Herein we report the details of attempts to produce phase pure Zr3AlC2. Though previous
methods have reportedly produced > 80% phase purity, through the addition of extra elements. It
is not consistent with cases of samples containing as low as 4 % MAX phase content using the same
method and elemental powders. It was determined through this work that the loss of aluminium
through potential evaporation is one of the major causes of poor MAX phase yield. Therefore
modifications to the heating regime were attempted to try and limit the rate of aluminium loss, so
far this has guaranteed > 70% phase purity consistently. Phase composition was measured through
XRD at different stages of heating and showed that there are key Zr-Al based intermetallics that
form at lower temperatures (600-700 ◦C), suggesting that the reaction pathway does not involve
carbon until higher temperatures. The production of phase pure material is desired so that the
materials properties can be directly studied. Of particular interest is the relationship between
structure and strain partitioning within the unit cell. This is complex to measure but Raman
spectroscopy, is sensitive to even slight changes in bond lengths. Therefore it allows a potential
method to measure these properties and has been explored here. It is possible to relate stresses
in materials to peak shifts observed. The MAX phases show peaks representative of shear and
vibrations along C, for both the M-A and M-X layers. Allowing for specific analysis of the strain
in the individual layers. Investigations were performed on the MAX phase T i3SiC2 as a common
MAX phase, with stress introduced through nano-indentation and compression. Currently this
can only produce qualitative results, however, it shows a far greater peak shift for the M-X layers
which was not expected as it is the less ductile of the two layers.