Functionalized graphene oxide papers are assembled materials with a wide range of potential applications; however, scientific studies about how the physical properties of functionalized graphene oxide papers are affected by the presence of new functional groups have not been addressed. Here, electrical resistance, optical band gap, and mechanical properties of flexible and free-standing functionalized graphene oxide papers with nitroxide moieties (NGOP’s) have been studied, and two of them (mechanicals and electricals) were correlated with the interlayer d spacing for the first time; herein, a new insight about the key role that an optimum amount of functionalization agent plays over the physical properties of NGOP’s is presented. In all cases, (functionalized or pristine) graphene oxide papers were prepared using anhydrous DMF instead water in order to study and highlight the pure effect of the functionalized groups over their physical properties. The functionalized nanomaterials exhibited significantly improved physical properties, which can be tuned by varying the interlayer d spacing, and this interlayer distance was systematically modified controlling the amount of functionalizing agent used. Thus, controlling the amount of functionalizing agent in the functionalization process is possible to obtain new assembled materials with modulated properties.

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A simple approach for the end‐functionalization of hydroxyl‐terminated polymers with nitroxide moieties using oxoammonium salts (OS) is presented. The functionalization is carried out using only one synthetic pathway in which high levels of functionalization (90%) are found. A mechanism for the functionalization with TEMPO moieties using OS is proposed in which the formation of peroxide groups is suggested. The structures of the functionalized polymers are characterized in detail by 1H NMR, 13C NMR, DQF‐COSY, and HETCOR. Bifunctional macroalkoxyamines are used to demonstrate how to extend the polymer chain for the synthesis of amphiphilic triblock copolymers by polymerizing St in a second block mediated by a nitroxide radical which provides the block length control. magnified image