Al matrix composite, reinforced with the in situ synthesized 3C–SiC, MgAl2O4, and MgO grains, was produced via the casting process using phenolic resin pyrolysis products in flash mode. The contents and microstructure of the composites’ fracture characteristics were analyzed by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Mechanical properties were tested by universal testing machine. Owing to the strong propulsion formed in turbulent flow in the pyrolysis process, nano-ceramic grains were formed in the resin pyrolysis process and simultaneously were homogeneously scattered in the alloy matrix. Thermodynamic calculation supported that the gas products, as carbon and oxygen sources, had a different chemical activity on in situ growth. In addition, ceramic (3C–SiC, MgAl2O4, and MgO) grains have discrepant contents. Resin pyrolysis in the molten alloy decreased oxide slag but increased pores in the alloy matrix. Tensile strength (142.6 ± 3.5 MPa) had no change due to the cooperative action of increased pores and fine grains; the bending and compression strength was increasing under increased contents of ceramic grains; the maximum bending strength was 378.2 MPa in 1.5% resin-added samples; and the maximum compression strength was 299.4 MPa. Lath-shaped Si was the primary effect factor of mechanical properties. The failure mechanism was controlled by transcrystalline rupture mechanism. We explain that the effects of the ceramic grains formed in the hot process at the condition of the resin exist in mold or other accessory materials. Meanwhile, a novel ceramic-reinforced Al matrix was provided. The organic gas was an excellent source of carbon, nitrogen, and oxygen to in situ ceramic grains in Al alloy.
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