Intensification of ultrasound-assisted process for the preparation of spindle-shape sodium zinc molybdate nanoparticles

In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO₃ at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80 °C. It is shown that the rate of reaction is significantly faster at 40 °C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.     

Photocatalytic activity of ZnO nanoparticles prepared via submerged arc discharge method

ZnO nanostructures were synthesized through arc discharge of zinc electrodes in deionized (DI) water. X-ray diffraction (XRD) analysis of the prepared nanostructures indicates formation of crystalline ZnO of hexagonal lattice structures. Transmission electron microscopy (TEM) images illustrate rod-like as well as semi spherical ZnO nanoparticles with 15–20 nm diameter range, which were formed during the discharge process with 5 A arc current. The average particle size was found to increase with the increasing arc current. X-ray photoelectron spectroscopy (XPS) analysis confirms formation of ZnO at the surface of the nanoparticles. Surface area of the sample prepared at 5 A arc current, measured by BET analysis, was 34 m²/g. Photodegradation of Rhodamine B (Rh. B) shows that the prepared samples at lower currents have a higher photocatalytic activity due to larger surface area and smaller particle size.     

Synthesis of nanocrystalline ZnO nanobelts via pyrolytic decomposition of zinc acetate nanobelts and their gas sensing behavior

The pyrolytic decomposition of layered basic zinc acetate (LBZA) nanobelts (NBs) into nanocrystalline ZnO NBs is investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and photoluminescence (PL). We also report on the gas sensing response of the resulting ZnO nanomaterial to CO. The LBZA NBs are grown at 65 °C in an aqueous solution of zinc acetate dihydrate. AFM and SEM results show as-grown products possess the characteristic layered structure of the LBZA crystals. XRD and XPS results show that annealing as-grown products at 210 °C in air causes a transformation from zinc acetate to nanocrystalline ZnO NBs via thermal decomposition. The ZnO crystalline domain size increases with temperature from 9.2 nm at 200 °C to 94 nm at 1000 °C, as measured from XRD. SEM shows evidence of sintering at 600 °C. The thickness of the NBs, determined via AFM, ranges from 10 to 50 nm and remains approximately constant with annealing temperature. XPS confirmed the chemical transformation from zinc acetate to ZnO and showed a significant remaining zinc hydroxide component for the ZnO NBs consistent with published results. PL measurements at room temperature show a blue shift in peak emission as the nanobelts change from LBZA to ZnO at 200 °C. Above this transition temperature, the ZnO nanobelts possess strong band edge emission at 390 nm and little broad band emission in the visible region. The AFM and SEM images reveal that the crystallites within the nanobelts orientate in rows along the long axis during annealing. This structure provides a high surface area to volume ratio of aligned nanoparticles which is beneficial for gas sensing applications. Gas sensors fabricated from 400 °C annealed nanobelts showed a response of 1.62 when exposed to 200 ppm of CO in dry air at 400 °C, as defined by the ratio of resistance before and during exposure. This indicates that ZnO nanostructures obtained by thermal decomposition of LBZA NBs could provide a cost effective route to high sensitivity gas sensors.     

Preferred orientation of ZnO nanoparticles formed by post-thermal annealing zinc implanted silica

High quality zinc oxide nanoparticles with (002) preferred orientation were prepared by post-thermal annealing zinc implanted silica at 700 °C using two methods. One method was annealing zinc implanted silica at 700 °C for 2 h in oxygen ambient; the other method was sequentially annealing zinc implanted silica at 700 °C in nitrogen and oxygen ambient for 1 h, respectively. X-ray diffraction (XRD), absorption and microphotoluminescence (micro-PL) results indicated that the latter method could create high quality ZnO nanoparticles with (002) preferred orientation and narrow size-distribution. X-ray photoelectron spectra (XPS) showed the formation of ZnO nanoparticles on a silica surface, where the ZnO nanoparticle content increased with increasing oxidation time in an oxygen environment. The processes of the transformation from Zn to ZnO are discussed.     

