Summary: | In this study, macroporous graphene aerogels (GAs) were synthesized by chemical reduction of graphene oxide sheets and were used as a support material for in situ synthesis of conductive poly(para-phenylenediamine) (p(p-PDA)). The in situ synthesis of p(p-PDA) in GA was carried out by using a simple oxidation polymerization technique. Moreover, the prepared conductive p(p-PDA) polymers in the networks of GAs were doped with various types of acids such as hydrochloric acid (HCl), nitric acid (HNO<sub>3</sub>), sulfuric acid (H<sub>2</sub>SO<sub>4</sub>), phosphoric acid (H<sub>3</sub>PO<sub>4</sub>), respectively. The prepared GA and different acid-doped forms as GA/p(p-PDA) composites were characterized by FT-IR, TGA, and conductivity measurements. The observed FT-IR peaks at 1574 cm<sup>−1</sup>, and 1491 cm<sup>−1</sup>, for stretching deformations of quinone and benzene, respectively, confirmed the in situ synthesis of P(p-PDA) polymers within GAs. The conductivity of GAs with 2.17 × 10<sup>−4</sup> ± 3.15 × 10<sup>−5</sup> S·cm<sup>−1</sup> has experienced an approximately 250-fold increase to 5.16 × 10<sup>−2</sup> ± 2.72 × 10<sup>−3</sup> S·cm<sup>−1</sup> after in situ synthesis of p(p-PDA) polymers and with HCl doping. Conductivity values for different types of acid-doped GA/p(p-PDA) composites were compared with the bare p(p-PDA) and their undoped forms. Moreover, the changes in the conductivity of GA and GA/p(p-PDA) composites upon CO<sub>2</sub> gas exposure were compared and their sensory potential in terms of response and sensitivity, along with reusability in CO<sub>2</sub> detection, were evaluated.
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