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Ti₃C₂T_xMXene membranes have attracted considerable interest due to their exceptional water transport properties, yet the role of cation intercalation on governing transport remains poorly understood. In this experimental and theoretical study, it shows how intercalation with K⁺, Na⁺, Li⁺, Ca²⁺, and Mg²⁺modulates both the nanochannel architecture and water flux of Ti₃C₂T_xmembranes. Unlike in graphene oxide analogs, cations with larger hydration diameters in Ti₃C₂T_xexpand the interlayer spacing, widening flow channels, enhancing slip length of these nanochannels, and boosting water flux from 31.45 to 61.86 L m⁻² h⁻¹. To overcome intrinsically poor adhesion of Ti₃C₂T_xto polymeric supports, this study incorporates a thin polyvinyl‐alcohol interlayer, which substantially enhances mechanical robustness and structural integrity. Together, these findings elucidate how cation hydration controls water transport and offer a flexible strategy for tailoring MXene membrane performance. 

The incorporation of a glassy material into a self-assembled nanoparticle (NP) film can produce highly loaded nanocomposites, with improved photostability under the right conditions. 

MXenes have demonstrated potential for various applications owing to their tunable surface chemistry and metallic conductivity. However, high temperatures can accelerate MXene film oxidation in air. Understanding the mechanisms of MXene oxidation at elevated temperatures, which is still limited, is critical in improving their thermal stability for high-temperature applications. Here, we demonstrate that Ti ${}_3$C ${}_2$T ${}_x$MXene monoflakes have exceptional thermal stability at temperatures up to 600 ${}^{°}$C in air, while multiflakes readily oxidize in air at 300 ${}^{°}$C. Density functional theory calculations indicate that confined water between Ti ${}_3$C ${}_2$T ${}_x$flakes has higher removal energy than surface water and can thus persist to higher temperatures, leading to oxidation. We demonstrate that the amount of confined water correlates with the degree of oxidation in stacked flakes. Confined water can be fully removed by vacuum annealing Ti ${}_3$C ${}_2$T ${}_x$films at 600 ${}^{°}$C, resulting in substantial stability improvement in multiflake films (can withstand 600 ${}^{°}$C in air). These findings provide fundamental insights into the kinetics of confined water and its role in Ti ${}_3$C ${}_2$T ${}_x$oxidation. This work enables the use of stable monoflake MXenes in high-temperature applications and provides guidelines for proper vacuum annealing of multiflake films to enhance their stability. 

In compositionally complex materials, there is controversy on the effect of enthalpy versus entropy on the structure and short-range ordering in so-called high-entropy materials. To help address this controversy, we synthesized and probed 40 M4AlC3 layered carbide phases containing 2 to 9 metals and found that short-range ordering from enthalpy is present until the entropy increases enough to achieve complete disordering of the transition metals in their atomic planes. We transformed all these layered carbide phases into two-dimensional (2D) sheets and showed the effects of the order vs. disorder on their surface properties and electronic behavior. This study suggests the key effect that the competition between enthalpy and entropy has on short-range order in multi-compositional materials.