Influence of post-deposition annealing on the structural and optical properties of ZnO thin films prepared by sol–gel and spin-coating method

Thin films of zinc oxide have been deposited onto (0001) sapphire substrate by sol–gel and spin-coating methods. The XRD pattern showed that the crystallinity of the annealed ZnO films had improved in comparison with that of the as-grown films. Photoluminescence spectra revealed a two-line structure, which is identified in terms of UV emission and defect-related emission. The emission intensity was found to be greatly dependent on heat treatment. Host phonons of ZnO and a shift of the _E2$E_2$ (high) peak from its position have been observed from Raman spectra. The surface morphologies of the film had been improved after annealing was observed from AFM images.     

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.     

Enhanced structural and magnetic properties of microwave sintered Li–Ni–Co ferrites prepared by sol–gel method

The properties of lithium ferrites are very sensitive to chemical composition, synthesis method, and sintering techniques. Li–Ni–Co ferrites with compositional formula Li_(0.45-0.5x)Ni_(0.1)Co_xFe_(2.45-0.5x)O_4, where 0.00 ≤ x ≤ 0.1 in steps of 0.02 were prepared by chemical sol–gel method and sintered by microwave sintering technique. The x-ray diffraction patterns confirmed the formation of single phase with spinel structure in all the samples. The structural parameter viz.lattice constant, crystallite size, and x-ray density for these samples were studied and compared with those measured from samples of similar composition prepared by the sol–gel method and sintered by conventional sintering technique. Enhancement in the magnetic properties like Curie temperature, hysteresis parameters was observed by employing sol–gel synthesis combined with microwave sintering. The results obtained and mechanisms involved are discussed in the paper.     

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.     

Particle size effects on magnetic properties of yttrium iron garnets prepared by a sol–gel method

We present detailed measurements of field—and temperature—dependence of magnetization in nanocrystalline YIG (Y₃Fe₅O₁₂) particles. The fine powders were prepared using sol–gel method. Samples with particle sizes ranging from 45 to 450 nm were obtained. We observe that the saturation magnetization decreases as the particle size is reduced due to enhancement of the surface spin effects. Below a critical diameter D_s≅190 nm, the particles become single domains and the coercive forces reaches a maximum at diameters close to the critical value. As the particle size decreases the coercivity diminishes and at D_p≃35 nm diameters the upper limit of superparamagnetic behavior is reached. A quantitative comparison of temperature and particle size dependence of coercivity shows a satisfactory agreement that is expected for an assembly of randomly oriented particles.     

Influence of drying conditions on the optical and structural properties of sol–gel-derived ZnO nanocrystalline films

Zinc oxide nanothin films were prepared on glass substrate by sol–gel dip-coating method using zinc acetate dihydrate, methanol, and monoethanolamine as precursor, solvent, and stabilizer, respectively. The relationship between drying conditions and the characteristics of ZnO nanocrystalline films (c-axis orientation, grain size, roughness and optical properties) was studied. The films were dried in an oven at different temperatures and by IR radiation. Then, the films were annealed at 500°C in a furnace. The chemical composition, transmission spectra, structure, and morphology of the samples were studied using infrared (IR) and UV–visible spectroscopy, X-ray diffraction (XRD), and atomic force microscopy (AFM), respectively. The XRD results show that the drying conditions affect the orientation of crystallization along the (0 0 2) plane. AFM images show that the thicknesses of the films decrease from 128 to 93 nm by changing the drying conditions. The photoluminescence (PL) of ZnO nanothin films shows the UV emission at near band edge and broad green radiation at about 465 nm wavelength.     

Characterization,electrical conduction and stability of Yb-doped barium cerate prepared by sol–gel method

Ceramics powder of BaCe_0.95Yb_0.05O_2.975 was successfully prepared by sol–gel method. Thermogravimetric analysis showed that the decomposition of the dried powder was completed at 1,000 °C. Three strongly exothermic peaks observed in differential thermogravimetric signal indicated three major stages of weight loss in the sample. The high crystallinity of sample with orthorhombic structure was confirmed by X-ray diffraction. The loose particles size obtained from scanning electron microscope was in the range of 65–100 nm, which is almost in the same range as that observed in particle size distribution. The sample showed a dc conductivity of ~1.3 × 10⁻⁴ S cm⁻¹ at 650 °C and the activation energy, E _a, was found to be 1.4 eV. Result of chemical stability test showed that the compound was unstable in atmosphere containing pure carbon dioxide.     

