Influence of pH on ZnO nanocrystalline thin films prepared by sol–gel dip coating method

ZnO nanocrystalline thin films have been prepared on glass substrates by sol?Cgel dip coating method. ZnO thin films have been coated at room temperature and at four different pH values of 4, 6, 8 and 10. The X-ray diffraction pattern showed that ZnO nanocrystalline thin films are of hexagonal structure and the grain size was found to be in the range of 25?C45?nm. Scanning electron microscopic images show that the surface morphology improves with increase of pH values. TEM analysis reveals formation of ZnO nanocrystalline with an average grain size of 44?nm. The compositional analysis results show that Zn and O are present in the sample. Optical band studies show that the films are highly transparent and exhibit a direct bandgap. The bandgap has been found to lie in the range of 3 $\boldsymbol\cdot$ 14?C3 $\boldsymbol\cdot$ 32?eV depending on pH suggesting the formation of ZnO nanocrystalline thin films.     

Microstructure,electrical and humidity sensing properties of TiO<Subscript>2</Subscript>/polyaniline nanocomposite films prepared by sol–gel spin coating technique

High sensitive resistive type humidity sensor based titanium oxide/polyaniline (TiO₂/PANI) nanocomposite thin films prepared by a sol–gel spin coating technique on an alumina substrate. The resultant nanocomposites were characterized by using X-ray diffraction (XRD), Field emission electron microscopy, Fourier transform infrared spectroscopy (FTIR), UV–Vis absorbance and energy dispersive spectra analysis. In the XRD patterns of both pure and TiO₂/PANI composite confirms the deposition of PANI on TiO₂ and the average size of the composite particle was found to be 32 nm. Large number of nano grain surface being covered by PANI, which agrees very well with the results obtained by XRD studies. FTIR and UV–Vis spectra reveal that the PANI component undergoes an electronic structure modification as a result of the TiO₂ and PANI interaction. The room temperature resistivity was found to be for TiO₂ and TiO₂/PANI nanocomposite films 1.42?×?10⁶ and 2.56?×?10³ Ω cm respectively. The obtained TiO₂/PANI nanocomposites sensor exhibited higher humidity sensing performance such as high sensitivity, fast response (20 s) and recovery time (15 s) and high stability.     

Structure and electrical properties of CuAlO<Subscript>2</Subscript> thin films derived by sol–gel processing

CuAlO₂ (CAO) thin films were prepared on quartz glass substrates by sol–gel spin-coating method. The effects of annealing temperatures, concentrations of sols and Al/Cu atomic ratios on structure, morphology and electrical properties have been investigated. It was found that CAO film with an Al/Cu atomic ratio of 0.8 approximately and the total metallic ion concentration of 0.7 M after heat treatment at 750 °C for 3 h in argon gas flow of 450 mL/min exhibited the lowest room temperature resistivity of 13.5 Ωcm.     

Microstructure,dielectric and photoluminescence properties of Tm-doped Ba<Subscript>0.8</Subscript>Sr<Subscript>0.2</Subscript>TiO<Subscript>3 </Subscript>thin films fabricated by sol–gel method

Ba_0.8Sr_0.2TiO₃ thin films doped by Tm from 0 to 7 mol% were fabricated by sol–gel method on silicon and Pt/Ti/SiO₂/Si substrates. X-ray diffraction, scanning electron microscopy, and Raman spectroscopy have been used to study variations of crystal structure, surface morphologies, and phase stability of Tm-doped BST films, respectively. The residual stress in BST films on silicon substrates can be reduced by Tm doping, as demonstrated by the blueshift of phonon peaks in Raman spectra. The dielectric measurements were conducted on metal-insulator-metal capacitors at the frequency from 1 kHz to 1 MHz. The grain size and dielectric constant decreased with increasing Tm concentration. While the variation of dielectric loss, tunability and the figure of merit were nonlinear with increasing Tm concentration. In addition, the photoluminescence property of 0.2 mol% Tm-doped BST was also studied. The effect of Tm doping on the microstructure, dielectric and photoluminescence properties were analyzed.     

