In situ synthesis of AlN nanoparticles by solid state reaction from plasma assisted ball milling Al and diaminomaleonitrile mixture

In this paper, Aluminum nitride (AlN) nanoparticles from solid state reaction of diaminomaleonitrile (DN) with aluminum (Al) are synthesized by plasma assisted high energy ball milling (p-milling). The structure and morphology of the p-milling products are characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier Transform infra red (FT-IR), Differential scanning calorimetry and Thermal gravimetry (DSC–TG). The XRD results show a correlation between milling time and crystallite size, lattice distortion, specific surface area, and conversion rate of AlN. About 90% AlN has been obtained and specific surface area can reach 52 m² g⁻¹ at p-milling 14 h. The FT-IR measurements show the solid reaction starts with the deammoniation of DN molecules, followed by the formation of AlN powder as the main solid products after p-milling 8 h. The DSC–TG results indicate that DN starts to disintegrate from 180 °C to 450 °C by the elimination of the N–H and C≡N groups, continue increasing temperature leads to the formation of AlN at 673 °C. The activation energy of reaction from p-milling Al and DN mixture is calculated by the Kissinger equation and is about 353.5 kJ/mol. Meanwhile, the formation mechanism of AlN in a p-milling process is also investigated.