To enhance the high temperature strength of aluminides, NiAl–iB2 composites with particulate contents up to 30 vol. pct. were made by XDTM synthesis and hot pressed to full density. Microstructures of these composites were characterized by optical, scanning and transmission electron microscopy (TEM). The average size of the TiB2 particles was about 1 μm, and the average grain size of the NiAl matrix was on the order of 10 μm. Elevated temperature compression testing was conducted on these composites in air at 1200 and 1300 K with strain rates varying from −10−4 to −10−7 s−1. Flow strengths were found to increase with increasing TiB2 content; for example, the 20 vol. pct. TiB2 composite was three times stronger than unreinforced NiAl. Post test TEM analysis showed that the primary feature of the dislocation substructure of deformed NiAl was well defined subgrain boundaries, whereas the structure of the higher volume fraction composites consisted of a very high density of tangled dislocations, loops and subgrain boundaries connecting particles. These observations suggest that TiB2 particles can stabilize a completely different dislocation structure than that normally found in NiAl.