Microwave synthesis and characterization of ZnO with various morphologies

ZnO micro- and nanostructures with a variety of morphologies have been synthesized using Zn(NO₃)₂·6H₂O and pyridine by a microwave-assisted aqueous solution method at 90 °C for 10 min. The pyridine has a significant influence on the morphology of ZnO. Various morphologies of ZnO (hexagonal columns, linked hexagonal needles, hollow structures, and hexagonal nanorings) were obtained by adjusting the concentration of pyridine. The effect of the type of other alkaline additive (aniline and triethanolamine) on the morphology of ZnO was also investigated. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM).     

Morphological syntheses of ZnO nanostructures under microwave irradiation

ZnO nanostructures with flower-, rod-, and flake-like morphologies have been controllably synthesized using Zn(acac)₂·H₂O (acac = acetylacetonate) as a single-source precursor through a facile and fast microwave-assisted method. The morphologies of ZnO nanostructures can be systematically adjusted by using various surfactants. The ZnO products are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. The results show that all ZnO nanostructures are of single-crystalline nature with hexagonal wurtzite structure. The possible formation mechanism for these ZnO nanostructures is proposed and their photoluminescence properties are also investigated.     

Facile synthesis of ZnO nanostructures and investigation of structural and optical properties

ZnO nanostructures were synthesized by chemical bath deposition method, using zinc nitrate [Zn(NO₃)₂] and hexa-methylene-tetra-amine [(HMT),C(H₂)₆N₄] as precursors. Controlled size and shape evolution of ZnO nanostructures were achieved by changing the HMT concentration from 0.025 M to 0.1 M, whereas Zn(NO₃)₂ concentration kept constant. X-ray diffraction (XRD) and Raman study confirmed the formation of single crystalline, hexagonal wurtzite ZnO structure. Sharp peaks in Raman spectra, corresponding to E₂(low) and E₂(high) referred to wurtzite structure with higher order of crystallinity. Transmission electron microscopy (TEM) revealed that the shape and size of the nanostructures reduced, with increasing concentration of HMT. Further, effect of structure's size was observed in the band gap (shift). Photoluminescence study showed two peaks at ~ 380 nm and ~ 540 nm corresponding to the band to band transition and defect transitions. Modifications of properties are explained in detail on the basis of shape and size change of the structures and possible mechanism is discussed.     

Fabrication and growth mechanism of hexagonal zinc oxide nanorods via solution process

This article presents, the fabrication of perfectly hexagonal zinc oxide nanorods performed via solution process using zinc nitrate hexahydrate (Zn(NO₃)₂·6H₂O) and hexamethylenetetramine (HMT) at various concentrations of i.e. 1 × 10⁻³ to 10 × 10⁻² M in 50 mL distilled water and refluxed at 100 °C for 1 h. We used HMT because it acts as a template for the nucleation and growth of zinc oxide nanorods, and it also works as a surfactant for the zinc oxide structures. The X-ray diffraction patterns clearly reveal that the grown product is pure zinc oxide. The diameters and lengths of the synthesized nanorods lie in the range of 200–800 nm and 2–4 μm, respectively as observed from the field emission scanning electron microscopy (FESEM). The morphological observation was also confirmed by the transmission electron microscopy (TEM) and clearly consistent with the FESEM observations. The chemical composition was analyzed by the FTIR spectroscopy, and it shows the ZnO band at 405 cm⁻¹. On the basis of these observations, the growth mechanism of ZnO nanostructures was also proposed.     

Dendritic and epitaxial growths of ZnO particle-rod and rod-rod nanostructures with quasi-one-dimensional and two-dimensional configurations

Quasi-one-dimensional and two-dimensional ZnO nanostructures have been fabricated through thermal evaporation approach. The microstructures of the ZnO nanostructures have been studied using scanning electron microscopy and high-resolution electron microscopy. Quasi-one-dimensional ZnO nanostructures are formed by dendritic growths of ZnO nanoparticles from the stem nanorods surfaces, forming particle-rod nanostructures. While epitaxial growths of branch nanorods from the stem nanorods configure two-dimensional ZnO nanostructures. The epitaxial growth orientation relationship can be described as [2? 110]_R1 || [2? 110]_R2 and (0001) _R1 || (011?0)_R2. The growth mechanism of the quasi-one-dimensional and two-dimensional ZnO nanostructures has been discussed.     

