Preparation and properties of VO2 thin films by a novel sol–gel process

Vanadium dioxide (VO₂) thin films were fabricated using a simple and novel sol–gel process in which V₂O₅ was used as the vanadium source; oxalic acid was used as the reducing agent; and polyvinyl alcohol was used as the film former to control the viscosity of the VO₂ precursor solution and bond vanadium ions. The microstructure and surface morphology of VO₂ films were studied by X-ray diffraction and scanning electron microscopy, respectively. The results showed that using polyvinyl alcohol forms porous nanostructure of VO₂ films with a uniform grain size of ~25 nm. The measured optical reflectance shows well-defined phase transition as observed by an increase of reflectance upon heating above the transition temperature from ~11 to ~30 % at 1,100 nm. Upon cooling, the expected hysteresis is observed.     

Formation of Zn–Al layered double hydroxide thin films intercalated with sulfonated spiropyran

We prepared Zn–Al layered double hydroxide (LDH) thin films intercalated with sulfonated 1,3′,3′-trimethyl-6-nitrospiro[2H-chromene-2,2′-indoline] anions (SP-SO₃ ^?) by immersion of sol–gel derived amorphous Al₂O₃–ZnO thin films in hot water containing SP-SO₃H. Extended interlayer spacing, in comparison to the Zn–Al LDH with carbonate anions, was observed after immersion in distilled water containing SP-SO₃H at 60 °C for 30 min, indicating that we formed Zn–Al LDH films with SP-SO₃ ^? directly on glass substrates. The merocyanine form of SP-SO₃ ^? was shown by UV spectra to have stabilized in the hydroxide layers of LDH.     

Preparation of nanostructured titania thin films by sol–gel technology

This study is concerned with the preparation of hydrolytically active heteroligand complex [Ti(OC₄H₉)_3.61(O₂C₅H₇)_0.39] from titanium butoxide and acetylacetone and with the gel formation kinetics in a solution of this complex upon hydrolysis and polycondensation. Single-layer and double-layer thin films of a solution of this precursor were coated on polished silicon substrates using the dip-coating method. The crystallization of nanostructured titania films during the heat treatment of these xerogel coatings was studied using various protocols; the anatase–rutile phase transition temperature was found to depend on the film thickness. The effects of the precursor solution viscosity on the film thickness and crystallite size were determined.     

Orientation degree dependence of magnetic properties of Co doped ZnO thin films by sol–gel process

Co-doped ZnO films were successfully fabricated on Si substrates by sol–gel process. The effects of Co concentration and preheating temperature on the structure and magnetic properties of the Zn_1−x Co _x O films were systematically studied. The results revealed that the films were highly c-axis oriented and contained no impurity phase. With preheating temperature increasing, the orientation degree of the films decreased. When the Co concentration and oxygen vacancy of the films are almost changeless, the enhancement of ferromagnetism in films originates from the orientation degree of the films increasing.     

Preparation and methodology for chemical mapping of sol–gel thin films containing lysozyme

Sol–gels are seeing widespread interest as suitable materials for the immobilization of biomolecules in applications ranging from optical coatings to specialty biocatalysts. Although there are numerous studies that have characterized these materials in terms of their macroscopic properties, few studies have examined and correlated these properties at the microscopic level. This study describes a spin-coating technique for the preparation of aluminum-supported sol–gel thin films containing immobilized lysozyme [E.C. 3.2.1.17] that are suitable for chemical mapping using FTIR microscopy operating in reflectance mode. This type of information can then be used to understand a variety of aspects of these materials which can be used for optimal engineering of these materials, as well as insightful design and modeling. A data analysis method was developed to extract information on chemical speciation and domain information on the materials from FTIR data matrices. Results from these studies indicated that, contrary to what might be expected, these sol–gels are not homogeneous on the microscopic level. Instead, they are heterogeneous in both the distribution of lysozyme and hydrophobic monomers at the scale investigated (20 μm resolution). The method described here has promise in terms of providing a non-invasive approach of chemically mapping concentrations of proteinaceous and related substances as well as chemical domains in situ in sol–gel thin films.     