Influence of Ag doping on structural and optical properties of ZnO thin films synthesized by the sol–gel technique

Thin films of Ag–ZnO samples deposited on glass substrates with a different percentage of Ag content (1, 2, and 3 at%) were synthesized, at room temperature, by a dip-coating sol-gel method. The obtained samples are hexagonal wurtzite structure. The average grain size of deposits is about 5 nm. Up to 3 at%, c-axis lattice parameter shifts toward a higher value, which indicates that silver atoms replace Zn atoms in the crystal lattice. As shown by the DRX spectra, growth rate in the (101) direction is favored by the presence of silver ions in the ZnO. The layers present a homogeneous crystallites distribution, as we can remark it on SEM micrographs and exhibit a very low roughness according to AFM images. The entire samples exhibit a transmission value greater than 80 %, in the visible region, while the maximum is obtained for those doped at 2 at%. Energy band varies between 3.15 eV and 3.25 eV. The wider gap obtained is that of the ZnO layer doped with 2 at%. It is worth noting a strong UV emission observed on PL spectrum, performed at very low temperature (liquid nitrogen temperature), for silver doped ZnO compared to that of pure ZnO.     

Effect of calcination atmosphere on photoluminescence properties of nanocrystalline ZrO2 thin films prepared by sol–gel dip coating method

Highly transparent and homogeneous nanocrystalline ZrO₂ thin films were prepared by the sol–gel dip coating method. The X-ray diffraction (XRD) pattern of ZrO₂ thin films calcined in air, O₂ or N₂ shows the formation of tetragonal phase with varying crystallite size. X-ray photoelectron spectroscopy (XPS) gives Zr 3d and O 1s spectra of thin film annealed in air, which reveal zirconium suboxide component (ZrO_x, 0<x<2), Zr–O bond and surface defects. An average transmittance greater than 85% (in UV–vis region) is observed in all calcined samples. Photoluminescence (PL) reveals an intense emission peak at 379 nm and weak peaks at 294, 586 and 754 nm for ZrO₂ film calcined in air. An enhancement of PL intensity and red-shift is observed in films calcined in O₂ and N₂ atmosphere. This is due to the reconstruction of zirconium nanocrystal interfaces and vacancies, which help passivate the non-radiative defects. The oxygen deficient defect, which is due to the distorted Zr–O bond, is suggested to be responsible for photoluminescence. The defect states in the nanocrystalline zirconia thin films play an important role in the energy transfer process. The luminescence defects in the film make it suitable for gas sensors development and tunable lasers.     

Effects of calcining temperature on structural and magnetic properties of nanosized Fe-doped NiO prepared by diol-based sol−gel process

Iron-doped nickel oxide (Fe_0.01Ni_0.99O, abbreviated as FNO) nanoparticles were prepared by sol–gel process using 1,3-propanediol as a solvent and also as a chelating agent, and calcined at the various temperatures (400–1000 °C) for 2 h. The phase composition and the microstructure of the calcined products were investigated by X-ray diffraction and scanning electron microscopy techniques, respectively. Magnetic properties were measured at room temperature using a vibrating sample magnetometer. All calcined samples showed the single phase of FNO cubic rock-salt structure without the presence of any impurity phases. The crystallite size from XRD and particle size from SEM increased as calcining temperature increased. The FNO powders calcined at 400?600 °C revealed the uniform and dense spherical particles in nanosize. The room-temperature ferromagnetism was observed for all samples. When the calcining temperature was increased, the saturation magnetization decreased whereas the coercivity increased, corresponding to the less dense and larger particles. The calcined sample at 400 °C had the best magnetic properties with the highest M_s of 5.34 emu/g (at 10 kOe) and the lowest H_c of 372 Oe.     

