In this study, we used one-pot polycondensation through Suzuki cross-coupling to prepare three three-dimensional (3D) conjugated microporous polymers (CMPs; Try-Ph-Th, Try-Ph-Py, and Try-Ph-TPE) containing triptycene (Try) moieties connected to thiophene (Th), pyrene (Py), and tetraphenylethene (TPE) units. Thermogravimetric analysis (TGA) revealed that the thermal stabilities of the Try-Ph-Py CMP (T d10 = 605 °C; char yield = 80 wt %) and the Try-Ph-TPE CMP (T d10 = 517 °C; char yield = 71 wt %) were higher than those of the Try-Ph-Th CMP (T d10 = 471 °C; char yield = 65 wt %) and other CMP materials. The Try-Ph-TPE CMP sample possessed a high specific surface area (up to 700 m 2 g −1 ) and pore volume (0.45 cm 3 g −1 ), based on N 2 adsorption/desorption analyses as well as superior electrochemical performance, characterized by a specific capacity of 245 F g −1 at a current density of 0.5 A g −1 . The Try-Ph-Th, Try-Ph-Py, and Try-Ph-TPE CMPs exhibited high-capacity retentions of 75.00, 85.71, and 92.85%, respectively. In addition to their extraordinary three-electrode performance, these CMPs provided high specific capacitances (53, 84.2, and 166 F g −1 , respectively) when used as real supercapacitors.
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