Fabrication of flower-like ZnO microstructures from ZnO nanorods and their photoluminescence properties

In the present work, we reported a novel method for the synthesis of well-dispersed flower-like ZnO microstructures derived from highly regulated, well-dispersed ZnO nanorods by using low temperature (100 °C) hydrothermal process and without using any additional surfactant, organic solvents or catalytic agent. The phase and structural analysis were carried out by X-ray diffraction (XRD) which confirms the high crystal quality of ZnO with hexagonal (wurtzite-type) crystal structure. The morphological and structural analyses were carried out by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) which indicate the formation of well-dispersed ZnO nanorods as well as flower-like ZnO. It has been shown that flower-like ZnO is made up of dozen of ZnO nanorods building block units. The high resolution transmission electron microscopy (HRTEM) and their corresponding selected area electron diffraction (SAED) pattern show that both ZnO nanorods and flower-like ZnO microstructures are single crystalline in nature and preferentially grow along [0 0 0 1] direction. Their optical property was characterized by photoluminescence spectroscopy; shows ZnO nanorods have only violet emission and no other emission while flower-like ZnO microstructures have a weak violet emission and a strong visible emission. A plausible growth mechanism of ZnO nanorods as well as flower-like ZnO microstructures has been given.     

Large-scale synthesis of ZnO flower-like and brush pen-like nanostructures by a hydrothermal decomposition route

In this present report, large-scale ZnO flower-like and brush pen-like nanostructures have been synthesized by a simple hydrothermal decomposition route. The flower-like nanostructure is composed of tens of radially oriented hexagonal nanorods. Field emission scanning electron microscopy was used to investigate the formation process of the brush pen-like nanostructures which ultimately lead to the formation of ZnO nanonunchakus. This facile low-cost controllable growth procedure holds promise in the future large-scale synthesis of ZnO nanostructures for many important applications in nano-/micro-scale devices. Room-temperature PL spectra from the ZnO flower-like and brush pen-like structures reveal weak UV emission and strong green emission.     

Gas sensing properties of ZnO nanorods prepared by hydrothermal method

ZnO nanorods are prepared by a hydrothermal process with cetyltrimethylammonium bromide (CTAB) and zinc powder at 182°C. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The gas sensing properties of the materials have been investigated. The results indicate that the as-prepared ZnO nanorods are uniform with diameters of 40–80 nm and lengths about 1 μm, the relatively high sensitivity and stability of these sensors made from ZnO nanorods demonstrate the potential for developing a new class of stable and very sensitive sensors.     

Morphological control of flower-like ZnO nanostructures

Flower-like ZnO nanostructures composed of different building blocks, such as hexagonal pyramids, hexagonal prisms, and cones, have been synthesized on a large scale by a simple hydrothermal method in the absence of surfactants or organic solvents. The effects of the concentration of NaOH, reaction temperature, and reaction time on the morphologies of the resulting products have been investigated. The morphologies and the crystal structures of flower-like ZnO nanostructures were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM).     

ZnO单晶堆垒纳米棒的制备与表征

在Au点阵模板上磁控溅射ZnO薄膜,然后在O2气氛下1000℃退火制备了ZnO单晶堆垒纳米棒。采用扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、X射线衍射(XRD)和傅立叶变换红外(FTIR)光谱对样品进行分析。结果表明,ZnO纳米棒是由诸多单晶堆垒而成,每个单晶均为六方纤锌矿结构,纳米棒直径在100nm左右。初步探讨了ZnO单晶堆垒纳米棒可能的生长机理。     

Synthesis of zinc oxide nanotetrapods and nanorods by thermal evaporation without catalysis

ZnO nanotetrapods and nanorods have been synthesized by a simple thermal evaporation of Zn powder (300 mesh, 99.99% purity) under simultaneous flow of oxygen and argon gases in two-zone furnace in two different temperature regions. These ZnO nanostructures have hexagonal structure, which grow along the [001] direction in the form of nanotetrapods (diameter approximately 60-150 nm, length approximately 1-4 microm) and nanorods (diameter approximately 30-60 nm, length approximately 2-5 microm). The morphologies of these ZnO nanostructures have been investigated by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It has been found that growth parameters like temperature, gas flow rate etc., control the diameter of the nanotetrapods and nanorods. These novel structures of ZnO nanorods and nanotetrapods may be attractive for optical and other nanodevices.     

