PZT nanofibers are piezoelectric and can produce a relatively high electrical output under strain that is useful for self-powered nanogenerators. To obtain maximum power output from these devices, their internal impedance needs to be matched with their applicable load impedance. Electrical impedance measurements of PZT nanofibers were performed using a variety of methods over a frequency spectrum ranging from DC to 3.0 GHz. These methods include Conductive AFM and Scanning Microwave Impedance Microscopy. Nanofibers formed by electro-spinning with diameters ranging from 3 to 150 nm were collected and measured. The nanofiber impedance was extremely high at low frequency, decreased considerably at higher frequency and varied with nanofiber diameter as well. The results are applicable for the analysis of many types of nanogenerators and nanosensors including those produced at Stevens.