<p>Two-dimensional (2D) transition metal carbides and nitrides, known as MXenes, are a fast-growing family of 2D materials. MXenes 2D flakes have <i>n </i>+ 1 (<i>n</i> = 1 – 4) atomic layers of transition metals interleaved by carbon/nitrogen layers, but to-date remain limited in composition to one or two transition metals. In this study, through the use of four transition metals, we report the synthesis of multi-principal element high-entropy M<sub>4</sub>C<sub>3</sub>T<i><sub>x</sub></i> MXenes. Specifically, we introduce two high-entropy MXenes, TiVNbMoC<sub>3</sub>T<i><sub>x</sub></i> and TiVCrMoC<sub>3</sub>T<i><sub>x</sub></i>, as well as their precursor TiVNbMoAlC<sub>3</sub> and TiVCrMoAlC<sub>3 </sub>high-entropy MAX phases. We used a combination of real and reciprocal space characterization (x-ray diffraction, x-ray photoelectron spectroscopy, energy dispersive x-ray spectroscopy, and scanning transmission electron microscopy) to establish the structure, phase purity, and equimolar distribution of the four transition metals in high-entropy MAX and MXene phases. We use first-principles calculations to compute the formation energies and explore synthesizability of these high-entropy MAX phases. We also show that when three transition metals are used instead of four, under similar synthesis conditions to those of the four-element MAX phase, two different MAX phases can be formed (<i>i.e.</i> no pure single-phase forms). This finding indicates the importance of configurational entropy in stabilizing the desired single-phase high-entropy MAX over multiphases of MAX, which is essential for the synthesis of phase-pure high-entropy MXenes. The synthesis of high-entropy MXenes significantly expand the compositional variety of the MXene family to further tune their properties, including electronic, magnetic, electrochemical, catalytic, high temperature stability, and mechanical properties. </p>
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