Flash synthesis of flower-like ZnO nanostructures by microwave-induced combustion process

Flower-like ZnO particles were fabricated from zinc nitrate and urea via the microwave-induced combustion technique (MICT). The structure and morphology of the products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). The effects of growth conditions such as microwave power, radiation time, and molar ratio of urea/Zn²⁺ were investigated. Results show that the morphologies and particle sizes of the final products depend on the molar ratio of urea/Zn²⁺. The SEM images of ZnO flowers grown in different periods were employed to explain the formation mechanism. This study provides a simple and efficient approach for synthesizing flower-like ZnO heterostructures.     

Facile synthesis and excellent electromagnetic wave absorption properties of flower-like porous RGO/PANI/Cu<Subscript>2</Subscript>O nanocomposites

Novel porous ternary nanocomposite systems containing reduced graphene oxide (RGO)/polyaniline (PANI)/cuprous oxide (Cu₂O) were prepared via one-step in situ redox method. The RGO/PANI/Cu₂O nanocomposites present a flower-like structure with an average size of 2.0 μm in diameter. The morphologies and properties of the products can be controlled by adjusting the molar ratios of aniline to Cu²⁺. When the molar ratio of aniline to Cu²⁺ is 1:1, the product exhibits excellent microwave absorption property in the frequency range of 2–18 GHz. It can be seen that the maximum reflection loss (RL) of the ternary composite is up to ?52.8 dB at 2.7 GHz with a thickness of only 2 mm, and the absorption bandwidth corresponding to ?10 dB (90% of EM wave absorption) is 13.2 GHz. The microwave absorption property of ternary RGO/PANI/Cu₂O composite is significantly improved due to its special flower-like porous structure, dielectric loss property and well impedance matching characteristics, which is 8.12 times than that of pure RGO and 5.28 times than that of pure PANI. Therefore, our study paves a new way to prepare the promising lightweight and high-performance composite materials combined with the characteristics of three components for electromagnetic absorption.     

Effect of α-Fe2O3 addition on the morphological,optical and decolorization properties of ZnO nanostructures

Visible light sensitive photocatalysts of Fe₂O₃/ZnO nanocomposites were prepared by a simple solid-state reaction method, using zinc acetate, α-Fe₂O₃ and sodium hydroxide at room temperature. The products were characterized by scanning electron microscopy, powder X-ray diffraction, N₂ adsorption–desorption measurement, UV–vis absorption, and photoluminescence spectroscopy and used for photodecolorization of Congo red. The characterization results showed that the morphology, crystallite size, BET surface area and optical absorption of the samples varied significantly with the Fe³⁺ to Zn²⁺ ratios. The nanocomposites show two absorption edges at ultraviolet and visible region. The optical band gap values of these nanocomposites were calculated to be about 3.98–3.81 eV and 2.88–2.98 eV, which show a red shift from that of pure ZnO. These red shifts are related to the formation of Fe s-levels below the conductive band edge of ZnO and effectively extend the absorption edge into the visible region. The growth mechanisms of the samples are proposed. These nanocomposites showed high decolorization ability in visible light with wavelength up to about 400 nm. Among the samples, Fe₂O₃/ZnO nanoflower (molar ratio of Fe³⁺ to Zn²⁺ is 1:100) exhibited higher decolorization efficiency than the other nanocomposites. It could be considered as a promising photocatalyst for dyes treatment.     

Structural and Magnetic Studies on Chromium substituted Ni-Zn Nano Ferrite Synthesized by Citrate Gel Auto Combustion Method

Nano crystalline Ni_0.5Zn_0.5Cr_xFe_2?xO₄ particles with x varying from 0.00 to 0.25 in steps of 0.05 have been synthesized through citrate gel autocombustion method. When Ni_0.5Zn_0.5Fe₂O₄ nano particles were annealed at 1000 °C, the crystallite size increased while the lattice constant decreased slightly. For, the Cr³⁺ substituted samples annealed at 1000 °C, the variation in lattice constant, bondlengths, M_e-M_e distances and other structural parameters have been attributed to the dissimilarity in the ionic radius of the displaced (Fe³⁺) ion and the substituted (Cr³⁺) ion. Thermal studies indicated the autocombustion process which is an exothermic reaction between the nitrates salt solutions and the citric acid took place at about a temperature of 400 °C for Ni_0.5Zn_0.5Fe₂O₄. The M-H loops for all samples indicated a soft ferrite nature for all samples. The non-saturated hysteresis loop and high coercivity for the as prepared Ni_0.5Zn_0.5Fe₂O₄ nano particles has been attributed to the core-shell structure of the fine particles. When annealed at 1000 °C the saturation magnetization of Ni_0.5Zn_0.5Fe₂O₄ nano particles increased and attained the bulk value (70emu/gm). The specific saturation magnetization has been observed to decrease with increasing Cr³⁺ substitution and is ascribed to the reduction in the predominant A-B exchange interaction mechanism. By considering the site preferences cations a suitable distribution of the cations among the A & B-sites has been proposed for Ni_0.5Zn_0.5Cr_xFe_2?xO₄ nano particles annealed at 1000 °C and has been verified using the X-ray diffraction line intensity calculations. The FT-IR spectra of the annealed ferrite powders showed two significant absorption bands in the wave numbers around 400 cm^?1 & 580 cm^?1 and an additional shoulder at 360cm^?1. The position and width of the bands have been observed to vary with Cr³⁺ substitution. The results of IR spectra are in support of the proposed cation distribution.     

