Structural and electrosurface characteristics of titanium dioxide xerogel prepared by the sol–gel method

Stable highly concentrated TiO₂ sol has been synthesized using binary titanyl ammonium sulfate monohydrate, (NH₄)₂TiO(SO₄)₂ · H₂O. Treatment of the sol with an ammonia solution has yielded a stable hydrogel, which, after being dried, is transformed into a TiO₂ xerogel. Study of the structure-related sorption and crystalline-chemical properties of the synthesized xerogel has shown that it represents a semicrystalline micro/mesoporous material with a rather developed specific surface area (S_sp = 120 m²/g). According to potentiometric titration data, the point of zero charge (PZC) of this material is located at pH 3.9. Measurements of the electrophoretic mobility (by microelectrophoresis) of TiO₂ xerogel particles in solutions of HCl, NaOH, and salts of mono-, bi-, and trivalent cations have shown that (1) the isoelectric point (IEP) of the particles lies in the vicinity of pH 6.2, i.e., at a much higher pH than that for PZC; (2) the presence of increasing amounts of 1: 1 and 2: 1 electrolytes causes a gradual and a dramatic reduction in the ζ potential of the particles, respectively; and (3), in the presence of an electrolyte with a trivalent counterion, the surface charge is reversed. The behavior of TiO₂ xerogel in an electric field is similar to that of lyophobic particles, with the difference that there is no maximum in the ζ potential versus 1: 1 electrolyte concentration dependence and the measured IEP of the xerogel is much higher than its PZC. Possible reasons for this discrepancy have been discussed.     

Titanium dioxide fibers prepared by sol–gel process and centrifugal spinning

A new study of the preparation of nanocrystalline titanium dioxide (TiO₂) fibers is reported in the paper, which were prepared by sol–gel process with titanium acetate [Ti(CH₃COO)₄] as precursor. After that, centrifugal spinning and steam atmosphere heat-treatment were used to obtain final fibers. Here, the molecule structure of precursor was analyzed and the TiO₂ fibers obtained were characterized. Additionally, the effects of the silica (SiO₂) doping were discussed in this paper. By the Fourier transformation infrared spectrum analysis, the chain structure of –O–Ti–O–Ti–O– was confirmed in the Ti(CH₃COO)₄ precursor, as a result the precursor spinning solution showed a good spinning performance. And the pyrolysis process of precursor fibers was analyzed with the help of DSC–TG method. The phase of TiO₂ fibers obtained after heat-treatment with steam atmosphere was characterized mainly by the X-ray diffractometer (XRD), from the XRD curves, the result that the SiO₂ doping can efficiently inhibit the grain growth of TiO₂ fibers could also be verified. The microstructure of the TiO₂ fibers was observed by scanning electron microscope, which showed that diameter of TiO₂ fibers obtained with excellent continuity are from 5 to 10 μm. At last, the photocatalytic property of TiO₂ fibers was also tested.     

Nitrogen doping into titanium dioxide by the sol–gel method using nitric acid

N-doped TiO₂ has been prepared by use of sol–gel systems containing titanium alkoxide, with nitric acid as the nitrogen source. The time needed for gelation of the systems was drastically reduced by ultrasonic irradiation. The peaks assigned to the nitrate and nitrous ions were observed by FT-IR measurement during the sol–gel reaction. The N-doping was confirmed by the observation of N–O peaks in the XPS spectrum of the sample heated at 400 °C. The nitrate ion acted as an oxidizer of the ethanol solvent and titanium species. The TiO₂ became doped with nitrogen oxide species as a result of reduction of nitrate ion incorporated into the dried gel samples. These results indicated that the added nitric acid was reduced during the sol–gel transition and heating process, and the resulting NO species were situated in the titania networks. The UV and visible photocatalytic activity of the samples was confirmed by the degradation of trichloroethylene.     

