The zip folder contains the dataset for the publication “Surface potential tailoring of PMMA fibers by electrospinning for enhanced triboelectric performance”. The dataset is divided in folders containing the data used to generate each figure of the paper. Figure 1 folder contains SEM images of the fibers and the .xls file of the fiber diameter histogram. Figure 2 folder contains KPFM images of fibers, the images are both in .png and in the format compatible with NanoScope Analysis 1.9 software. Figure 3 folder contains rubbing KPFM images of fibres, the images are both in .png and in the format compatible with NanoScope Analysis 1.9 software. Figure 4 folder contains the voltage, current and power data of triboelectric devices built using the fibers. The data is saved in .xls format. Figure S2 folder contains the data of the XPS Oxygen1 and Oxygen2 spectra. Figure S3 folder contains the KPFM data of Au coated silicon wafer. The data is available as .png and in the format compatible with NanoScope Analysis 1.9 software. The line scan values of the KPFM image is in .xls format. Figure S4 folder contains the KPFM data of PMMA film. The data is available as .png and in the format compatible with NanoScope Analysis 1.9 software. The line scan values of the KPFM image is in .xls format. Figure S5 folder contains the rubbing KPFM data of PMMA film. The data is available as .png and in the format compatible with NanoScope Analysis 1.9 software. The line scan values of the KPFM image is in .xls format. Figure S6 folder contains the open circuit voltage and short circuit current data of the PMMA fibers and film in .xls format. Figure S7 folder contains the voltage, current and power data of triboelectric devices built using PMMA film. The data is in .xls format. Figure S8 folder contains the open circuit voltage and short circuit current data of the PMMA fibers under fatigue testing. The data is in .xls format. Table 1 folder contains the XPS data of PMMA fibers and film in .xls format.