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The chemical bonding within the transition-metal carbide materials MAX phaseTi3AlC2 and MXene Ti3C2Tx is investigated by X-ray absorption near-edgestructure (XANES) and extended X-ray absorption fine structure (EXAFS)spectroscopies. MAX phases are inherently nanolaminated materials that consistof alternating layers of Mn+1Xn and monolayers of an A-element from the IIIA orIVA group in the periodic table, where M is a transition metal and X is eithercarbon or nitrogen. Replacing the A-element with surface termination species Txwill separate the Mn+1Xn-layers forming two-dimensional (2D) flakes ofMn+1XnTx. For Ti3C2Tx the Tx corresponds to fluorine (F) and oxygen (O)covering both sides of every single 2D Mn+1Xn-flake. The Ti K-edge (1s) XANESof both Ti3AlC2 and Ti3C2Tx exhibit characteristic pre-edge absorption regionsof C 2p - Ti 3d hybridization with clear crystal-field splitting's while themain-edge absorption features originate from the Ti 1s -> 4p excitation, whereonly the latter shows sensitivity towards the fcc-site occupation of thetermination species. The coordination numbers obtained from EXAFS show thatTi3AlC2 and Ti3C2Tx are highly anisotropic with a strong in-plane contributionfor Ti and with a dynamic out-of-plane contribution from the Al monolayers andtermination species, respectively. As shown in the temperature-dependentmeasurements, the O contribution shifts to shorter bond length while the Fdiminishes as the temperature is raised from room temperature up to 750{\deg}C.

Local chemical bonding and structural properties in Ti3AlC2 MAX phase and Ti3C2Tx MXene probed by Ti 1s X-ray absorption spectroscopy