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MXenes have gained great attention in various fields because of their fascinating properties; however, the preparation of few-layered MXene powders is still limited by serious restacking of MXene nanosheets. Herein, for the first time, we have demonstrated an effective ammonium ion route to fundamentally address restacking and aggregation of the MXene nanosheets, using a solution-phase flocculation method (NH4+ method and modified NH4+ method) for large-scale preparation of few-layered Ti3C2T x MXene powders in large quantities. The as-prepared few-layered MXene nanosheet powders show large size in the ab plane without the restacking phenomenon even at scanning electron microscopy measurements of 400× magnification, demonstrating the effectiveness of the proposed method. The method is also suitable for large-scale synthesis of other few-layered MXene powders, including Nb4C3T x , V2CT x , Nb2CT x , etc., providing a general approach for the preparation of various few-layered MXene nanosheet powders, which represents a significant result for the development of MXenes.

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