Annealing effect on the characteristics of La0.67Sr0.33MnO3 polycrystalline thin films produced by the sol–gel dip-coating process

The effect of annealing temperature on selected characteristics of polycrystalline La_0.67Sr_0.33MnO₃ films, which have been produced on quartz substrates, was investigated. X-Ray powder diffraction patterns showed that the phase formation started at 873 K and all the films had perovskite structure. By increasing the annealing temperature, the lattice parameters were decreased. Scanning electron microscope indicated that the film thicknesses were approximately 3 μm and the average grain size of the samples varied between 30–100, 50–110, 70–120, and 100–150 nm for films annealed at 873, 973, 1,073, and 1,173 K, respectively. All the films showed a paramagnetic–ferromagnetic (T_C) and metal–insulator (T_IM) phase transition. The T_C indicated a small variation [from 131 K (S4) to 124 K (S1)] as a function of annealing temperature, whereas the T_IM went down from 212 K (S4) to 110 K (S1), a strong decrease of 102 K. A colossal magneto resistance with magneto resistance ratios of 130, 139, 156, and 163% were observed near T_C and at 6 T magnetic field.     

Effect of annealing temperature on electrical and nano-structural properties of sol–gel derived ZnO thin films

Zinc oxide (ZnO) thin films have been prepared on silicon substrates by sol–gel spin coating technique with spinning speed of 3,000 rpm. The films were annealed at different temperatures from 200 to 500 °C and found that ZnO films exhibit different nanostructures at different annealing temperatures. The X-ray diffraction (XRD) results showed that the ZnO films convert from amorphous to polycrystalline phase after annealing at 400 °C. The metal oxide semiconductor (MOS) capacitors were fabricated using ZnO films deposited on pre-cleaned silicon (100) substrates and electrical properties such as current versus voltage (I–V) and capacitance versus voltage (C–V) characteristics were studied. The electrical resistivity decreased with increasing annealing temperature. The oxide capacitance was measured at different annealing temperatures and different signal frequencies. The dielectric constant and the loss factor (tanδ) were increased with increase of annealing temperature.     

Influence of annealing temperature and oxygen atmosphere on the optical and photoluminescence properties of BaTiO3 amorphous thin films prepared by sol–gel method

Homogeneous and transparent BaTiO₃ thin films were prepared by sol–gel dip coating method. The prepared BaTiO₃ thin films were annealed in air and O₂ atmosphere at different temperatures. The annealed BaTiO₃ thin films were amorphous in nature. Scanning electron microscopy (SEM) revealed the nucleation and particle growth on the films. Energy-dispersive X-ray (EDX) analysis data revealed the adsorption of oxygen atoms in the BaTiO₃ film. The direct energy band gap was found to vary (3.84–3.58 eV) as functions of annealing atmosphere and temperature. Photoluminescence (PL) revealed intense emission peaks at 393 and 675 nm. Quenching of PL intensity was observed in films annealed at high temperature and in O₂ atmosphere. This is due to reduction in the oxygen vacancy by the adsorption of oxygen in the film. Luminescence spectra also have been related to the results obtained by SEM and EDX analysis. The change in luminescence intensity of BaTiO₃ thin films makes it suitable for optoelectronic temperature sensor applications.     

Effect of temperature on dielectric and electrical properties of Co–Zr doped barium hexaferrites prepared by sol–gel method

In the present research, temperature dependence of dielectric properties of cobalt–zirconium substituted barium hexaferrites, fabricated using citric acid sol gel method, has been reported. The dielectric constant, loss tangent and A.C. conductivity were investigated on the circular pellets in temperature range 30–350 °C and frequency range 10 kHz–1 MHz using impedance analyzer. This paper also presents impedance (Z*) and electric modulus (M*) analysis of all the samples. The single semi-circular arcs, observed in impedance Nyquist plots, suggest the dominance of grain boundaries in the conduction process. Dielectric constant and dielectric loss tangent show very small variation up to 200–250 °C temperature and abrupt increase afterwards up to 350 °C. Thus, these ferrites can be successfully implemented in the practical applications like capacitors, microwave devices etc. up to 250 °C, without any significant change in properties.     

