Synthesis and antimicrobial activity of mesoporous hydroxylapatite/zinc oxide nanofibers

The aim of this study is to develop antimicrobial mesoporous hydroxylapatite/zinc oxide (meso-HA/ZnO) nanofibers from polyvinyl alcohol/hydroxylapatite/zinc acetate (PVA/HA/Zn(OAc)₂) electrospun nanofibers by calcination process. The antibacterial activities of meso-HA/ZnO nanofibers towards Staphylococcus aureus (S. aureus, ATCC6538) and Escherichia coli (E. coli, 8099) were evaluated. The meso-HA/ZnO nanofibers were composed of hexagonal HA and wurtzite ZnO phases. The representative meso-HA/ZnO nanofibers with ZnO/HA ratio at 1:5 showed a wormhole-like shape, main pore diameter around 25 nm and specific surface area at 24.81 m²/g. The inhibition efficiency of meso-HA/ZnO nanofibers increased with the increase of ZnO/HA ratio, however, S. aureus was more sensitive to meso-HA/ZnO nanofibers than E. coli. The meso-HA/ZnO nanofibers with ZnO/HA ratio at 1:10 exhibited effective antibacterial activity towards S. aureus, whereas, the ZnO/HA ratio was raised up to 1:5 towards E. coli. The experimental results suggested that the meso-HA/ZnO nanofibers might have potential as an antimicrobial activity material in biomaterial applications.     

Microwave-assisted hydrothermal synthesis of zinc oxide particles starting from chloride precursor

Zinc oxide (ZnO) was synthesized using a microwave assisted hydrothermal (MAH) process based on chloride/urea/water solution and under 800 W irradiation for 5 min. In the bath, Zn²⁺ ions reacted with the complex carbonate and hydroxide ions to form zinc carbonate hydroxide hydrate (Zn₄CO₃(OH)₆·H₂O), and the conversion from Zn₄CO₃(OH)₆·H₂O to ZnO was synchronously achieved by a MAH process. The as-prepared ZnO has a sponge-like morphology. However, the initial sponge-like morphology of ZnO could change to a net-like structure after thermal treatment, and compact nano-scale ZnO particles were finally obtained when the period of thermal treatment increased to 30 min. Pure ZnO nanoparticles was obtained from calcination of loose sponge-like ZnO particles at 500 °C. The analysis of optical properties of these ZnO nanoparticles showed that the intensity of 393 nm emission increased with the calcination temperature because the defects were reduced and the crystallinity was improved.     

Preparation and characterization of the bismuth sodium titanate (Na0.5Bi0.5TiO3) ceramic doped with ZnO

This study investigates effects of the zinc oxide (ZnO) addition and the sintering temperature on the microstructure and the electrical properties (such as dielectric constant and loss tangent) of the lead-free piezoelectric ceramic of bismuth sodium titanate (Na_0.5Bi_0.5TiO₃), NBT, which was prepared using the mixed oxide method. Three kinds of starting powders (such as Bi₂O₃, Na₂CO₃ and TiO₂) were mixed and calcined. This calcined NBT powder and a certain weight percentage of ZnO were mixed and compressed into a green compact of NBT–ZnO. Then, this green compact of NBT–ZnO was sintered to be a disk doped with ZnO, and its characteristics were measured. In this study, the calcining temperature was 800 °C, the sintering temperatures ranged from 1000 to 1150 °C, and the weight percentages of ZnO doping included 0.0, 0.5, 1.0, and 2.0 wt%. At a fixed wt% ZnO, the grain size increases with increase in the sintering temperature. The largest relative density of the NBT disk obtained in this study is 98.3% at the calcining temperature of 800 °C, the sintering temperature of 1050 °C, and 0.5 wt% ZnO addition. Its corresponding dielectric constant and loss tangent are 216.55 and 0.133, respectively.     

