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Transition metal dichalcogenides (TMDCs) have received attention as atomically thin post‐silicon semiconducting materials. Tuning the carrier concentrations of the TMDCs is important, but their thin structure requires a non‐destructive modulation method. Recently, a surface‐charge transfer doping method was developed based on contacting molecules on TMDCs, and the method succeeded in achieving a large modulation of the electronic structures. The successful dopant is a neutral benzyl viologen (BV 0 ); however, the problem remains of how to effectively prepare the BV 0  molecules. A reduction process with NaBH 4  in water has been proposed as a preparation method, but the NaBH 4  simultaneously reacts vigorously with the water. Here, a simple method is developed, in which the reaction vial is placed on a hotplate and a fragment of air‐stable metal is used instead of NaBH 4  to prepare the BV 0  dopant molecules. The prepared BV 0  molecules show a strong doping ability in terms of achieving a degenerate situation of a TMDC, MoS 2 . A key finding in this preparation method is that a convection flow in the vial effectively transports the produced BV 0  to a collection solvent. This method is simple and safe and facilitates the tuning of the optoelectronic properties of nanomaterials by the easily‐handled dopant molecules.

Convection‐Flow‐Assisted Preparation of a Strong Electron Dopant, Benzyl Viologen, for Surface‐Charge Transfer Doping of Molybdenum Disulfide