Ti3C2Tx MXene, a new 2D nanosheet material, is expected to be an attractive reinforcement of metal matrix composites because its surfaces are terminated with Ti and/or functional groups of –OH, –O, and –F which improve its wettability with metals. Thus, new Ti3C2Tx/Al composites with strong interfaces and novel properties are desired. To prepare such composites, the chemical stability of Ti3C2Tx with Al at high temperatures should be investigated. This work first reports on the chemical stability of Ti3C2Tx MXene with Al in the temperature range 500–700 °C. Ti3C2Tx is thermally stable with Al at temperatures below 700 °C, but it reacts with Al to form Al3Ti and TiC at temperatures above 700 °C. The chemical stability and microstructure of the Ti3C2Tx/Al samples were investigated by differential scanning calorimeter, X-ray diffraction analysis, scanning electron microscopy, and transmission electron microscopy.