In this work core/shell composite polymer/TiO₂ nanofibers and from those TiO₂ nanotubes were prepared. First, poly(vinyl alcohol) (PVA) and poly(vinylpyrrolidone) (PVP) fibers were synthetized by electrospinning. They were covered with a 100 nm thick amorphous TiO₂ layer by atomic layer deposition at 50 °C. Later the polymer core was removed by two different methods: dissolution and annealing. In the case of dissolution in water, the as-prepared TiO₂ nanotubes remained amorphous, while when annealing was used to remove the polymers, the TiO₂ crystallized in anatase form. Due to this, the properties of amorphous and crystalline TiO₂ nanotubes with exactly the same structure and morphology could be compared. The samples were investigated by SEM-EDX, ATR-IR, UV-Vis, XRD and TG/DTA-MS. Finally, the photocatalytic properties of the TiO₂ nanotubes were studied by decomposing methyl-orange dye under UV light. According to the results, crystalline anatase TiO₂ nanotubes reached the photocatalytic performance of P25, while amorphous TiO₂ nanotubes had observable photocatalytic activity.

In this paper, we combine the atomic layer deposition synthesis method of inverse opal with the hydrothermal growth of nanorods. From 460 nm polystyrene nanospheres opal crystals were produced using vertical deposition on Si wafers. The opal templates were covered with ZnO by atomic layer deposition. High temperature annealing was used to remove the polystyrene nanospheres to obtain the inverse opal structure. For the hydrothermal growth of ZnO nanorods, two production routes were analysed: hydrothermal reaction before and after the removal of the template. The two paths produced two distinct structures, one with plate like formations and one with nanorods, respectively. Also, the sample modified by the hydrothermal growth after the annealing showed slight differences in optical properties compared to the regular inverse opal. Morphology, composition and structure of the samples were explored using SEM, EDX and XRD. Optical properties were investigated with reflectance UV–Vis spectroscopy. Thermal stability of the polystyrene opal was determined using TG.

In comparison to conventional nano-infiltration approaches, the atomic layer deposition (ALD) technology exhibits greater potential in the fabrication of inverse opals (IOs) for photocatalysts. In this study, TiO₂ IO and ultra-thin films of Al₂O₃ on IO were successfully deposited using thermal or plasma-assisted ALD and vertical layer deposition from a polystyrene (PS) opal template. SEM/EDX, XRD, Raman, TG/DTG/DTA-MS, PL spectroscopy, and UV Vis spectroscopy were used for the characterization of the nanocomposites. The results showed that the highly ordered opal crystal microstructure had a face-centered cubic (FCC) orientation. The proposed annealing temperature efficiently removed the template, leaving the anatase phase IO, which provided a small contraction in the spheres. In comparison to TiO₂/Al₂O₃ plasma ALD, TiO₂/Al₂O₃ thermal ALD has a better interfacial charge interaction of photoexcited electron–hole pairs in the valence band hole to restrain recombination, resulting in a broad spectrum with a peak in the green region. This was demonstrated by PL. Strong absorption bands were also found in the UV regions, including increased absorption due to slow photons and a narrow optical band gap in the visible region. The results from the photocatalytic activity of the samples show decolorization rates of 35.4%, 24.7%, and 14.8%, for TiO₂, TiO₂/Al₂O₃ thermal, and TiO₂/Al₂O₃ plasma IO ALD samples, respectively. Our results showed that ultra-thin amorphous ALD-grown Al₂O₃ layers have considerable photocatalytic activity. The Al₂O₃ thin film grown by thermal ALD has a more ordered structure compared to the one prepared by plasma ALD, which explains its higher photocatalytic activity. The declined photocatalytic activity of the combined layers was observed due to the reduced electron tunneling effect resulting from the thinness of Al₂O₃.

Vertically aligned carbon nanotubes (VACNTs or “CNT forest”) were decorated with semiconductor particles (TiO₂ and ZnO) by atomic layer deposition (ALD). Both the structure and morphology of the components were systematically studied using scanning (SEM) and high resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX), Raman spectroscopy, and X-ray diffraction (XRD) methods. Characterization results revealed that the decoration was successful in the whole bulk of VACNTs. The effect of a follow-up heat treatment was also investigated and its effect on the structure was proved. It was attested that atomic layer deposition is a suitable technique for the fabrication of semiconductor/vertically aligned carbon nanotubes composites. Regarding their technological importance, we hope that semiconductor/CNT forest nanocomposites find potential application in the near future.

Among the chemical methods in the liquid phase, the sol–gel technique is a versatile and efficient method for pure or doped metal oxide films or powders preparation, showing some advantages over other preparation techniques (high homogeneity, the possibility to introducing dopants in large amount, low processing temperature and control over the stoichiometry). Combining the sol–gel (SG)method with the effect of ultrasounds(US) or microwaves (MW) leads to improving the sol–gel procedure. The microwave-assisted sol–gel method is most frequently used for obtaining nanocrystalline, monodispersed oxide nanoparticles, or to transform amorphous gels into well-crystallized nanopowders. Less studied is the influence of the microwaves on the sol–gel reactions in solutions. The benefit of using microwave-assisted sol–gel preparation highly depends on the reagents used and on the composition of the studied systems. In the present chapter, results on the influence of the microwaves on the chemical reactions that take place during the sol–gel synthesis and on the properties of the resulted samples are discussed.