Growth of ZnO nanorod forests and characterization of ZnO-coated nylon fibers

ZnO nanorod forests were grown wrapping nylon fibers using a two-step process. In the first step, the formation of ZnO seeds at nylon fiber surfaces was induced by the dip coating of ZnO nanosols; in the second step, the growth of the ZnO seeds into nanorod forests was carried out via a wet chemical route in a bath containing an equimolar solution of zinc nitrate hexahydrate and hexamethylenetetramine. The as-obtained ZnO-coated nylon fibers were characterized by scanning electron microscopy, Energy dispersive X-ray spectrum imaging, and X-ray diffraction, respectively. Thermal gravimetric analysis of the pristine and the ZnO-coated nylon fibers was also conducted.     

Superhydrophobic properties of cotton fabrics functionalized with ZnO by electroless deposition

Cotton fabrics were coated with arrays of ZnO hexagonal prisms using an electroless (catalytic/autocatalytic) deposition process. A typical three step method, similar to those used for electroless deposition of metals on insulating substrates, consisting of pre-activation, activation and deposition steps was employed. The low-dimensional ZnO particles were grown from an aqueous solution containing zinc nitrate as source of zinc ions and dimethylamineborane as reducing agent. The as-obtained ZnO-coated cotton fabrics were characterized from the point of view of structure by X-ray diffraction (XRD) and morphology by scanning electron microscopy (SEM). The XRD studies demonstrate that the ZnO particles have a hexagonal wurtzite crystalline structure. The SEM observations prove that the cotton fibers are homogeneously covered by hexagonal prisms which have uniform base size of approximately 500 nm and height of 1 μm. Optical spectroscopy measurements show that the functionalization with ZnO strongly decreases the transmittance in the UV–vis region of the cotton fabrics. An important characteristic is that the ZnO-functionalized cotton fabrics exhibit superhydrophobicity, with water contact angles exceeding 150°. The technique described is highly reproducible, easy scalable and cheap, allowing a wide range of applications.     

Facile synthesis of ZnO hollow fibres

In this paper, cotton fibres were used as bio-template to successfully synthesize new ceramic materials, ZnO hollow fibres and in an effort to explore the synthesis condition, and simplify the synthesis procedure. In this synthesis, a direct thermal decomposition of zinc acetate dihydrate coated on the surface of cotton fibres was explored. The wall porosity of the ZnO hollow fibres was controlled by changing the concentration of zinc acetate aqueous solution.     

Rapid growth of thick particulate film of crystalline ZnO in an aqueous solution

Thick particulate films of crystalline ZnO were developed in an aqueous solution. ZnO crystallized in the solution of zinc nitrate hexahydrate and ethylenediamine at 60 °C. ZnO crystalline particles were then gradually deposited on a glass substrate to form thick particulate films. The thick films were constructed of multi-needle ZnO particles having an ultrafine surface relief structure, and thus had high specific surface area. The thick films can be applied to dye-sensitized solar cells supported by low-heat-resistant polymer films.     

Electron field emission characteristics of different surface morphologies of ZnO nanostructures coated on carbon nanotubes

The optimal carbon nanotube (CNT) bundles with a hexagonal arrangement were synthesized using thermal chemical vapor deposition (TCVD). To enhance the electron field emission characteristics of the pristine CNTs, the zinc oxide (ZnO) nanostructures coated on CNT bundles using another TCVD technique. Transmission electron microscopy (TEM) images showed that the ZnO nanostructures were grown onto the CNT surface uniformly, and the surface morphology of ZnO nanostructures varied with the distance between the CNT bundle and the zinc acetate. The results of field emissions showed that the ZnO nanostructures grown onto the CNTs could improve the electron field emission characteristics. The enhancement of field emission characteristics was attributed to the increase of emission sites formed by the nanostructures of ZnO grown onto the CNT surface, and each ZnO nanostructure could be regarded as an individual field emission site. In addition, ZnO-coated CNT bundles exhibited a good emission uniformity and stable current density. These results demonstrated that ZnO-coated CNTs is a promising field emitter material.     

Fabrication of ZnO nanowhiskers array film by forced-hydrolysis-initiated-nucleation technique using various templates

ZnO nanowhiskers array films were successfully fabricated using an aqueous solution deposition at 88 °C based on the forced-hydrolysis-initiated-nucleation technique of a template layer. Several zinc salts template layers (anhydrous zinc acetate, layered hydroxide zinc acetate, fibrous monohydrate zinc hydroxonitrate, and two types of layered hydroxide zinc nitrate) were investigated. In-situ forced hydrolysis of low-solubility zinc salts to ZnO nanocrystals at an initial stage promoted homoepitaxial growth of ZnO nanowhiskers array by heterogeneous nucleation on the substrate surface, which were clarified by XRD and FE–SEM. ZnO nanowhiskers array film was successfully fabricated on the low heat-resistant plastic substrate by this technique.     

