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Summary Triboelectric nanogenerators (TENGs) are promising new generation systems with their basic motion‐based working principle using both triboelectric and electrostatic effects. Today, the energy densities of TENGs are insufficient for many electronic devices and new strategies are needed to increase their power conversion efficiency. In this study, two different Perylene‐based organic structures were added to the triboelectric layers as well as the electrochemical properties of these structures, and the device parameters related to these properties were investigated. A large variety of instrumental analyses, including cyclic voltammetry, contact angle, scanning electron microscopy, atomic force microscopy, and so on, have been used to identify the relationship between doped molecules, their doping ratios, and obtained fiber structures. Depending on molecular structure and even any small variations in side groups of molecules, different doping rates brought about various device outputs. Compared with undoped layers, doping of small molecules led to a ~3.3 times increase in the maximum power of the best‐performed devices, and a very high voltage value of 500 V was obtained. The analysis of doping with small molecules undertaken here has extended our knowledge of how material design improves the electrical output and contributes to the device performance in TENGs.