The effect of repeated annealing temperature on the structural,optical, and electrical properties of TiO<Subscript>2</Subscript> thin films prepared by dip-coating sol–gel method

In this study, we have studied the effect of repeated annealing temperatures on TiO₂ thin films prepared by dip-coating sol–gel method onto the glasses and silicon substrates. The TiO₂ thin films coated samples were repeatedly annealed in the air at temperatures 100, 200, and 300 °C for 5 min period. The dipping processes were repeated 5 to 10 times in order to increase the thickness of the films and then the TiO₂ thin films were annealed at a fixed temperature of 500 °C for 1 h period. The effect of repeated annealing temperature on the TiO₂ thin films prepared on glass substrate were investigated by means of UV–VIS spectroscopy, X-ray diffraction (XRD), and atomic force microscopy (AFM). It was observed that the thickness, average crystallite size, and average grain size of TiO₂ samples decreased with increasing pre-heating temperature. On the other hand, thickness, average crystallite size, and average grain size of TiO₂ films were increased with increasing number of the layer. Al/TiO₂/p-Si metal–insulator–semiconductor (MIS) structures were obtained from the films prepared on p-type single silicon wafer substrate. Capacitance–voltage (C–V) and conductance–voltage (G/ω–V) measurements of the prepared MIS structures were conducted at room temperature. Series resistance (R _s) and oxide capacitance (C _ox) of each structures were determined by means of the C–V curves.     

Piezoelectric BNT-BT<Subscript>0.11</Subscript> thin films processed by sol–gel technique

0.89(Na_0.5Bi_0.5)TiO₃–0.11BaTiO₃, (BNT-BT_0.11) thin film was fabricated by sol–gel/spin coating process, on platinized silicon wafer. Perovskite structure with random orientation of crystallites has been obtained at 700 °C. Piezoelectric activity of BNT-BT_0.11 thin film was detected using piezoresponse force microscopy (PFM). Effective piezoelectric coefficient d _33eff of such film, recorded at 5 V applied dc voltage, was ~29 pm/V, which is similar to other BNT-BT _x thin films. The complex refractive index and dielectric function of BNT-BT_0.11 thin films were also investigated. The high leakage current density significantly influences the dielectric, ferroelectric, and piezoelectric properties of the BNT-BT_0.11 films.     

Effect of V substitution on microstructure and ferroelectric properties of Bi<Subscript>3.6</Subscript>Ho<Subscript>0.4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by sol–gel method

Bi_3.6Ho_0.4Ti₃O₁₂ and (Bi_0.9Ho_0.1)_4−x/3Ti_3−x V _x O₁₂ (BHTV) (x = 0.3, 1.2, 3.0 and 6.0%) thin films were prepared on Pt/Ti/SiO₂/Si substrates by sol–gel method. The effect of V content on their microstructure and ferroelectric properties were investigated. All the BHTV samples consisted of the single phase of Bi-layered Aurivillius phase. The B-site substitution with high-valent cation of V⁵⁺, in Bi_3.6Ho_0.4Ti₃O₁₂ films, enhanced the remanent polarizations (2P_r) and reduced the coercive field (2E_c). The BHTV film with x = 0.3% exhibited the better electrical properties with 2P_r 45.5 μC/cm², 2E_c 257 kV/cm, good insulting behavior, as well as the fatigue-free characteristic.     

Synthesis and piezoelectric properties of (Na<Subscript>0.5</Subscript>Bi<Subscript>0.5</Subscript>)<Subscript>0.94</Subscript>Ba<Subscript>0.06</Subscript>TiO<Subscript>3</Subscript> ceramics prepared by sol–gel auto-combustion method

In this study, NaNO₃, Bi(NO₃)₃·5H₂O, Ba(NO₃)₂, Ti(OC₄H₉)₄ and citric acid were successfully introduced to fabricate lead-free piezoelectric (Na_0.5Bi_0.5)_0.94Ba_0.06TiO₃ [NBBT] nanopartical powders by a novel modified sol–gel auto-combustion method. The resultant products were characterized by the X-ray diffraction analysis and transmission electron microscope method. (Na_0.5Bi_0.5)_0.94Ba_0.06TiO₃ + Mn(NO₃)₂ [NBBTM] can be sintered by the traditional solid-state reaction, and the effects of NBBT doped different amounts of Mn(NO₃)₂ at various sintering temperatures upon phase formation, microstructure as well as piezoelectric properties were further studied. The experimental results show that it was helpful to control their chemical ingredients and microstructure to prepare nanocrystalline single phase NBBT powders. Where is the X-ray diffraction result of the corresponding ceramics to prove the existence of the mixing between rhombohedral and tetragonal phases at the MPB compositions. Doping 0.015 mol% Mn(NO₃)₂ into NBBT at 1,090 °C, piezoelectric constant (d ₃₃) and relative dielectric constant (ε_r) reach the superior value of 159pC/N and 1,304, respectively, and dielectric loss (tan δ) and electromechanical coupling factor (K _t) are 2.5% and 65%, respectively.     

