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.     

Structural and optical characterization of Ag-doped TiO2 nanoparticles prepared by a sol–gel method

Undoped and silver-doped TiO₂ nanoparticles (Ti_1?x Ag _x O₂, where x?=?0.00?C0.10) were synthesized by a sol?Cgel method. The synthesized products were characterized by X-ray diffraction (XRD), particle size analyzer (PSA), scanning electron microscope (SEM), and UV?CVisible spectrophotometer. XRD pattern confirmed the tetragonal structure of synthesized samples. Average crystallite size of synthesized nanoparticles was determined from X-ray line broadening using the Debye?CScherrer formula. The crystallite size was varied from 8 to 33?nm as the calcination temperature was increased from 300 to 800?°C. The incorporation of 3 to 5% Ag⁺ in place of Ti⁴⁺ provoked a decrease in the size of nanocrystals as compared to undoped TiO₂. The SEM micrographs revealed the agglomerated spherical-like morphology of particles. SEM, PSA, and XRD measurements show that the particles size of the powder is in nanoscale. Optical absorption measurements indicated a red shift in the absorption band edge upon silver doping. Direct allowed band gap of undoped and Ag-doped TiO₂ nanoparticles measured by UV?CVis spectrometer were 3.00 and 2.80?eV, respectively, at 500?°C.     

Development of TiO2 pastes modified with Pechini sol–gel method for high efficiency dye-sensitized solar cell

A titanium oxide layer used for a dye-sensitized solar cell (DSSC) has to meet two opponent properties to assure a high efficiency DSSC: good connection between TiO₂ grains and a large inner surface area. Three different paste formulations based on commercial nanocrystalline TiO₂ powder (Degussa P25) are studied. Results confirm that modification of the TiO₂ paste with the Pechini sol–gel method increases the surface area of the TiO₂ layer while maintaining good connections between the nanocrystalline grains, consequently the efficiency of the DSSC increases from 1.8% to 5.3%. The structure and morphology of the TiO₂ layers are described by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD).     

TiO2 and TiO2/SiO2 nanoparticles obtained by sol–gel method and applied on dye sensitized solar cells

In this work we show the synthesis and characterization of TiO₂ and TiO₂/SiO₂ nanoparticles synthesized by sol–gel method using HF and HCl as catalysts. The obtained nanoparticles were analyzed by N₂ adsorption–desorption isotherms, transmission electronic microscopy, Ultraviolet–visible spectroscopy and X-ray diffractometry. Mesoporous, homogeneously polycondensed TiO₂/SiO₂ materials, containing nanocrystalline anatase phase with band gap similar to pure titania were obtained. Films of the powdered oxides were applied to assemble dye sensitized solar cells that presented electrical parameters, Fill Factor and efficiencies similar to devices obtained by only TiO₂. The sol–gel route arises as an alternative way to prepare TiO₂/SiO₂ materials for solar cells.     

Structural,morphological and optical properties of SnO2 nanoparticles obtained by a proteic sol–gel method and their application in dye-sensitized solar cells

Journal of Sol-Gel Science and Technology - Tin dioxide nanoparticles were synthesized by the proteic sol–gel method. Tin chloride (SnCl4·5H2O) was used as source of Sn4+ and commercial...     

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.     

Structural stability and electrochemical properties of Gd-doped ZrO2 nanoparticles prepared by sol–gel

Cubic, tetragonal and monoclinic Gd-doped zirconia nanoparticles with nominal composition Gd_xZr_1?xO₂ in the range 0 ≤ x ≤ 0.2, were prepared by annealing dried gels of Gd-containing zirconia at temperatures over the range between 450 and 1,300 °C. The synthesized zirconia-based nanoparticles with increased gadolinium load were characterized by X-ray powder diffraction, infrared and Raman spectroscopies, and transmission electron microscopy. The stabilization of the crystalline forms of Gd-doped ZrO₂ solid solutions depends on the amount of Gd dopant and the annealing temperature. For low Gd loads in Gd_xZr_1?xO₂ being x < 0.05, the tetragonal form is the single phase up to 1,100 °C, whereas the monoclinic is the crystalline form detected up to 1,300 °C. Within the range of compositions 0.05 ≤ x < 0.1, is the tetragonal the only stabilized zirconia crystalline structure over the whole range of temperature up to 1,300 °C. For higher Gd-contents, in the range 0.1 ≤ x ≤ 0.2, is the cubic zirconia form the only stable phase for the whole range of annealing temperatures. Solid-state electrochemistry of the gadolinium-doped zirconia performed by the voltammetry of microparticles approach allowed distinguishing different electrochemical answers of Gd cation associated with slightly different local coordination surrounding of cations. Enantioselective electrocatalytic effect of monoclinic Gd-doped ZrO₂ on the oxidation of l-(+)-tartaric acid and d-(?)-tartaric was also studied.     