Preparation and characterization of polyindole–ZnO composite polymer electrolyte with LiClO<Subscript>4</Subscript>

This paper describes the preparation and conductivity studies of polyindole–ZnO composite polymer electrolyte (CPE) with LiClO₄. Polyindole–ZnO-based polymer nanocomposites were prepared by chemical method and characterized by XRD, infrared (IR), scanning electron microscope (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The IR spectrum confirms the intermolecular interaction between polyindole and ZnO. The significant spectral changes of polyindole and ZnO nancomposites reveal the strong interaction between polyindole and ZnO nanoparticles. The structural morphologies of the ZnO, polyindole, and polyindole–ZnO are obtained from SEM. The TEM image of polyindole nanocomposite shows that ZnO is embedded in polyindole matrix. An enhanced conductivity of 4.405 × 10⁻⁷ S cm⁻¹ at 50 °C for the CPE was determined from impedance studies.     

Synthesis and surface modification of ZnO:Cu nanoparticles by silica and PMMA

ZnO nanoparticles doped with Cu were synthesized by solid state reaction using different precursor routes and varying growth environment. Average crystallite size varied from 40 to 100 nm depending upon synthesis temperature, lower temperature favouring smaller particle size. Scanning electron microscope (SEM) images showed that particles synthesized at 250 °C were in the shape of nanorods but those synthesized at 900 °C had spherical shape. Luminescence emission showed marked dependence on the growth conditions varying from ultraviolet (UV) emission to green emission. For making the luminescent nanoparticles bio-compatible, a bioinorganic interface on ZnO:Cu nanoparticles was created by coating them with inert silica. Surface modification of ZnO:Cu was also done with lipophilic polymethylmethacrylate (PMMA). ZnO:Cu nanoparticles showed hexagonal wurtzite structure and the coating of silica was confirmed with the presence of two extra peaks due to silica in the XRD spectra. Thermogravimetric analysis (TGA) and FTIR spectroscopy indicated that PMMA molecules were adsorbed on the surface of ZnO:Cu nanoparticles. SEM images revealed that PMMA adsorption improved the dispersibilty of ZnO:Cu nanoparticles.     

Nanocomposite ZnO/Au formation by pulsed laser irradiation

The ZnO/Au nanocomposite formation involves synthesis of Au and ZnO colloidal solutions by 532 nm pulse laser ablation of metal targets in deionized water followed by laser irradiation of the mixed colloidal solution. The transmission electron microscope (TEM) and high-resolution transmission electron microscope (HRTEM) images show evolution of spherical particles into ZnO/Au nanonetworks with irradiation time. The formation mechanism of the nanonetwork can be explained on the basis of near resonance absorption of 532 nm irradiation by gold nanoparticles which can cause selective melting and fusion of gold nanoparticles to form network. The ZnO/Au nanocomposites show blue shift in the ZnO exciton absorption and red shift in the Au plasmon resonance absorption due to interfacial charge transfer.     

The influence of annealing temperature on the structure,morphologies and optical properties of ZnO nanoparticles

ZnO nanoparticles (NPs) have been successfully synthesized by the simple solution method at low temperature. The effects of annealing temperature on the structure and optical properties of ZnO NPs were investigated in detail by X-ray diffraction, transmission electron microscopy (TEM), ultraviolet–visible (UV–vis) spectroscopy and photoluminescence (PL) measurements. As the annealing temperature was increased above 180 ^°C the particles morphology evolved from spherical to hexagonal shape, indicating that the average particle size increased from 11 nm to 87 nm. The UV-vis and PL spectra showed a red-shift from 3.62 to 3.33 eV when the annealing temperature was increased.     