Effect of Ni Doping on Structural,Morphological, Optical and Magnetic Properties of Zn1−x Ni x O Dilute Magnetic Semiconductors

Ni²⁺-doped ZnO diluted magnetic semiconducting materials (Zn_1?x Ni _x O with x=0.01,0.02,0.03,0.04,0.05) were synthesised by the co-precipitation method. All synthesised samples were sintered at 600 °C for 6 hours. The effects of Ni²⁺ ion-doping on the structural, morphological, optical and magnetic properties of ZnO were investigated using powder X-ray diffraction, field emission SEM, UV–DRS spectroscopy, photoluminescence and vibrating sample magnetometry. The XRD patterns of pure and Ni-doped ZnO samples revealed single phase hexagonal wurtzite structure. The SEM analysis revealed the morphology of prepared samples, and the chemical compositions of all samples were analysed using exhibit energy density X-ray analysis (EDAX) characterisation. The absorption and emission properties revealed the effect of Ni²⁺ doping in ZnO samples. All Ni²⁺ ion-doped samples showed ferromagnetism at room temperature. The observed results are here analysed and reported.     

ZnO hierarchical nanostructures and application on high-efficiency dye-sensitized solar cells

Uniform hierarchical ZnO nanostructures are synthesized on a large scale based on a solution approach at low temperature. The primary ZnO hexagonal prisms are firstly produced by the reaction of Zn(NO₃)₂ with hexamethylenetetramine, and then ZnO branches grow on the primary prisms by using ethylenediamine molecules as an evocator. The morphology of the hierarchical nanostructure can be controlled conveniently by adjusting the molar ratio of [EDA]/[Zn²⁺]. The hierarchical structure provides an effective pathway for carrier transport as well as larger surface area for dye adsorption, when ZnO hierarchical nanostructures serve as photoanode materials, the solar cells show higher conversion efficiency than that of primary ZnO nanowires.     

Large-scale controlled synthesis of magnetic FeCo alloy with different morphologies and their high performance of electromagnetic wave absorption

Magnetic materials of FeCo alloy with different morphologies (nanocube, nanoplate and flower-like structure) have been synthesized by controlling the molar ratio of Fe²⁺ to Co²⁺, concentrations of cyclohexane and PEG-400. The structure and morphology were characterized by several analytical techniques, including XRD, SEM, TEM, XPS and VSM. The microwave-absorbing properties were measured by a vector network analyzer. The SEM and TEM photographs reveal that the edge length of FeCo nanocube is about 215 nm, the diameter and thickness of the nanoplate is 100 and 15 nm, respectively. The average diameter of flower-like FeCo is about 1.5 μm. The investigation of the electromagnetic wave absorbability revealed that flower-like FeCo exhibited excellent electromagnetic wave absorption properties compared with FeCo nanocube and FeCo nanoplate due to the special structure. The maximum reflection loss of flower-like FeCo was up to ?43 dB at 13.1 GHz and the absorption bandwidth with the reflection loss below ?10 dB was 5.8 GHz (from 2.7 to 5.4 GHz and from 12 to 15.1 GHz) with a thickness of 3.4 mm. Furthermore, this work offers a simple solvothermal route to fabricate shape and size-controlled FeCo alloy, which can be used as an attractive candidate for new type of electromagnetic wave absorbers.     

Room-temperature ferromagnetism in Fe-doped, Fe- and Cu-codoped ZnO diluted magnetic semiconductor

Magnetic properties of Zn_0.975Fe_0.025O and Zn_0.97Fe_0.025Cu_0.005O crystallites fabricated by hydrothermal method are investigated. X-ray diffraction and Raman measurements indicate that the samples have pure ZnO wurtzite structure and Fe²⁺ ions have substituted Zn²⁺ sites. Magnetic measurements indicate that Fe doping can induce room-temperature ferromagnetism, while codoping with Cu might enhance the magnetic moment but reduce the Curie temperature in ZnO.     

