Ti–4Al–2Fe alloy and Ti–4Al–2Fe/TiB nano-composite were processed by a novel spark plasma sintering route. KBF4 was used as an alternative and inexpensive boron precursor to form TiB reinforcement in situ during sintering. Fe was used as an alternative to vanadium to make the (α + β) Ti matrix. The processed Ti–4Al–2Fe alloy exhibited excellent mechanical properties (CS = 1798 MPa). The TiB whiskers were distributed homogeneously and were fine (widths 130 nm and lengths from 100 nm to 3 µm). No residual TiB2 was found in the composite, in contrast with other methods. The TiB homogenised and refined the microstructure, while the hardness (710 HV), compressive strength (2414 MPa) and elastic modulus (140 GPa) all increased significantly when compared to the unreinforced alloy. © 2018, © 2018 Institute of Materials, Minerals and Mining.