Rapid growth of nanotubes and nanorods of würtzite ZnO through microwave-irradiation of a metalorganic complex of zinc and a surfactant in solution

Large quantities of single-crystalline ZnO nanorods and nanotubes have been prepared by the microwave irradiation of a metalorganic complex of zinc, in the presence of a surfactant. The method is simple, fast, and inexpensive (as it uses a domestic microwave oven), and yields pure nanostructures of the hexagonal würtzite phase of ZnO in min, and requires no conventional templating. The ZnO nanotubes formed have a hollow core with inner diameter varying from 140–160 nm and a wall of thickness, 40–50 nm. The length of nanorods and nanotubes varies in the narrow range of 500–600 nm. These nanostructures have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods and nanotubes are found by SAED to be single-crystalline. The growth process of ZnO nanorods and nanotubes has been investigated by varying the surfactant concentration and microwave irradiation time. Based on the various results obtained, a tentative and plausible mechanism for the formation of ZnO nanostructures is proposed.     

Fabrication of single-crystal ZnO nanorods and ZnS nanotubes through a simple ultrasonic chemical solution method

A simple and rapid method has been developed for the preparation of rod-like ZnO nanocrystals via ultrasonic irradiation. The as-synthesized ZnO nanocrystals were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The ZnO nanorods had an average diameter of 15-70 nm that varied from the ultrasonic operation mode. The results showed that Zn powder played an important role in the synthesis of ZnO nanorods. Through adding a sulfur source in the reaction system, ZnO/ZnS nanocables and ZnS nanotubes could be obtained with continuous ultrasonic irradiation. The formation mechanism of ZnS nanotubes could be attributed to the Kirkendall effect.     

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.     

A simple microwave-assisted decomposing route for synthesis of ZnO nanorods in the presence of PEG400

In the paper, a simple microwave-assisted decomposing reaction in the presence of PEG400 has been successfully developed to synthesize ZnO nanorods with 10-25 nm of diameter and 60-200 nm of length. The product was analyzed and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and HRTEM. Ultraviolet-visible (UV-vis) absorption peak of ZnO nanorods shows a distinct blue shift from that of the bulk and the Photoluminescence (PL) spectrum exhibits a strong near-band-edge emission at 385 nm. Further experiments have also been designed, and the results show that microwave radiation and surfactant PEG400 all played an important role on the formation of ZnO nanorods.     

Growth and characterization of flower-like Ag/ZnO heterostructure composites with enhanced photocatalytic performance

Flower-like Ag/ZnO heterostructure composites were prepared through a solvothermal method without surfactants or templates. The products were characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, and photoluminescence (PL) spectroscopy. Results demonstrate that flower-like Ag/ZnO heterostructure composites were composed of wurtzite ZnO flowers coated by face-center-cubic Ag nanoparticles. The growth process of flower-like ZnO crystals was investigated, and a possible growth mechanism was proposed. The photocatalytic activity of the as-prepared flower-like Ag/ZnO samples, pure ZnO samples, and commercial TiO₂ (Degussa, P-25) was tested with the photocatalytic degradation of methylene blue. Results show that the Ag/ZnO heterostructures were superior in photocatalytic activity to the pure ZnO samples and the commercial TiO₂ (Degussa, P-25), but the mixture of Ag (0.1 wt%) particles and ZnO flowers did not, which implies that the heterostructure promoted the separation of photogenerated electron–hole pairs, enhancing the photocatalytic activity. That was primarily verified by the PL results.     

Self-assembly of ZnO nanosheets into nanoflowers at room temperature

A singularity flower-like ZnO nanostructure was prepared on a large scale through a very simple solution method at room temperature and under ambient pressure in a very short time. The flower-like ZnO nanostructures were self-assembled by thin and uniform nanosheets, with a thickness of around 5 nm. X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM) were used to characterize the structure and morphology. The possible growth mechanism was discussed based on the reaction process. The blue shift in the UV-vis spectra of the ZnO nanostructures was also observed.     

Deposition and characterization of a novel integrated ZnO nanorods/thin film structure

One-dimensional (1-D) ZnO (zinc oxide) nanostructures have received a lot of attention due to their superior properties. Various techniques have been developed to synthesize ZnO nanorods at high-temperature process using vapor–liquid–solid (VLS) mechanism. In this paper, we report a novel process to synthesize integrated ZnO nanorods/thin film structures using an RF magnetron sputter deposition under different deposition parameters and substrate conditions. The substrate used was glass plated with electroless Cu prepared using various conditions. The resulting specimens are analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD). The effect of the copper surface roughness was found to be significant. ZnO nanorods were found only when the copper layer is rough enough. The roughness of the copper in general increases with the plating time and/or the ratio of V_HCHO/V_Cu used in the plating bath. Post-plating annealing of the copper was also found to increase the surface roughness of the copper.     

