An Al-rich AlFeSi ternary intermetallic (alpha' phase) of composition of 32.1 wt% Fe + 8.7 wt% Si + balance Al, was produced in pure form by combustion synthesis of a mixture of pure Al, Fe and Si powders. The synthesis was done in a hot press to minimise porosity and distortion. The effect of hot pressing pressure on the crystal structure and apparent density of the product was studied which showed that use of an excessive pressure leads to leakage of the transient liquid phase that is produced just prior to reaction. This results in mixtures of different AlFeSi intermetallics instead of the intended alpha' phase. Good quality alpha'' intermetallic discs of diameter 13 nm were successfully produced at 10 MPa. pressure and 600degreesC temperature. Various physical and mechanical properties of the discs are measured and reported.