Morphologies of Sol–Gel Derived Thin Films of ZnO Using Different Precursor Materials and their Nanostructures

We have shown that the morphological features of the sol–gel derived thin films of ZnO depend strongly on the choice of the precursor materials. In particular, we have used zinc nitrate and zinc acetate as the precursor materials. While the films using zinc acetate showed a smoother topography, those prepared by using zinc nitrate exhibited dendritic character. Both types of films were found to be crystalline in nature. The crystallite dimensions were confined to the nanoscale. The crystallite size of the nanograins in the zinc nitrate derived films has been found to be smaller than the films grown by using zinc acetate as the precursor material. Selected area electron diffraction patterns in the case of both the precursor material has shown the presence of different rings corresponding to different planes of hexagonal ZnO crystal structure. The results have been discussed in terms of the fundamental considerations and basic chemistry governing the growth kinetics of these sol–gel derived ZnO films with both the precursor materials.

Fabrication and Characterization of Pure and Pb-doped ZnO Thin Films Prepared by Sol–Gel and Dip-coeting Method

In this paper, undoped and Pb-doped ZnO thin films have been prepared by sol gel method and deposited on glass substrate using dip-coating technique. The structural, morphological, and optical properties of the films were investigated as a function of Pb doping. The results of the structural tests showed that these films are of a polycrystalline hexagonal structure with a preferred orientation in the (002) direction. The grain size values of Pb-doped films were lower than that of pure ZnO, but the strain and the dislocation density values inecrease with increase Pb doping ratio. The atomic force microscopy (AFM) images showed that the particle size and Root Mean Square (RMS) of ZnO decrease with increasing Pb doping. The optical band gap values were found to increase from (3.19 to 3.30 eV) and the Urbach energy decrease from (322 to 313 meV). PL spectra exhibit an increased amount of defects with increasing Pb, which leads to a red shift in the UV region.

     

Modified Sol–Gel Based Nanostructured Zirconia Thin Film: Preparation,Characterization, Photocatalyst and Corrosion Behavior

In this work, AISI 316L stainless steel was coated by nanostructured zirconia using the sucrose assisted sol–gel dip-coating route. Then, the effect of different calcination temperatures and the thickness of the coating on the corrosion protection of 316L stainless steel was investigated. Here, Zr(acac)₄ and sucrose were used as starting materials and gelation agents, respectively. Thermogravimetry and differential thermal analysis, X-ray powder diffraction (XRD), Fourier transform infrared, scanning electron microscopy and energy dispersive X-ray spectroscopy were used to characterize the coatings. XRD revealed that the pure tetragonal phase of zirconia was obtained at the calcination temperature of 300–500 °C. However, the mixture of monoclinic (m) and tetragonal (t) phase found in the zirconia coating calcined at 650 °C. Also, by increasing the calcination temperature from 300 to 650 °C, the mean of the crystallite size of structures was increased from 7 to 27 nm. AFM result show that the average roughness value of the sample calcined at 300 °C is 10.5 nm and the dimensions of the particles on the surface of this sample smaller than 50 nm. The potentiodynamic polarization and electrochemical impedance spectroscopy results revealed that the as-synthesized nanostructured sol–gel zirconia coatings exhibited a barrier property for the protection of the substrate. However, the highest corrosion resistance was obtained by the zirconia coating calcined at 300 °C. This was as a result of the desirable compromise of good adhesion, low defect density, and high barrier behaviour. Furthermore, zirconia nanoparticles were synthesized by calcination of the gel at the different temperature. The photocatalytic activity of samples was tested for degradation of methyl orange solutions. It is found that ZrO₂ nanoparticles calcined at 500 °C have higher photocatalytic activity than the other samples under UV light.     

