Incorporation of layers of noble metals in non-van der Waals layered materials may be used to form novel layered compounds.Recently, we demonstrated a high-temperature-induced exchange process of Au with Si in the layered phase Ti 3 SiC 2 , resulting in the formation of Ti 3 AuC 2 and Ti 3 Au 2 C 2 . Here, we generalize this technique showing that Au/Ti 2 AlC and Au/Ti 3 AlC 2 undergo an exchange reaction at 650 8C to form Ti 2 Au 2 C and Ti 3 Au 2 C 2 and determine their structures by electron microscopy, X-ray diffraction, and ab initio calculations. These results imply that noble-metal-containing layered phases should be possible to synthesize in many systems.The metal to be introduced should be inert to the transition-metal carbide layers, and exhibit negative heat of mixing with the initial A element in a liquid phase or two-phase liquid/solid region at the annealing temperature.Phases with nanolaminated or atomically layered structures are an extensive research topic for the synthesis of novel materials and two-dimensional structures. Layered ceramics constitute a large class of materials including both van der Waals (vdW) materials, such as graphite or transition-metal dichalcogenides, and non-vdW solids. vdW materials are commonly applied for the formation of new two-dimensional materials, and allow for intercalation of foreign species, both ionic such as in Li-ion batteries 1,2 and neutral as in the case of intercalation of zerovalent noble metals in vdW solids. [3][4][5] In contrast, incorporation of noble-metal layers in non-vdW layered materials to form novel compounds is an outstanding challenge. Recently, we demonstrated a high-temperature-induced exchange process of Au with Si in the layered phase Ti 3 SiC 2 , resulting in the formation of the novel Ti 3 AuC 2 and Ti 3 Au 2 C 2 phases by an ordered replacement of the A-layer crystal planes; from Si-planes to Au or Au 2 planes.6 Furthermore, Ir-exchange with Au in Ti 3 AuC 2 yielded the new phase Ti 3 IrC 2 . 6 The starting phase Ti 3 SiC 2 is an archetype member of the M n+1 AX n phases, a large family of layered transition-metal carbides and nitrides [7][8][9][10]