Microwave-assisted synthesis and characterization of flower shaped zinc oxide nanostructures

A microwave-assisted solution-phase approach has been applied for the synthesis of zinc oxide nanostructures. The synthesis procedure was carried out by using two reagents: hydrazine hydrate and ammonia. Flower shaped particles were obtained with hydrazine hydrate whereas mainly spherical agglomerated particles were observed with ammonia. The nanostructures were influenced by microwave irradiation time, reagent concentration and molar ratio of the precursors. High crystalline materials were found without the need of a post-synthesis treatment. The average crystalline size of ZnO nanostructures has been analyzed by X-ray Diffraction (XRD) pattern and estimated to be 18 nm. The presence of flower shaped zinc oxide with nanorods arranged has been confirmed from Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) micrographs. The samples were further analyzed by Fourier Transform InfraRed (FT-IR), Thermogravimetric Analysis (TGA) and photoluminescence spectroscopic techniques.     

Face-selective electrostatic control of hydrothermal zinc oxide nanowire synthesis

Rational control over the morphology and the functional properties of inorganic nanostructures has been a long-standing goal in the development of bottom-up device fabrication processes. We report that the geometry of hydrothermally grown zinc oxide nanowires can be tuned from platelets to needles, covering more than three orders of magnitude in aspect ratio (~0.1-100). We introduce a classical thermodynamics-based model to explain the underlying growth inhibition mechanism by means of the competitive and face-selective electrostatic adsorption of non-zinc complex ions at alkaline conditions. The performance of these nanowires rivals that of vapour-phase-grown nanostructures, and their low-temperature synthesis (<60 °C) is favourable to the integration and in situ fabrication of complex and polymer-supported devices. We illustrate this capability by fabricating an all-inorganic light-emitting diode in a polymeric microfluidic manifold. Our findings indicate that electrostatic interactions in aqueous crystal growth may be systematically manipulated to synthesize nanostructures and devices with enhanced structural control.     

Recent progress in hydrothermal synthesis of zinc oxide nanomaterials

Hydrothermal synthesis is of considerable interest due to its low cost, simplicity and relatively low growth temperature (typically below 200 °C). Since the synthesis is performed in aqueous solutions (no organic solvents), it can also be safe and environmentally friendly (depending on precursor chemicals). Consequently, it has been a subject of intense research in recent years. In this article, we review recent progress in hydrothermal synthesis of zinc oxide nanomaterials, with focus on practical relevance for a variety of applications.     

Microwave-assisted synthesis and characterization of zinc oxide/carbon nanotube composites

A composite material of zinc oxide and carbon nanotubes were successfully synthesized via a sol process using zinc acetate dihydrate and treated multi-wall carbon nanotubes under microwave irradiation. The morphology, microstructure and chemical bonding of as-obtained composites were well characterized using X-ray diffraction, scanning electron microscope, transmission electron microscope, and Fourier transform infrared spectroscopy. Zinc oxide nanoparticles were dispersively coated on the surface of carbon nanotube when the precursor was dried under microwave irradiation without post-annealing. X-ray diffraction results obviously showed the mixture of two phases of carbon nanotube and wurzite zinc oxide whose size is approximately 15 nm. The formation of zinc oxide nanoparticles on carbon nanotube surface in the composite prepared by microwave heating is much better than the composite heated by conventional annealing. Fourier transform infrared spectroscopic results suggest that carboxylic groups and uniform heating by microwave heating could play key roles on the nucleation of zinc oxide on carbon nanotube surface.     

Microwave-assisted hydrothermal synthesis of nanocrystalline SnO powders

Tin oxide (SnO) powders were obtained by the microwave-assisted hydrothermal synthesis technique using SnCl₂·2H₂O as a precursor. By changing the hydrothermal processing time, temperature, the type of mineralizing agent (NaOH, KOH or NH₄OH) and its concentration, SnO crystals having different sizes and morphologies could be achieved. The powders were characterized by X-ray diffraction (X-ray), Field Emission Scanning Electron Microscopy (FE-SEM), High Resolution Transmission Electron Microscopy (HR-TEM) and Selected Area Electron Diffraction (SAED). The results showed that plate-like form is the characteristic morphology of growth and the TEM analyses indicate the growth direction as (200).     

Microwave-assisted hydrothermal synthesis and photocatalytic activity of ZnO

The effect of synthesis temperature on the morphology of fine zinc oxide powders prepared by microwave-assisted hydrothermal processing of Zn(OH)₂ suspensions has been studied using x-ray diffraction and low-temperature nitrogen BET measurements. The photocatalytic activity of the powders for Methyl Orange photodegradation has been assessed as a function of synthesis temperature. The results indicate that the specific surface of ZnO powders plays a key role in determining their photocatalytic activity.     

Microwave-assisted hydrothermal synthesis of coralloid nanostructured nickel hydroxide hydrate and thermal conversion to nickel oxide

Coralloid nanostructured nickel hydroxide hydrate has been successfully synthesized by a simple microwave-assisted hydrothermal process using nickel sulfate hexahydrate as precursor and urea as hydrolysis-controlling agent. A pure coralloid nanostructured nickel oxide can be obtained from the nickel hydroxide hydrate after calcination at 400 °C. The thermal property, structure and morphology of samples were characterized by thermogravimetry (TG), temperature-programmed reduction (TPR), X-ray (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).     