Preparation of Highly Adhesive and Superhydrophobic Epoxy-Based Thin Film by Sol–Gel Process

In this study the preparation of a superhydrophobic epoxy-based thin film with excellent high adhesion properties was carried out by mixing epoxy polymer solution, MTMOS solution, and silica powder. It was found that the adhesion between the film and a substrate could be improved by adding PET fibers to the above solution. The characteristic properties of the as-prepared films were analyzed by contact angle measurements, scanning electron microscopy (SEM) and by atomic force microscopy (AFM). The adhesion between the film and the substrate was estimated by the cross-cut method. The experimental parameters were: the mole fraction of MTMOS, weight fraction of silica powder, weight fraction of PET fibers, and the curing temperature. The result indicated that the contact angle and the sliding angle of the hybrid film were 153° and 4°, respectively, and the adhesion test result was very good (5B degree), while the mole fraction of MTMOS was 0.4, the silica powder concentration was 30 wt%, and the PET fibers concentration was 0.15 wt%, with the curing temperature in the range of 130–180°C.     

Preparation of Nano-TiO2/Diatomite Composites by Non-hydrolytic Sol–Gel Process and its Application in Photocatalytic Degradation of Crystal Violet

Silicon - The dispersion of anatase TiO2 on diatomic material was a prospective route to avoid agglomerates of these particles. In this work, the TiO2/diatomite composites were prepared using a...     

An Amalgam of Mg-Doped TiO2 Nanoparticles Prepared by Sol–Gel Method for Effective Antimicrobial and Photocatalytic Activity

In this study, undoped and Magnesium doped TiO₂ nanoparticles (Mg-TiO₂ NPs) are successfully synthesized via a simple sol–gel method cost-effectively. The prepared Mg- TiO₂ NPs is characterized by UV–Vis, FTIR, PL, XRD, FESEM, TEM, and EDAX. UV–Visible Spectroscopy showed that an increase in the optical bandgap concerning the concentration of dopant Mg increases. The bandgap values were found to be 3.57–3.54 eV. FTIR spectra shows that the presence of the characteristic stretching and bending vibrational band of Ti–O bonding at 468 cm^?1 and shifts in vibrational bands were observed for Mg-TiO₂ NPs. PL spectra of Mg- TiO₂ NPs at different concentrations exhibit a strong UV emission band. X-ray diffraction confirmed the formation of the tetragonal anatase phase. The average crystallite size of synthesized samples was found to be 22–19 nm. The average crystallite size of Mg- TiO₂ NPs decreases with increasing the concentration of dopant Mg. The FESEM and TEM analysis confirmed that the spherical morphology for both TiO₂ and Mg-TiO₂ NPs. SAED pattern confirms the crystalline nature of prepared samples. EDAX spectra confirm the presence of Ti, O, and Mg and confirm that Mg²⁺ ions are present in the TiO₂ lattices. The prepared samples were investigated against gram-positive and gram-negative bacteria. The prepared samples exhibit potent antibacterial activity against gram-negative bacteria than the gram-positive bacteria. The prepared samples exhibit significant photocatalytic degradation for Methylene blue (MB).

     

Electrochemical Sensor for Detection of Trichlorfon Based on Molecularly Imprinted Sol–Gel Films Modified Glassy Carbon Electrode

Thin films of molecularly imprinted sol–gel polymer with specific binding sites for trichlorfon were prepared, fixed on glassy carbon electrodes and used as recognition material. The binding characteristic of the imprinted films to trichlorfon was evaluated by equilibrium binding experiments; and, the morphology was studied by scanning electronic microscope. A novel electrochemical sensor for determination of trichlorfon was developed based on the reaction between trichlorfon and the molecularly imprinted sol–gel film, which was a modified glassy carbon electrode. The sensor displayed excellent selectivity and high sensitivity. The linear response range of the sensor was 10⁻⁸ –10⁻⁶ g mL⁻¹, and the limit of detection was 2.8 × 10⁻⁹ g mL⁻¹. The relative standard deviation for the determination of 10⁻⁷ g mL⁻¹ trichlorfon was 3.5%. The sensor was applied to the determination of trichlorfon in vegetables with satisfactory results.     