Effect of stabilizer on optical and structural properties of MgO thin films prepared by sol–gel method

The effects of monoethanolamine (MEA) and acetylacetone (ACAC) addition as stabilizer on the crystallization behaviour, morphology and optical properties of magnesium oxide were investigated using thermogravimetry (TG/DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible, photoluminescence (PL) and Fourier transform infrared (FTIR) spectroscopy. Stabilizer addition reduces transparency of the films. MgO films prepared at 500 °C showed weak orientation of (200). However, the films prepared by addition of stabilizer are amorphous. MgO powders were prepared for exhibiting the structural properties. The patterns of MgO powders showed a preferred orientation of (200). The addition of stabilizer causes a reduction in grain size. SEM micrographs show that a homogenous and crack-free film can be prepared at 500 °C and addition of stabilizer causes an increase in packing density.     

Effect of concentration and temperature on the properties of the microspheres prepared using an emulsion–solvent extraction process

Methylaluminoaxane (MAO) microspheres of average size smaller than 100 μm were prepared using a solvent extraction process; excess of perfluorocarbon (PFC) was added to the hydrocarbon-in-perfluorocarbon emulsion to solidify the MAO droplets. The effect of the MAO concentration in the dispersed phase, the temperature of the PFC added to the emulsion and the preparation temperature on the size, the size distribution and the morphology of the MAO microspheres was studied. MAO droplets broke up more easily with decreasing dispersed phase viscosity and hence the size of the MAO microspheres decreased. The temperature of the PFC added to the emulsion did not significantly affect the size and the morphology of the MAO microspheres. The size of the MAO microspheres increased with increasing preparation temperature. The main reason for the increased size of the MAO microspheres was the increased coalescence with increasing preparation temperature. In addition the porosity of the MAO microspheres increased with increasing preparation temperature.     

Effect of Zn doping on structure and ferroelectric properties of PST thin films prepared by sol–gel method

(Pb _y Sr_1−y )Zn _x Ti_1−x O_3−x thin films were prepared on ITO/glass substrate by sol–gel process using dip-coating method. The phase structure, morphology and ferroelectric property of the thin film were studied. All the thin films show the typical perovskite phase structure. Both the crystallinity and c/a ratio of the perovskite phase increases initially and then decreases gradually with doping Zn in the thin film. Ferroelectric properties of the Zn-doped PST thin films, including ferroelectric hysteresis-loop, remnant polarization and coercive force, decrease gradually with increasing Zn. And the effect of Zn on ferroelectric properties is more obvious in PST thin film with high content of Pb than that with low Pb although the high lead thin film exhibits high intrinsic ferroelectric properties.     

Influence of annealing temperature on the structural,topographical and optical properties of sol–gel derived ZnO thin films

This investigation deals with the effect of annealing temperature on the structural, topographical and optical properties of Zinc Oxide thin films prepared by sol–gel method. The structural properties were studied using X-ray diffraction and the recorded patterns indicated that all the films had a preferred orientation along (002) plane and the crystallinity along with the grain size were augmented with annealing temperature. The topographical modification of the films due to heat treatment was probed by atomic force microscopy which revealed that annealing roughened the surface of the film. The optical properties were examined by a UV–visible spectrophotometer which exhibited that maximum transmittance reached nearly 90% and it diminished with increasing annealing temperature.     

Effect of solution concentration on the structural, optical and conductive properties of ZnO thin films prepared by sol–gel method

ZnO thin films with different solution concentrations (0.1–0.9 mol/L) were prepared by a simple sol–gel dip-coating technique. X-ray diffraction, ultraviolet–visible spectroscopy, Hall effect measurements and photoluminescence (PL) spectroscopy were employed to investigate the effect of solution concentration on the structural,optical and electrical conductive properties of the ZnO thin films. The results showed that the ZnO thin films preferentially oriented along the (002) direction at higher solution concentration. The careful study of the optical and electrical conductive properties showed that the resistivity decreased monotonously, while the transmittance increased first and then decreased when solution concentrations changed from 0.1 to 0.9 mol/L. Photoluminescence spectra indicated that the defect-related blue emission was increased with the enhancement of solution concentration. The mechanism of the blue emission, and the reasons why high solution concentration was favorable for forming high c-axis oriented ZnO thin films and obtaining low resistivity were also discussed in detail.     