Porous structure to improve microwave absorption properties of lamellar ZnO

The novel porous ZnO nanoflakes were fabricated by a facile two-step method containing preparation of precursor ZnCO₃ and subsequently calcination of ZnCO₃. The as-prepared products were analyzed by X-ray diffraction, scanning electron microscopy, and thermalgravimetric analysis. The results reveal that the porous ZnO nanoflakes were in the diameter and thickness of several to tens micrometers and 100–500 nm, respectively. The microwave absorption properties of porous ZnO nanoflakes were investigated by the network analyzer, which exhibit the minimal reflection loss of ?34.5 dB at 10.7 GHz with only thickness of 1.5 mm. The effective absorption (below ?10 dB) bandwidth can be tuned between 7.0 GHz and 17.1 GHz by tuning absorber thickness of 1.0–2.2 mm. Thus, the porous lamellar ZnO could be used as a promising absorbing material with the features of high efficiency absorption, wide-band and light weight.     

Preparation and microwave absorption of porous hollow ZnO by CO2 soft-template

The porous hollow ZnO samples were prepared by calcination of ZnCO₃ precursor at 450 °C. The structural properties were investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), thermogravimetric analysis and differential thermal analysis (TG-DTA). A possible mechanism for the formation of porous hollow microstructure was proposed. The microwave absorption properties of the porous hollow structural ZnO have been investigated. The reflection loss (RL) of the ZnO was calculated based on the relative complex permeability and permittivity. A minimum reflection loss of the wax-composite with 25 wt% porous hollow ZnO is −36.3 dB at 12.8 GHz with a thickness of 4.0 mm. The results indicate that porous hollow structural ZnO can be used as a desirable material for the microwave absorption.     

Effect of aluminum oxide doping on the structural,electrical, and optical properties of zinc oxide (AOZO) nanofibers synthesized by electrospinning

Zinc oxide nanofibers doped with aluminum oxide were prepared by sol–gel processing and electrospinning techniques using polyvinylpyrrolidone (PVP), zinc acetate and aluminum acetate as precursors. The resulting nanofibers were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–Vis spectroscopy, and current–voltage (I–V) properties. The nanofibers had diameters in the range of 60–150 nm. The incorporation of aluminum oxide resulted in a decrease in the crystallite sizes of the zinc oxide nanofibers. Aluminum oxide doped zinc oxide (AOZO) nanofibers exhibited lower bandgap energies compared to undoped zinc oxide nanofibers. However, as the aluminum content (Al/(Al + Zn) × 100%) was increased from 1.70 at.% to 3.20 at.% in the electrospinning solution, the bandgap energy increased resulting in lower conductivity. The electrical conductivity of the AOZO samples was found to depend on the amount of aluminum dopant in the matrix as reflected in the changes in oxidation state elucidated from XPS data. Electrospinning was found to be a productive, simple, and easy method for tuning the bandgap energy and conductivity of zinc oxide semiconducting nanofibers.     

Photocatalytic degradation of reactive brilliant blue X-BR in aqueous solution using quantum-sized ZnO

Quantum-sized ZnO was prepared using sol–gel method with zinc acetate dehydrate (Zn(CH₃COO)₂·2H₂O) and lithium hydroxide monohydrate (LiOH·H₂O) as raw material. The ZnO particles annealed at different temperature were characterized by means of X-ray diffraction (XRD), Infrared absorption spectroscopy (IR) and UV–vis spectroscopy. The degradation rate of reactive brilliant blue X-BR in aqueous solution was used to evaluate the photocatalytic performance of the quantum-sized ZnO. The experimental results indicated that the photocatalytic property of the ZnO was excellent. The photocatalytic efficiency of quantum-sized ZnO was significantly influenced by the calcining heat. When calcined at 300 °C, its size is 6.78 nm and the photocatalytic performance is the best. The degradation rate of reactive brilliant blue X-BR could exceed 90% in 15 min at 35 °C, when the concentration of the quantum-sized ZnO was 0.35 mg/L.     

