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Aluminium nitride (AlN) is an important technical ceramic with outstanding strength and thermal conductivity that has important applications for advanced heat sink materials and as a reinforcement for metal-based composites. In this study, we report a novel, straightforward and low-cost method to prepare AlN powder using a vacuum tube furnace for the direct nitridation of loose aluminium powder at low temperatures (down to 500 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><msup><mrow></mrow><mo>∘</mo></msup></semantics></math></inline-formula>C) under flowing high-purity nitrogen. Small amounts of magnesium powder (1 wt.%), combined with aluminium, promote nitridation. Here, we characterise the effects of time (up to 12 h) and temperature (490 to 560 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><msup><mrow></mrow><mo>∘</mo></msup></semantics></math></inline-formula>C) on nitridation with the aim to establish an effective regimen for the controlled synthesis of an aluminium nitride reinforcement powder for the production of metal matrix composites. The extent of nitridation and the morphology of the reaction products were assessed using scanning electron microscopy and X-ray diffraction analyses. AlN was detected for all nitriding temperatures ≥ 500 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><msup><mrow></mrow><mo>∘</mo></msup></semantics></math></inline-formula>C, with the highest yields of 80% to 85% obtained at 530 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><msup><mrow></mrow><mo>∘</mo></msup></semantics></math></inline-formula>C for times ≥ 1 h. At this temperature, nitridation proceeded rapidly, and there was extensive agglomeration of the reaction products making it difficult to reprocess into powder. At lower temperatures around 510 <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><msup><mrow></mrow><mo>∘</mo></msup></semantics></math></inline-formula>C, a relatively high proportion of AlN was attained (>73% after 6 h) while retaining excellent friability so that it could be manually reprocessed to powder. The synthesised reinforcement consisted of micro- or nano-crystalline AlN comingled with metallic aluminium. The ratio of AlN and metallic aluminium can be readily controlled by varying the nitriding temperature. This provides a flexible and accessible method for the production of AlN-reinforcement powders suited to the production of metal matrix composites.