The effect of reinforcements and thermal exposure on the tensile properties of aluminium AA 5083–silicon carbide (SiC)–fly ash composites were studied in the present work. The specimens were fabricated with varying wt.% of fly ash and silicon carbide and subjected to T6 thermal cycle conditions to enhance the properties through “precipitation hardening”. The analyses of the microstructure and the elemental distribution were carried out using scanning electron microscopic (SEM) images and energy dispersive spectroscopy (EDS). The composite specimens thus subjected to thermal treatment exhibit uniform distribution of the reinforcements, and the energy dispersive spectrum exhibit the presence of Al, Si, Mg, O elements, along with the traces of few other elements. The effects of reinforcements and heat treatment on the tensile properties were investigated through a set of scientifically designed experimental trials. From the investigations, it is observed that the tensile and yield strength increases up to 160 °C, beyond which there is a slight reduction in the tensile and yield strength with an increase in temperature (i.e., 200 °C). Additionally, the % elongation of the composites decreases substantially with the inclusion of the reinforcements and thermal exposure, leading to an increase in stiffness and elastic modulus of the specimens. The improvement in the strength and elastic modulus of the composites is attributed to a number of factors, i.e., the diffusion mechanism, composition of the reinforcements, heat treatment temperatures, and grain refinement. Further, the optimisation studies and ANN modelling validated the experimental outcomes and provided the training models for the test data with the correlation coefficients for interpolating the results for different sets of parameters, thereby facilitating the fabrication of hybrid composite components for various automotive and aerospace applications.