Recently, the ultrasound-assisted sol-gel synthesis procedure of mesoporous titania (TiO₂) photocatalysts caught the researcher’s attention, due to the physicochemical properties enhancement of the resulting titania nanomaterials. Thus, by varying different synthesis parameters particular characteristics could be obtained. In the present study, the ultrasound pulse on/off ratio has been considered and the effect of the envisaged parameter on the textural, morphological, and optical features of titania nanomaterial has been investigated. Therefore, X-ray Diffraction (XRD), Fourier-Transform Infrared spectroscopy (FTIR), N₂-sorption measurements, SEM imaging, and UV-Vis Diffuse Reflectance spectroscopy (UVDR) have been used. And further, the photocatalytic activity of the prepared TiO₂ materials was evaluated by the features developed about the applied ultrasound pulse on/off ratio as 1/1, 2/1, 3/1, 4/1, 1/3 and 2/2. It was found that the ultrasound pulse on/off ratio considered in the synthesis procedure of titania leads to TiO₂ materials with different textural (S_BET = 98–156 m²/g), morphological, and optical (E_g = 3.1–3.2 eV) characteristics. For this reason, TiO₂ nanomaterials prepared were found to exhibit suitable features for photocatalytic applications. Thus, the TiO₂ 4.1 sample prepared at 4/1 ultrasound pulse on/off ratio revealed the highest photodegradation efficiency of Congo Red dye (98.28%) as the results of photocatalytic tests show. More than that, a possible reaction mechanism of the CR photodegradation process through the contribution of reactive oxygen species (·HO, ·O₂⁻), holes (h⁺), and electrons (e⁻) of developed titania photocatalyst was proposed.

A mesoporous titania structure has been prepared using the ultrasound-assisted sol-gel technique in order to find out a way to tailor its structure. The TiO₂ obtained was compared to the same version of titania but synthesized by a conventional sol-gel method with the objective of understanding the effect of ultrasound in the synthesis process. All synthesis experiments were focused on the preparation of a titania photocatalyst. Thus, the anatase photocatalytic active phase of titania was proven by X-ray diffraction. Additionally, the ultrasonation treatment proved to increase the crystallinity of titania samples, being one of the requirements to having good photocatalytic activity for titania. The influence of surfactant/titania precursor weight ratio on the structural (XRD), textural (N₂-sorption measurements), morphological (TEM), surface chemistry (FTIR) and optical properties (UVDR) was investigated. It was observed that the crystallite size, specific surface area, band gap energy and even photocatalytic activity was affected by the synergism occurring between cavitation effect and the surfactant/titania precursor weight ratio. The study yielded interesting great results that could be considered for further application of ultrasound to tailor mesoporous titania features via sol-gel soft template synthesis, against conventional sol-gel process.

Up to now, the use of TiO₂ has been considered a promising advanced technology for organic pollutants removal from air or water, since it has high biological and chemical stability, high photoactivity, low toxicity, and low-cost production. However, there are issues to be addressed in enhancing TiO₂ performance, and one of the current key issues is redesigning UV-active photocatalysts and making them active in the visible region of the electromagnetic spectrum. This way, solar light absorption will be insured, and thus, a more efficient photocatalyst could be obtained. For this reason, conjugated polymers and their derivatives are considered to act as photosensitizers, being able to shift the TiO₂ activity from the UV to the visible region. Therefore, this study focuses on the synthesis of TiO₂/conjugated polymer systems, which was accomplished by the deposition of poly-3,4-ethylene-dioxy-thiophene (PEDOT [-C₆H₄O₂S-]_n), a low-band semiconductor with an excellent stability due to its extending π-conjugated electron system, on titania nanoarchitecture. First of all, a TiO₂ nanoarchitecture was synthesized by an ultrasound-assisted sol–gel method. Then, TiO₂/PEDOT systems were obtained and characterized by using different techniques such as X-ray diffraction, Fourier Transform Infrared Spectroscopy, Scanning Electron Microscopy, UV–Vis diffuse reflectance, and N₂ sorption measurements. The synthesized composites confirmed their mesoporosity and lower band gap values compared to bare titania, which clearly shows the ability to work as photocatalysts under visible-light activity. Further, we demonstrated that an organic pollutant, Congo Red dye, used as a model molecule could be photodegraded with the synthesized TiO₂/PEDOT systems, with efficiencies of up to 95% in the case of T_convPEDOT under UV light and up to 99% for T_convPEDOT under visible-light irradiation, accomplishing in this way a successful synthesis of visible-light-activated titania photocatalyst.

Porous titania was successfully synthesized by an ultrasound-assisted sol-gel route. The synthesis process was empirically modeled and optimized using the response surface methodology (RSM). Input variables adopted for optimization dealt with the weight ratio of precursors (r) and the sonication time (t), representing the used factors in the synthesis procedure. With regard to application, the synthesized TiO₂ samples were tested for the photodegradation of two water-soluble organic pollutants under UV–Vis irradiation. Optimal conditions for the efficient pollutants’ photodegradation were found to involve a precursors ratio of 3 and a sonication time of 60 min. Thus, the M5 sample prepared under the founded optimal conditions yielded the maximal removal efficiencies of 98.4% and 46.3% for the photodegradation of CR dye and 2,4-D herbicide, respectively. In addition, the photodegradation kinetics revealed the pseudo first-order rate constants, showing the photodegradation of CR (k₁ = 8.86 × 10⁻² min⁻¹) by M5 sample is about 1.3-fold faster than the photodegradation of 2,4-D pesticide (k₂ = 6.84 × 10⁻² min⁻¹).

CoFe 2 O 4 and NiFe 2 O 4 spinel ferrites were obtained by microwave-assisted sol–gel combustion synthesis using three different types of chelating/combustion agents: maleic acid, citric acid, and urea. The nanomaterials produced were characterized from the structural, morphological, textural, and magnetic viewpoints. The spinel ferrites prepared were employed as adsorbents for the removal of Orange-II dye from synthetic wastewaters. The nickel ferrite sample prepared using urea as fuel exhibited distinctive properties such as the smallest crystallite size and the highest specific surface area. Likewise, this material was the most efficient for the adsorption of the organic pollutant (50.32 mg/g) from aqueous solutions.