Solvothermal synthesis of Ag/ZnO micro/nanostructures with different precursors for advanced photocatalytic applications

Micro/nanostructured systems based on metallic oxide (ZnO) with noble metal (Ag) on the surface (Ag/ZnO) are synthesized by solvothermal method from zinc nitrate hexahydrate (Zn(NO₃)₂·6H₂O), zinc acetate dehydrate (Zn(CH₃COO)₂·2H₂O), zinc acetylacetonate hydrate (Zn(C₅H₇O₂)₂·xH₂O) and silver nitrate (Ag(NO₃)) as precursors. In these systems, polyvinylpyrrolidone (PVP) is used as surfactant for controlling particle morphology, size and dispersion. The obtained materials are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), UV–vis diffuse reflectance spectroscopy (DRS), N₂ gas adsorption–desorption (BET) and Raman spectroscopy (RS). By XRD results, all major peaks are indexed to the hexagonal wurtzite-type structure of the ZnO and samples with noble metal, extra diffraction peaks are detected which correspond to the face-centered-cubic (fcc) structure of the metallic Ag. Depending on used precursor, different morphologies have been obtained. Mainly, ZnO prims-like rods – NRs (with 0.8 ? aspect ratio ? 3.4) – have been observed. Quasi-spherical particles of metallic Ag (with diameters between 558 ± 111 μm and 22 ± 1 nm) have been detected on the ZnO surface. Photocatalytic results (all samples studied >30% MB degradation) verify the important effect of surfactant and the viability of synthesized Ag/ZnO micro/nanocomposites for environmental applications.     

Effects of optical band gap energy,band tail energy and particle shape on photocatalytic activities of different ZnO nanostructures prepared by a hydrothermal method

The dependence of the crystallite size and the band tail energy on the optical properties, particle shape and oxygen vacancy of different ZnO nanostructures to catalyse photocatalytic degradation was investigated. The ZnO nanoplatelets and mesh-like ZnO lamellae were synthesized from the PEO₁₉-b-PPO₃ modified zinc acetate dihydrate using aqueous KOH and CO(NH₂)₂ solutions, respectively via a hydrothermal method. The band tail energy of the ZnO nanostructures had more influence on the band gap energy than the crystallite size. The photocatalytic degradation of methylene blue increased as a function of the irradiation time, the amount of oxygen vacancy and the intensity of the (0 0 0 2) plane. The ZnO nanoplatelets exhibited a better photocatalytic degradation of methylene blue than the mesh-like ZnO lamellae due to the migration of the photoelectrons and holes to the (0 0 0 1) and (0 0 0 −1) planes, respectively under the internal electric field, that resulted in the enhancement of the photocatalytic activities.     

ZnO films and nanorod/shell arrays electrodeposited on PET-ITO electrodes

In this work, ZnO films, nanorod and nanorod/shell arrays were synthesized on the surface of PET-ITO electrodes by electrochemical methods. ZnO films with high optical transmittance were prepared from a zinc nitrate solution using a pulsed current technique with a reduced pulse time (3 s). The X-ray diffraction pattern of ZnO film deposited on PET-ITO electrode showed that it has a polycrystalline structure with preferred orientations in the directions [0 0 2] and [1 0 3]. ZnO nanorods were synthesized on electrochemical seeded substrate in an aqueous solution containing zinc nitrate and hexamethylenetetramine. In order to increase the stability of PET-ITO electrode to electrochemical and chemical stresses during ZnO nanorods deposition the surface of the electrode was treated with a 17 wt% NH₄F aqueous solution. Electrochemical stability of PET-ITO electrode was evaluated in a solution containing nitrate ions and hexamethylenetetramine. ZnO nanorod/shell arrays were fabricated using eosin Y as nanostructuring agent. Photoluminescence spectra of ZnO nanorod and ZnO nanorod/shell arrays prepared on the surface of PET-ITO electrode were discussed comparatively. By employing the 1.5 μm-length ZnO nanorod/shell array covered with a Cu₂O film a photovoltaic device was fabricated on the PET-ITO substrate.     

