Kamal M.S. Khalil

Humidity sensing properties of NiO/Al2O3 nanocomposite materials

Abstract Humidity sensing properties measured by impedance spectroscopy (IS) and DC conductivity for a group of high surface area nanostructured 5–30% w/w NiO/Al 2 O 3 composite materials are reported. The nanocomposites were prepared via a sol–gel method, which involved mixing of the respective sol–gel precursors and the subsequent drying and calcination at 873 K for 3 h. Accordingly, nanosized NiO particles dispersed in γ-Al 2 O 3 matrix were formed. Conductivity changes amount to six orders of magnitudes were observed in response to 5–90% relative humidity (RH) change in the measuring chamber. Results indicate that humidity sensing was increased with the increase of NiO content in the composite. Moreover, conductance kinetics and conduction mechanism are discussed in terms of surface texture and nanostructured morphology of the composite materials that facilitate ionic transport mechanism.

Preparation and characterization of sol-gel derived mesoporous titania spheroids

The formation of mesoporous spherical titania particles via hydrolysis of pure titanium tetra-isopropoxide in n-heptane solution upon the application of a slow stirring rate is described. Calcination of the dry hydrolysis product produced pure anatase at 400–600°C, and rutile at 800°C. Nitrogen adsorption results indicate high surface area (SBET 132 m2/g) and uniform mesopores peaking at 10 nm for the material calcined at 400°C. Upon calcination at 600°C, the pore size remained at 10 nm, whereas the SBET value was decreased. The material calcined at 400°C was found by scanning electron microcopy to be shaped into spherical particles about 2 μm in diameter. Sizes of the spherical particles were unchanged at 400°C and up to 800°C. This was ascribed to the spherical morphology of the particles which prevented primary particles from growing beyond the boundary of the host aggregate even when the rutile phase transition occurred at 800°C.

Catalytic activity of a zirconium(IV) oxide surface supported with transition metal ions

The kinetics of H2O2 decomposition have been investigated using ZrO2 supported with transition metal ions including CuII, AgI, HgII, CoII, MnII, NiII and FeIII. At pH = 6.8, the reaction rate exhibits a first order dependence on the initial H2O2 concentration at low concentrations. The order of activity of the different catalysts is strongly dependent on the [H2O2]0 used. The reaction proceed via the formation of the peroxo-intermediate which has an inhibiting effect on the reaction rate. The rate increases with increasing pH, and attains a limiting rate at higher pHs. A reaction mechanism is proposed involving liberation of HO2 radicals from the peroxo-intermediate as the rate-determining step.

Dielectric behavior and ac conductivity study of NiO∕Al2O3 nanocomposites in humid atmosphere

Humidity sensing characteristics of NiO∕Al2O3 nanocomposites, prepared by sol-gel method, are studied by impedance spectroscopy. Modeling of the obtained impedance spectra with an appropriate equivalent circuit enables us to separate the electrical responses of the tightly bound chemisorbed water molecules on the grain surfaces and the loosely associated physisorbed water layers. Dependence of the dielectric properties and ac conductivity of the nanocomposites on relative humidity (RH) were studied as a function of the frequency of the applied ac signal in the frequency range of 0.1–105Hz. The electrical relaxation behavior of the investigated materials is presented in the conductivity formalism, where the conductivity spectra at different RHs are analyzed by the Almond-West formalism [D. P. Almond et al., Solid State Ionics 8, 159 (1983)]. The dc conductivity and the hopping rate of charge carriers, determined from this analysis, show similar dependences on RH, indicating that the concentration of mobile...

Direct formation of thermally stabilized amorphous mesoporous Fe2O3/SiO2 nanocomposites by hydrolysis of aqueous iron III nitrate in sols of spherical silica particles.

Nanocomposite materials containing 10% and 20% iron oxide/silica, Fe2O3/SiO2 (w/w), were prepared by direct hydrolysis of aqueous iron III nitrate solution in sols of freshly prepared spherical silica particles (Stöber particles) present in their mother liquors. This was followed by aging, drying, calcination up to 600 degrees C through two different ramp rates, and then isothermal calcinations at 600 degrees C for 3 h. The calcined and the uncalcined (dried at 120 degrees C) composites were characterized by thermogravimetric analysis, differential scanning calorimetry, Fourier transform infrared spectroscopy, X-ray diffraction (XRD), N2 adsorption/desorption techniques, and scanning electron microscopy as required. XRD patterns of the calcined composites showed no line broadening at any d-spacing positions of iron oxide phases, thereby reflecting the amorphous nature of Fe2O3 in the composite. The calcined composites showed nitrogen adsorption isotherms characterizing type IV isotherms with high surface area. Moreover, surface area increased with the increasing of the iron oxide ratio and lowering of the calcination ramp rate. Results indicated that iron oxide particles were dispersed on the exterior of silica particles as isolated and/or aggregated nanoparticles. The formation of the title composite was discussed in terms of the hydrolysis and condensation mechanisms of the inorganic FeIII precursor in the silica sols. Thereby, fast nucleation and limited growth of hydrous iron oxide led to the formation of nanoparticles that spread interactively on the hydroxylated surface of spherical silica particles. Therefore, a nanostructured composite of amorphous nanoparticles of iron oxide (as a shell) spreading on the surface of silica particles (as a core) was formed. This morphology limited the aggregation of Fe2O3 nanoparticles, prevented silica particle coalescence at high temperatures, and enhanced thermal stability.

Direct formation of iron oxide/MCM-41 nanocomposites via single or mixed n-alkyltrimethylammonium bromide surfactants.

Iron oxide/MCM-41 nanocomposites, Fe(2)O(3)/MCM-41, containing 5%, 10%, and 20% (w/w) iron oxide, were prepared via a direct nonhydrothermal method at room temperature. The preparations were preformed by using iron(III) nitrate, tetra-ethoxysilane (TEOS), and cetyltrimethylammonium bromide (CTAB) mixed or unmixed with dodecyltrimethylammonium bromide (DTAB). The produced materials were dried and calcined at 550 °C for 3 h. Test materials were characterized by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), N(2) gas adsorption/desorption isotherms, small angle and wide angle X-ray diffraction (XRD). Results indicate that mixing of CTAB with DTAB does not harm the formation of blank MCM-41 structure. For the composite Fe(2)O(3)/MCM-41 materials, results showed formation of more stable MCM-41 structure with higher surface area and improved porosity in the presence of mixed (CTAB+DTAB) than in the presence of single (CTAB) surfactants for up to 10% Fe(2)O(3)/MCM-41 (w/w). This was explained in terms of the effect DTAB on contraction of the template micellar size to compensate for the expected size expansion upon the addition of ionic iron(III) nitrate precursor. Highly dispersed Fe(2)O(3) nanoparticles were formed in all cases even with the highest iron oxide percentage. Formation of the nanocomposites was postulated to be determined by fast nucleation and slow growth of iron oxide species, which facilitated formation of well dispersed iron oxide nanoparticles inside and on the wall of the MCM-41 material.

VARIABLE RANGE HOPPING CONDUCTION IN NiO/Al2O3 NANOCOMPOSITES

The formation and electrical properties of high surface area NiO/Al2O3 nanocomposite materials with composition ranging from 5 to 30% w/w have been studied. The temperature dependence of the DC electrical resistivity was monitored in the temperature range 350–600 K. The results revealed correlation between electrical resistivity and textural properties. The conductivity results were discussed in terms of variable-range-hopping mechanism.