Effect of functional groups on condensation and properties of sol–gel silica nanoparticles prepared by direct synthesis from organoalkoxysilanes

Silsesquioxane nanoparticles were synthesized from organotrialkoxysilanes in ethanol/water medium by a two-step hydrolysis–condensation process. Regular shaped spheres functionalized by vinyl, methyl, ethyl, phenyl, amyl, octyl, 3-aminopropyl groups were obtained, with sizes in the range 100–400 nm. The integrity of the organic functional groups and the condensation degree of the silsesquioxane networks were detected by multinuclear solid state Nuclear Magnetic Resonance (NMR). The nanoparticles thermal behavior was studied by thermogravimetric analyses, and N₂ sorption was used to measure the particles porosity. Coatings were obtained from particles suspensions by spin coating technique and the surface properties were studied by contact angle measurements. The emission of Rhodamine 6G doped nanoparticles was analyzed in the visible light region. The fluorescence experiments highlight the influence of the different matrices on amount of dye retained into the network and fluorescence intensity.     

Sol–gel synthesis,characterization and microwave absorbing properties of nano sized spherical particles of La0.8Sr0.2Mn0.8Fe0.2O3

LSMFO (La_0.8Sr_0.2Mn_0.8Fe_0.2O₃) nano sized powders were synthesized by modified EDTA assisted sol–gel synthesis using EDTA:metal ion = 0.5. Another new synthesis method, sol–gel self combustion using PVA, was also devised for the synthesis of LSMFO and the effects of the PVA mole ratio was investigated. The characterization techniques, XRD, FE-SEM, TG/DTA and ICP, confirmed the formation of the pure phase LSMFO by both the methods. The material attained spherical morphology instead of previously reported rod like structure. Sizes of synthesized powders vary from 14.5 nm to 23 nm. TG/DTA results suggest that LSMFO can be synthesized by the self combustion at temperatures as low as 200 °C. Synthesized LSMFO has excellent microwave absorbing properties in the range of 0.05–18 GHz and appreciable effective bandwidth, 2 GHz, with microwave absorption in excess of 10 dB and peak reflection loss of 25 dB which suggests that the materials can be used as effective microwave absorbers.     

Orientation-dependent microwave dielectric properties of Ba0.6Sr0.4TiO3 thin films prepared by sol–gel method

Barium strontium titanate (Ba_0.6Sr_0.4TiO₃, BST) thin films have been prepared on the (100) LaAlO₃ single-crystal substrates by sol–gel technique. The X-ray diffraction study indicated that the thin films exhibited (100) preferred orientation and random orientation depending upon the concentration of precursor solution. The nonlinear dielectric properties of the BST films were measured using an interdigital capacitor. The temperature dependence of dielectric constant of the BST thin films was measured at 1 MHz in the temperature range from ?100 to 80 °C. The Curie temperature T _c of the films derived from 0.1, 0.2 and 0.3 M was found to be ?18.5, ?32.5 and ?39.9 °C, respectively. The tunability of BST films with the (100) preferred orientation was 30.74 %, which was much higher than that of thin films with random orientation at the frequency of 10 kHz with an applied electric field of 80 kV/cm. The microwave dielectric properties of the BST thin films were measured by a vector network analyser from 1 to 10 GHz.     