Sol–gel auto-combustion synthesis,structural and enhanced magnetic properties of Ni substituted nanocrystalline Mg–Zn spinel ferrite

Nanocrystalline arrays of Ni²⁺ substituted Mg–Zn spinel ferrite having a generic formula Mg_0.7−xNi_xZn_0.3Fe₂O₄ (x=0.0, 0.2, 0.4 and 0.6) were successfully synthesized by sol–gel auto-combustion technique. The fuel used in the synthesis process was citric acid and the metal nitrate-to-citric acid ratio was taken as 1:3. The phase, crystal structure and morphology of Mg–Ni–Zn ferrites were investigated by X-ray diffraction, scanning electron microscopy, and Fourier transformer infrared spectroscopy techniques. The lattice constant, crystallite size, porosity and cation distribution were determined from the X-ray diffraction data method. The FTIR spectroscopy is used to deduce the structural investigation and redistribution of cations between octahedral and tetrahedral sites of Mg–Ni–Zn spinel structured material. Morphological investigation suggests the formation of grain growth as the Ni²⁺ content x increases. The saturation magnetization and magneton number were determined from hysteresis loop technique. The saturation magnetization increases with increasing Ni²⁺ concentration ‘x’ in Mg–Zn ferrite.     

Structural studies on the yttrium-doped cobalt ferrite powders synthesized by sol–gel combustion method

Y_0.2CoFe_1.8O₄ nanopowders were prepared using a sol–gel combustion method. Metal nitrates, such as yttrium nitrate, cobalt nitrate and ferric nitrate, were used as the source materials. Citric acid and polyvinyl alcohol were used as the burning agent and agglomeration reducing agent, respectively. The pH of the precursor was maintained at 7. The mean crystallite size of the prepared ferrite was in the range of ∼20–70 nm. The inverse spinel structure, cubic morphology, and the identification of functional groups of the yttrium-doped cobalt ferrite were analyzed systematically using several analytical tools.     

Effects of Cd concentration on structure and optical properties of the ternary Zn1−xCdxO nanopowder prepared by sol–gel method

Zn_1−xCd_xO nanocrystalline powder with different Cd contents (0≤x≤1) has been prepared by new facile sol–gel route. The crystal structure and optical properties were investigated by X-ray diffraction patterns, Transmission electron microscope, X-ray photoelectron spectroscopy, Photoluminescence. As x varied from x=0 to 0.25, the Zn_1−xCd_xO nanopowder exhibits a hexagonal wurtzite structure of pure ZnO without any significant formation of a separated CdO phase. For the samples with 0.5≤x≤0.85, the Zn_1−xCd_xO nanopowder exhibits the coexistence of hexagonal ZnO and cubic CdO phase, meanwhile, the content of ZnO phase decreases while that of CdO increases with increasing the Cd content x. The ultra-violet near-band-edge emission of the Zn_1−xCd_xO nanopowder was monotonously red-shifted from 389 nm (x=0) to 406 nm (x=0.25) due to the direct modulation of band gap caused by Cd substitution.     

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.     

Enhanced soft magnetic properties of iron powders through coating MnZn ferrite by one-step sol–gel synthesis

The MnZn ferrite coating formed on the surface of iron-based soft magnetic powders via facile and modified sol–gel process has been fabricated to obtain better magnetic performance due to its higher permeability compared with traditional nonmagnetic insulation coatings. The influence of the MnZn ferrite contents on the magnetic performance of the soft magnetic composites(SMCs) has been studied. As the MnZn insulation content increases, the core loss first experiences a decreasing trend that is followed by progressive increase, while the permeability follows an increasing trend and subsequently degrades. The optimized magnetic performance is achieved with 2.0 wt% MnZn ferrite, which results from the decrement of inter-particle eddy current losses based on loss separation. A uniform and compact coating layer composed of MnZn ferrite and oxides with an average thickness of 0.38 ± 0.08 μm is obtained by utilizing ion beam technology, and the interface between the powders and the coating shows satisfied adhesiveness compared with the sample directly prepared by mechanical mixing. The evolution of the coating layers during the calcination process has been presented based on careful analysis of the composition and microstructure.     