Synthesis and characterization of Mg-doped ZnO hollow spheres

Mg-doped ZnO nanoparticles were synthesized by a simple chemical method at low temperature with Mg:Zn atomic ratio from 0 to 7%. The synthesis process is based on the hydrolysis of zinc acetate dihydrate and magnesium acetate tetrahydrate were heated under refluxing at 65 °C using methanol as a solvent. X-ray diffraction analysis reveals that the Mg-doped ZnO crystallizes in a wurtzite structure with crystal size of 5–12 nm. These nanocrystals self-aggregated themselves into hollow spheres of size of 800–1100 nm. High resolution transmission electron microscopy images show that each sphere is made up of numerous nanoparticles of average diameter 5–11 nm. The XRD patterns, SEM and TEM micrographs of doping of Mg in ZnO confirmed the formation of hollow spheres indicating that the Mg²⁺ is successfully substituted into the ZnO host structure of the Zn²⁺ site. Furthermore, the UV–Vis spectra and photoluminescence (PL) spectra of the ZnO nanoparticles were also investigated. The band gap of the nanoparticles can be tuned in the range of 3.36–3.55 eV by the use of the dopants.     

Structural and optical properties of Mn-doped ZnO nanocrystalline thin films with the different dopant concentrations

The transparent nanocrystalline thin films of undoped zinc oxide and Mn-doped (Zn_1−xMn_xO) have been deposited on glass substrates via the sol–gel technique using zinc acetate dehydrate and manganese chloride as precursor. The as-deposited films with the different manganese compositions in the range of 2.5–20 at% were pre-heated at 100 °C for 1 h and 200 °C for 2 h, respectively, and then crystallized in air at 560 °C for 2 h. The structural properties and morphologies of the undoped and doped ZnO thin films have been investigated. X-ray diffraction (XRD) spectra, scanning electron microscopy (SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) were used to examine the morphology and microstructure of the thin films. Optical properties of the thin films were determined by photoluminescence (PL) and UV/Vis spectroscopy. The analyzed results indicates that the obtained films are of good crystal quality and have smooth surfaces, which have a pure hexagonal wurtzite ZnO structure without any Mn related phases. Room temperature photoluminescence is observed for the ZnO and Mn-doped ZnO thin films.     

Experimental investigation on the structural,dielectric, ferroelectric and piezoelectric properties of La doped ZnO nanoparticles and their application in dye-sensitized solar cells

Pure and lanthanum (La) doped ZnO nanorods were synthesized via co-precipitation method. The structure and morphology of as grown ZnO and La-ZnO nanoparticles were studied using transmission electron microscopy (TEM) and powder X-ray diffraction (XRD) methods. The values of remnant polarization and coercive field were found to be 0.027 μC/cm² and 1.33 kV/cm, respectively, for as grown La-ZnO nanostructures. High Curie temperature (276 °C) for doped ZnO was observed in dielectric study. Piezoelectric coefficient at room temperature was found to be 101.30 pm/V. I-V characteristics were studied for both pure and doped ZnO nanoparticles. Photo-anodes of dye-sensitized solar cells (DSSCs) were made using ZnO and La-ZnO nanorods. The conversion efficiency and short circuit current density of La-ZnO nanorods based DSSC were 0.36% and 1.31 mA/cm², respectively, which were found to be largely enhanced when compared with that of pure ZnO based DSSC (0.20% and 0.94 mA/cm²).     

Nanostructure materials for destruction of warfare agents and eco-toxins prepared by homogeneous hydrolysis with thioacetamide: Part 1—zinc oxide

Zinc sulphide (ZnS) nanoparticles were prepared by homogeneous hydrolysis of zinc sulphate and thioacetamide (TAA) at 80 °C. After annealing at temperature above 400 °C in oxygen atmosphere, zinc oxide (ZnO) nanoparticles were obtained. The ZnS and ZnO nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission microscopy (HRTEM), selected area electron diffraction (SAED), by BET and BJH methods used for surface area and porosity determination. The photocatalytic activity of the as-prepared ZnO samples was determined by the decomposition of Orange II in the aqueous solution under UV irradiation of 365 nm of wavelength.     