Doughnut-shaped zinc oxide particles

Zinc oxide doughnut-shaped particles were synthesized using a chemical route. A possible growth model has been proposed from a detailed experiment in which samples were picked from the reaction chamber at various time intervals and characterized using scanning electron microscopy (SEM). Particles were also characterized using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS).     

Microwave-assisted hydrothermal synthesis of zeolite films on ceramic supports

Zeolite films were formed on ceramic supports by a novel microwave-assisted hydrothermal method and were characterized by XRD, SEM, FTIR and BET surface area. The two-stage synthesis technique consists of microwave heating of supports saturated with precursor solution to form a thin layer of zeolite nano-seeds, followed by hydrothermal treatment to crystallize MFI zeolite. The resulting zeolite formation time was drastically reduced and the BET surface area of the product was double that obtained using conventional hydrothermal method. The dipping time, microwave heating time, power and hydrothermal heating time influence the amount of zeolite formation, the BET surface area and preferred orientation of the zeolite film. This new method of seed-film growth using a simple domestic microwave oven has the advantages of a two-stage synthesis technique, allowing independent control of nucleation and crystallization to obtain an optimum zeolite film and reduce the synthesis time.     

Continuous production of fine zinc oxide nanorods by hydrothermal synthesis in supercritical water

Continuous production of highly crystalline ZnO nanorods by supercritical hydrothermal synthesis was reported in this article. Zinc nitrate aqueous solution was pressurized to 30 MPa at room temperature and rapidly heated to 673 K by mixing with supercritical water and then fed into a tubular reactor. Residence time is about 10 s. Production of ZnO nanorod particles with uniform particle size distribution showed a strong ultraviolet light emission at room temperature. This article also reported in-situ surface modification of ZnO nanorods with organic reagents by the supercritical hydrothermal synthesis.     

Basic zinc carbonate as a precursor in the solvothermal synthesis of nano-zinc oxide

ZnO nanoparticles were synthesized solvothermally in various diols (ethylene glycol, di(ethylene glycol), tetra(ethylene glycol), 1,2-propanediol, 1,4-butanediol), using basic zinc carbonate (2ZnCO₃·3Zn(OH)₂) as a precursor for the first time. Since ZnCO₃ was sparingly soluble in diols the transformation reaction proceeded at a low reaction rate. Ethylene glycol was found as the most suitable medium among five diols studied yielding the smallest ZnO particles (~ 55 nm) and short reaction time, t_r (2 h). Diols with shorter chain length produced smaller ZnO particles. p-Toluene sulfonic acid (p-TSA) acted as a catalyst and reduced t_r from 8 h to 2 h in concentration of 0.02 M. Optimum reaction conditions for the synthesis in ethylene glycol were 185 °C and 2 h. At higher p-TSA concentrations (0.04–0.08 M) the size of ZnO particles was reduced from 500–800 nm to 50–100 nm and crystallite size to 25–30 nm. Benzene sulfonic acid (BSA) and inorganic bases (LiOH, NaOH, and KOH) also showed catalytic activities. Raman and photoluminescence spectroscopies revealed high concentration of defects on ZnO surface causing the emission of visible light and giving this type of ZnO higher potential in various (opto)-electronic application in comparison to Zn(II) acetate based ZnO.     

Effects of initial precursor and microwave irradiation on step-by-step synthesis of zinc oxide nano-architectures

ZnO nano-architectures were produced with the aid of a fast, simple and low cost microwave-assisted synthesis method. Solid semispherical ZnO nanoparticles on the order of 600 nm in diameter along with rice-like ZnO nanorods 95 nm thick were produced from butanol, triethanolamine (TEA), and zinc acetate dihydrate. Solid spherical ZnO nano-architectures with an average diameter of 250 nm were produced from the same starting materials in addition to NaOH. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy were used to characterize the ZnO nano-architectures as well as the precursor. This method is cheap, fast and simple; capable of producing large quantities of each ZnO nanostructure. Investigation of the step-by-step formation mechanism for each ZnO nanostructure was conducted.     

Microwave-assisted synthesis and characterization of tin oxide nanoparticles

Tin oxide nanoplatelets (SnO) and nanoparticles (SnO₂) were prepared by microwave assisted technique with an operating frequency of 2.45 GHz. This technique permits to produce gram quantity of homogeneous nanoparticles in just 10 min. The crystalline size was evaluated from XRD and found to range from 26 to 34 nm. SEM and TEM analyses showed that the nanoparticles present a platelet-like shaped particle or, a pseudo spherical morphology, after calcination at moderate temperature during which the phase transformation from SnO to SnO₂ takes place. Additional FT-IR, density and resistivity measurements were also presented.     