Facile ultrasound-assisted synthesis of ZnO nanorods in an ionic liquid

ZnO nanocrystals have been synthesized by ultrasound-assisted synthesis from Zn(CH₃COO)₂2H₂O and NaOH in the neat room-temperature ionic-liquid 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide, [C₄mim][Tf₂N]. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) show that the formed ZnO nanocrystals are of rod like shape with lengths from 50 to 100 nm and diameters of about 20 nm. X-ray diffraction (XRD) confirms the crystallinity as well as the sample purity. The band gap of the as-prepared ZnO nanorods was estimated to be 3.31 eV from UV–Vis absorption measurements. The photoluminescence spectrum shows the characteristic greenish emission of ZnO at room temperature (λ_max = 563 nm). The ZnO bonding levels have been determined by X-ray photoelectron spectroscopy (XPS). Nitrogen adsorption–desorption measurements show typical samples to have a specific surface area of 49.93 m²/g.     

Tailor of ZnO morphology by heterogeneous nucleation in the aqueous solution

The umbrella-like ZnO nanostructures have been prepared by the morphological tailoring in the aqueous solution at 95 °C in the addition of heterogeneous seeds such as MnO₂ and CdS nanoparticles. The morphology and structure of as-synthesized umbrella-like ZnO nanostructures have been characterized by transmission electron microscopy (TEM), high-resolution transmission electron microscope (HRTEM), electron energy loss spectroscopy (EELS), field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The heterogeneous seeds play the critical role for the formation of umbrella-like ZnO nanostructures. Furthermore, the formation mechanism of the umbrella-like nanostructures has been phenomenally presented.     

Selective H2S detection by CuO functionalized ZnO nanotetrapods at room temperature

ZnO nanotetrapods have been synthesized by carbothermal method. The structure, phase, morphology of the synthesized sample were investigated by X-ray diffraction and X-ray photoelectron spectroscopy, Scanning electron microscopy, Transmission electron microscopy and Selected area electron diffraction. The gas-sensing characteristics of thick films of pure and CuO-functionalized ZnO Nanotetrapods have been compared. Pure ZnO nanotetrapod films were found to be sensitive to both H₂S and NO with similar sensitivities, at a temperature of 250–300 °C. It is demonstrated that functionalization of ZnO nanotetrapods with CuO, results in selectivity towards H₂S at a lower temperature of 50 °C.     

Facile tailoring of titanate nanostructures at low alkaline concentration by a solvothermal route

Nanostructured titanates with different morphologies such as nanoflakes, nanotubes, and nanofibers have been selectively synthesized by a simple solvothermal treatment of commercial anatase TiO₂ using the mixed water–ethanol cosolvent at low alkaline concentration. The effects of solvothermal temperature, volume ratio of H₂O to C₂H₅OH, amount of NaOH and solvents on the formation of titanate nanostructures have been systematically studied through X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). At low concentration of NaOH solution (the actual concentration of OH⁻ in the solution is only 0.58 M), different titanate nanostructures are achieved by simply changing the volume ratio of H₂O to C₂H₅OH at 180 °C and titanate nanotubes can be synthesized between 100 and 180 °C. A probable formation mechanism is proposed based on XRD, SEM and TEM analysis. The influence of cosolvent on the transformation from anatase TiO₂ to titanate is also investigated.     

Self-assembly into temperature dependent micro-/nano-aggregates of 5,10,15,20-tetrakis(4-carboxyl phenyl)-porphyrin

Various nanostructures of 5,10,15,20-tetrakis(4-carboxyl phenyl)-porphyrin (H₂TCPP) can be easily synthesized by a surfactant-assisted self-assembly (SAS) method at different temperatures. When the DMF solution of porphyrin monomer was injected into cetyltimethylammonium bromide (CTAB) aqueous solution by a syringe, diverse H₂TCPP nanostructures dependent on the different temperatures, including hollow nanospheres, solid nanospheres and nanospheres with holes, were successfully obtained. As a result, the suitable concentration of the CTAB aqueous solution used to form nanostructues of porphyrin ranges from 0.15 to 0.2 mM. The various morphologies of porphyrin nanostructures were characterized by transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM). UV–vis adsorption spectra showed that the micro-/nano-aggregate properties of porphyrin transformed from H-aggretates to J-aggregates during the process of self-assembly of porphyrin at different temperatures. Fluorescence spectra revealed a greater fluorescence quenching of various micro-/nano-aggregatess of porphyrin formed at different temperatures in aqueous solution, compared to the DMF solution of porphyrin monomer.     