Synthesis and optical properties of nanocrystalline ZnO powders prepared by a direct thermal decomposition route

This paper reports the synthesis and optical properties of nanocrystalline ZnO powders with crystallite sizes of 32.5 (±1.4)–43.4 (±0.4) nm prepared by a direct thermal decomposition of zinc acetate at the temperatures of 400, 500, 600, and 700°C for 4 h. The structure of the prepared samples was studied by XRD and FTIR spectroscopy, confirming the formation of wurtzite structure. The morphology of the samples revealed by SEM was affected by the thermal decomposition temperature, causing the formations of both nanoparticles and nanorods with different size and shape in the samples. The synthesized powders exhibited the UV absorption below 400 nm (3.10 eV) with a well defined absorption peak at around 285 nm (4.35 eV). The estimated direct bandgaps were obtained to be 3.19, 3.16, 3.14, and 3.13 eV for the ZnO samples thermally decomposed at 400, 500, 600, and 700°C, respectively. All the samples exhibited room-temperature photoluminescence (PL) showing a strong UV emission band at ∼395 nm (3.14 eV), a weak blue band at ∼420 nm (2.95 eV), a blue–green band at ∼485 nm (2.56 eV), and a very weak green band at ∼529 nm (2.35 eV). The mechanisms responsible for photoluminescence of the samples are discussed.     

Evolution of ZnO nanostructures in sol–gel synthesis

Evolution of the microstructure and optical properties of ZnO nanoparticles in a mild sol–gel synthesis process is studied. The ZnO nanostructures were prepared by reacting zinc acetate dihydrate with NaOH in water at 50−60 °C. Evolution of ZnO nanostructures with reaction time is studied using UV–Vis spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), and Fourier transform infrared (FT-IR) spectroscopy techniques. During the process of Zn²⁺ hydroxylation, well defined rod-like crystals were formed within 15 min. Further hydroxylation leads to the formation of a gel-like structure within about 45 min. However, XRD, FT-IR and energy dispersive spectroscopy (EDS) confirmed that these initial products were zinc hydroxyl double salts (Zn-HDS), not ZnO. On ageing the reaction mixture, ZnO nanoparticles with wurtzite structure evolved.     

Effect of annealing temperature on optical and electrochemical properties of chitosan–ZnO nanostructure

Chitosan–ZnO nanostructures were prepared by chemical precipitation method using different concentration of zinc chloride and sodium hydroxide solutions. Nanorod-shaped grains with hexagonal structure for samples annealed at 300 °C and porous structure with amorphous morphology for samples annealed at 600 °C were revealed in SEM analysis. X-ray diffraction patterns confirmed the hexagonal phase ZnO with crystallite size found to be in the range of ~24.15–34.83 nm. Blue shift of UV–Vis absorption shows formation of nanocrystals/nanorods of ZnO with marginal increase in band gap. Photoluminescence spectra show that blue–green emission band at 380–580 nm. The chitosan–ZnO nanostructures used on surface of a glassy carbon electrode gives the oxidation peak potential at ~0.6 V. The electrical conductivity of chitosan–ZnO composites were observed at 2.1?×?10^?5 to 2.85?×?10^?5?S/m. The nanorods with high surface area and nontoxicity nature of chitosan–ZnO nanostructures observed in samples annealed at 300 °C were suitable as a potential material for biosensing.     

Synthesis and characterisation: Zinc oxide–sulfide nanocomposites

A novel synthesis method is presented for the preparation of nanosized-semiconductor zinc oxide–sulphide (ZnO/ZnS) core–shell nanocomposites, both formed sequentially from a single-source solid precursor. ZnO nanocrystals were synthesized by a simple co-precipitation method and ZnO/ZnS core–shell nanocomposites were successfully fabricated by sulfidation of ZnO nanocrystals via a facile chemical synthesis at room temperature. The as-obtained samples were characterized by X-ray diffraction and transmission electron microscopy. The results showed that the pure ZnO nanocrystals were hexagonal wurtzite crystal structures and the ZnS nanoparticles were sphalerite structure with the size of about 10 nm grown on the surface of the ZnO nanocrystals. Optical properties measured reveal that ZnO/ZnS core–shell nanocomposites have integrated the photoluminescent effect of ZnO and ZnS. Based on the results of the experiments, a possible formation mechanism of ZnO/ZnS core–shell nanocomposites was also suggested. This treatment is suggested to improve various properties of optoelectronically valuable ZnO/ZnS nanocomposites. These nanosized semiconductor nanocomposites can form a new class of luminescent materials for various applications.     

