A solvent-free mechanochemical route for the preparation of poly(2,5-dimethoxyaniline) hydrochloride nanostructures is developed and reported in the article. High conductivity, good crystallinity, and nanostructured morphology are observed for the prepared polymer. This polymeric powder is utilized as a cathode material in hybrid supercapacitor and its electrochemical performance is evaluated and discussed in this short report. The maximum specific capacitance of the poly(2,5-dimethoxyaniline) hydrochloride/ activated carbon hybrid supercapacitor is found to be 125 F g −1 at 1 mA cm −2 current density. The cell delivers a specific energy as high as 50 Wh kg −1 at a specific power of 97 W kg −1 and also exhibits an excellent cycle performance with more than 99% coulombic efficiency and the maintenance of 85% of its initial capacitance after 1,000 cycles.
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