Sharif Digital Repository

To improve the biocompatibility and corrosion resistance of 316L SS (Stainless Steel) metal implants, HAp(hydroxyapatite)/TiO2/Al2O3 nanocomposite coating was created using dip sol-gel method sintered at 550 °C. The weight percentage of TiO2+ Al2O3 in these coatings was 20, 30, and 40% wt. In this study, characterization was performed using FTIR (Fourier-Transform Infrared Spectroscopy), XRD, FE-SEM (Field Emission Scanning Electron Microscope), EDS (Energy Dispersive Spectroscopy), DLS (Dynamic Light Scattering), Pull-off, and AFM (Atomic Force Microscopy) analysis. The potentiodynamic polarization and EIS (Electrochemical Impedance Spectroscopy) were performed in the simulated body fluid... 

A facile sol-gel synthesis for self-agglomeration of metallic silver nanoparticles, with fcc crystalline structure, on the silica surface in a low annealing temperature has been introduced. X-ray photoelectron spectroscopy (XPS) revealed initial agglomeration (∼30 times greater than the nominal concentration of Ag) of the nanoparticles on the surface of the dried film (100 °C) and also their oxidation as well as easy diffusion (with 0.08 eV required activation energy) into the porous silica thin films, by increasing the annealing temperature (200-400 °C). By raising the Ag concentration from 0.2 to 1.6 mol% in the sol, the average size of the Ag nanoparticles increased from ∼5 to 37 nm... 

A novel amino-functionalized polymer was synthesized using 3-(trimethoxysilyl) propyl amine (TMSPA) as precursor and hydroxy-terminated polydimethylsiloxane (OH-PDMS) by sol-gel technology and coated on fused-silica fiber. The synthesis was designed in a way to impart polar moiety into the coating network. The scanning electron microscopy (SEM) images of this new coating showed the homogeneity and the porous surface structure of the film. The efficiency of new coating was investigated for headspace solid-phase microextraction (SPME) of some environmentally important chlorophenols from aqueous samples followed by gas chromatography-mass spectrometry (GC-MS) analysis. Effect of different... 

To evaluate the selectivity and efficiency of solid phase microextraction (SPME) fiber coatings, synthesized by sol-gel technology, roles of precursors and coating polymers were extensively investigated. An on-line combination of capillary microextraction (CME) technique and high performance liquid chromatography (HPLC) was set up to perform the investigation. Ten different fiber coatings were synthesized in which five of them contained only the precursor and the rests were prepared using both the precursor and coating polymer. All the coatings were chemically bonded to the inner surface of copper tubes, intended to be used as the CME device and already functionalized by self-assembly... 

A method based on solid-phase microextraction (SPME) followed by on-fiber derivatization and gas chromatography-mass spectrometry detection (GC-MS) for determination of phenol in air was developed. Three different types of SPME fibers, polar and non-polar poly(dimethylsiloxane) (PDMS) and polyethylene glycol (PEG) were synthesized using sol-gel technology and their feasibility to the sampling of phenol were investigated. Different derivatization reagents for post on-fiber derivatization of phenol were studied. Important parameters influencing the extraction and derivatization process such as type of fiber coating, type and volume of derivatizing reagent, derivatization time and temperature,... 

CeO 2-TiO 2 nanoparticles were prepared by the sol-gel process using 2-hydroxylethylammonium formate as room-temperature ionic liquid and calcined at different temperatures (500-700°C). CeO 2-TiO 2-graphene nanocomposites were prepared by hydrothermal reaction of graphene oxide with CeO 2-TiO 2 nanoparticles in aqueous solution of ethanol. The photocatalysts were characterized by X-ray diffraction, BET surface area, diffuse reflectance spectroscopy, scanning electron microscopy, and Fourier transformed infrared techniques. The results demonstrate that the room-temperature ionic liquid inhibits the anatase-rutile phase transformation. This effect was promoted by addition of CeO 2 to TiO 2.... 

A new technique for preparation of an unbreakable solid-phase microextraction (SPME) fiber, using sol-gel technology is developed. Primarily, an ultrathin two-dimensional intermediate film was prepared by hydrolysis of 3-(trimethoxysilyl)-1-propanthiol self-assembled monolayer grafted onto gold, then a stationary phase by electrodeposition of 3-(trimethoxysilyl) propylmethacrylate as a precursor, tetramethyl orthosilicate and polyethylene glycol as a coating polymer was produced. The scanning electron microscopy images revealed that the new fiber exhibits a rather porous and homogenous surface. The thermal stability of the fabricated fiber was investigated by thermogravimetric analysis. The... 

Nanostructured TiO2-ZrO2 thin films and powders were prepared by a straightforward aqueous particulate sol-gel route. Titanium (IV) isopropoxide and zirconium (IV) acetate hydrate were used as precursors, and hydroxypropyl cellulose was used as a polymeric fugitive agent in order to increase the specific surface area. X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy revealed that the powder were crystallised at the low temperature of 500 °C, containing anatase-TiO 2 and tetragonal-ZrO2 phases. Furthermore, it was found that ZrO2 retarded the anatase-to-rutile transformation up to 900 °C. The activation energies for crystallite growth of TiO2 and ZrO2 components in... 

