Hierarchical SnO2 nanoflowers, assembled from single‐crystalline SnO2 nanosheets with high‐index (11$ \bar 3 $) and (10$ \bar 2 $) facets exposed, are prepared via a hydrothermal method using sodium fluoride as the morphology controlling agent. Formation of the 3D hierarchical architecture comprising of SnO2 nanosheets takes place via Ostwald ripening mechanism, with the growth orientation regulated by the adsorbate fluorine species. The use of Sn(II) precursor results in simultaneous Sn2+ self‐doping of SnO2 nanoflowers with tunable oxygen vacancy bandgap states. The latter further results in the shifting of semiconductor Fermi levels and extended absorption in the visible spectral range. With increased density of states of Sn2+‐doped SnO2 selective facets, this gives rise to enhanced interfacial charge transfer, that is, high sensing response, and selectivity towards oxidizing NO2 gas. The better gas sensing performance over (10$ \bar 2 $) compared to (11$ \bar 3 $) faceted SnO2 nanostructures is elucidated by surface energetic calculations and Bader analyses. This work highlights the possibility of simultaneous engineering of surface energetics and electronic properties of SnO2 based materials.
Hierarchical assembly of Ti(IV)/Sn(II)-doped SnO₂ nanosheets along titanate nanowires serving as both sacrificial templates and a Ti(IV) source is demonstrated, using SnCl2 as a tin precursor and Sn(II) dopants and NaF as the morphology controlling agent. Excess fluoride inhibits the hydrolysis of SnCl2, promoting heterogeneous nucleation of Sn(II)-doped SnO₂ on the titanate nanowires due to the insufficient oxidization of Sn(II) to Sn(IV). Simultaneously, titanate nanowires are dissolved forming Ti(4+) species under the etching effect of in situ generated HF resulting in spontaneous Ti(4+) ion doping of SnO₂ nanosheets formed under hydrothermal conditions. Compositional analysis indicates that Ti(4+) ions are incorporated by substitution of Sn sites at a high level (16-18 at.%), with uniform distribution and no phase separation. Mössbauer spectroscopy quantified the relative content of Sn(II) and Sn(IV) in both Sn(II)-doped and Ti(IV)/Sn(II) co-doped SnO₂ samples. Electrochemical properties were investigated as an anode material in lithium ion batteries, demonstrating that Ti-doped SnO₂ nanosheets show improved cycle performance, which is attributed to the alleviation of inherent volume expansion of the SnO₂-based anode materials by substituting part of Sn sites with Ti dopants.
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