Ferrocene (Fc) functionalization of macroporous polyacrylamide‐based cryogel (PAAm‐Epx) is achieved by click chemistry. For this purpose, firstly, PAAm‐Epx cryogel with azide functionality (PAAm‐N3) is prepared by using acryalmide (AAm) as the monomer and allyl glycidyl ether (AGE) as the co‐monomer followed by subsequent ring opening reaction of epoxide ring of AGE in acidic medium. Azide groups of PAAm‐N3 is then modified with ethynyl ferrocene, leading to the redox active cryogel (PAAm−Fc) together with preserving the unique characteristic properties of the virgin PAAm‐Epx cryogel. Swelling, mechanical and morphological behaviours of PAAm‐Epx, PAAm‐N3 and PAAm−Fc are investigated. Detailed characterization of the PAAm−Fc is carried out by several techniques such as FTIR (Fourier Transform Infrared Spectroscopy), Scanning electron microscopy with energy dispersive X‐ray spectroscopy (SEM‐EDX), Inductively Coupled Plasma Optical Emmision Spectrometry (ICP‐OES, Cyclic (CV), and Differential Pulse Voltammetry (DPV). Electrochemical analysis confirms the electroactivity and the presence of chemically linked ferrocene unit to the cryogel.
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