In this study, flakes of molybdenum disulfide (MoS2) with controlled size and thickness are prepared through sequential solvent exchange method by sonication in dimethylformamide (DMF) and N-methyl-2-pyrrolidone (NMP) solvents. While NMP acts more effectively in reducing the thickness of flakes, DMF shows better potential in conserving the lateral size of nanosheets. The distribution of size and thickness of nanoflakes as a function of sonication time verifies that extended sonication results in dramatic drop of the dimension of the exfoliated flakes. This technique leads to the formation of few-layered MoS2 flakes without further drop of their lateral dimensions. It has been observed that by exposing the bulk MoS2 powders to oxygen plasma, the exfoliation process is accelerated without converting to 2H-MoS2 structures. Finally, a phototransistor has been fabricated based on few-layered MoS2 layers with a field effect mobility of ∼2.1 cm2 V–1 s–1 showing a high response to laser excitation of 532 nm wavelength.