Cu-doping effect on structure and magnetic properties of Fe-doped ZnO powders

Fe-doped and Cu, Fe co-doped ZnO diluted magnetic semiconductors powders were synthesized by sol–gel method. The x-ray diffraction (XRD) results showed that Zn_0.97−xFe_0.03Cu_xO (x ≤ 0.02) samples were single phase with the ZnO-like wurtzite structure. X-ray photoelectron spectroscopy (XPS) showed that Fe²⁺ and Fe³⁺ existed in Zn_0.97Fe_0.03O, while Fe²⁺, Fe³⁺and Cu⁺, Cu²⁺ were found in Zn_0.95Fe_0.03Cu_0.02O. Both Zn_0.97Fe_0.03O and Zn_0.95Fe_0.03Cu_0.02O exhibited ferromagnetic performance at room temperature. But the Cu incorporation reduced the saturation magnetization of Fe-doped ZnO diluted magnetic semiconductors.     

Structural,dielectric, ac conductivity and electromagnetic shielding properties of polyaniline/Ni<Subscript>0.5</Subscript>Zn<Subscript>0.5</Subscript>Fe<Subscript>2</Subscript>O<Subscript>4</Subscript> composites

A conducting polymer, polyaniline (PANI)/Ni_0.5Zn_0.5Fe₂O₄ composites with high dielectric absorbing properties and electromagnetic shielding effectiveness at low frequencies were successfully synthesized through a simple in situ emulsion polymerization. PANI was doped with hydrochloric acid to improve its electrical properties and interactions with ferrite particles. PANI/Ni_0.5Zn_0.5Fe₂O₄ composites were characterized by X-ray diffraction analysis, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and thermal gravimetric analysis. Frequency dependence of dielectric and ac conductivity (σ_ac) studies have been undertaken on the PANI/Ni_0.5Zn_0.5Fe₂O₄ composites in the frequency range 50 Hz–5 MHz. The electrical conduction mechanism in the PANI/Ni_0.5Zn_0.5Fe₂O₄ is found to be in accordance with the electron hopping model. Further, frequency dependence of electromagnetic interference (EMI) shielding effectiveness (SE) is studied. The EMI shielding effectiveness is found to decrease with an increase in the frequency. The maximum value 55.14 dB of SE at 50 Hz was obtained at room temperature for PANI/Ni_0.5Zn_0.5Fe₂O₄ composites in the 50 Hz–5 MHz frequency range. PANI/Ni_0.5Zn_0.5Fe₂O₄ composites were demonstrated as a promising functional material for the absorbing of electromagnetic waves at low frequencies because of a large amount of dipole polarizations in the polymer backbone and at the interfaces of the Ni–Zn ferrite particles and PANI matrix.     

The structure and ferromagnetic properties of (Fe0.12CuxZn0.88−x)O thin films deposited on Si substrates by R.F. sputtering

Fe–Cu co-doped ZnO thin films deposited on silicon substrates were prepared by R.F. magnetron sputtering. The effects of various amounts of copper on the microstructure, surface morphology, composition, and magnetic properties of ZnO thin films were examined. The results of the experiments show that the structures of the ZnO thin films grown on the silicon substrate have a preferred orientation of (002). By increasing the copper concentration, the Fe ions exist as Fe²⁺ in the Fe_0.12Cu_xZn_0.88−xO system, but Cu²⁺ and Cu¹⁺ ions coexist when the Cu replaces the Zn. In addition, the ZnO thin films show ferromagnetic behaviour at room temperature and the largest saturation magnetization (Ms) is 5.64 × 10⁴ A/m for the as-grown Fe_0.12Cu_0.02Zn_0.86O thin film.     

基于纳米镍锌铁氧体以Co2+逐步替代Ni2+制备钴锌铁氧体及吸波性能对比

应用水热法掺杂钴离子到纳米镍锌铁氧体粉末中,制备处纳米镍锌钴铁氧体,继而用钴离子代替镍离子制备钴锌铁氧体.并利用XRD、TEM、VNA对其进行表征和分析,研究了纳米镍锌钴铁氧体和纳米钴锌铁氧体的样品粒度、形貌、电磁损耗性能及吸收性能.结果表明：纳米镍锌钴铁氧体由原先纳米镍锌铁氧体的类球形转变为不规则四边形结构.掺杂钴离子后增加吸收器的带宽, 改善材料在低频率的吸波性能。钴锌铁氧体中当Co²⁺: Zn²⁺=1: 1时,对于电磁波吸收性能比镍锌钴铁氧体要好,在16.47 GHz处到达33.9 dB.     