Electrochemical characterization of sodium and potassium doped lanthanum–titanium mixed oxides prepared by sol–gel method

Varying amounts of Na and K doped lanthanum–titanium oxides were synthesized by gel entrapment technique. These ceramics were characterized by X-ray diffraction. Microstructural investigations revealed grain growth in the doped material compared to undoped sample. Dielectric relaxations of these compounds were investigated in the temperature range 250–900 °C. A high degree of dispersion of the permittivity of un-doped lanthanum–titanium oxide and K and Na doped lanthanum–titanium oxide was observed in the frequency range <100 kHz which was attributed to oxygen vacancies. An increase in the permittivity values were observed with 1 % Na and K doped samples. The permittivity values further deteriorated with the dopant concentration. Using the Cole–Cole model, an analysis of the dielectric loss with frequency was performed, assuming a distribution of relaxation time. The dielectric loss was found to decrease by doping K in lanthanum–titanium oxide matrix. The dc conductivity studies showed that a temperature dependent hopping type mechanism is responsible for electrical conduction in the system.     

High-efficiency TiO2/ZnO nanocomposites photocatalysts by sol–gel and hydrothermal methods

Journal of Sol-Gel Science and Technology - TiO2/ZnO nanocomposites with ratio of Ti/Zn of 1:0, 1:1, 2:1, 3:1 and 0:1 was synthesized by sol–gel and hydrothermal methods. The performance and...     

Anticorrosive cerium-based coatings prepared by the sol–gel method

The development of efficient anti-corrosion and environmentally friendly coating systems are needed for the replacement of the highly toxic Cr-based conversion coatings for corrosion protection of aluminum alloys. In this study, we demonstrate that the direct application of ceramic cerium-based sol–gel coatings to AA7075-T6 substrates produces high-performance anti-corrosion layers. Electrochemical experiments and analyses of the microstructure demonstrate that the protective layers are very efficient for the passivation of the alloy surfaces operating as both passive and active barrier for corrosion protection.     

Sensing abilities of materials prepared by sol–gel technology

The advantages of the sol–gel technology are undoubtedly simplicity and versatility. It enables to obtain for example oxides in the form of layers, powders, monoliths or fibers. These materials can be successfully applied for sensing purposes due to their properties such as transparency, porosity, and high surface areas. In this article, the basis of operation of mainly optical and semiconductor sensors are presented. A brief overview of various kinds of sensors is submitted. The utility of optical fibers and planar waveguides in these systems is discussed. The paper contains also some results obtained by the authors in the field of thin film-based sensors.     

Synthesis of titanium dioxide nano-powder via sol–gel method at ambient temperature

Titanium dioxide is a semiconductor with excellent photo catalytic properties and an important material with high regarded in nanotechnology. In this study, titanium dioxide nanoparticles was successfully synthesized via sol–gel method using tetra-n-butyl orthotitanate, hydrochloric acid and ammonia. Tetra-n-butyl orthotitanate was used as precursor. The ingredients were mixed at ambient temperature for 9 h on a magnetic stirring, sol was formed and converted to gel by adding ammonia. X-ray diffraction analysis clearly showed anatase and rutile phases so that, with increasing calcination temperature anatase converts to the rutile. Scanning electron microscopy was used for agglomerate observations. Energy-dispersive detector analysis was carried out and confirmed the formation of titanium dioxide. The influences of calcination temperature and pH value on particles size were studied. The results indicate that synthesis at room temperature reduced the particle size to 15 nm.     

Physical and optical properties of organo-modified silica nanoparticles prepared by sol–gel

A comparative study on the physical and optical properties of silica nanoparticles prepared by sol–gel has been carried out. Post-modification of as-synthesized silica nanoparticles produced organo-functionalized silica nanoparticles slightly increased in size (~20%) and relatively high aggregation. However, in situ method produced sixfold bigger functionalized particles with good dispersion and less aggregation. Higher organic content was observed for in situ modified nanosilica, leading to a higher surface hydrophobicity that improved compatibility and dispersion in preparation of silica-polymer nanocomposite. Furthermore, in situ and post-modified nanosilica demonstrated a distinct optical activity, photoluminescence and UV compared to the unmodified nanoparticles.     

