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Transition metal dichalcogenide (TMD) alloys and heterostructures are attracting increasing attention thanks to their unique electronic, optical, and interfacial properties. However, the growth fundamental of TMD alloys and heterostructures during one-step growth is still beyond understanding. Here, thermogravimetric (TG/DTG) technology is introduced to predict the evolution of the precursor (MoO3 and WO3) concentration in the vapor during growth. We establish the correlation between precursor concentration and the corresponding growth behavior. TG/DTG predication suggests that tuning precursor temperature and powder ratio can alter their concentration in the vapor, well explaining the formation of MoxW1-xSe2 alloy or MoSe2-WSe2 heterostructure at different growth conditions. Based on the TG/DTG analysis, we further design and grow a complex MoSe2-MoxW1-xSe2-WSe2 heterostructure and MoxW1-xS2 monolayer alloys, confirming the validity of TG/DTG prediction in TMD crystal synthesis. Thus, employing TG/DTG to predict the synthesis of two-dimensional materials is of importance to understand the TMD growth behavior and provide guidance to the desired TMD heterostructure formation for future photoelectric devices.