Sol–Gel Assisted Preparation of Chromia–Silica Catalysts for Non-Oxidative Dehydrogenation of Propane

Preparation of continuous silica gel in the presence of dissolved Cr(NO₃)₃ leads to a hard high surface area (710 m²/g) microporous xerogel. Formation of the gel in the pore structure of mesoporous Pore-Expanded MCM-41 (PE-MCM-41) and macroporous commercial Cab–O–Sil silica results in retention of the mesoporous structure in the case of PE-MCM-41, and the formation of a powder with a broad pore size distribution in the case of Cab–O–Sil silica. Comparison of the catalytic activities in non-oxidative dehydrogenation of propane revealed a linear correlation of the initial conversion with the surface area for all three samples. The sample prepared from PE-MCM-41 through a sol–gel assisted procedure was the most active, particularly with respect to the catalysts prepared by simple wet impregnation with chromium nitrate.     

Using the Sol–Gel Technology for the Treatment of Barley Seeds

Silica sols obtained by acidic or alkaline hydrolysis of tetraethoxysilane in an excess of water or ethanol in the presence of a number of salts and/or acids are used to treat the surface of barley seeds. The surface state and the elemental composition of the seeds are studied before and after their treatment in silica sols. The conditions of the sol–gel synthesis of silica sols, their effect on the state and chemical composition of the seed surface, and the sowing characteristics are analyzed. The plant’s resistance to phytopathogen, the causative agent of root rot is studied.     

Methods and Approaches of the Sol–Gel Technology for the Surface Modification of Aluminum Oxide Powders

The results of studies, sol–gel synthesis, and the sedimentation stability of complex multicomponent sol–gel systems of the “silica sol modified with Co(NO₃)₂ · 6H₂O, Al(NO₃)₃ · 9H₂O with α-Al₂O₃ or γ-Al₂O₃ as highly dispersed filler” type are generalized. The physical–chemical processes accompanying the formation of modifying layers on the powder oxide particles are examined. The promising prospects of applying α-Al₂O₃ powders modified with a silicate layer of the composition (wt %) 1.2K₂O · 3Al₂O₃ · 3.2CaO · 12.5Na₂O · 28.1B₂O₃ · 52SiO₂ in the fabrication of ceramic materials with improved strength characteristics are demonstrated.     

Sol–Gel Pd Exhaust Catalysts and Hydrocarbon Speciation

Sol–gel Pd/alumina promoted by oxygen-storing CeO₂ or CeO₂–Tb₄O₇ catalysts has higher hydrocarbon oxidation activity than commercial three-way catalysts. It is active in hydrocarbon (and CO) oxidation even under net reducing conditions albeit over short periods of time. This observation is relevant to cold start conditions. Cryo-focussing GCMS and pulse RGA experiments suggest that mechanistically interesting by-product hydrocarbon species evolve from the catalysts under just these conditions, even when the fuel is LPG in type. Further catalyst developments and analytical refinements are likely to go hand in hand as the mode of operation of these environmental catalysts is better understood from their by-product fingerprint.     

Sol–Gel Aluminum Hydroxides and Their Thermal Transformation Studies for the Production of α-Alumina

This work reports the formation of α-alumina from pseudoboehmite synthesized from three different hydrated inorganic aluminum salts such as aluminum nitrate, aluminum chloride and aluminum sulfate using the sol–gel method in aqueous medium at 80 °C. All the aluminum hydroxides were thermally treated and all showed similar crystalline conversion behavior; and, their solid-phase transformations to aluminum oxides were investigated. Following the synthesis, all products were characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry–thermogravimetric analysis and X-ray diffraction. The hydrolysis products were calcined at 200, 300, 600, 800, 1100 and 1200 °C for 1-h. The eta (η) and theta (θ) transitional aluminas were detected until complete transformation to highly crystalline α-alumina occurred at ~1200 °C. Moreover, starting at 1100 °C the sample derived from the sulfate salt showed intense crystalline peaks corresponding to α-alumina. The morphological study for the samples of α-alumina calcined at 1200 °C was carried out by field emission scanning electron microscopy where a vermicular structure was observed. These α-alumina samples were also analyzed by high resolution-transmission electron microscopy. In addition, fast Fourier transform and selected area electron diffraction patterns of α-alumina samples calcined at the highest temperature were obtained to calculate the experimental interplanar distances whose values were compared to reported theoretical values.     

