The solid state reaction of diaminomaleonitrile (DAMN) with aluminum via both mechanochemical and thermal treatment routes was studied by X-ray diffraction and Fourier transform infrared spectroscopy. During the milling process, the reaction starts with the deammoniation of the DAMN molecules, followed by the formation of nanostructured AlN powder as the main solid product after milling for 7 h. The reactivity of the mixed powder was also investigated during conventional thermal treatment process using differential scanning calorimetry, derivative thermogravimetry and thermogravimetric analysis. The results reveal that DAMN starts to be polymerized at 192 °C by the elimination of the amine groups. Furthermore, increasing the annealing temperature leads to the formation of a nitrogen-containing carbonaceous material with the structure similar to non-crystalline carbon. However, no evidence for the formation of AlN was observed in the annealed samples even at temperatures as high as the Al melting point.

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