Growth of p-type ZnO thin films by using an atomic layer epitaxy technique and NH3 as a doping source

Nitrogen-doped, p-type ZnO thin films have been grown successfully on sapphire (0001) substrates by atomic layer epitaxy (ALE) using Zn(C₂H₅)₂ [Diethylzinc, DEZn], H₂O and NH₃ as a zinc precursor, an oxidant and a doping source gas, respectively. The lowest electrical resistivity of the p-type ZnO films grown by ALE was 210 Ω cm with a hole concentration of 3.41 × 10¹⁶ cm^− 3. Low temperature-photoluminescence analysis results support that the nitrogen ZnO after annealing is a p-type semiconductor. Also a model for change from n-type ZnO to p-type ZnO by annealing is proposed.     

Self-assembly of small ZnO nanoparticles toward flake-like single crystals

Flake-like single-crystalline ZnO nanocrystals with porous structure have been achieved, in which precursor of Zn₄CO₃(OH)₆·H₂O was first prepared by mild hydrothermal method with urea as the homogeneous precipitant and decomposed into small ZnO nanocrystals after being calcined at 400 °C, then the small ZnO nanocrystals self-assemble to form flake-like ZnO aggregates. The ZnO nanoflakes have lateral dimensions up to micrometer with the plane normal to [0 0 1] direction. The UV–vis absorption reveals that the ZnO nanoflakes have strong absorption in the UV region. The advantages of our method for the synthesis lie in the low temperature and mild reaction condition, which permit large-scale production at low cost.     

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.     

La-doped ZnO nanoparticles: Simple solution-combusting preparation and applications in the wastewater treatment

La-doped ZnO nanoparticles have been successfully synthesized by a simple solution combustion method via employing a mixture of ethanol and ethyleneglycol (v/v = 60/40) as the solvent. Zinc acetate and oxygen gas in the atmosphere were used as zinc and oxygen sources, and La(NO₃)₃ as the doping reagent. The as-obtained product was characterized by means of powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray spectrometry and X-ray photoelectron spectroscopy. Experiments showed that La-doped ZnO nanoparticles exhibited the higher capacities for the removal of Pb²⁺ and Cu²⁺ ions in water resource than undoped ZnO nanoparticles.     

Synthesis and adsorption property of zinc rust of zinc hydroxynitrate

In order to clarify the formation condition of zinc rusts such as layered zinc hydroxynitrate (Zn₅(OH)₈(NO₃)₂·2H₂O: ZHN), ZnO particles were aged with aqueous Zn(NO₃)₂·6H₂O solution at 6–140 °C for 48 h. Further, adsorption of H₂O and CO₂ on ZHN was examined for simulating study of atmospheric corrosion of galvanized steel. The ZHN was formed at 6 °C and the ZnO completely disappeared, meaning the hydrolysis of ZnO particles in aqueous Zn(NO₃)₂·6H₂O solution to recrystallize as ZHN. Increasing the aging temperature improved the crystallinity of layered structure of ZHN, showing a maximum at 85 °C. The formed ZHN was hexagonal plate-like particles. The particle size was dependent of the crystallinity of layered structure of ZHN. The specific surface area of ZHN was decreased on elevating the aging temperature, showing a minimum at 85 °C. The adsorption of H₂O and CO₂ was enhanced on increasing the crystallinity of layered structure of ZHN, meaning that these molecules are adsorbed not only on particle surface but also in interlayer of ZHN. These facts infer that the preferred orientation of plate-like ZHN particles leads to the formation of compact rust layer on galvanized steel and to the enhancement of corrosion resistance.     

Structural and microstructural behaviour of SnO2 dense ceramics doped with ZnO and WO3

SnO₂-based varistors doped with ZnO and WO₃ were prepared by mixed oxide method. Experimental evidence shows that the increase in ZnO amount increases the volume and microstrain of unit cell while the WO₃ promotes a decrease. The effect of ZnO and WO₃ additives could be explained by the substitution of Sn^4 +  by Zn^2 +  and W^6 + . The addition of WO₃ inhibits the grain growth due to the segregation in the grain boundary without influence in the densification of the samples. Besides that, an increase in the electrical resistance of the SnO₂–ZnO–WO₃ system was observed independent of the WO₃ concentration.     

