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In this work, the redispersion of three nanocrystalline TiO2 colloids is studied: one pure and two Fe-doped titania. These three colloids are produced by an easy aqueous sol–gel synthesis using precipitation-acidic peptization of Ti precursor. For the two Fe-doped TiO2, one is doped during synthesis (primary doping) and the other is doped after the synthesis (secondary doping). The initial colloids are composed of crystalline TiO2 particles around 7 nm with good photocatalytic properties, tested on PNP degradation under visible light (wavelength >390 nm). The powders obtained by air drying of these three colloids are redispersed in water to produce colloids, which are compared to the initial colloid produced. For each colloid, five cycles of drying redispersion are achieved. The colloids are characterized by dynamic light scattering, zeta potential measurements, inductively coupled plasma–atomic emission spectroscopy, X-ray diffraction, nitrogen adsorption–desorption measurements, Mossbauer spectroscopy, diffuse reflectance spectroscopy, and photocatalytic tests. The results show that similar products are obtained between the cycles, maintaining homologous properties of colloids. This property of redispersion is mainly due to the acid (HNO3, HCl, or H2SO4) which protonates the surface of the TiO2 nanoparticle leading to high-surface charges and electrostatic repulsions between aggregates. This property can be very useful for industrial applications of this synthesis, especially as it allows the volume and weight to be reduced for transportation and storage. Moreover, results show that the pure TiO2 powder can be doped during its redispersion step. The redispersion of the TiO2 developed here is possible without surface functionalization or multiple step processes, contrary to commercial Degussa P25. A 2-year stability study of all the produced colloids has been performed by following the evolution of the macroscopic aspect and the physicochemical properties of these sols. This study showed high stability of the produced colloids.

Nanoparticulate TiO2/Rh3+ sols have been synthesized by the colloidal sol–gel route. The combination of the data measured with optical techniques such as laser diffraction, dynamic light scattering and multiple light scattering with a near-infrared light allows us to follow up the evolution of the peptization process and to establish the effect of the presence of Rh3+ on it. It is observed that the presence of rhodium ions retards the peptization step (t2) and decreases both the average particle size of the nanoparticles and the viscosity of the nanoparticulate sols. In addition, when Rh3+ is present the isoelectric point shifts up to higher pH, which suggests that chemical adsorption of the rhodium (III) cations onto the surface of the TiO2 nanoparticles is produced. The xerogels and cryogels obtained from the sols are constituted by anatase as major phase and traces of brookite. The phase transition is observed at lower temperatures for the xerogels containing rhodium (III) and at higher temperatures in the case of the cryogels. Finally, photocatalytic activity is higher in the case of the TiO2/Rh3+ sols due to the rhodium (III) effect on the electronic transitions from the valence band to the conduction band.

The stable alumina sol with an ASB/water molar ratio of 1:30 could not be obtained via the general peptization process because gelation occurred immediately. With the addition of EAcAc the stability of this sol was greatly improved. The studies using TEM, UV-V is and IR spectra revealed that a surface modification layer was formed around the Al2O3 colloidal particle through the chelating reaction of EAcAc with the surface HO-Al groups. The Al2O3 colloidal particles were therefore sufficiently capped and the growth of the colloidal particles was effectively prevented.

Hafnia nanofiltration membranes were prepared by sol-gel process from hafnium 1-methoxy-2 propoxide via colloidal route. This original molecular precursor has been synthesized and characterized by 1H NMR, mass spectroscopy, infrared and elemental analysis. Its peptization revealed to be the most efficient method to provide a highly reactive powder at a low sintering temperature. The porous volume variation and the pore diameter distribution of the hafnia powder have been studied as a function of the sintering temperature and the TGA, DTA and dilatometry study are reported. The membrane sintered at 450°C exhibited a defect-free texture with a cut-off equals to 420 Daltons and pore diameters equal to 1.9 nanometers.

The capacity of the sol-gel process of producing highly pure, homogeneous alumina-silica based materials had been demonstrated in the last few years. However, a full understanding on the mechanisms associated to sol formation and sol to gel transition has not yet been achieved and is required for the development of a new generation of nano-structurally tailored materials that will significantly enhance the technological importance of the sol-gel process. In this work, tetraethyl orthosilicate (TEOS) and aluminum isopropoxide were used to prepare materials within the entire silica-alumina system. Process parameters, such as gelation time, were correlated to variables of the initial stage of the process, such as pH, temperature of hydrolysis and water/alkoxide ratio. The obtained gels were dried at 105°C and subsequently heat treated at 500 and 1100°C for 3 hours. X-ray diffraction and infrared spectroscopy were used to characterize the materials and phase transformations. Structural information obtained from phase characterization and phase transformations was correlated to the effects of the process variables on sol formation and gelation, providing insights related to the mechanisms involved. The influence of temperature of aluminum isopropoxide hydrolysis on peptization and gelation of the mixtures was noted. The different behavior of mixtures hydrolyzed at low and high temperatures was suggested to be caused by different mechanisms of surface charge formation on the structurally different aluminum hydroxides. Monophasic and diphasic mullite xerogels were produced by changing temperature of aluminum isopropoxide hydrolysis, and led to formation of mullite and Al-Si spinel phases respectively, when treated at 1100°C.

Formation of boehmite sols from aluminium alkoxides was studied by X-ray diffraction, IR-spectroscopy, DLS (Dynamic Light Scattering) and other methods. It was found that the distortion of the boehmite crystal lattice occurs under the electrolyte sol formation processes. The surface charges were evaluated to explain the observed changes in X-ray patterns and IR-spectra of the boehmite samples and the causes that bring about these changes. The influence of the peptizing process on γ-Al2O3 specific surface was also studied.

SnO2 sols were prepared in the following way: (1) precipitation of metastannic acid with aqueous ammonia from aqueous solutions of SnCl4, (2) washing the precipitates with NH4NO3 solution and water, (3) peptization of precipitates in water, sometimes with an addition of HNO3, at elevated temperature using mechanical stirring. In those sols, sometimes diluted with water or ethanol, substrates (glass or silica derived wafers) were dipped and withdrawn at various rates. Gel coatings were converted into crystalline SnO2 by thermal treatment at 600°C. Coatings with thickness between 300–2000 A were prepared.