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SnO 2 nanoparticles are regarded as attractive, functional materials because of their versatile applications. SnO 2 nanoaggregates with single-nanometer-scale lumpy surfaces provide opportunities to enhance hetero-material interfacial areas, leading to the performance improvement of materials and devices. For the first time, we demonstrate that SnO 2 nanoaggregates with oxygen vacancies can be produced by a simple, low-temperature sol-gel approach combined with freeze-drying. We characterize the initiation of the low-temperature crystal growth of the obtained SnO 2 nanoaggregates using high-resolution transmission electron microscopy (HRTEM). The results indicate that Sn (II) hydroxide precursors are converted into submicrometer-scale nanoaggregates consisting of uniform SnO 2 spherical nanocrystals (2~5 nm in size). As the sol-gel reaction time increases, further crystallization is observed through the neighboring particles in a confined part of the aggregates, while the specific surface areas of the SnO 2 samples increase concomitantly. In addition, X-ray photoelectron spectroscopy (XPS) measurements suggest that Sn (II) ions exist in the SnO 2 samples when the reactions are stopped after a short time or when a relatively high concentration of Sn (II) is involved in the corresponding sol-gel reactions. Understanding this low-temperature growth of 3D SnO 2 will provide new avenues for developing and producing high-performance, photofunctional nanomaterials via a cost-effective and scalable method.

Elucidation of the Crystal Growth Characteristics of SnO2 Nanoaggregates Formed by Sequential Low-Temperature Sol-Gel Reaction and Freeze Drying