples have been studied by X-ray diffraction, transmission electron microscope, X-ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm, and photoluminescence spectroscopy. The ZnO/SBA-15 nanocomposite has the ordered hexagonal mesostructure of SBA-15. ZnO clusters of a high loading are distributed in the channels of SBA-15. Photoluminescence spectra show the UV emission band around 368 nm, the violet emission around 420 nm, and the blue emission around 457 nm. The UV emission is attributed to band-edge emission of ZnO. The violet emission results from the oxygen vacancies on the ZnO–SiO₂ interface traps. The blue emission is from the oxygen vacancies or interstitial zinc ions of ZnO. The UV emission and blue emission show a blue-shift phenomenon due to quantum-confinement-induced energy gap enhancement of ZnO clusters. The ZnO clusters encapsulated in SBA-15 can be used as light-emitting diodes and ultraviolet nanolasers.     

氧化锌纳米晶的制备及表征研究

采用溶胶-凝胶法以醋酸锌、草酸为原料制备ZnO纳米晶,借助X射线粉末衍射(XRD)、扫描电子显微镜(SEM)等表征手段进行了物相分析和微观形貌表征.结果 表明,制备ZnO纳米晶适宜工艺条件为:凝胶化温度80℃,凝胶化时长1.5h,焙烧温度600℃,焙烧时间3h.X射线衍射图表明ZnO纳米晶在(101)晶面出现取向生长....     

Synthesis of Porous NiO and ZnO Submicro- and Nanofibers from Electrospun Polymer Fiber Templates

Porous nickel oxide (NiO) and zinc oxide (ZnO) submicro- and nanofibers were synthesized by impregnating electrospun polyacrylonitrile (PAN) fiber templates with corresponding metal nitrate aqueous solutions and subsequent calcination. The diameter of the NiO and ZnO fibers was closely related to that of the template fibers and larger diameters were obtained when using the template fibers with larger diameter. SEM results showed that the NiO and ZnO fibers have a large amount of pores with diameters ranging from 5 nm to 20 nm and 50 nm to 100 nm, respectively. Energy dispersive X-ray (EDX) spectra and X-ray diffraction (XRD) patterns testified that the obtained materials were NiO and ZnO with high purity.     

Preparation of nanostructure CuO/ZnO mixed oxide by sol–gel thermal decomposition of a CuCO3 and ZnCO3: TG,DTG, XRD,FESEM and DRS investigations

Nanostructure CuO/ZnO mixed oxide was systematically prepared via the sol–gel route using zinc and copper carbonates as precursors (molar ratio of 2:1) under thermal decomposition. The zinc and copper carbonates precursors have been synthesized by a simple chemical reaction in high yield and characterized by its melting point, FT-IR and thermal analysis (TG/DTG). The TG/DTG analysis proved that the thermal decomposition of zinc and copper carbonates precursors at 255 °C and 289 °C respectively. Thermo-gravimetric analysis (TG-DTG), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and diffuse reflectance spectroscopy (DRS) studies were undertaken to investigate the thermal properties and electronic structure of the CuO/ZnO mixed oxide catalysts. XRD data of the samples proved the formation of the nano-crystalline CuO/ZnO mixed oxide. Scanning electron microscopy (SEM) showed that the spherical-like particles have a diameter in the range 35–45 nm. Optical spectra of the nanostructure show a band peaked at 1.35 eV which is associated to near band gap transitions of CuO and a band centered at about 3.00 eV related to band gap transitions of ZnO nanostructures.     

Temperature-dependent growth of ZnO structures by thermal oxidation of Zn coatings electrodeposited on steel substrates and their photocatalytic activities

In this work, zinc oxide (ZnO) nanostructures were successfully synthesized by thermal oxidation of zinc (Zn) coated steel substrates. Zn coatings were electrodeposited on the mild carbon steel sheet in the sulfate bath by DC current. The zinc coated samples were oxidized in air at distinct annealing temperatures between 400 °C and 800 °C. The phase structure and surface morphology of the ZnO films were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic activity of these ZnO layers was examined by means of decomposition of methylene blue (MB) aqueous solutions under UV lamp irradiation for various duration. The findings illustrated that annealing temperatures had a big effect on the morphology and structure of the ZnO layers. The annealed layers showed significantly enhanced photoactivity activity than the pure Zn layer under UV-irradiation. The sample with ZnO nanostructures oxidized at 800 °C exhibited a better photocatalytic degradation of MB than the other samples. This paper can provide an important contribution to the development of efficient photocatalysts for the solution of the environmental pollution problems.     