In this work a novel unbreakable sol-gel-based in-tube device for on-line solid phase microextraction (SPME) was developed. The inner surface of a copper tube, intended to be used as a high performance liquid chromatography (HPLC) loop, was electrodeposited by metallic Cu followed by the self assembled monolayers (SAM) of 3-(mercaptopropyl) trimethoxysilane (3MPTMOS). Then, poly (ethyleneglycol) (PEG) was chemically bonded to the -OH sites of the SAM already covering the inner surface of the copper loop using sol-gel technology. The homogeneity and the porous surface structure of the SAM and sol-gel coatings were examined using the scanning electron microscopy (SEM) and adsorption/desorption... 

A new type of composite material based on carbon nanotubes (CNTs) and sol-gel chemistry was prepared and used as sorbent for needle trap device (NTD). The synthesized composite was prepared in a way to disperse CNTs molecules in a sol-gel polymeric network. CNT/silica composites with different CNT doping levels were successfully prepared, and the extraction capability of each composite was evaluated. Effects of surfactant and the oxidation duration of CNTs on the extraction efficiency of synthesized composites were also investigated. The applicability of the synthesized sorbent was examined by developing a method based on needle trap extraction (NTE) and gas chromatography mass spectrometry... 

Nanostructured TiO2-CeO2 thin films and powders were prepared by a straightforward aqueous particulate sol-gel route. Titanium (IV) isopropoxide and cerium chloride were used as precursors, and hydroxypropyl cellulose was used as a polymeric fugitive agent in order to increase the specific surface area. The effect of Ce:Ti molar ratio was studied on the crystallisation behaviour of the products. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed that the powders crystallised at the low temperature of 500 °C, containing anatase-TiO2, rutile-TiO2 and cubic-CeO2 phases, as well as Ti 8O15, Ti3O5 and Ce 11O20 depending on annealing temperature and Ce:Ti molar... 

Nanocrystalline neodymium titanium oxide thin films and powders with different phase compositions with mesoporous structure were produced by a straightforward particulate sol-gel route. The sols were prepared in various Nd:Ti molar ratios and they showed a narrow particle size distribution in the range 20-26 nm. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed that the powders contained mixtures of Nd4Ti9O24, Nd2Ti4O11, Nd3Ti4O12 for titanium dominant powders (Nd:Ti ≤ 45:60), mixtures of Nd2TiO5 and Nd2O3 for neodymium dominant powders (Nd:Ti ≥ 75:25) and pure Nd3Ti4O12 phase for equal molar ratio of Nd:Ti, depending on the annealing temperature and Nd:Ti... 

TiO2 and transition metal (Cr, Mn, Fe, Co, Ni, Cu, and Zn) doped TiO2 nanoparticles were synthesized by the sol-gel method using 2-hydroxylethylammonium formate as an ionic liquid. All the prepared samples were calcined at 500 °C and characterized by X-ray diffraction (XRD), BET surface area determination, energy dispersive X-ray (EDX) analysis, diffuse reflectance spectroscopy (DRS), and Fourier transformed infrared (FT-IR) techniques. The studies revealed that transition metal (TM) doped nanoparticles have smaller crystalline size and higher surface area than pure TiO2. Dopant ions in the TiO2 structure caused significant absorption shift into the visible region. The results of... 

Monometallic and bimetallic supported metal oxides catalysts on γ-alumina were prepared by heterogeneous deposition-precipitation. The γ-alumina used as a support was synthesized by the sol-gel and the co-precipitation methods. Supports and catalysts were characterized by Brunauer–Emmett–Teller (BET) surface area, X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS). The performance of the prepared catalysts was studied for total oxidation of toluene in air at different relative humidity and oxidation temperatures. Efficiency of bimetallic catalysts for deep oxidation of toluene was... 

A method based on direct immersion solid-phase microextraction (DI-SPME) coupled with high performance liquid chromatography combined with post-column photochemically induced fluorimetry derivatization and fluorescence detection (HPLC-PIF-FD) was developed to extract three pyrethroid insecticides, i.e. cyfluthrin, cypermethrin, and flumethrin from water samples. A sol-gel based coating fiber using 3-(trimethoxysilyl propyl) amine as precursor was prepared and used for the extraction of the pyrethroids from groundwater samples. A post-column photochemical reactor was designed and constructed for the derivatization of these environmentally important pollutants to increase their fluorescence... 

A systematic comparison of single and binary metal oxide TiO2, TiO2-Er2O3 and TiO2-Ta2O5 thin film gas sensors with nanocrystalline and mesoporous microstructure, prepared by sol-gel route, was conducted. The gas sensitivity was increased by secondary phase introduction into TiO2 film via two mechanisms, firstly due to the inhibition of anatase-to-rutile transformation, since the anatase phase accommodates larger amounts of adsorbed oxygen, and secondly due to the retardation of grain growth, since the higher surface area provides more active sites for gas molecule adsorption. The binary metal oxide gas sensors exhibited a remarkable response towards low concentrations of CO and NO2 gases at...