ZnO nanomaterials based surface acoustic wave ethanol gas sensor

ZnO nanomaterials based surface acoustic wave (SAW) gas sensor has been investigated in ethanol environment at room temperature. The ZnO nanomaterials have been prepared through thermal evaporation of high-purity zinc powder. The as-prepared ZnO nanomaterials have been characterized with scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray Diffraction (XRD) techniques. The results indicate that the obtained ZnO nanomaterials, including many types of nanostructures such as nanobelts, nanorods, nanowires as well as nanosheets, are wurtzite with hexagonal structure and well-crystallized. The SAW sensor coated with the nanostructured ZnO materials has been tested in ethanol gas of various concentrations at room temperature. A network analyzer is used to monitor the change of the insertion loss of the SAW sensor when exposed to ethanol gas. The insertion loss of the SAW sensor varies significantly with the change of ethanol concentration. The experimental results manifest that the ZnO nanomaterials based SAW ethanol gas sensor exhibits excellent sensitivity and good short-term reproducibility at room temperature.     

A simple one-step solvothermal synthesis of hierarchically structured ZnO hollow spheres for enhanced selective ethanol sensing properties

A simple one-step solvothermal method, using ethanolamine as solvent without any additives except zinc source, has been employed to synthesize hierarchically structured ZnO hollow spheres consisting of numerous orderly and radical nanorods with diameter of several tens nanometers and length of 2–3 μm. The ethanolamine and the solvothermal process play the critical role in the synthesis of the ZnO hollow spheres by the primary formation of ZnO crystal nucleus and subsequent transformation into nanorods, which self-assemble into hollow spheres. The morphology and structure of the spheres have been characterized by transmission electron microscopy, field emission scanning electron microscopy, X-ray powder diffraction, high-resolution transmission electron microscopy, and Brunauer–Emmett–Teller N₂ adsorption–desorption analyses. The results also indicate that the sensor based on the prepared ZnO hollow spheres exhibit good ethanol sensing performance, which can be attributed to its structural defects and high surface-to-volume ratio that significantly facilitate the absorption of oxygen species and diffusion of target gas. Besides, the sensor shows high selectivity to ethanol because ZnO as a basic oxide is favored for dehydrogenation of ethanol.     

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.     

Fabrication of ordered flower-like ZnO nanostructures by a microwave and ultrasonic combined technique and their enhanced photocatalytic activity

Ordered flower-like zinc oxide (ZnO) nanostructures were fabricated via a facile microwave and ultrasonic combined technique. The product was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction pattern (SAED). The flower-like ZnO nanostructures were assembled by a central petal and six symmetrical petals which grew radially from the center. The flower-like ZnO sample showed an enhanced photocatalytic performance compared with the ZnO microrods for the methylene blue (MB) degradation, which could be attributed to its special structure feature. Au/ZnO and Ag/ZnO nanocomposites were also synthesized and exhibited enhanced photocatalytic efficiency after decorating noble metal nanoparticles on the surface of flower-like ZnO nanostructures.     

Synthesis, characterization, and hydrophobic properties of Bi2S3 hierarchical nanostructures

Novel Bi₂S₃ hierarchical nanostructures self-assembled by nanorods are successfully synthesized in mild benzyl alcohol system under hydrothermal conditions. The hierarchical nanostructures exhibit a flower-like shape. X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) were used to characterize the as-synthesized samples. Meanwhile, the effect of various experimental parameters including the concentration of reagents and reaction time on final product has been investigated. In our experiment, PVP plays an important role for the formation of the hierarchical nanostructures and the possible mechanism was proposed. In addition, Bi₂S₃ film prepared from the flower-like hierarchical nanostructures exhibits good hydrophobic properties, which may bring nontrivial functionalities and may have some promising applications in the future.     

Catalyst-free MOCVD growth of ZnO nanorods and their structural characterization

We have synthesized ZnO nanorods on ZnO-coated Si(100) substrates without a metal catalyst by a reaction of a diethylzinc (DEZn) and oxygen (O₂) mixture. By adjusting the argon (Ar)/O₂ gas flow ratio, we have obtained ZnO nanorods of various densities at a temperature of 450°C. The ZnO nanorods had an average diameter of 30–70 nm, and transmission electron microscopy (TEM) showed a single crystalline structure.     

Synthesis of flower-like silver nanoarchitectures at room temperature

Novel flower-like silver nanoarchitectures were synthesized via a facile and environmentally benign route in the presence of citric acid and ascorbic acid. The flower-like structures are composed of nano-petals of ca. 20 nm in thickness. The products were characterized with X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The growth mechanism of flower-like silver nanoarchitectures involves a film-fold process. Some crucial factors affect the nanocrchitectures growth, such as, pH, the concentration of citric acid, and the concentration of ascorbic acid, have also been discussed.