In this study, we have used the one-pot polycondensation method to prepare novel 2D conjugated microporous polymers (Th-F-CMP) containing thiophene (Th) and fluorene (Fl) moieties through the Suzuki cross-coupling reaction. The thermogravimetric analysis (TGA) data revealed that Th-F-CMP (Td10 = 418 °C, char yield: 53 wt%). Based on BET analyses, the Th-F-CMP sample displayed a BET specific surface area of 30 m2 g−1, and the pore size was 2.61 nm. Next, to show the effectiveness of our study, we utilized Th-F-CMP as a fluorescence probe for the selective detection of Fe3+ ions at neutral pH with a linear range from 2.0 to 25.0 nM (R2 = 0.9349). Furthermore, the electrochemical experimental studies showed that the Th-F-CMP framework had a superior specific capacity of 84.7 F g−1 at a current density of 0.5 A g−1 and outstanding capacitance retention (88%) over 2000 cycles.
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