Electrochemical performance of Co–Al layered double hydroxide nanosheets mixed with multiwall carbon nanotubes

Regular hexagonal Co–Al layered double hydroxides (Co–Al LDH) were synthesized by urea-induced homogeneous precipitation. This material proved to be nanosheets by scanning electron microscopy and X-ray diffraction measurements. The electrochemical capacitive behavior of the nanosheets in 1 M KOH solution were evaluated by constant current charge/discharge and cyclic voltammetric measurements, showing a large specific capacitance of 192 F·g⁻¹ even at the high current density of 2 A·g⁻¹. When multiwall carbon nanotubes (MWNTs) were mixed with the Co–Al LDH, it was found that the specific capacitance and long-life performance of all composite electrodes at high current density are superior to pure LDH electrode. When the added MWNTs content is 10 wt%, the specific capacitance increases to 342.4 F·g⁻¹ and remains at a value of 304 F·g⁻¹ until the 400th cycle at 2 A·g⁻¹, showing that this is a promising electrode material for supercapacitors working at heavy load. According to the electrochemical impedance spectra, MWNTs greatly increase the electronic conductivity between MWNTs and the surface of Co–Al LDH, which consequently facilitates the access of ions in the electrolyte and electrons to the electrode/electrolyte interface.     

Deposition of silica thin films formed by sol–gel method

Deposition of silica thin films on silicon wafer was investigated by in situ mass measurements with a microbalance configured for dip coating. Mass change was recorded with respect to deposition time when the substrate was fully immersed in the silica sol. Mass gain during deposition was higher than predicted from monolayer coverage of silica nano particles. This implied that deposition was facilitated by gelling of the nanoparticles on the substrate. The rate of deposition was enhanced by increasing the particle concentration in the sol and by decreasing the particle size from 12 to 5 nm. Increasing the salt concentration of the silica sol at constant pH enhanced the deposition of the silica particles. Reducing the pH of the sol from 10 to 6 decreased the deposition rate due to aggregation of the primary silica particles.     

Microstructure and performance of AZO thin films prepared by sol–gel processing

Al-doped zinc oxide (AZO) films were prepared by a wet-chemical coating technique, their microstructure and crystal growth were characterized as a function of the single layer thickness. When similar final thicknesses are attained by more multiple subsequent coating-firing cycles, film porosity is reduced from over 14 to 2 %. Simultaneously the AZO crystallite size is increased from approximately 23 to 60 nm, a preferential c-axis oriented growth is observed. Different substrates (soda-lime glass, soda-lime glass with a SiO₂ barrier coating, borosilicate glass and alkali-free display glass) were used and the resulting AZO films were compared. It is found that the substrate composition primarily affects grain growth and subsequently the electrical performance of the AZO films.     

Simultaneous formation of ferrite nanocrystals and deposition of thin films via a microwave-assisted nonaqueous sol–gel process

Combination of the surfactant-free nonaqueous sol–gel approach with the microwave technique makes it possible to synthesize Fe₃O₄, CoFe₂O₄, MnFe₂O₄, and NiFe₂O₄ nanoparticles of about 5–6 nm and with high crystallinity and good morphological uniformity. The synthesis involves the reaction of metal acetates or acetylacetonates as precursors with benzyl alcohol at 170 °C under microwave irradiation of 12 min. Immersion of glass substrates in the reaction solution results in the deposition of homogeneous metal ferrite films whose thickness can be adjusted through the precursor concentration. If preformed nickel nanoparticles are used as a type of curved substrate, the ferrite nanoparticles coat the seeds and form core–shell structures. These results extend the microwave-assisted nonaqueous sol–gel approach beyond the simple synthesis of nanoparticles to the preparation of thin films on flat or curved substrates.     

