SnO nanosheets were prepared at room temperature through a reaction between an aqueous solution of SnCl2, N2F4, and NaOH and were converted into SnO2 nanosheets without a morphological change. The SnO nanosheets were formed through a dissolution-recrystallization mechanism. Uniform and well-dispersed SnO nanosheets with the round-shape morphology were attained when the solution was treated by ultrasonic sound immediately after the addition of NaOH. The SnO2 nanosheets prepared by means of solution reduction under the ultrasonic treatment, and subsequent oxidation at 600˚C showed a high level of gas sensitivity to C2H5OH and CH3COCH3.