Synthesis conditions and processing parameters profoundly affect the growth and morphology of nanostructures. In particular, when nanostructures are fabricated through a chemical technique such as hydrothermal, the process parameters such as reaction time, temperature, precursor concentration, and substrate orientation play a crucial role in determining the structure-property relationships. In this work, we report the hydrothermal growth of Titanium dioxide (TiO2) nanostructures as a function of these parameters and show that specific morphologies can be obtained by a variation of these parameters. A systematic study is carried out to understand the influence of reaction time (from 0.5 h to 3.0 h), reaction temperature (180 °C–200 °C), titanium precursor concentration (0.25 ml and 0.50 ml in 20 ml solution of HCl and deionized water) and substrate orientation (horizontal and tilted at an angle), and we show that significant variation in morphology- from nanowires to nanorods and then dandelions can be achieved. In particular, we demonstrate that high surface area multidirectional growth of nanorods leading to flower-like nanostructures or dandelions resulting from precipitation during the hydrothermal process. This is in contrast with previous reports on similar structures, where the role of precipitations was not analyzed. The work shows a possibility to control such growth by manipulating substrate position inside the autoclave during the hydrothermal process and will be useful for surface-dependent applications.
Designing a photocatalyst material with reduced recombination of photogenerated charges is one of the most important aspects of hydrogen generation through solar water splitting. Here, we report hydrogen generation using the TiO2/ultrathin g-C3N4 (U-g-CN) heterostructure fabricated using a unique in situ thermal exfoliation process. Multilayer g-CN is converted into U-g-CN having a high surface (∼190 m2/g) area by calcination at ∼550 °C through oxygen-induced exfoliation, which also forms a robust heterostructure with TiO2. In addition, the presence of g-CN also inhibits further growth of TiO2 nanoparticles, thereby retaining a high specific surface area. The presence of U-g-CN causes a redshift (∼0.13 eV) in the absorption edge of heterostructure compared to that of bare TiO2, which extends the light absorption capability. Addition of 40 wt. % of multilayer g-CN to TiO2 shows an enhanced H2 evolution rate, which is ∼15 times and ∼4 times higher compared to that of bare TiO2 and U-g-CN, respectively. Photoluminescence (PL) and time-resolved PL (TRPL) studies indicate a reduced recombination rate of photogenerated charge carriers with an increase in the average lifetime from 10.53 (TiO2) to 13.32 ns (TiO2/U-g-CN40). The interfacial charge transport characteristics studied through impedance spectroscopy reveal a reduced charge transfer resistance at the semiconductor–electrolyte interface, which facilitates faster charge separation due to the heterostructure formation. The band edge positions are estimated through flatband potential from the Mott–Schottky measurements and optical absorption data, indicating a type-II heterojunction. More light absorption and enhanced separation of photogenerated charges at the heterojunction interface lead to better photocatalytic H2 generation.
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