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Three-dimensional (3D) SnO hierarchical architectures were synthesized via a one-step dissolution–precipitation route under room temperature using SnCl2 · 2H2O and Na2CO3 as the initial reagents. The morphology and size of the prepared SnO structures could be easily tailored by alternating the solvent from deionized water with absolute ethanol. The SEM observation showed that the prepared 3D SnO hierarchical architectures consisted of nanosheets. The size of the SnO hierarchical architectures could be effectively reduced from 4–10 μm to 1–2 μm when the solvent was changed from water to ethanol while the thickness of the assembling nanosheets was reduced from 200–500 nm to 20–30 nm at the same time. The possible formation mechanism of the 3D SnO hierarchical architectures is proposed in this paper. The photodegradation of methylene blue revealed that the SnO hierarchical structures prepared using ethanol as the solvent exhibit much better photocatalytic activity due to its smaller particle size, larger specific surface area, and appropriate band structure as well. [ABSTRACT FROM AUTHOR]