Synthesis of Ag–ZnO powders by means of a mechanochemical process

Nowadays, Ag–CdO alloys are widely used in electrical contact applications, because of their good electrical and thermal conductivity is as well as high resistance to arc erosion and contact welding. Considering the restricted use of Cd due to its toxicity, it is necessary to find a material that can replace those alloys. The objective of this work was to study the possibility of obtaining an Ag–ZnO alloy from an Ag–Zn solid solution powders by means of a mechanochemical method. The mechanochemical process was carried out in a SPEX 8000D mill, under air and with ethanol as a reaction agent. Based on the results obtained, it can be concluded that an Ag–ZnO alloy with a fine and uniform ZnO distribution in the Ag matrix can be obtained by applying the mechanochemical process for 25 h.     

Nanostructures and luminescence properties of porous ZnO thin films prepared by sol–gel process

ZnO thin films containing nano-sized pores were synthesized on solid substrates through a sol–gel process by accommodating cetyl-trimethyl-ammonium bromide (CTAB) as an organic template in the precursor solution. By X-ray diffraction the resultant ZnO films were found to possess ordered pore arrays forming lamellar structure with the spacing between two adjacent pores being ∼3.0 nm. Photoluminescence measurements indicated that the surfactants effectively passivated the surface defects of the ZnO films responsible for the green emission. Al doping was found to improve not only the lamellar structure of the pore arrays but also the near-band-gap emission intensity while the suppression effect of CTAB on the green emission remained undisturbed. With a proper control of doping level, the optical property as well as the structural integrity can be tailored to augment the potential of ZnO films for the optoelectronics and sensor applications.     

Effect of preheating temperatures on microstructure and optical properties of Na-doped ZnO thin films by sol–gel process

The chemical composition, crystalline structure, surface morphology and photoluminescence spectra of Na-doped ZnO thin films with different heat treatment process were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, atomic force microscopy and a fluorescence spectrometer. The results show that preferred orientation, residual stress, average crystal size and surface morphology of the thin films are strongly determined by the preheating temperature. The effects of preheating temperature on microstructure and surface morphology have been discussed in detail. The photoluminescence spectra show that there are strong violet & UV emission, blue emission and green emission bands. The violet & UV emission is ascribed to the electron transition from the localized level below the conduction band to the valence band. The blue emission is attributed to the electron transition from the shallow donor level of oxygen vacancies to the valence band, and the electron transition from the shallow donor level of interstitial zinc to the valence band. The green emission is assigned to the electron transition from the level of ionized oxygen vacancies to the valence band.     

Optical, electrical and morphological properties of p-type Mn-doped SnO2 nanostructured thin films prepared by sol–gel process

SnO₂ thin films doped with various manganese concentrations were prepared on glass substrates by sol–gel dip coating method. The decomposition procedure of compounds produced by alcoholysis reactions of tin and manganese chlorides was studied by thermogravimetric analysis (TGA). The effects of Mn doping on structural, morphological, electrical and optical properties of prepared films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), Hall effect measurement, Fourier Transform Infrared (FTIR) spectral analysis, UV–Vis spectrophotometry, and photoluminescence (PL) spectroscopy. The results of the X-ray diffraction show that the samples are crystalline with a tetragonal rutile structure and the grain size decreases with increasing the doping concentration. The SEM and AFM images demonstrate that the surface morphology of the films was affected from the manganese incorporation. The Sn_1?x Mn _x O₂ thin films exhibited electrically p-type behavior in doping level above x=0.035 and electrical resistivity increases with increase in Mn doping. The optical transmission spectra show a shift in the position of absorption edge towards higher wavelength (lower energy). The optical constants (refractive index and extinction coefficient) and the film thickness were determined by spectral transmittance and using a numerical approximation method. The oscillator and dispersion energies were calculated using the Wemple–DiDomenico dispersion model. The estimated optical band gap is found to decrease with higher manganese doping. The room-temperature PL measurements illustrate the decrease in intensity of the emission lines when content of Mn is increased in Mn-doped SnO₂ thin films.     