Preparation and characterization of nanocrystalline Ca-doped CeO2 by sol–gel process

The reactivity of CeO₂ is determined by grain size and oxygen vacancies, which can be achieved by doping elements with less oxidation state into CeO₂. In this study nanocrystalline Ca-doped CeO₂ sol was synthesized from the reaction of hydrate cerium (III) nitrate and calcium nitrate tetrahydrate in alcohol solution after being calcined at 600?°C. X-ray diffraction as well as selected area electron diffraction gave evidence that the synthesized Ca-doped CeO₂ samples were well crystalline and had a cubic fluorite structure. TEM observation revealed that Ca-doped CeO₂ was composed by nanoparticles with grain size around 8?nm. The Raman spectrum of pure CeO₂ consists of a single triple degenerate F_2g model characteristic of the fluorite-like structure. In the Ca-doped CeO₂ sample, two additional low-intensity Raman bands were detected, thus confirming the formation of the solid solution. The synthesized nanometric powder is expected to be used in solid oxide fuel cells as well as in the catalytic treatment of automobile exhaust fumes.     

Resistive switching behavior in amorphous and crystalline TiO2 thin films by sol–gel process

We present recent studies on amorphous and crystalline TiO₂ resistive switching nonvolatile memory devices. A chemical sol–gel process is demonstrated for preparing amorphous and crystalline TiO₂ thin films with different calcination temperature. Glass/SnO₂:F/TiO₂/Cu sandwich structures are fabricated and their current–voltage characteristics are examined. We found that the switching voltage goes from 4.8 to 3.5 V and the current compliance also drops from 10 to 1 mA when calcination temperatures increased. Smooth surface of TiO₂ thin films are also observed by XRD, AFM and XPS.     

Preparation and characterization of boron-based bioglass by sol−gel process

45S5 bioglass has been widely studied in the last few decades because of its bioactivity and promising applications in the biomedical field. Boron, even few studied, represents a potential element to improve the properties of the 45S5 bioglass derivatives. The bioglasses are conventionally prepared by heat treatment of oxides and silicon. Here, the sol?gel method is proposed for the preparation of the boron-based 45S5 bioglass (45S5B) and the classical 45S5 bioglass (45S5), using water-soluble salts as raw materials. The bioglasses were characterized by FTIR, XRD, and SEM, indicating the success of the sol?gel method for preparation of the samples. The bioglasses were also tested in vitro for bioactivity in biological conditions and cytotoxicity against eukaryotic cells. The bioactivity of 45S5B was similar to the bioactivity of 45S5 bioglass, indicated by the deposition of hydroxyapatite crystals at the surface of the pristine bioglasses. The results of cytotoxicity tests revealed that the IC₅₀ of 45S5B (IC₅₀?=?7.56?mg?mL^?1) was similar to the IC₅₀ of 45S5 (IC₅₀?=?8.15?mg?mL^?1), indicating its safety for application in the biomedical field.

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Preparation of durable superhydrophobic surface by sol–gel method with water glass and citric acid

Durable superhydrophobic surface on cotton fabrics has been successfully prepared by sol–gel method. Cellulose fabric was first coated with silica sol prepared with water glass and citric acid as the acidic catalyst. The silica coated fabric was then padded with hydrolyzed hexadecyltrimethoxysilane afterwards obtaining low surface energy. Water contact angle and hydrostatic pressure were used to characterize superhydrophobicity and washing durability. Scanning electron microscopy was used to characterize the surface morphology changes after certain washing times. All results showed good durable hydrophobicity on cellulose fabrics. In addition, the influence of citric acid and sodium hypophosphite (NaH₂PO₂) on the durability of hydrophobicity was also investigated. The durability of treated cotton improved with the increase of concentration of citric acid in the presence of NaH₂PO₂. It could be concluded that citric acid acted as multi-functional heterogeneous grafting chemicals to improve washing durability of hydrophobicity by forming the ester bonds between cotton fabric and silica sol and improved the durability of hydrophobicity.     

