Rapid solidification techniques, such as gas atomisation, have been widely implemented in metallic alloys/composites to increase solid solubility, avoid or mitigate segregation phenomena, and favour metastable phase formation to enhance performance. Particularly, gas atomisation can enhance the solid solubility of low diffusion coefficient elements like Fe, Ni, Mn, Zr, and Cr in the α-Al matrix, yielding metastable phases. As a result, Al alloys exhibit excellent strength at high temperatures. In this study, the AISI 304L alloy was employed to introduce Fe, Ni, and Cr elements into the AlSi10Mg alloy through gas atomisation, resulting in the formation of two distinct hypereutectic AlFe-based alloys: AlFe9Si8Cr2Ni and AlFe18Si8Cr5Ni2. Gas-atomised alloy powders were separated into different size fractions by sieving and characterised using X-ray diffraction, differential scanning calorimetry, optical microscopy, and scanning electron microscopy. Microstructural analyses revealed dendritic patterns with distinct phases, highlighting the influence of the alloying element content on the solidification processes. Furthermore, a synergic evaluation of the XRD and EDS analysis results allowed the identification of intermetallic phases and their distribution in the two systems.