Study of NiCuZn ferrite powders and films prepared by sol gel method

This paper reports that a series of NiCuZn ferrite powders and films are prepared by using sol-gel method.The effects of raw material composition and the calcinate temperature on magnetic properties of them are investigated.The NiCuZn ferrite powders are prepared by the self-propagating high-temperature synthesis method and subsequently heated at 700 C～1000 C.The results show that NiCuZn ferrite powders with single spinel phase can be formed after heat-treating at 750 C.Powders obtained from Ni 0.4 Cu 0.2 Zn 0.4 Fe 1.9 O 4 gel have better magnetic properties than those from gels with other composition.After heat-treating at 900 C for 3 h,coercivity H c and saturation magnetization M s are 9.7 Oe (1 Oe=80 A/m) and 72.4 emu/g,respectively.Different from the powders,NiCuZn films produced on Si (100) from the Ni 0.4 Cu 0.2 Zn 0.4 Fe 2 O 4 gel formed at room temperature possess high properties.When heat-treating condition is around 600 C for 6 min,samples with low H c and high M s will be obtained.The minimal H c is 16.7 Oe and M s is about 300 emu/cm 3.In comparison with the films prepared through long-time heat treating,the films prepared through short heat-treating time exhibits better soft magnetic properties.     

Synthesis of self-light-scattering wrinkle structured ZnO photoanode by sol–gel method for dye-sensitized solar cells

A special morphological zinc oxide (ZnO) photoanode for dye-sensitized solar cell was fabricated by simple sol–gel drop casting technique. This film shows a wrinkled structure resembling the roots of banyan tree, which acts as an effective self scattering layer for harvesting more visible light and offers an easy transport path for photo-injected electrons. These ZnO electrode of low thickness (~5 μm) gained an enhanced short-circuit current density of 6.15 mA/cm², open-circuit voltage of 0.67 V, fill factor of 0.47 and overall conversion efficiency of 1.97 % under 1 sun illumination. This shows a high conversion efficiency and a superior performance than that of ZnO nanoparticle-based photoanode (η ~ 1.13 %) of high thickness (~8 μm).     

Synthesis and characterization of tin oxide (SnO2) nanocrystalline powders by a simple modified sol–gel route

This paper reports the synthesis and characterization of nanocrystalline tin oxide (SnO₂) powders by a simple method using a chitosan–polymer complex solution. To obtain SnO₂ nanocrystalline powders, the precursor was calcined at 500–600 °C in air for 2 h. The phase composition of calcined samples was studied by X-ray diffraction (XRD). The XRD results confirmed the formation of a SnO₂ phase with tetragonal structure. The particle sizes of the powder were found to be 22–23 nm as evaluated by the XRD line broadening method. TEM investigation revealed that the SnO₂ samples consist of crystalline particles of 19–21 nm. The corresponding selected area electron diffraction analysis further confirmed the formation of the tetragonal structure of SnO₂ without any impurity phases. The optical properties of the samples were explored by Fourier transform infrared spectroscopy, optical absorption and Raman studies. The estimated band gaps of the samples were in the range of 3.44–3.73 eV.     

Structural analysis of cobalt titanate nanoparticles obtained by sol–gel process

In this work we report the synthesis of nanocomposites based on nanoparticles of cobalt titanate and titanium dioxide in their anatase crystalline phase by a sol–gel process. The synthesized nanoparticles of titanate vary from 1 to 6 nm in size. They are embedded in the anatase matrix, and they were obtained from TiO₂ monoliths doped with Co²⁺. The formation of cobalt titanate nanoparticles showed a linear dependence on the cobalt concentration. The cobalt titanate nanocrystals are very stable even at temperatures higher than 1000 °C. The crystalline structures of the samples were examined using high-resolution transmission electron microscopy and X-ray diffraction. Molecular simulation methods were utilized for a better understanding and for improving the analytical data interpretation of the experimental results. PACS 61.16.Bg; 79.60.Jv; 61.46.+w; 61.50.Ah     

Structural,optical and photocatalytic properties of (Mg,Al)-codoped ZnO powders prepared by sol–gel method

Structural and optical properties of 1 at % Al-doped Zn_1−xMg_xO (x=0–8%) powders prepared by sol–gel method were systematically investigated by means of X-ray diffraction, scanning electron microscopy, ultraviolet–visible absorbance measurement, photoluminescence and Raman scattering spectra. All the powders retained the hexagonal wurtzite structure of ZnO. The band gap and near band emission energies determined from absorbance and photoluminescence spectra increased linearly with increasing Mg content, respectively, which implied that the Mg worked effectively on ZnO band gap engineering, irrespective of Al codoping. However, according to the PL and Raman scattering studies, for the sample of x=8%, the Al doping efficiency was decreased by higher Mg codoping. On the other hand, the effect of Mg codoping on photocatalytic degradation of methylene orange was explored experimentally. The substitution of Mg ions at Zn sites shifted the conduction band toward higher energies and then enhanced the photocatalytic activity, while the incorporation of interstitial Mg ions and decreased Al doping efficiency for higher Mg doping sample (x=8%) reduced the photocatalytic activity.     