Structure,morphology, photocatalytic and antibacterial activities of ZnO thin films prepared by sol–gel dip-coating method

ZnO thin films were deposited on soda lime glass substrates by the sol–gel dip-coating method with variations of the initial Zn²⁺ concentrations. Various techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM) were used to investigate the effects of the initial Zn²⁺ concentrations on the structure, and surface morphology and topography of the prepared films. All prepared ZnO thin films showed a high transparency of over 88% in the visible region. The particle size increased with an increased initial Zn²⁺ concentration. This also reduced the surface denseness and the energy band gap of the ZnO thin films. All the prepared films showed photocatalytic properties through photodegradation of the methylene blue (MB) dye. The ZnO thin film prepared from the 0.1 M Zn²⁺ concentration showed the greatest efficiency as it had the highest surface area because of its greatest surface roughness. Furthermore, the prepared ZnO thin film showed antibacterial activities against the Escherichia coli bacterium.     

New insights in photo-patterned sol–gel-derived TiO<Subscript>2</Subscript> films

Specific sol–gel formulations and protocols have been adapted to the fine patterning of TiO₂ films using a very simplified UVA three-step lithography method. Mechanisms occurring during the photo-patterning procedure and a post-patterning thermal treatment have been studied by Fourier transform infrared spectroscopy, atomic force microscopy, X-ray diffraction, and ellipsometry. Discussions are proposed to support the influence of the photo-patterning procedure and post-patterning treatment on the shape and the dimension of so-formed microstructures. Original additional functionalities arising from such structures are also presented.     

Study on structural,optical and electrical properties of CdO and Cd<Subscript>0.98</Subscript>Al<Subscript>0.02</Subscript>O films prepared by innovative sol–gel screen-printing method

In present work for the first time we report the synthesis and characterization of pure CdO and Cd_0.98Al_0.02O films by innovative sol–gel screen-printing technique. The prepared films were characterized for their structural, morphological, optical and electrical properties. XRD studies reveals the polycrystalline nature of the films, exhibiting cubic structure with preferred orientation of grains along (111) plane. SEM image of CdO and Cd_0.98Al_0.02O indicates that surface of the films were uniformly covered and have smooth surface area on the entire film. EDAX analysis confirms the presence of Cd, O, Al along with some impurities as films were prepared on glass substrate. A UV–Visible spectroscopy confirms the direct band gap of 2.53 eV for CdO and 2.51 eV for Cd_0.98Al_0.02O films. The refractive index for the Cd_0.98Al_0.02O films firstly increases and then decreases with photon energy. The emission features of pure CdO and Cd_0.98Al_0.02O films were studied through PL spectra. Semiconducting nature of films was confirmed by the DC electrical conductivity measurement via standard two-probe method.     

Facile synthesis and characterization of CdTiO<Subscript>3</Subscript> nanoparticles by Pechini sol–gel method

In this work, CdTiO₃ nanoparticles were synthesized through reaction between Cd(CH₃COO)₂.2H₂O, Ti(OC₄H₉)₄, trimesic acid as a new chelating agent and ethanol as solvent by Pechini sol–gel method. X-ray diffraction (XRD) patterns showed that CdTiO₃ nanostructures have rhombohedral structure with diameter of about 35.61 nm. The structure, morphology and size of CdTiO₃ nanoparticles were characterized by FT-IR, XRD, SEM and EDAX. The optical properties of the products were studied by DRS. Based on the results of experiments, it was found that temperature and time of calcination, pH and the solvent of reaction are important parameters for formation of CdTiO₃ nanoparticles. Utilizing trimesic acid (benzene-1,3,5-tricarboxylic acid) as a new chelating agent for preparation of CdTiO₃ nanostructures was initiative of this work.     

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.     