Surface properties of palladium catalysts supported on ternary ZrO2–Al2O3–WOx oxides prepared by the sol–gel method: Study of the chemical state of the support

The surface properties of Pd and Pd–Pt catalysts supported on binary ZrO₂–WOx and ternary ZrO₂–Al₂O₃–WOx oxides prepared by the sol–gel method were studied. Special attention was paid to the study of the texture of the catalysts as well as the chemical state of tungstated zirconia and tungstated zirconia promoted with alumina in the palladium catalysts. The catalysts were tested in the isomerization of n-hexane and were characterized by N₂ physisorption, XRD, TPR, Raman spectroscopy, XPS and FT-IR of adsorbed pyridine. The catalysts had bimodal pore size distributions with mesopores in the range 55–70 Å and macropores of 1000 Å in diameter. The catalysts had a surface WOx coverage (4.4–6.0 W nm^?2) lower than that of the theoretical monolayer (7.0 W nm^?2). A lower acidity of the ternary ZrO₂–Al₂O₃–WOx oxide as compared to the binary ZrO₂–WOx oxide was found. Higher activity in the isomerisation of n-hexane was obtained in the Pd–Pt catalysts supported on ternary ZrAlW oxides prepared by sol–gel that is correlated with the coexistence on the surface of W⁴⁺ (WO₂) or W⁰ and W⁶⁺ (Al₂(WO₄)₃) species, ZrO₂ in the tetragonal phase and a high amount of ZrOx suboxides species in a low oxidation state (Zr³⁺ and Zr²⁺).     

Influence of post-deposition annealing on the structural,optical and electrical properties of Li and Mg co-doped ZnO thin films deposited by sol–gel technique

Lithium (Li) and magnesium (Mg) co-doped zinc oxide (ZnO) thin films were deposited by sol–gel method using spin coating technique. The films were deposited on glass substrates and annealed at different temperatures. The effects of annealing temperature on the structural, optical and electrical properties of the deposited films were investigated using X-ray diffraction (XRD), Ultraviolet–Visible absorption spectra (UV–VIS), photoluminescence spectra (PL), X-ray photo electron spectroscopy (XPS) and Hall measurements. XRD patterns indicated that the deposited films had a polycrystalline hexagonal wurtzite structure with preferred (0 0 0 2) orientation. All films were found to exhibit a good transparency in the visible range. Analysis of the absorption edge revealed that the optical band gap energies of the films annealed at different temperatures varies between 3.49 eV and 3.69 eV. Room temperature PL spectra of the deposited films annealed at various temperatures consist of a near band edge emission and visible emission due to the electronic defects, which are related to deep level emissions, such as oxide antisite (O_Zn), interstitial zinc (Zn_i), interstitial oxygen (O_i) and zinc vacancy (V_Zn) which are generated during annealing process. The influence of annealing temperature on the chemical state of the dopants in the film was analysed by XPS spectra. Ion beam analysis (Rutherford back scattering) experiments were performed to evaluate the content of Li and Mg in the films. Hall measurements confirmed the p-type nature of the deposited films.     

Iron-based soft magnetic composites with Mn–Zn ferrite nanoparticles coating obtained by sol–gel method

This paper focuses on iron-based soft magnetic composites which were synthesized by utilizing Mn–Zn ferrite nanoparticles to coat iron powder. The nanocrystalline iron powders, with an average particle diameter of 20 nm, were obtained via the sol–gel method. Scanning electron microscopy, energy dispersive X-ray spectroscopy and distribution maps show that the iron particle surface is covered with a thin layer of Mn–Zn ferrites. Mn–Zn ferrite uniformly coated the surface of the powder particles, resulting in a reduced imaginary permeability, increased electrical resistivity and a higher operating frequency of the synthesized magnets. Mn–Zn ferrite coated samples have higher permeability and lower magnetic loss when compared with the non-magnetic epoxy resin coated compacts. The real part of permeability increases by 33.5% when compared with the epoxy resin coated samples at 10 kHz. The effects of heat treatment temperature on crystalline phase formation and on the magnetic properties of the Mn–Zn ferrite were investigated via X-ray diffraction and a vibrating sample magnetometer. Ferrites decomposed to FeO and MnO after annealing above 400 °C in nitrogen; thus it is the optimum annealing temperature to attain the desired permeability.     

Effect of annealing temperature on nanocrystalline TiO2 thin films prepared by sol–gel dip coating method

Nanocrystalline TiO₂ thin films have been prepared by sol–gel dip coating method. X-ray diffraction results showed the formation of anatase phase TiO₂ with grain size in the range of 18–26 nm. The HRTEM studies show that the average particle size of TiO₂ is 24 nm. The EDX analysis confirmed that Ti and O elements are present in the samples. The optical absorption spectra reveal that the absorption edge shifts towards longer wavelength side with increase in annealing temperature.