Enhancement in ethanol sensing response by surface activation of ZnO with SnO2

A surface functionalized gas sensing material convincingly giving enhanced response to ethanol is demonstrated by SnO₂ activated ZnO. Zinc oxide was synthesized by a chemical route, deposited on an alumina substrate and activated by tin dioxide obtained by on-site oxidation of tin chloride. The XRD study of samples confirmed wurtzite hexagonal structure of zinc oxide and FESEM investigation revealed that surface of activated ZnO microrods was covered by nanoparticles of tin dioxide. Sensing response of sensing elements activated with different concentrations of tin chloride solution has been investigated. It was found that response to ethanol vapor significantly enhanced (eight times) by surface activation with tin dioxide, which optimized at a concentration of 3 wt.%.     

Preparation of aluminum foil-supported nano-sized ZnO thin films and its photocatalytic degradation to phenol under visible light irradiation

The zinc oxide thin films on aluminum foil have been successfully prepared by sol–gel method with methyl glycol as solvent. The film was characterized by means of XRD, TG, UV–vis, SEM and AFM, which show that the ZnO/Al film is formed by a layer of ZnO nano-sized particles with average diameter of 52.2 nm. Under the initial concentration of 20 mg/L phenol solution (500 mL) and visible light irradiation time of 3 h, more than 40% of the initial phenol was totally mineralized using two pieces of ZnO/Al thin film as photocatalyst with an efficient irradiation area of 400 cm². It is a promising visible light responded photocatalyst for the activation of O₂ at room temperature to degrade organic pollutants.     

New natively textured surface Al-doped ZnO-TCOs for thin film solar cells via magnetron sputtering

Natively textured surface aluminum doped zinc oxide (ZnO:Al) thin films were directly deposited via pulsed direct current (DC) reactive magnetron sputtering on glass substrates. During the reactive sputtering process, the oxygen gas flow rate was varied from 8.5 sccm to 11.0 sccm. The influences of oxygen flow rate on the structural, electrical and optical properties of naturally textured ZnO:Al TCO thin films with milky surface were investigated in detail. Gradual oxygen growth (GOG) technique was developed in the reactive sputtering process for textured ZnO:Al thin films. The light-scattering ability and optical transmittance of the natively textured ZnO:Al TCO thin films can be improved through gradual oxygen growth method while maintaining a low sheet resistance. Typical natively textured ZnO:Al TCO thin film with crater-like surface exhibits low sheet resistance (R_s ～ 4 Ω), high transmittance (T_a > 85%) in visible optical region and high haze value (12.1%).     

Apatite-forming ability and magnetic properties of glass-ceramics containing zinc ferrite and calcium sodium phosphate phases

Fine particles of zinc ferrite (ZnFe₂O₄) and calcium sodium phosphate [NaCaPO₄] were crystallized in bulk x(ZnO, Fe₂O₃)(65?x)SiO₂20(CaO, P₂O₅)15Na₂O (6 ≤ x ≤ 21 mol %) glassy matrix by heat treatment. Initial magnetization curves reveal that samples with x = 6 and 9 mol % zinc–iron oxide exhibit both ferrimagnetic and paramagnetic contributions, whereas, samples with x > 9 mol % zinc–iron oxide exhibit only ferrimagnetic contribution. This observation is supported by the disappearance of the electron paramagnetic resonance (EPR) absorption line centered at g ≈ 4.3 in samples with x > 9 mol % zinc–iron oxide. Apatite-forming ability of the glass-ceramic samples was investigated by examining apatite formation on the surface of the samples treated in simulated body fluid (SBF). Increase in apatite-forming ability was observed with an increase in zinc–iron oxide content. The results obtained have been used to understand the evolution of the apatite surface layer as a function of immersion time in SBF and glass-ceramic composition. A good correlation has also been observed between the magnetic nature of the samples and their apatite-forming ability. These materials are expected to find application as thermo-seeds in hyperthermia treatment of bone cancer.