Effect of precursor on epitaxially grown of ZnO thin film on p-GaN/sapphire (0 0 0 1) substrate by hydrothermal technique

Single crystalline ZnO thin film on p-GaN/sapphire (0 0 0 1) substrate, using two different precursors by hydrothermal route at a temperature of 90 °C were successfully grown. The effect of starting precursor on crystalline nature, surface morphology and optical emission of the films were studied. ZnO thin films were grown in aqueous solution of zinc acetate and zinc nitrate. X-ray diffraction analysis revealed that all the thin films were single crystalline in nature and exhibited wurtzite symmetry and c-axis orientation. The thin films obtained with zinc nitrate had a more pitted rough surface morphology compared to the film grown in zinc acetate. However the thickness of the films remained unaffected by the nature of the starting precursor. Sharp luminescence peaks were observed from the thin films almost at identical energies but deep level emission was slightly prominent for the thin film grown in zinc nitrate.     

Photocatalytic self-cleaning properties of cellulosic fibers modified by nano-sized zinc oxide

Nano-sized zinc oxide was synthesized and deposited onto cellulosic fibers using the sol-gel process at ambient temperature. The prepared materials were characterized using several techniques including scanning electron microscopy, transmission electron microscopy, diffuse reflectance spectroscopy, X-ray diffraction and thermogravimetric analysis. X-ray diffraction studies of the ZnO-coated fiber indicate formation of the hexagonal crystal phase which was satisfactory crystallized on the fiber surface. The electron micrographs show formation of zinc oxide nanoparticles within 10-15 nm in size which have been homogeneously dispersed on the fiber surface. The prepared materials show significant photocatalytic self-cleaning activity, which was monitored by diffuse reflectance spectroscopy. The photoactivity was studied upon measuring the photodegradation of methylene blue and eosin yellowish under UV-Vis irradiation. The photocatalytic activity of the treated fabrics was fully maintained performing several cycles of photodegradation.     

Fabrication of TiO2/Tin-doped indium oxide-based photoelectrode coated with overlayer materials and its photoelectrochemical behavior

The photoelectrochemical properties of TiO2-based photoelectrodes with metal oxide overlayers (e.g., ZnO, ZrO2, MgO, and Al2O3) were investigated. The metal oxides were deposited on TiO2/tin-doped indium oxide (ITO) films by spin-coating metal-alkoxide precursors. The formation of the overlayers was confirmed by energy dispersive X-ray spectroscopy (EDS) and high resolution transmission electron microscopy (HRTEM). Each overlayers were well-coated on the TiO2-based films and have approximately 2 nm thickness. The prepared films were used as photoanodes in a photoelectrochemical system with a Pt counter electrode to evaluate hydrogen production performance. Comparing with other overlayers, the ZnO-coated photoelectrode exhibits the highest rate of hydrogen evolution and which is better than the uncoated one. From the photoelectrochemical and spectroscopic study, the superior hydrogen production property of the ZnO-coated TiO2 photoelectrode was attributed to both the higher light absorbance of ZnO compared to TiO2 and the formation of hydroxyl groups at the ZnO surface.     

Low temperature growth and optical properties of ZnO nanowires using an aqueous solution method

ZnO nanowires were grown on indium tin oxide (ITO) coated glass substrates at a low temperature of 90 degrees C using an aqueous solution method. The ZnO seeds were coated on the ITO thin films by using a spin coater. ZnO nanowires were formed in an aqueous solution containing zinc nitrate hexahydrate (Zn(NO3)2 x 6H2O) and hexamethylenetetramine (C6H12N4). The pH value and concentration of the solution play an important role in the growth and morphologies of ZnO nanowires. The size of ZnO naonowires increased as the concentration of the solution increased. It was formed with a top surface of hexagonal and tapered shape at low and high pH values respectively. Additionally, the single crystalline structure and optical property of the ZnO nanowires were investigated using high-resolution transmission electron microscopy and photoluminescence spectroscopy.     

