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The importance and widespread need for accurate pH monitoring necessitates the fabrication of new pH sensors with high sensitivity that can be used in a variety of environments. However, typical pH sensors have certain limitations ( e.g. , glass electrodes are fragile and require consistent upkeep, colorimetric pH strips are single use and inaccurate). Herein, we examine the pH-response of multilayers consisting of Ti 3 C 2 T x nanosheets and polycations fabricated using layer-by-layer (LbL) assembly. The MXene sheets themselves are pH-responsive due to their hydroxyl surface groups, and this effect may be amplified with the choice of an appropriate polycation. Specifically, the performance of multilayers assembled with the strong electrolyte poly (diallyldimethylammonium) (PDADMA) or pH-sensitive branched polyethylenimine (BPEI) is compared. As expected, the use of a pH-sensitive constituent leads to a 464% increase in pH sensitivity (116 kΩ pH −1 unit vs. 25 kΩ pH −1 unit) as compared to PDADMA. This is due to the conformational changes that BPEI undergoes with (de)protonation as pH changes. Further comparisons with reduced graphene oxide (rGO), which is far less pH responsive, confirm the unique pH responsivity of MXene nanosheets themselves. The ability to enhance response to particular stimuli by changing the constituent polycation demonstrates promise for future use of MXenes in resistive sensors for a variety of stimuli. 

The oxidation of 2D MXenes jeopardizes their shelf life, both in colloidal dispersions and in functional devices. Certain compounds have been shown to effectively mitigate oxidation of MXenes (such as sodium L‐ascorbate, ascorbic acid, and polyanions), but the nature of interaction between these antioxidants and MXene remains unknown, which impedes the future selection and design of improved protection. This work systematically examines the interactions between three classes of organic antioxidant candidates, α‐hydroxy acids, polycarboxylic acids, and phenols with Ti_n+1C_nT_xMXenes, specifically Ti₃C₂T_xand Ti₂CT_x. Interestingly, while some antioxidants provide no protection for the MXenes, and some antioxidants even accelerate their degradation, three antioxidants (e.g., citric acid, tartaric acid, and oxalic acid) protect the MXene nanosheets exceptionally well, showing minimum MXene degradation after the 14‐day storage period. Analysis of the antioxidants’ molecular structure and efficacy suggests that chelation interactions with the transition metal atoms of the nanosheets play a key role in effective protection of MXenes from oxidation.