Aerogel is a high-performance thermal resistance material desired for high-temperature applications like dye-sensitized solar cells, batteries, and fuel cells. To increase the energy efficiency of batteries, an aerogel is required to reduce the energy loss arising from the exothermal reaction. This paper synthesized a different composition of inorganic− organic hybrid material by growing the silica aerogel inside a polyacrylamide (PAAm) hydrogel. The hybrid PaaS/silica aerogel was synthesized using different irradiation doses of gamma rays (10−60 kGy) and different solid contents of PAAm (6.25, 9.37, 12.5, and 30 wt %). Here, PAAm is used as an aerogel formation template and carbon precursor after the carbonization process at a temperature of (150, 350, and 1100 °C). The hybrid PAAm/silica aerogel was converted into aluminum/silicate aerogels after soaking in a solution of AlCl 3 . Then, the carbonization process takes place at a temperature of (150, 350, and 1100 °C) for 2 h to provide C/Al/Si aerogels with a density of around 0.18−0.040 gm/cm 3 and porosity of 84−95%. The hybrid C/Al/Si aerogels presented interconnected networks of porous structures with different pore sizes depending on the carbon and PAAm contents. The sample with a solid content of 30% PAAm in the C/Al/Si aerogel was composed of interconnected fibrils whose diameter was about 50 μm. The structure after carbonization at 350 and 1100 °C was a condensed opening porous 3D network structure. This sample gives the optimum thermal resistance and a very low thermal conductivity of 0.073 (w/m•k) at low carbon content (2.71% at temperature 1100 °C) and high v pore (95%) compared with carbon content 42.38% and v pore (93%) which give 0.102 (w/m•k). This is because at 1100 °C, the carbon atoms evolve to leave an area between Al/Si aerogel particles, increasing the pore size. Furthermore, the Al/Si aerogel had excellent removal ability for various oil samples.