Synthesis and characterization of tellurium-doped CdO nanoparticles thin films by sol–gel method

In this work, tellurium (Te) doped CdO nanoparticles thin films with different Te concentrations (1, 3, 5, 7 and 10 %) were prepared by sol–gel method. The effects of Te doping on the structural, morphological and optical properties of the CdO thin films were systematically studied. From X-ray diffraction spectra, it has seen that all of thin films were formed polycrystalline and cubic structure having (111), (200) and (311) orientations. The structure of CdO thin films with Te-dopant was formed the unstable CdTeO₃ monoclinic structure crystal plane ( $ {\bar{\text{1}}\text{22}} $ 1 ¯ 22 ), however, the intensity of this unstable peak of the crystalline phase decreased with the increase of Te-doping ratio. The strain in the structure is also studied by using Williamson-Hall method. From FE-SEM images, it has seen that particles have homogeneously distributed and well hold onto the substrate surface. Additionally, grain size increases from 27 to 121 nm with the increase of Te-doping ratio. Optical results indicate that 1 % Te-doped CdO thin film has the maximum transmittance of about 87 %, and the values of optical energy band gap increases from 2.50 to 2.64 eV with the increase of Te-doping ratio. These results make Te-doped CdO thin films an attractive candidate for thin film material applications.     

Preparation and characterization of nanorods Sb doped CdO films by sol–gel technique

Pure and antimony (Sb) doped CdO films were grown using sol–gel spin coating technique. The structural properties of the films were investigated using atomic force microscopy. The structure of CdO film is converted from microrods to nanorods with Sb dopant. The analysis of optical absorption revealed that optical bandgap of the films changes with doping. The optical bandgap for 0.1, 0.5, 1.0, and 2.0% Sb doped CdO was determined to be 2.28, 2.30, 2.56, and 2.42 eV, respectively. Other optical constants such as refractive index, extinction coefficient, and dielectric constants were calculated using the optical data. The refractive index dispersion of the films obeys the single oscillator model. The volume and surface energy loss functions were calculated and observed to increase with increase in the photon energy.     

Photocatalytic and antibacterial activities of Ag-doped ZnO thin films prepared by a sol–gel dip-coating method

Silver-doped ZnO thin films with various loadings of Ag in the range of 0–10 mol% were prepared by the sol–gel dip-coating method. All prepared films show X-ray powder diffraction patterns that matched with ZnO in its würtzite structure. The grain size decreased as the Ag loading increased. The prepared films, under UV blacklight illumination, produced a photocatalytic degradation of methylene blue, rhodamine B and reactive orange solutions. Furthermore, they inhibited the growth of Escherichia coli bacteria under UV blacklight irradiation and to a lesser extent in dark conditions. The photocatalytic and antibacterial activities of the prepared films increased with Ag loading, presumably because Ag enhanced the efficiency of generation of superoxide anion radicals (^•O₂ ⁻) and hydroxyl radicals (^•OH).     

Removal of chromate from aqueous solution by reduction with nanoscale Fe–Al layered double hydroxide

Nanoscale layered double hydroxides of Fe^II and Al^III (Fe–Al LDH) have been applied for removal of chromate (Cr^VI) from aqueous solution. Given the reaction stoichiometry, Cr^VI was completely reduced to Cr^III and coprecipitated with Fe^III and Al^III oxyhydroxides. The extent of Cr^VI removal decreased with increasing initial pH and decreasing molar ratio of Cr^VI/structural Fe^II in the LDH. The chromate reduction rate at different initial concentrations of Cr^VI was well described by the pseudo-second-order model with reaction rate constant ranging from 197.4 to 13.53 (mmol min)^?1. Initial pH and substitution of various amounts of Fe^III in the LDH structure had little effect on the reaction rate. Backtransformation of Cr^III to Cr^VI by birnessite Mn oxide (δ-MnO₂) after 40 days of reaction was less than 1% of the initial Cr (as Cr^III solid), indicating high stability of the final reaction products and high efficiency of nanoscale Fe–Al LDHs for removal of chromate from aqueous solution.