Preparation of Thermally Stable Mesostructured Nano-sized TiO2 Particles by Modified Sol–Gel Method Using Ionic Liquid

The mesoporous anatase form of TiO₂ was prepared by modified sol–gel method using ionic liquid as a template agent. The prepared nanosize TiO₂ particle was characterized by N₂-physisorption, XRD, TEM, and SEM. The physical properties of prepared TiO₂ particles were compared with that prepared by conventional sol–gel method without template. It has been proved that the anatase phase prepared by modified sol–gel process using ionic liquid was preserved well even if the TiO₂ samples were treated at high temperatures up to 800 °C while those prepared by conventional sol–gel method were transformed from anatase to rutile phase gradually during calcinations at 600 °C. Moreover, there was no phase transition in the sample obtained by sol–gel method with ionic liquid in spite of prolonged calcination for 60 h at 600 °C. However, in case of those samples prepared by conventional sol–gel method, the portion of rutile form was continuously increased with the increase in the calcination period.     

Electrostatic Spray Deposition of Copper–Indium Thin Films

Electrostatic spray deposition is an innovative coating technique that produces fine, uniform, self-dispersive (due to Coulombic repulsion), and highly wettable, atomized droplets. Copper–indium salts are dissolved in an alcohol-based solvent; this precursor is then electrostatically sprayed onto a moderately heated, molybdenum-coated substrate. Precursor flowrates range from 0.02 to 5 mL/h under applied voltages of 1–18 kV, yielding droplet sizes around a few hundred nanometers. Comparing scanning electron microscope images of the coated samples showed that the substrate temperature, applied voltage, and precursor flowrate were the primary parameters controlling coating quality. Also, the most stable electrostatic spray mode that reliably produced uniform and fine droplets was the cone-jet mode with a Taylor cone issuing from the nozzle.     

Non-hydrolytic Sol–Gel Preparation of Silver Alumina Based Catalysts for the HC-SCR of NOx

The preparation of Ag/Al₂O₃ catalysts by nonhydrolytic sol–gel process leads to highly efficient HC-deNOx materials thanks to the silver ability to diffuse toward the surface. The presence of niobium as co-catalyst, with a Nb content comprised between 1 and 3 wt%, enhances the NO reduction efficiency at low temperatures (<250 °C).     

Effect of Zr–Al Co-Doping on Structure and Photocatalytic Performance of ZnO Photocatalyst

利用水热处理结合焙烧的方法分别制备了Zr、Al掺杂及Zr–Al共掺的ZnO光催化剂。研究了制备的光催化剂样品的相结构和光谱性能;以紫外光（λ=254nm）为光源,酸性橙Ⅱ为降解对象,进行光催化活性测试;考察了Zr、Al掺杂对ZnO光催化剂反应活性的影响。研究表明,制备的产物均为六方晶系纤锌矿结构的ZnO;Zr、Al掺杂及Zr–Al共掺的ZnO样品的光催化活性相对于纯ZnO均有较大程度的提高,而且Zr–Al共掺的ZnO的光催化性能明显优于单一掺杂的。Zr–Al共掺可以明显改善ZnO表面状态,使ZnO具有更丰富的表面羟基,同时可以抑制光生电子–空穴对的复合,从而有利于光催化活性和稳定性的提高。     

Co/SiO2 Sol–Gel Catalysts for Fischer–Tropsch Synthesis

Six catalysts with a different cobalt content were prepared following the sol–gel method. The samples were tested by the Fischer–Tropsch synthesis performed both at low and high temperature and pressure. All the catalytic performances are well correlated with the characterization results which highlighted the good metal distribution and the presence of a large amount of metallic cobalt (but not the whole) on the surface of both 10 and 30% Co catalysts. As a result, high CO conversions were observed with a particular sensitivity to the reaction pressure and also the limitation of the produced hydrocarbons fraction to C₆ or C₉ at low or high pressure, respectively.