Since 1976 NiAl–Ni2AlTi alloys have been known to possess elevated temperature mechanical properties approaching those of Ni-base superalloys; however, due to their apparent brittleness, little additional work has been undertaken to exploit this strength. In an attempt to instill ductility in these materials, small grain size single (Ni–45Al–5Ti) and two (Ni–40Al–10Ti) phase intermetallics were fabricated by XDTM technology and tested (XDTM is a trademark of Martin Marietta Corporation). As these compositions have the potential for being the matrix material in high temperature composites, Ni–40Al–10Ti and Ni–45Al–5Ti with 20 vol.% TiB2 in the form of ∼1 μm diameter particles were also investigated. The as-fabricated materials were fully dense and polycrystalline. The grain sizes measured ∼8 μm for Ti-poor and about 15 μm for the Ti-rich unreinforced materials but could not be determined for either TiB2 containing composite. Elevated temperature compression testing was conducted to about 8% deformation between 1200 and 1400 K with strain rates varying from ∼10−4 to ∼10−7 s−1. The majority of the tests exhibited diffuse yielding over approximately 1% strain followed by negative strain hardening. However, a few experiments resulted in steady state behavior where deformation continued under a constant stress. The flow strengths on yielding of both forms of Ni–40Al–10Ti were higher than those for the Ni–45Al–5Ti versions. For each matrix composition the addition of 20 vol.% TiB2 decreased the strength at the higher strain rates in comparison to the TiB2-free forms. During slow deformation conditions, however, the particles do provide reinforcement. Light optical microscopy of tested specimens revealed that these materials are generally quite brittle as numerous longitudinal and transverse cracks were found irrespective of the type of stress-strain behavior.