Synthesis and characterization of organic–inorganic hybrid materials prepared by sol–gel and containing CdS nanoparticles prepared by a colloidal method using poly(N-vinyl-2-pyrrolidone)

This paper describes the synthesis and characterization of CdS nanoparticles (NPs) stabilized with poly(N-vinyl-2-pyrrolidone) and their further immobilization on a hybrid organic–inorganic matrix produced by the sol–gel process. The production of the hybrid matrix doped with CdS NPs was carried out in two steps. In the first step a precursor, designated diureasil precursor, was synthesized from the reaction between the terminal amine groups of α,ω-diamine-poly(oxyethylene-co-oxypropylene) and the isocyanate group of 3-isocyanatopropyltriethoxysilane. The next step involved the hydrolysis and condensation reactions of ethoxy groups attached to silicon, this step resulting in the formation of a crosslinked siliceous network linked through urea bonds to a poly(oxyethylene)/poly(oxypropylene) chain. The NPs were added to the diureasil precursor before the gelation process to allow a homogeneous dispersion of the NPs within the matrix. The developed method allowed the transfer of colloidal NPs to a solid matrix without the need of exchange the capping agents or the solvent. The materials were characterized by absorption, steady-state photoluminescence spectroscopy and by TEM. The results obtained showed the presence of CdS NPs with quantum size effect dispersed within the diureasil matrix. The obtained nanocomposites show a high transparency in the visible range accounting for the good dispersion of the NPs within the matrix. The TEM analysis confirmed that the NPs are uniformly dispersed within the diureasil matrix.     

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.     

Preparation of ZnO nanoparticles by a surfactant-assisted complex sol–gel method using zinc nitrate

This paper presents a surfactant-assisted complex sol–gel method for the controlled preparation of Zinc Oxide (ZnO) nanoparticles using zinc nitrate and citric acid as starting material. ZnO nanoparticles with a pure wurtzite structure were obtained after calcination at 773 K. The effects of the citric acid concentration, the pH, and the surfactants on the average particle size and morphology of the ZnO nanoparticles were investigated using X-ray diffraction and scanning electron microscopy. Well dispersed ZnO nanoparticles with a uniform size distribution were obtained using polyethylene glycol (PEG) 2000 as a surfactant. During sintering, the ZnO nanoparticles revealed isotropic growth below 1,373 K and anisotropic growth above 1,473 K. The particles’ activation energy was calculated to be 140 ± 6 kJ/mol between 773 and 1,373 K.     

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.     

Fabrication and electrical characterization of transparent NiO/ZnO p–n junction by the sol–gel spin coating method

Sol–gel spin technique was used to fabricate transparent p–n junction between NiO and ZnO semiconductors. Atomic force microscopy studies indicated that ZnO film had a fibrous structure, while NiO film showed very smooth surface morphology. The optical transmittance of these films was about 75 %. The optical band gaps of ZnO and NiO films were obtained to be 3.25 and 3.89 eV, respectively. The current–voltage characteristics of NiO/ZnO junction showed a good rectifying behavior. The junction parameters such as ideality factor and barrier height were calculated using thermionic emission model. The barrier height and ideality factor values of the diode were obtained to be 0.48 and 2.91 eV, respectively. The variation of photocurrent with wavelength indicates that this device had high efficiency in wavelength range of 450–475 nm.     

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.     

Preparation of CuCrO2 nanoparticles with narrow size distribution by sol–gel method

Copper chromium oxide (CuCrO₂) nanoparticles were synthesized by sol–gel method. The effect of annealing temperature, duration of heat treatment and metallic ion concentration in precursor solution on the structural properties of the nanoparticles was investigated. The delafossite structure of CuCrO₂ powder was confirmed by X-ray diffractometer. It was found that the crystallite sizes as well as the size of the nanoparticles increased with annealing temperature and duration of heat treatment but decreased with metallic ion concentration. Nanoparticles’ size was obtained using particle size analyzer. The synthesized CuCrO₂ nanoparticles with 0.7 M metallic ion concentration have the lowest crystallite and particle sizes with a narrow size distribution in the range of 13.5–15.6 nm. In the presence of this metallic ion concentration, we could also produce single crystal CuCrO₂ nanoparticles. Moreover, the CuCrO₂ nanoparticles exhibit a large optical band gap that increases with metallic ion concentration. The optical band gap of the nanoparticles fabricated with 0.7 M metallic ion concentration in precursor solution is about 3.99 eV.