In this study, Carbon Aerogels (CAs) were prepared by high-temperature supercritical drying (HTSD) in ethanol for supercapacitors (SCs). HTSD eliminates the acetone-liquid CO2 exchange step and offers a time-efficient alternative to traditional liquid CO2 drying methods. This study investigated the effect of varying carbonization temperatures (600, 700, 800, and 900 °C) on resorcinol-formaldehyde aerogel and assessed their impact on structural, morphological, compositional, and surface area properties. Amongst, CA carbonized at 700 °C (CA-7) exhibited superior performance with a specific capacitance (Cs) of 78 F/g, energy density (Ed) of 39 Wh/kg at 2 A/g in 1 M Na2SO4. After KOH activation, CA-7 demonstrated two-fold enhancement in Cs (184 F/g at 2 A/g) and three-fold in Ed (93 Wh/kg) while maintaining 98 % capacitance retention over 7000 cycles. The symmetric aqueous device (ACA\\SSM||ACA\\SSM) exhibited a Cs of 32 F/g, Ed of 25 Wh/kg, Pd of 2308 W/kg, and 88.6 % retention over 2500 cycles at 2.4 V. This research highlights the advantages of HTSD-based CA synthesis and the potential of activated CA and Na2SO4 to achieve high Ed for SCs.
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