Fabrication and characterization of tetrapod-like ZnO nanostructures prepared by catalyst-free thermal evaporation

Tetrapod-like ZnO nanostructures were fabricated on ZnO-coated sapphire (001) substrates by two steps: pulsed laser deposition (PLD) and catalyst-free thermal evaporation process. First, the ZnO films were pre-deposited on sapphire (001) substrates by PLD. Then the ZnO nanostructures grew on ZnO-coated sapphire (001) substrate by the simple thermal evaporation of the metallic zinc powder at 900 °C in the air without any catalysts. The pre-deposited ZnO films by PLD on the substrates can provide growing sites for the ZnO nanostructures. The as-synthesized ZnO nanostructures were characterized by using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectrum (FTIR). The results show that the tetrapod-like ZnO nanostructures are highly crystalline with the wurtzite hexagonal structure. Photoluminescence (PL) spectrum of as-synthesized nanostructures exhibits a UV emission peak at ～ 389 nm and a broad green emission peak at ～ 513 nm. In addition, the growth mechanism of ZnO nanostructures is also briefly discussed.     

Preparation of nano-sized flower-like ZnO bunches by a direct precipitation method

In this work, nano-sized ZnO particles were prepared by a direct precipitation method with Zn(NO₃)₂·6H₂O and NH₃·H₂O as raw materials, and the impact of the synthesis process was studied. The optimal thermal calcined temperature of precursor precipitates of ZnO was obtained from the differential thermal analysis (DTA) and the thermal gravimetric analysis (TGA) curves. The purity, microstructure, morphology of the calcined ZnO powders were studied by X-ray diffraction (XRD), energy dispersive X-ray spectrum (EDS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The synthesized ZnO powders had a wurtzite structure with high purity. The final products were of flower-like shape and the nanorods which consisted of the flower-like ZnO bunches were 20–100 nm in diameter and 0.5–1 μm in length. The effect of process conditions on the morphology of ZnO was discussed.     

Microwave-assisted method for preparation of Zn1−xMgxO nanostructures and their activities for photodegradation of methylene blue

Nanostructures of Zn_1−xMg_xO (0 ⩽ x ⩽ 0.2) were prepared in water by one-pot method under microwave irradiation for 5 min. In this method, zinc acetate, magnesium nitrate and sodium hydroxide were used as starting materials without using any additive and post preparation treatment. The nanostructures were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), diffuse reflectance spectroscopy (DRS), electrochemical impedance spectroscopy (EIS), Fourier transform-infrared (FT-IR), and the Brunauer–Emmett–Teller (BET) techniques. The nanostructures have wurtzite hexagonal crystalline phase and doping of Mg²⁺ ions does not change the phase of ZnO. The SEM and TEM images show that morphology of the samples is changing by doping of Mg²⁺ ions. The EIS data show that by doping the ion, interfacial charge transfer resistance of the nanostructures decreases. Photocatalytic activity of the nanostructures was evaluated by degradation of methylene blue (MB) under UV irradiation. The degradation rate constant on the nanostructures with 0.15 mol fraction of Mg²⁺ ions is about 2-fold greater than for ZnO. Moreover, influence of various operational parameters such as microwave irradiation time, calcination temperature, weight of catalyst, concentration of MB, pH of solution and scavengers of reactive species on the degradation rate constant was investigated and the results were discussed.     

Microwave synthesis of SrCO3 one-dimensional nanostructures assembled from nanocrystals using ethylenediamine additive

One-dimensional SrCO₃ nanostructures assembled from nanocrystals have been successfully synthesized by a microwave-assisted aqueous solution method at 90 °C using Sr(NO₃)₂, (NH₄)₂CO₃ and ethylenediamine (C₂H₈N₂). Our experiments show that the microwave heating time plays an important role in the size and morphology of SrCO₃. A rational mechanism based on the oriented attachment self-assembly is proposed for the formation of SrCO₃ nanostructures. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected-area electron diffraction (SAED). This method is simple, fast, low-cost and suitable for large-scale production of SrCO₃ nanostructures with different morphologies. We expect that this method may be extended to the preparation of nanostructures of other kinds of carbonates.     