Effect of heat and time-period on the growth of ZnO nanorods by sol–gel technique

Sol–gel routes to metal oxide nanoparticles in organic solvents under exclusion of water have become a versatile alternative to aqueous methods. We focus on the preparation of well-aligned ZnO nanorod arrays using non-aqueous sol–gel synthesis route, where ZnO nanorods arrays have been grown on glass substrates. This work provides a systematic study of controlled morphology and crystallinity of ZnO nanorod arrays. The investigation demonstrates that the synthesis process conditions of ZnO thin film have strong influences on the morphology and crystallinity of the ZnO nanorod arrays grown thereon, where non-aqueous process offers the possibility of better understanding and controlling the reaction pathways on the molecular level, enabling the synthesis of nanomaterials with high crystallinity and well-defined, uniform particle morphologies. Here the annealing temperature plays an important role on the growth of nanostructures of the ZnO grains and nanorod arrays. The scanning electron microscopy (SEM) image shows that the growth of ZnO nanorod arrays are high-quality single crystals growing along the c-axis perpendicular to the substrates. A detailed analysis of the growth characteristics of ZnO nanostructures as functions of growth time is also reported.     

Electrical and optical properties of Sb-doped ZnO thin films synthesized by sol–gel method

Sb-doped ZnO thin films with different values of Sb content （from 0 to 1.1 at.%） are deposited by the sol-gel dip- coating method under different sol concentrations. The effects of Sb-doping content, sol concentration, and annealing ambient on the structural, optical, and electrical properties of ZnO films are investigated. The results of the X-ray diffraction and ultraviolet-visible spectroscopy （UV-VIS） spectrophotometer indicate that each of all the films retains the wurtzite ZnO structure and possesses a preferred orientation along the c axis, with high transmittance （〉 90%） in the visible range. The Hall effect measurements show that the vacuum annealed thin films synthesized in the sol concentration of 0.75 mol/L each have an adjustable n-type electrical conductivity by varying Sb-doping density, and the photoluminescence （PL） spectra revealed that the defect emission （around 450 nm） is predominant. However, the thin films prepared by the sol with a concentration of 0.25 mol/L, despite their poor conductivity, have priority in ultraviolet emission, and the PL peak position shows first a blue-shift and then a red-shift with the increase of the Sb doping content.     

Synthesis and magnetic properties of barium–calcium hexaferrite particles prepared by sol–gel and microemulsion techniques

The preparation of W-type hexaferrite particles with the composition BaCa₂Fe₁₆O₂₇ by microemulsion and a stearic acid sol–gel method with and without surfactant has been investigated at various sintering temperatures. The structural and magnetic characteristics have been studied by X-ray diffraction (XRD), a vibrating sample magnetometer (VSM), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetric (DSC) and Fourier transform infrared (FTIR) techniques. The effect of sintering temperature on the properties of BaCa₂Fe₁₆O₂₇ hexaferrites has been studied. The value of saturation magnetization (M_s) depends on types of surfactant used. The sample prepared in the presence of polyoxyethylene (20) sorbitan monooleat (Tween 80) shows low saturation magnetization (M_s=15.10 emu/g), whereas the other sample prepared in the presence of a surfactant cetyltrimethylammonium bromide (CTAB) exhibits high saturation magnetization (M_s=24.60 emu/g) compared to the normal sample.     

Synthesis and characterization of nanostructured strontium hexaferrite thin films by the sol–gel method

Nanostructured single phase strontium hexaferrite, SrFe₁₂O₁₉, thin films have been synthesized on the (100) silicon substrate using a spin coating sol–gel process. The thin films with various Fe/Sr molar ratios of 8–12 were calcined at different temperatures from 500 to 900 °C. The composition, microstructure and magnetic properties of the SrFe₁₂O₁₉ thin films were characterized using Fourier transform infrared spectroscopy, differential thermal analysis, thermogravimetry, X-ray diffraction, electron microscopy and vibrating sample magnetometer. The results showed that the optimum molar ratio for Fe/Sr was 10 at which the lowest calcination temperature to obtain the single phase strontium hexaferrite thin film was 800 °C. The magnetic measurements revealed that the sample with Fe/Sr molar ratio of 10, exhibited higher saturation magnetization (267.5 emu/cm³) and coercivity (4290 Oe) in comparison with those synthesized under other Fe/Sr molar ratios.     