Crystallographic and magnetic properties of Fe-doped SnO<Subscript>2</Subscript> nanopowders obtained by a sol–gel method

We prepared Sn_1?x Fe _x O₂ (x = 0, 0.03, 0.05, 0.10, and 1.0) nanoparticles by the polymeric precursor method based on the modified Pechini process. Two types of starting reactants for both tin and iron were explored: Sn(II)/Fe(II) and Sn(IV)/Fe(III) precursors. Thermogravimetric analysis revealed that the precursor powders prepared from Sn(IV) have higher excess in ethylene glycol in comparison to precursor samples prepared from Sn(II). XRD patterns for those samples prepared from Sn(IV) and Fe(III) were adequately fitted by introducing only the cassiterite phase of SnO₂. Micro-Raman spectra also support these findings, and additionally it is found that the presence of iron broadened and reduced the intensities of the principal bands. ¹¹⁹Sn Mössbauer spectra indicated only the presence of Sn⁴⁺, whereas RT ⁵⁷Fe Mössbauer spectra suggested the presence of two Fe³⁺ sites located at different distorted sites. On the other hand, micro-Raman and ⁵⁷Mössbauer spectrometry showed the formation of hematite as impurity phase for those samples with iron concentrations above ~5 at.%, prepared from Fe(II) and Sn(II) precursors. In addition, their XRD patterns revealed larger average grain sizes for the cassiterite phase of SnO₂ in comparison to those samples prepared from Sn(IV) and Fe(III).     

Synthesis and characterization of TiO<Subscript>2</Subscript>–NiO and TiO<Subscript>2</Subscript>–WO<Subscript>3</Subscript> nanocomposites

TiO₂–NiO and TiO₂–WO₃ nanocomposites were prepared by hydrothermal and surface modification methods. The samples were analyzed using X-ray diffraction, Scanning Electron Microscope images, Transmission Electron Microscope, Energy dispersive analysis, Zeta potential, Electrophoretic mobility and Photocatalysis activity measurement. XRD data sets of TiO₂–NiO, TiO₂–WO₃ powder nanocomposite have been studied for the inclusion of NiO, WO₃ on the anatase-rutile mixture phase of TiO₂ by Rietveld refinement. The cell parameters, phase fraction, the average grain size, strain and bond lengths between atoms of individual phases have been reported in the present work. Shifted positional co-ordinates of individual atoms in each phase have also been observed.     

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.     

Dielectric properties of Erbium doped CaCu<Subscript>3</Subscript>Ti<Subscript>4</Subscript>O<Subscript>12</Subscript> prepared by sol–gel self combustion method

The dielectric properties of Erbium doped CaCu₃Ti_(4–x)Er_xO_(12–δ) with x = 0, 0.05, 0.1 were synthesized by the sol–gel self combustion method. XRD (X-ray powder diffraction) analysis confirmed the formation of single-phase material in the samples calcined at 800 °C. Crystal structure does not change on doping with Erbium and it remains cubic in all the three compositions studied. It is found that lattice parameter increases slightly with Erbium doping. The surface morphology of CaCu₃Ti_(4–x)Er_xO_(12–δ) powders sintered at 950 °C in air for 3 h was observed using high resolution—scanning electron microscope and it shows that the grain size is in the range of 1–8 μm for these samples. Energy dispersive X-ray spectroscopy pattern confirmed the presence of Erbium with 1.9 and 4.86 atomic percentages with doping concentration. The dielectric characteristics of CaCu₃Ti_(4–x)Er_xO_(12–δ) were studied by LCR meter in the frequency range (100 Hz–1 MHz) at various temperatures (RT to 500 °C). Interestingly, the dielectric constant increases and dielectric loss had lower values than those of undoped CCTO.     

Optical properties and electrical resistivity of boron-doped ZnO thin films grown by sol–gel dip-coating method

Sol–gel dip-coating was used to grow ZnO thin films doped with various concentrations of B ranging from 0 to 2.5 at.% on quartz substrates. The effects of B doping on the absorption coefficient (α), optical band gap (E_g), Urbach energy (E_U), refractive index (n), refractive index at infinite wavelength (n_∞), extinction coefficient (k), single-oscillator energy (E_o), dispersion energy (E_d), average oscillator strength (S_o), average oscillator wavelength (λ_o), moments M₋₁ and M₋₃, dielectric constant (ε), optical conductivity (σ), and electrical resistivity (ρ) of the BZO thin films were investigated. The transmittance spectra of the ZnO and BZO thin films show that the transmittance of the BZO thin films was significantly higher than that of the ZnO thin films in the visible region of the spectrum and that the absorption edge of the BZO thin films was blue-shifted. The BZO thin films exhibited higher E_g, E_U, and E_o and lower E_d, λ_o, M₋₁ and M₋₃ moments, S_o, n_∞, and ρ than the ZnO thin films.