表面活性剂对纳米氧化锌形貌和发光性能的影响

以二水合乙酸锌和氢氧化钠为原料,分别以表面活性剂十六烷基三甲基溴化铵(CTAB)和聚乙烯吡咯烷酮(PVP)为结构导向剂,采用简单的水热法制备了不同形貌的纳米氧化锌。研究了两种表面活性剂对纳米氧化锌形貌和光致发光性能的影响,并探讨了表面活性剂的作用机理。采用X射线衍射(XRD)、扫描电子显微镜(SEM)和室温光致发光光谱(PL)等测试方法对样品的结构、形貌和发光性能进行了表征。结果表明:添加了表面活性剂后,样品形貌和尺寸都更加均匀,紫外发射峰强度相对增加。     

Synthesis of porous ZnO nanostructures using bamboo fibers as templates

In this study, we fabricated ZnO nanostructures using bamboo fibers as templates. The starting material used was zinc acetate, and the nanostructures were synthesized by soaking and calcining the bamboo fibers. The fabricated nanostructures were characterized using X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM), and ultraviolet-visible spectrophotometry. The results showed that the size of the ZnO nanoparticles was approximately 20–100 nm. When the ZnO nanoparticles were used as the catalyst in the photodegradation of methyl orange, the dye degraded by 95.98 % in 80 min. The response and recovery times of a gas sensor based on the ZnO nanoparticles were 25 and 24 s, respectively, during the detection of C₂H₅OH in a concentration of 10 ppm at 270 °C.     

Large-scale synthesis and characterization of fan-shaped rutile TiO2 nanostructures

Large-scale fan-shaped rutile TiO₂ nanostructures have been synthesized by means of a simple hydrothermal method using only TiCl₄ as titanium source and chloroform/water as solvents. The physicochemical features of the fan-shaped TiO₂ nanostructures are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), nitrogen absorption-desorption, diffuse reflectance ultraviolet-visible spectroscopy (UV-vis) and Fourier transform infrared spectroscopy (FTIR). Structural characterization indicates that the fan-shaped TiO₂ nanostructures are composed of several TiO₂ nanorods with diameters of about 5 nm and lengths of 300-350 nm. The average pore size and BET surface area of the fan-shaped TiO₂ nanostructures are 6.2 nm and 59 m²/g, respectively. Optical adsorption investigation shows that the fan-shaped TiO₂ nanostructures possess optical band gap energy of 3.11 eV.     

The effects of different acids on the preparation of TiO2 nanostructure in liquid media at low temperature

Titania of different crystalline structures and morphology was prepared by the low temperature dissolution–reprecipitation process (LTDRP) of amorphous precursors in various acidic mediums at 70 °C for 8 h. The effects of different acids on the crystalline and morphology of titania nanostructures were investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Results showed that HCl, HNO₃ and their mixture favored the formation of rod-like rutile TiO₂, while H₂SO₄ and its mixture with HCl or HNO₃ retarded the formation of rutile but favored the formation of the anatase phase of with an irregular shape. The mechanism of the formation of various titania nanostructures was also discussed.     

A simple route to V2O5·xH2O bundle-like nanostructures

V₂O₅·xH₂O bundle-like nanostructures composed of nanobelts have been synthesized by a simple hydrothermal method with the aid of Co²⁺. The widths, thickness and lengths of V₂O₅·xH₂O nanobelts are 80–100 nm, 10–20 nm, and several micrometers, respectively. The morphologies and the crystallographic structures of the V₂O₅·xH₂O bundle-like nanostructures were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The effects of the inorganic ions and reaction temperature on the morphologies of the resulting products have been investigated.     

Synthesis and comparative study of Ho and Y doped ZnO nanoparticles

Ho and Y doped ZnO nanoparticles were synthesized using a wet chemical route followed by structural, electrical and magnetic property characterization of the same. We present a comparison of the properties of Ho and Y (having same ionic radii) doped ZnO nanoparticles. X-ray diffraction studies of the diffraction data exhibit a monophasic wurtzite crystal structure similar to that of the parent compound, ZnO. Microstructural investigations of these samples by scanning electron microscopy show the presence of nanostructures. The optical measurements show an increase in the band gap of doped samples as compared to the undoped sample. DC magnetization measurements of Ho doped ZnO point towards the presence of hysteresis loop at 5 K with an H_c of about 110 Oe for a nominal 1 mol% Ho doped sample. The resistivity of Ho doped sample is found to be higher as compared to the undoped and Y doped sample.