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In this study, silicone rubber (SiR) with 0, 90, and 180 parts of aluminum hydroxide (Al(OH)3, ATH) contents prepared in the laboratory was treated in a certain concentration of NO2 for 0, 12, 24, and 36 h. Fourier transform-infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and thermogravimetry (TG) were used to study the changes in the surface structure and thermal stability of SiR, as well as the influence of Al(OH)3 on the properties of SiR. According to AFM, the root-mean-square roughness of ATH-90 SiR was 192 nm, which was 2.7 times of ATH-0 SiR. With the incorporation of ATH, the surface of SiR became more susceptible to corrosion by NO2. According to FT-IR and XPS, with the increase in aging time, the side chain Si-CH3 of polydimethylsiloxane (PDMS) was oxidized gradually and a few of nitroso -NO2 groups were formed. According to TG, the incorporation of ATH caused the maximum decomposition rate temperature of PDMS to advance from 458.65 °C to 449.37 and 449.26 °C, which shows that the thermal stability of SiR degraded by adding ATH. After NO2 aging, a new decomposition stage appeared between 75 and 220 °C (stage Ⅰ), and this decomposition trend was similar to aluminum nitrate, which was proven to reduce the thermal stability of PDMS. The effects of NO2 on the surface structure and thermal stability of different ATH contents of silicone rubber were preliminarily clarified by a variety of characterization methods, which provided ideas for the development of silicone rubber resistant to NO2 aging. [ABSTRACT FROM AUTHOR]