ZnO nanocrystallites/cellulose hybrid nanofibers fabricated by electrospinning and solvothermal techniques and their photocatalytic activity

ZnO nanocrystallites have been in situ embedded in cellulose nanofibers by a novel method that combines electrospinning and solvothermal techniques. Zn(OAc)₂/cellulose acetate (CA) precursor hybrid nanofibers with diameter in the range of 160–330 nm were first fabricated via the electrospinning technique using zinc acetate as precursor, CA as the carrier, and dimethylformamide (DMF)/acetone(2 : 1) mixture as cosolvent. The precursor nanofibers were transformed into ZnO/cellulose hybrid fibers by hydrolysis in 0.1 mol/L NaOH aqueous solution. Subsequently, these hybrid fibers were further solvothermally treated in 180°C glycerol oil bath to improve the crystallite structure of the ZnO nanoparticles containing in the nanofibers. The structure and morphology of nanofibers were characterized by scanning electron microscopy, transmission electron microscopy, and X‐ray diffraction. It was found that hexagonal structured ZnO nanocrystallites with the size of ～ 30 nm were dispersed on the nanofiber surfaces and within the nanofibers with diameter of about 80 nm. The photocatalytic property of the ZnO/cellulose hybrid nanofibers toward Rhodamine (RhB) was tested under the irradiation of visible light. As a catalyst, it inherits not only the photocatalytic ability of nano‐ZnO, but also the thermal stability, good mechanical property, and solvent‐resistibility of cellulose nanofibers. The key advantages of this hybrid nanofiber over neat ZnO nanoparticles are its elasticity, dimensional stability, durability, and easy recyclability. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Formation of 1-D ZnTe nanocrystals by aerosol-assisted spray pyrolysis

One-dimensional (1-D) ZnTe nanowires were prepared by aerosol-assisted spray pyrolysis using a mixture of ZnO (1 mmol)/OA (4 mL)/TOPO (0.8 g)/ODE (4 mL) as Zn precursor and Te/TOP (3 mL of 0.75M) as Te precursor. The shape, size, and crystal structure of products were characterized by means of transmission electron microscope (TEM) and X-ray diffraction (XRD). The shape evolution of ZnTe nanocrystals from nanodots to nanowires was achieved by controlling the reaction temperature. ZnTe nanodots with average diameter of 8.3 nm were synthesized at 300 °C. “Earthworm-like” shaped ZnTe (linear ZnTe aggregates) consisting of primary ZnTe nanodots of about 16 nm in diameter were obtained at 400 °C. In addition, 1-D ZnTe nanowires were prepared at reaction temperature higher than 450 °C. Those experimental results suggest that ZnTe nanowires with zinc blende structure are formed from ZnTe nanodots by the oriented attachment due to insufficient surface capping of surfactant molecules and by strong dipole-dipole interaction of nanodots, followed by self-organization of linear aggregates at higher reaction temperatures. The linear ZnTe aggregates consisting of primary ZnTe nanodots may be an intermediate stage in the formation process of nanowires from nanodots.     

Preparation and Optical Property of Long Single Crystalline ZnO Nanofibers

Long single crystal ZnO nanofibers were synthesized on a large-scale by a simple solvothermal method at low temperature in the presence of dodecyl benzene sulfonic acid sodium salt and hydrazine. X-ray diffraction, scanning electron microscopy, transmission electron microscopy and high-resolution transmission electron microscopy were used to characterize the product. The diameter of the single crystal nanofiber is 50–70 nm and the length is 30–50 μm. Due to the oxygen or the zinc vacancy in the nanofibers, the wide emission in the visible light region is increased, while the sharp UV emission still exists at 388.5 nm.