Influence of Fe dopant concentration and annealing temperature on the structural and optical properties of ZnO thin films deposited by sol–gel method

Nanostructured Fe doped ZnO thin films were deposited onto glass substrates by sol–gel spin coating method. Influence of Fe doping concentration and annealing temperature on the structural, compositional, morphological and optical properties were investigated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV–Vis spectroscopy and photoluminescence (PL) measurements. XRD analysis showed that all the films prepared in this work possessed a hexagonal wurtzite structure and were preferentially oriented along the c-axis. Pure ZnO thin films possessed extensive strain, whereas Fe doped films possessed compressive strain. In the doped films, least value of stress and strain was observed in the 0.5 at.% Fe doped thin film, annealed at 873 K. Average crystallite size was not significantly affected by Fe doping, but it increased from 15.57 to 17.79 nm with increase in annealing temperature from 673 to 873 K. Fe ions are present in +3 oxidation state as revealed by XPS analysis of the 0.5 at.% Fe doped film. Surface morphology is greatly affected by changes in Fe doping concentration and annealing temperature which is evident in the SEM images. The increase in optical band gap from 3.21 to 3.25 eV, with increase in dopant concentration was attributed to Moss–Burstein shift. But increase in annealing temperature from 673 to 873 K caused a decrease in band gap from 3.22 to 3.20 eV. PL spectra showed emissions due to excitonic combinations in the UV region and defect related emissions in the visible region in all the investigated films.     

Enhanced electrical properties of PZT thick films prepared by sol–gel technique through step-by-step crystallization process

[Pb(Zr_xTi_1-x)O₃: PZT] films at morphotropic phase boundary composition (x = 0.52) were deposited on bare Si, ZrO₂/Si and Pt/Ti/SiO₂/Si substrates by sol–gel spin on technique. Films deposited on the bare Si and ZrO₂/Si substrates had low degree of crystallization and micro cracks. Well crystallized films with smooth microstructure were obtained on Pt/Ti/SiO₂/Si substrates. Further, the thickness of the films on Pt/Ti/SiO₂/Si substrate was increased up to ~1 μm by step-by-step crystallization process. The single perovskite phase of the above films was confirmed with X-ray diffraction analysis. Films had enhanced dielectric properties at room temperature and the dielectric constant values were comparable to those of bulk values at Curie temperature (T_c) from the temperature dependent dielectric measurements. Films exhibit higher remnant polarization (P_r) and lower coercive field (E_c) values. Further, capacitance–voltage (C–V), current–voltage (I–V) measurements and rough estimation of piezoelectric coefficient of the films were carried out.     

Effect of solvents on the preparation of lithium aluminate by sol–gel method

γ-Lithium aluminate was prepared by sol–gel method using lithium methoxide and aluminum-sec-butoxide precursors in i-propanol, n- and tert-butanol. Clear gels could be obtained due to the addition of ethylacetoacetate and the dried solids were calcined at 550 and 900 °C. The resulting solids were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), thermo-gravimetric analysis/differential thermal analysis (TGA/DTA). γ-Lithium aluminate with the highest purity was obtained with t-butanol solvent and LiAl₅O₈ was the second major phase.     

Improvement of physical properties of IGZO thin films prepared by excimer laser annealing of sol–gel derived precursor films

Indium gallium zinc oxide (IGZO) transparent semiconductor thin films were prepared by KrF excimer laser annealing of sol–gel derived precursor films. Each as-coated film was dried at 150 °C in air and then annealed using excimer laser irradiation. The influence of laser irradiation energy density on surface conditions, optical transmittances, and electrical properties of laser annealed IGZO thin films were investigated, and the physical properties of the excimer laser annealed (ELA) and the thermally annealed (TA) thin films were compared. Experimental results showed that two kinds of surface morphology resulted from excimer laser annealing. Irradiation with a lower energy density (≤250 mJ cm⁻²) produced wavy and irregular surfaces, while irradiation with a higher energy density (≥350 mJ cm⁻²) produced flat and dense surfaces consisting of uniform nano-sized amorphous particles. The explanation for the differences in surface features and film quality is that using laser irradiation energy to form IGZO thin films improves the film density and removes organic constituents. The dried IGZO sol–gel films irradiated with a laser energy density of 350 mJ/cm² had the best physical properties of all the ELA IGZO thin films. The mean resistivity of the ELA 350 thin films (4.48 × 10³ Ω cm) was lower than that of TA thin films (1.39 × 10⁴ Ω cm), and the average optical transmittance in the visible range (90.2%) of the ELA 350 thin films was slightly higher than that of TA thin films (89.7%).