Preparation of Fe2O3/Al composite powders by homogeneous precipitation method

The Fe₂O₃/Al composite powders were prepared by homogeneous precipitation method. The influence of the concentration of Fe²⁺ and the molar ratio of raw materials on the preparation of Fe₂O₃/Al composite powders were investigated. X-ray diffractometer, scanning electron microscope, Fourier transform infrared spectroscopy and differential thermal analysis were used to analyze the morphology and structure of the Fe₂O₃/Al composite powders. The results show that the content of iron oxide in the composite powders could be effectively controlled by adjusting the concentration of Fe²⁺ and the molar ratio of raw materials in the plating solution. The surface of Al particle was coated with a layer of thick and dense iron oxide. The core-shell Fe₂O₃/Al composite powders with Fe₂O₃ content of 14.1% were produced, the coating efficiency of Fe₂O₃ reaches more than 77%. The iron oxide, which coated on the surface of the aluminium particle is flower-like cluster structure, each flower-like cluster is constituted by nano-flaky iron oxide.     

Shape-controlled synthesis of bare ZnO nanomaterials with improved photoactivity and photostability

ABSTRACT

Understanding the growth mechanisms of nanomaterials usually leads to the successful preparation of targeted micro-structures with excellent properties. In this paper, flower-like and roughly spherical ZnO nanocrystals have been successfully synthesised through facile wet chemical methods, i.e. hydrothermal pathways and homogeneous precipitation method. The photocatalytic activities of the prepared photocatalysts were evaluated by degradation of rhodamine B (RhB) and phenol under ultraviolet (UV) irradiation. Remarkably, the ZnO powder via homogeneous precipitation (urea/Zn²⁺?=?2.0) exhibited better photocatalytic performance and photostability than those of flower-like ZnO substrate. The enhanced photocatalytic properties could be attributed to more active catalytic sites and effective separation of carriers, which were confirmed by low-temperature nitrogen adsorption, photocurrent responses, and photoluminescence spectral analysis. A possible mechanism for the excellent photocatalytic activity of ZnO substrates was proposed.     

Synthesis and characterization of Ni1−xZnxFe2O4 spinel ferrites from tailored layered double hydroxide precursors

In this paper, a series of pure Ni_1 − xZn_xFe₂O₄ (0 ≤ x ≤ 1) spinel ferrites have been synthesized successfully using a novel route through calcination of tailored hydrotalcite-like layered double hydroxide molecular precursors of the type [(Ni + Zn)_{1 − x − y}Fe_y²⁺Fe_x³⁺(OH)₂]^x+(SO₄²⁻)_x/2·mH₂O at 900 °C for 2 h, in which the molar ratio of (Ni²⁺ + Zn²⁺)/(Fe²⁺ + Fe³⁺) was adjusted to the same value as that in single spinel ferrite itself. The physico-chemical characteristics of the LDHs and their resulting calcined products were investigated by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and Mössbauer spectroscopy. The results indicate that calcination of the as-synthesized LDH precursor affords a pure single Ni_1 − xZn_xFe₂O₄ (0 ≤ x ≤ 1) spinel ferrite phase. Moreover, formation of pure ferrites starting from LDHs precursors requires a much lower temperature and shorter time, leading to a lower chance of side-reactions occurring, because all metal cations on the brucite-like layers of LDHs can be uniformly distributed at an atomic level.     

Morphology controllable synthesis of ZnO crystals—pH-dependent growth

ZnO crystals were grown through a solution-based chemical route at ambient pressure and low temperature. It was found that the solution pH is a dominative factor in determining the morphology of crystals: Rod-like ZnO crystals are apt to be formed at near neutral condition, whereas flower-like structured ZnO crystals are preferred to be formed at higher solution pH. By monitoring the reaction intermediates during the ZnO growth process, it was realized that the crucial role of solution pH in determining the morphology of ZnO crystals is to control the structure of the primary reaction intermediates at the early stage of ZnO growth. Moreover, by appreciate controlling the solution pH together with Zn²⁺ concentration, various ZnO crystals of rod-like, dumbbell-like and even more complex flower-like structures were obtained without any template, and a pH-dependent morphology controllable growth mechanism is suggested.     

