The shift from traditional, single‐component metals and alloys continues, and researchers are currently investigating alternative materials. This evolution has led to the creation of innovative materials, including hybrid metal‐matrix composites. The present study aims to investigate the microstructural, surface morphological, and thermal properties of a novel Al7075/TiO2/Kaoline hybrid metal‐matrix composite prepared using high‐energy ball milling and sintering methods. In this study, phases related to the composite components are formed depending on the milling time, no undesirable phase is formed, but the peak intensities decreas as the milling time increases. Particle size increases from 63 to 215 μm with increasing milling time. Increasing the kaoline reinforcement ratio and sintering temperature increases the microhardness from 62.27 ± 2 to 75.83 ± 2 HV, and reduces the friction coefficient from 0.82 ± 0.01 to 0.62 ± 0.01. The wear rate of the composite without kaoline addition is 2.1 (mm3 m−1) × 10−3, while with 6 wt% kaoline addition, it decreases to 1.5 (mm3 m−1) × 10−3. There are no cracks in the composite other than plastic deformation due to sintering and wear. Peaks indicating endothermic and exothermic reactions during continuous heating occurr in the 635–750 °C temperature range.
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