Cathodic electrodeposition of nanoporous ZnO thin films from new electrochemical bath and their photoinduced hydrophilic properties

The cathodic electrodeposition of nanocrystalline zinc oxide (ZnO) thin films from an aqueous zinc acetate containing electrochemical bath is reported. Scanning electron microscopic examination of the resultant films reveals the formation of nanoporous ZnO. X-ray diffraction (XRD) analysis indicates that the ZnO thin films deposited with crystallite sizes as small as 10 nm are possible with this method. The surface wettability of the electrodeposited ZnO thin films was also investigated. Reversible hydrophobicity to super-hydrophilicity transition was observed and nicely controlled by alternation of UV light irradiation and dark storage.     

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.     

A comparative study on the NO2 gas sensing properties of ZnO thin films, nanowires and nanorods

ZnO thin films were fabricated using the spin coating method, ZnO nanowires by cathodically induced sol-gel deposition by the means of an anodic aluminum oxide (AAO) template, and ZnO nanorods with the hydrothermal technique. For thin film preparation, a clear, homogeneous and stable ZnO solution was prepared by the sol-gel method using zinc acetate (ZnAc) precursor which was then coated on a glass substrate with a spin coater. Vertically aligned ZnO nanowires which were approximately 65 nm in diameter and 10 μm in length were grown in an AAO template by applying a cathodic voltage in aqueous zinc nitrate solution at room temperature. For fabrication of the ZnO nanorods, the sol-gel ZnO solution was coated on glass substrate by spin coating as a seed layer. Then ZnO nanorods were grown in zinc nitrate and hexamthylenetetramine aqueous solution. The ZnO nanorods are approximately 30 nm in diameter and 500 nm in length. The ZnO thin film, ZnO nanowires and nanorods were characterized by X-ray diffraction (XRD) analysis and scanning electron microscope (SEM). The NO₂ gas sensing properties of ZnO thin films, nanowires and nanorods were investigated in a dark chamber at 200 °C in the concentration range of 100 ppb-10 ppm. It was found that the response times of both ZnO thin films and ZnO nanorods were approximately 30 s, and the sensor response was depended on shape and size of ZnO nanostructures and electrode configurations.     

Influence of precursor source on sol–gel deposited ZnO thin films properties

Zinc oxide thin films were deposited by sol gel technique on glass substrates using different precursors (zinc acetate, zinc nitrate and zinc chloride). In the present work we investigate the precursor nature influence on structural, morphological, optical, electrical properties and photocatalytic activity of ZnO thin films. For this purpose we have used X-rays diffraction (XRD), atomic force microscopy (AFM), UV–visible spectroscopy and Hall effect measurements for films characterization. The obtained results indicated that ZnO films properties are strongly influenced by the nature of the used precursor as reactant. Films photocatalytic activity was evaluated by the photo-degradation of methylene blue (MB) dissolved in aqueous solution under UV-A light. The obtained results indicated that ZnO thin films prepared from zinc acetate are more efficient than those prepared from zinc nitrate and zinc chloride.     

Growth and characterization of electrosynthesised zinc oxide thin films

Zinc oxide (ZnO) films have been electrodeposited from an aqueous solution containing 0.1 M zinc nitrate as the electrolyte with pH around 5±0.1. The deposition was carried out by galvanostatic reduction with an applied cathodic current density in the range between 5 and 20 mA cm⁻². The influence of bath composition on the preparation of ZnO films is studied. The effects of zinc nitrate concentration and cathodic current density on the deposition rate of ZnO films were also studied. An optimum current density of 10 mA cm⁻² is identified for the growth of ZnO film with improved crystallinity and optical transmittance. The crystalline structure of the deposits studied by X-ray diffraction reveals the possibility of growing hexagonal ZnO films under suitable electrochemical conditions. The surface morphological studies by scanning electron micrographs revealed the presence of nodular appearance for films deposited at 800 °C bath temperatures.     

SiO2/TiO2 multilayer films grown on cotton fibers surface at low temperature by a novel two-step process

A novel two-step process was developed to synthesize and deposit SiO₂/TiO₂ multilayer films onto the cotton fibers. In the first step, SiO₂ particles on cotton fiber surface were synthesized via tetraethoxysilane hydrolysis in the presence of cotton fibers, in order to protect the fibers against photo-catalytic decomposition by TiO₂ nanoparticles. In the second step, the growth of TiO₂ nanoparticles into the modified cotton fiber surface was carried out via a sol-gel method at the temperature as low as 100 °C. The as-obtained SiO₂/TiO₂ multilayer films coated on cotton fibers were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, atomic force microscopy and X-ray diffraction, respectively.     