ZnO nanoparticles obtained by mechanochemical technique and the optical properties

Crystalline ZnO nanoparticles were synthesized by mechanochemical method. Mechanochemical processing involves the mechanical activation of solid-state displacement reactions at low temperatures in a ball mill. Statistical design was used to investigate the effect of main parameters (i.e. time, milling rate and calcination temperature) on ZnO crystallite size and morphology. After annealing at 400 °C in air, zinc oxide (ZnO) nanoparticles were obtained. The milled powders are analyzed by X-ray diffraction (XRD), TG/DTA and transmission electron microscope (TEM).The crystallite size of ZnO samples calculated from XRD is consistent with the TEM images and estimated to be less than 20 nm. The optical properties of the samples were studied by UV-vis spectrophotometer.     

A study on optical,photoluminescence and thermoluminescence properties of ZnO and Mn doped-ZnO nanocrystalline particles

Pure ZnO and Mn (1%wt.) doped-ZnO nanocrystalline particles were synthesized by reverse micelle method. The structural properties of the nanoparticles were investigated by X-Ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) techniques. UV–vis and photoluminescence (PL) spectroscopy was used for analyzing the optical properties of the nanoparticles. XRD and TEM results revealed the formation of ZnO and Mn doped-ZnO nanocrystalline particles with pure wurtzite crystal structure and average particle size of 18–21 nm. From UV–vis studies, the optical band gap energy of 3.53 and 3.58 eV obtained for ZnO and Mn doped-ZnO nanoparticles, respectively. Further optical analysis showed that the refractive index decreases from 2.35 to 1.35 with the change of wavelength. Room-temperature photoluminescence analysis of all samples showed four main emission bands including a strong UV emission band, a weak blue band, a week blue–green band, and a weak green band which indicated their high structural and optical quality. Moreover, the samples exposed to gamma rays sources of ¹³⁷Cs and ⁶⁰Co and their thermoluminescence properties were investigated. The thermoluminescence response of ZnO and Mn doped-ZnO nanocrystalline particles as a function of dose exhibited good linear ranges, which make them very promising detectors and dosimeters suitable for ionizing radiation.     

Preparation of pure ZnO nanoparticles by a simple solid-state reaction method

ZnO nanoparticles are synthesized by the one-step solid-state reaction using ZnSO₄·7H₂O and NaOH as the reagents. By adjusting the molar ratio of the reagents, the unwanted component Zn(OH)₂, which is the intermediate product of the reaction, can be fully removed in the final product, and the preparation of pure ZnO nanoparticles are achieved at room temperature. The X-ray diffraction pattern and transmission electron microscopic observations show that these nanoparticles are of hexagonal phase ZnO mostly in round shapes with a minority of rod shape with a mean grain size of about 40 nm. PACS  61.46.Df; 81.07.-b; 61.46.-w; 81.07.wx; 81.16.-c     

Zinc impregnated cellulose nanocomposites: Synthesis,characterization and applications

Nanocomposite materials have broad applicability due to synergistic effect of combined components. In present investigation, cellulose isolated from citrus peel waste is used as a supporting material; impregnation of zinc oxide nanoparticles via co-precipitation method. The characterization of nano composite is carried out through Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) analysis, scanning electron microscopy (SEM) and Thermo-gravimetric analysis (TGA) resulting less than 10 µm cellulose fiber and approx. 50 nm ZnO NPs. Zinc oxide impregnated cellulose (ZnO–Cel) exhibited significant bacterial devastation property when compared to ZnO NPs or Cellulose via disc diffusion and colony forming unit methods. In addition, the ZnO–Cel exhibited significant total antioxidant, and minor DPPH free radical scavenging and total reducing power activities. The nano composite also showed time dependent increase in photocatalytic by effectively degrading methylene blue dye up to 69.5% under sunlight irradiation within 90 min. The results suggest effective utilization of cellulose obtained from citrus waste and synthesis of pharmacologically important nano-composites that can be exploited in wound dressing; defence against microbial attack and healing due to antioxidative property, furthermore can also be used for waste water treatment.