ZnO micro and nanocrystals with enhanced visible light absorption

In this paper, we investigate the effect of the particle size and morphology on the optical properties of ZnO. A series of ZnO micro and nanocrystals were synthesized by the hydrothermal processing of zinc acetate dihydrate and sodium hydroxide as the starting materials, and polyvinylpyrrolidone (PVP) as the polymer surfactant. The particle size and morphology were tailored by adjusting the reactant molar ratios [Zn²⁺]/[OH⁻], while the reaction temperature and the time remained unchanged. X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and high-resolution TEM (HRTEM) have shown that the micro and nanocrystals have a high crystalline pure wurtzite-type hexagonal structure with nanosized crystallites. The size and morphology of the ZnO micro and nanocrystals were investigated by field emission scanning electron microscopy (FE-SEM), which showed a modification from micro-rods via hexagonal-faceted prismatic morphology to nanospheres, caused by simple adjustment of the reactant molar ratio [Zn²⁺]/[OH⁻] from 1:1 to 1:5. The optical properties of the ZnO micro and nanocrystals, as well as their dependence on the particle size and morphology were investigated by Raman and ultraviolet–visible (UV–vis) diffuse reflectance spectroscopy (DRS). The UV–vis spectra showed that the modification of the particle size and morphology from nanospheres to micro-rods resulted in increased absorption, and a slight red-shift of the absorption edge (0.06 eV). Besides, the band gap energy of the synthesized ZnO micro and nanocrystals showed the red shift (∼0.20 eV) compared to bulk ZnO. According to the results of a Raman spectroscopy, the enhanced visible light absorption of the ZnO micro and nanocrystals is related to two phenomena: (1) the existence of lattice defects (oxygen vacancies and zinc interstitials), and (2) the particle surface sensitization by PVP.     

Coprecipitation of 60Co from aqueous solutions with triethylenediamine complexes of d-element nitrates

Formation of complexes of Co²⁺ with triethylenediamine (CH₂-CH₂)₃N₂ (Q) in aqueous solution and coprecipitation of microamounts of ⁶⁰Co with triethylenediamine complexes of Cu²⁺, Ni²⁺, and Zn²⁺ nitrates were studied. Microamounts of ⁶⁰Co poorly coprecipitate with triethylenediamine complexes of Cu²⁺ and Zn²⁺ nitrates. At practically 100% precipitation of Cu²⁺ and Zn²⁺ from solutions in the form of the corresponding complexes, the degree of coprecipitation of ⁶⁰Co with these complexes does not exceed 15%. With the Ni²⁺ complexes formed from 10⁻¹ M aqueous solutions at the molar ratios Ni²⁺: Q = 1 : 1 and 1 : 2, the degree of coprecipitation of ⁶⁰Co is about 45 and 90%, respectively.     

Divalent ion uptake of heavy metal cations by (aluminum + alkali metals) – substituted synthetic 1.1 nm-tobermorites

The reactions of Mn²⁺, Fe²⁺, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺, Pb²⁺, Cd²⁺ or Hg²⁺ synthetic (Al + alkali metal) – substituted tobermorites were studied. Among these cations, Mn²⁺, Fe²⁺, Cu²⁺, Zn²⁺, pb²⁺ and Hg²⁺ appears to exchange with outer planar surface of Ca²⁺ of tobermorites due to the break down of structural Ca-O bonds, in addition to the substituted alkali metals in the structure. But it is difficult to delineate the extent of this reaction from the precipitation of the concerned ions as carbonates, hydroxy carbonates, hydroxy nitrates or hydroxides. The uptake of metal ions by these solids led to their amorphization in many cases due to the partial exchange and the acidic nature of metal solutions, and hence their reactions are not strictly analogous to cation exchange in zeolites and clays. The order of ion uptake has been found in the following order: Fe²⁺ > Ni²⁺ > Co²⁺ > Zn²⁺ > Cu²⁺ > Mn²⁺ > Hg²⁺ > Cd²⁺ > pb²⁺.     

Ni-doped vertically aligned zinc oxide nanorods prepared by hybrid wet chemical route

Ni-doped zinc oxide (Ni:ZnO) nanorods were synthesized by incorporating nickel in vertically aligned ZnO nanorods. Ni was evaporated onto ZnO nanorods and the composite structure was subjected to rapid thermal annealing for dispersing Ni in ZnO nanorods. The optical band gap decreased with increasing amount of Ni incorporation. The origin of the photoluminescence peak at ∼ 400 nm was related to the defect levels introduced due to substitution of Ni²⁺ in the Zn²⁺ site with annealing. The Raman spectra indicated the presence of the characteristic peak at ∼ 436 cm^− 1 which was identified as high frequency branch of E₂ mode of ZnO. The Fourier Transformed Infrared spectra indicated the existence of the distinct characteristic absorption peak at 481 cm^− 1 for ZnO stretching modes. Current-voltage characteristics indicated that the current changed linearly with voltage for both the doped and undoped samples.