Growth and characterisation of electrodeposited ZnO thin films

The electrochemical method has been used to deposit zinc oxide (ZnO) thin films from aqueous zinc nitrate solution at 80 °C onto fluorine doped tin oxide (FTO) coated glass substrates. ZnO thin films were grown between − 0.900 and − 1.025 V vs Ag/AgCl as established by voltammogram. Characterisation of ZnO films was carried out for both as-deposited and annealed films in order to study the effect of annealing. Structural analysis of the ZnO films was performed using X-ray diffraction, which showed polycrystalline films of hexagonal phase with (002) preferential orientation. Atomic force microscopy was used to study the surface morphology. Optical studies identified the bandgap to be ∼ 3.20 eV and refractive index to 2.35. The photoelectrochemical cell signal indicated that the films had n-type electrical conductivity and current-voltage measurements showed the glass/FTO/ZnO/Au devices exhibit rectifying properties. The thickness of the ZnO films was found to be 0.40 μm as measured using the Talysurf instrument, after deposition for 3 min. Environmental scanning electron microscopy was used to view the cross-section of glass/FTO/ZnO layers.     

Low-temperature crystallization of oriented ZnO film using seed layers prepared by sol–gel method

Transparent zinc oxide (ZnO) films were coated on seed layers prepared by the sol–gel method by chemical solution deposition method. Firstly, seed layers were prepared from zinc acetate and monoethanolamine, 2-methoxyethanol by the sol–gel method on a silicon substrate or a slide glass. Next, the substrate coated with a seed layer was immersed in zinc nitride solution with hexamethylenetetramine, and ZnO films were obtained. The transmittance of the ZnO films depended on the morphology and crystallinity of the seed layers. When the seed layer were dried on a hot plate, the seed layer had flat surface and transparent ZnO film could be obtained on the seed layers dried at temperatures above 200 °C. When the seed layer was prepared from zinc acetate dihydrate dried in a petri dish, the seed layer were smooth without cracks and the transparent ZnO films were obtained at temperature below 100 °C.     

Fabrication and characterization of tetrapod-like ZnO nanostructures prepared by catalyst-free thermal evaporation

Tetrapod-like ZnO nanostructures were fabricated on ZnO-coated sapphire (001) substrates by two steps: pulsed laser deposition (PLD) and catalyst-free thermal evaporation process. First, the ZnO films were pre-deposited on sapphire (001) substrates by PLD. Then the ZnO nanostructures grew on ZnO-coated sapphire (001) substrate by the simple thermal evaporation of the metallic zinc powder at 900 °C in the air without any catalysts. The pre-deposited ZnO films by PLD on the substrates can provide growing sites for the ZnO nanostructures. The as-synthesized ZnO nanostructures were characterized by using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectrum (FTIR). The results show that the tetrapod-like ZnO nanostructures are highly crystalline with the wurtzite hexagonal structure. Photoluminescence (PL) spectrum of as-synthesized nanostructures exhibits a UV emission peak at ～ 389 nm and a broad green emission peak at ～ 513 nm. In addition, the growth mechanism of ZnO nanostructures is also briefly discussed.     

Influence of ammonia, lithium hydroxide, and hexamine on ZnO films synthesized by successive ionic layer adsorption and reaction technique

Various nanostructured zinc oxide (ZnO) films have been developed on non-seeded soda-lime glass substrates by successive ionic layer adsorption and reaction (SILAR) method, employing different baths of aqueous zinc sulfate solution using complexing agents of ammonia, lithium hydroxide, and hexamine. Influence of complexing agents on the structural, morphological, chemical compositional, optical and electrical properties of the films were investigated and compared among and with the samples annealed at 400 °C. Role of complexing agents on the growth process was discussed. X-ray diffraction analysis revealed that the ZnO films were polycrystalline dominating with (100), (002), and (101) oriented crystallites of hexagonal wurtzite structure. The lattice constants, c/a ratio, internal relaxation parameter, anion–cation (Zn–O) bond length, and the tetrahedral angles of ZnO films were determined. Cauliflower, flower, and flower-like nanorod morphologies of the films from the respective baths were exposed by scanning electron microscopic studies. Optical analysis of all films except that prepared from hexamine showed low absorbance and a higher transmittance 70–85 % in the entire visible region. Resistivity of annealed films was one order of magnitude lower than that of the as-grown films. We demonstrated utility of SILAR as an efficient single step soft chemical route for obtaining high-quality crystalline ZnO films having high-specific surface area on non-seeded substrates.