Microwave-assisted hydrothermal synthesis of ZnO rod-assembled microspheres and their photocatalytic performances

ZnO rod-assembled microspheres were successfully fabricated by using the microwave-assisted hydrothermal method in the existence of the poly ethylene glycol (PEG) with the molecular weight of 2000. The structure and morphology of as-prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The experimental results exhibit that the as-prepared ZnO microspheres with a diameter about 1.5–2.0 μm were composed of many rods with the diameter of 300 nm and the length of 1 μm, respectively. Photoluminescene measurement shows a broad visible emission band centered at around 500–560 nm. The improved catalytic activity may be attributed to structural difference, including morphology, surface orientation and surface defects. Furthermore, the possible growth and photodegradation mechanism of the as-prepared sample is also briefly discussed.     

独特形貌碳酸钙的微波水热合成与表征

以醋酸钙和尿素为原料,在无添加剂的条件下采用微波水热法合成技术,直接制得了高度对称的双头矛状、双头扁平铲形、拉长六边形、拉长四边形、侧表面为六边形的多面体和六瓣花状等奇异形貌的碳酸钙晶体,利用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、傅里叶红外光谱仪(FT-IR)等对样品进行了表征,并对碳酸钙晶体的形成过程进行了分析。结果表明醋酸钙用量、尿素用量和微波辐照能量对碳酸钙晶体的结构与形貌具有重要调控作用。     

Influence of pH and HPC concentration on the synthesis of zinc oxide photocatalyst particle from zinc-dust waste by hydrothermal treatment

This work aimed to use the waste zinc-dust from a hot-dip galvanizing plant for the synthesis of nanosized ZnO photocatalyst powder via hydrothermal treatment. ZnO particles with different morphologies and sizes were obtained by varying the solution pH (8–12) and the amount of hydroxypropyl cellulose (HPC) dispersant (0–0.15% (w/v)) under hydrothermal treatment at 170 °C for 8 h. The influence of the preparation conditions on the properties of resultant ZnO particles were evaluated by X-ray diffraction, scanning electron microscopy with energy dispersive X-ray analysis, laser light scattering and Brunauer–Emmett–Teller analyses. The solution pH affected the crystallinity, particle morphology and specific surface area of the obtained ZnO, which in turn influenced its photocatalytic activity. The addition of the optimum amount of HPC (0.1% (w/v)) in the starting solution acted as a dispersant to reduce ZnO particle agglomeration but had the opposite effect at higher levels. Moreover, ZnO nanorods with various aspect ratios and a diameter and length range of 20–70 nm and 100–400 nm, respectively, were obtained depending on the amount of added HPC. The photocatalytic activity of the synthesized ZnO powder was improved by the addition of the optimal amount of HPC, and correlated to the particle dispersion and specific surface area.     

The hydrothermal synthesis of super-paramagnetic barium hexaferrite particles

Superparamagnetic Ba-hexaferrite nanoparticles were prepared using modified hydrothermal synthesis. The precursor and hydroxide [OH⁻] concentrations were optimized and the synthesis temperature and time were drastically reduced. The size and the morphology of synthesized nanoparticles was confirmed by transmission electron microscopy (TEM) images. The crystal structure of the nanoparticles was characterized by X-ray diffraction data. Powders synthesized at 160 °C exhibit a bimodal particle size distribution while those synthesized at T_S = 150 °C show a monomodal particle size distribution. Zero-field-cooling (ZFC) and field-cooling (FC) magnetization measurements were performed using a superconducting quantum interference device magnetometer from 2 to 300 K to investigate the magnetic properties of nanoparticles. The FC/ZFC magnetization measurements showed a typical superparamagnetic behavior. The synthesized superparamagnetic particles exhibit a disc-like shape, in average 11 nm wide and 3 nm thick with a room temperature magnetization of approximately 10 Am²/kg at 5 T.     

Microwave-assisted synthesis and magnetic studies of cobalt oxide nanoparticles

An efficient microwave-assisted route has been used to synthesize nanoparticles of cobalt oxide. The particles were well characterized by transmission electron microscopy (TEM) which showed that the average diameter of the particles is around 6 nm. X-ray diffraction (XRD) studies further confirmed the formation of the spinel Co₃O₄. Purity of the products was detected by Fourier transform infrared spectroscopy (FTIR) combined with thermal gravimetric analysis (TG/DTG). The magnetic measurements revealed a small hysteresis loop at room temperature indicating a weak ferromagnetic nature of the synthesized Co₃O₄ nanoparticles. The magnetic moment of the particles was measured to be 4.27 μ_eff.     

Nanocrystalline copper doped zinc oxide produced from copper doped zinc hydroxide nitrate as a layered precursor

Undoped and copper doped nanostructured zinc oxides were synthesized by using a series of synthetic layered material, undoped and copper doped zinc hydroxide nitrates at various molar percentages of copper (2–10) within the layers as precursors. The layered materials were heat-treated at 500 °C to produce zinc oxide nanostructures with crystallite sizes in the range of 23–35 nm. Optical studies of the nanostructured copper doped zinc oxides showed the decrease in band gap with increasing content of the doping agent, copper.