Abstract The response to thermal exposure of ball-milled Al/K 2 TiF 6 /KBF 4 powder blends was investigated to explore the potential of PM processing for the manufacture of Al–Ti–B alloys. K 2 TiF 6 starts to be reduced by aluminium as early as 220 °C when ball-milled Al/K 2 TiF 6 /KBF 4 powder blends are heated. The reaction of KBF 4 with aluminium follows soon after. The Ti and B thus produced are both solutionized in aluminium before precipitating out as Al 3 Ti and TiB 2 . All these reactions take place below the melting point of aluminium. The ball-milled Al/K 2 TiF 6 /KBF 4 powder blends heat treated at approximately 525 °C can be compacted to produce Al–Ti–B pellets with in situ formed Al 3 Ti and TiB 2 particles. These pellets are shown to be adequate grain refiners for aluminium alloys.