Mechanically alloyed aluminum–iodoform composites were prepared with iodine concentration of 20 wt%. Ball milling at both room temperature and liquid nitrogen temperature was explored. Material characterization by electron microscopy and X-ray diffraction showed no difference between samples milled at different temperatures. However, samples prepared at room temperature aged rapidly. Thermo-gravimetric measurements quantifying release of iodine upon heating confirmed that cryogenic milling was necessary to stabilize iodoform in the Al-matrix. Iodine was released upon heating in four distinct stages. The oxidation of the prepared materials was also studied using thermo-gravimetric analysis and two main oxidation steps were detected. The ignition temperatures were determined for powders coated onto a metal filament heated electrically at 103–104 K min−1. The ignition temperatures of the prepared materials were noticeably lower compared to the Al · I2 composite prepared using a similar cryo-milling approach. The combustion characteristics determined using constant volume explosions of aerosolized powders were found to be similar to those of Al · I2 composite. The maximum pressure and rate of pressure rise observed in the latter experiments were greater than for pure aluminum powders with comparable particle sizes.