Temperature dependent structural and optical properties of nanocrystallineCdO thin films deposited by sol–gel process

Nanocrystallites of cadmium oxide (CdO) thin films were deposited by sol–gel dip coating technique on glass and Si substrates. XRD and TEM diffraction patterns confirmed the nanocrystalline cubic CdO phase formation. TEM micrograph of the film revealed the manifestation of nano CdO phase with average particle size lying in the range 1.6–9.3 nm. UV–Vis spectrophotometric measurement showed high transparency (nearly 75% in the wavelength range 500–800 nm) of the film with a direct allowed bandgap lying in the range 2.86–3.69 eV. Particle size has also been calculated from the shift of bandgap with that of bulk value for the films for which the particles sizes are comparable to Bohr exitonic radius. The particle size increases with the increase in annealing temperature and also the intensity of XRD peaks increases which implies that better crystallinity takes place at higher temperature.This revised version was published online in August 2005 with a corrected issue number.     

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.     

Microstructure and electro-optical properties of sol–gel derived Cd-doped ZnO films

The microstructure, and the electrical and optical properties of undoped zinc oxide (ZnO) and cadmium-doped ZnO (CZO) films deposited by a sol–gel method have been investigated. The films have a polycrystalline structure with hexagonal wurtzite ZnO. Scanning electron microscopy (SEM) images indicated that the films have a wrinkle network with uniform size distributions. The elemental analyses of the CZO films were carried out by energy dispersive X-ray analysis. The fundamental absorption edge changed with doping. The optical band gap of the films decreased with Cd dopant. The optical constants of the films such as refractive index, extinction coefficient and dielectric constants changed with Cd dopant. A two-probe method was used to investigate the electrical properties, and the effect of Cd content on the electrical properties was investigated. The electrical conductivity of the films was improved by incorporation of Cd in the ZnO film.     

Fabrication and characterization of pure and Sn/Sb-doped ZnO thin films deposited by sol–gel method

Undoped and doped ZnO thin films were prepared by sol–gel method and deposited on tin-doped indium oxides (ITO) substrate using spin coating technique. The effects of Sn and Sb dopants on structural and optical properties were investigated. The starting material was zinc acetate dihydrate, 2-methoxyethanol was used as solvent and monoethanolamine (MEA) as stabilizer. ZnO films were doped with 2% and 7% Sn and Sb concentrations. Optical measurements show an important effect of Sn and Sb dopants on optical band gap.     

Indium doping effect on properties of ZnO nanoparticles synthesized by sol–gel method

Pure ZnO and indium-doped ZnO(In–ZO) nanoparticles with concentrations of In ranging from 0 to 5% are synthesized by a sol–gel processing technique. The structural and optical properties of ZnO and In–ZO nanoparticles are characterized by different techniques. The structural study confirms the presence of hexagonal wurtzite phase and indicates the incorporation of In~(3+) ions at the Zn~(2+) sites. However, the optical study shows a high absorption in the UV range and an important reflectance in the visible range. The optical band gap of In–ZnO sample varies between 3.16 e V and 3.22 e V. The photoluminescence(PL) analysis reveals that two emission peaks appear: one is located at 381 nm corresponding to the near-band-edge(NBE) and the other is observed in the green region. The aim of this work is to study the effect of indium doping on the structural, morphological, and optical properties of ZnO nanoparticles.     

Molybdenum oxide-organosilane hybrids through sol–gel process

From reactions between tetraethylortosilicate (TEOS) and nitrogen containing organosilanes of general formula (C₂H₅O)₃Si–R; R=–(CH₃)₂NH₂, –(CH₃)₂NH(CH₂)₂NH₂ and –(CH₃)₂NH(CH₂)₂NH(CH₂)₂NH₂, with lamellar molybdenum trioxide (α-MoO₃), four hybrid matrices, named here as MoSil, MoN1, MoN2 and MoN3, respectively, were synthesized, through sol–gel process. The obtained matrices were characterized by elemental analysis, Infrared spectroscopy, thermogravimetry, scanning electron microscopy, X-ray diffraction patterns, surface area measurements and ²⁹Si CPMAS NMR spectroscopy. The organic moiety contents are 1.7, 2.0 and 0.9 mmol g⁻¹ for MoN1, MoN2 and MoN3 matrices, respectively. The measured surface areas are 0.61; 78.12; 1.85; 0.59 and 2.53 m² g⁻¹ for MoO₃, MoSil, MoN1, MoN2 and MoN3 matrices, respectively. Molybdenum oxide exhibts a single mass loss step in TG curve, due to the sublimation of the oxide, starting at 730 °C.The MoSil matrix exhibits a similar TG curve profile, but the thermal degradation takes place at 704 °C. MoN1, MoN2 and MoN3 matrices shows mass loss steps of 20%, 30% and 23%, respectively, associated with the organic moiety. The 2θ values for the 001 diffraction plane were 12.64, 13.20, 12.82, 12.84 and 12.90° for MoO₃, MoSil, MoN1, MoN2 and MoN3 matrices, respectively, indicating that the organic species are at the surface, and not inside the interlayer space.