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.     

Study of tri-layer antireflection coatings prepared by sol–gel method

Antireflective coatings (ARCs) on tri-layer thin film stacks were studied in this paper. Silica sols have been prepared by acid-catalyzed or base-catalyzed hydrolysis and condensation reactions of tetraethyl orthosilicate. Antireflective nanometric SiO₂/TiO₂ films are formed on both sides of the glass substrates by combining the sol–gel method and the dip-coating technique. Seen from the transmittance spectra of different films, a maximum light transmittance of 99.9% was obtained at the band of 300–800 nm. Scanning electron microscope (SEM) and atomic force microscopy (AFM) confirm the well-covered surface morphology. By the SEM observations we can see that the films are full of coverage on glass surface and containing no voids or cracks. The image root mean square roughness of the two types of ARCs provided by the AFM is 1.21 and 3.04 nm, respectively. Furthermore, a surface profiler was used to determine the thickness of each layer in the obtained multi-layer coating system.     

The properties of nickel aluminate nanoparticles prepared by sol–gel and impregnation methods

Nickel aluminates were prepared by sol–gel and impregnation methods and calcined at 1100 °C. The sol–gel made samples were prepared with different amounts of nickel (Ni/Al molar ratio equal to 0, 0.25, 0.5, and 0.75) and aging times (24 and 48 h). The samples were characterized by X-ray diffraction, induced couple plasma, nitrogen physisorption, transmission and scanning electron microscopy, and ammonia temperature programmed desorption (NH₃-TPD). In the sol–gel made samples, only the NiAl₂O₄ structure of nickel aluminate was defined, while for impregnation, NiAl₁₀O₁₆ was formed as well. The sol–gel made samples had low specific surface areas (7.7–12.4 m²/g), but a sample prepared by impregnation method had higher specific surface area (67.2 m²/g). The surface acidity density decreased by increasing the amount of nickel and was the lowest for impregnation method.     

Synthesis and characterization of nitrogen-doped TiO2 nanoparticles prepared by sol–gel method

The N-doped TiO₂ has been synthesized by sol?Cgel method, using titanium isopropoxide, isopropanol and an aqueous solution of ammonia with ratio 2:1:10. The concentrations used for the NH₃ aqueous solution were 3, 7, 10 and 15?%. The samples have been analysed by X-ray diffraction, electron microscopy (SEM and TEM) thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), micro-Raman spectroscopy and diffuse reflectivity. TEM, SEM, DSC and TGA showed that the morphology is influenced by the presence of N^3? ions but not by the concentration of the solution. Instead reflectance gave us a relation between values of the energy gap and the concentration of N^3? ions: the gap between valence and conduction band lowers as the concentration of NH₃ in the starting solution increases. From these results we can say that the properties of the material have been tuned by doping with nitrogen ions because the particles absorb more light in the visible range, and this is important for photovoltaic and photocatalytic applications.     

Effects of diethanolamine on the evolution of silver/titanium dioxide sol–gel process

In order to clarify the effects of diethanolamine (DEA) in the silver (Ag)/titanium dioxide (TiO₂) sol–gel process, sols with and without DEA, and films derived from these sols were prepared. The samples were investigated by X-ray diffraction, transmission electron microscopy, electron diffraction and optical absorption spectra. The results showed that metallic Ag clusters were formed in the sol with DEA and was absent in the sol without DEA. This indicated that DEA worked not only as the stabilizer but also as the reduce agent in Ag/TiO₂ sol–gel process. After annealed, Ag metallic nanoparticles were generated in the films derived from both the sols with and without DEA. The particles in the films derived from the sol with DEA were smaller than those from the sol without DEA. This can be ascribed to the limitation of the growth of Ag cluster formed in the sol with DEA during heat treatment. Mechanisms for the formation of metallic Ag in the Ag/TiO₂ sols and films were discussed. The effects of DEA in the sols and films were studied in detail.