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A class of 2D layered materials exhibits substantial potential for high‐performance electrocatalysts due to high specific surface area, tunable electronic properties, and open 2D channels for fast ion transport. However, liquid‐phase exfoliation always utilizes organic solvents that are harmful to the environment, and the active sites are limited to edge sites. Here, an environmentally friendly exfoliator in aqueous solution is presented without utilizing any toxic or hazardous substance and active site self‐assembly on the inert base of 2D materials. Benefiting from thin 2D/2D heterostructure and strong interfacial coupling, the resultant highly disordered amorphous NiFe/2D materials (Ti3C2 MXene, graphene and MoS2) thin nanosheets exhibit extraordinary electrocatalytic performance toward oxygen evolution reaction (OER) in alkaline media. DFT results further verify the experimental results. The study emphasizes a viable idea to probe efficient electrocatalysts by means of the synergistic effect of environmentally friendly exfoliator in aqueous solution and active site self‐assembly on the inert base of 2D materials which forms the unique thin 2D/2D heterostructure in‐suit. This new type of heterostructure opens up a novel avenue for the rational design of highly efficient 2D materials for electrocatalysis.

Two-dimensional molybdenum disulfide (2D MoS) has drawn persistent interests as one of the most promising alternatives to Pt catalysts for the hydrogen evolution reaction (HER). It is generally accepted that the edge sites of 2D MoS are catalytically active but the basal planes are inert. Activating the MoS basal plane is an obvious strategy to enhance the HER activity of this material. However, few approaches have sought to activate the basal plane. Here, for the first time, we demonstrate that the inert basal planes can be activated via the synergistic effects of nitrogen and fluorine codoping. Our first-principles calculations reveal that nitrogen in the basal plane of the fluorine- and nitrogen-codoped MoS (NF-MoS) can act as a new active and further tuneable catalytic site. The as-prepared NF-MoS catalyst exhibited an enormously enhanced HER activity compared to that of pure MoS and N-doped MoS due to the chemical codoping effect. This work will pave a novel pathway for enhancing the HER activity using the synergistic effects of chemical codoping.

Gas sensors lie at the heart of various fields ranging from medical to environmental sciences, and the demand of gas sensors is instantly expanding. However, in the face of complex gas samples, how to maintain high sensitivity while performing multiplex detection still puzzles the researchers. Here, by introducing Ti 3 C 2 T x MXene into a microfluidic gas sensor with a three-dimensional (3D) transferable SERS substrate, a powerful gas sensor having both multiplex detecting ability and high sensitivity is demonstrated. The employ of MXene endows the sensor with a universal high adsorption efficiency for various gases while the generation of in situ gas vortices in the sophisticated nanomicro structure extends the molecule residence time in SERS-active area, both leading to the increased sensitivity. In the proof-of-concept experiment, a limit of detection (LOD) of 10−50 ppb was achieved for three typical volatile organic compounds (VOCs) according to the intrinsic SERS signals of gas molecules. Besides, the welldesigned periodic 3D structure solves the general repeatability problem of SERS substrates. In addition, the detailed composition of gas mixture was revealed using classic least-square analysis (CLS) with an average accuracy of 90.6%. Further, a chromatic barcode was developed based on the results of CLS to read out the complex composition of samples visually. KEYWORDS: surface-enhanced Raman spectroscopy (SERS), volatile organic compounds (VOCs), self-assembly, MXene, Ti 3 C 2 T x , classic least-square analysis (CLS)