Nanoindentation is a standard analysis technique for quantifying the mechanical properties of materials. Traditionally nanoindentation measurements have consisted of only force-depth data, however, recent advances have enabled the electrical properties to be collected at the same time. Exploring the relationship between electrical and mechanical properties is an important area of research, especially for materials that display piezoelectric behaviours. A technique designed to measure this behaviour, NanoECR^® (Nanoscale Electrical Contact Resistance) is capable of making simultaneous in-situ measurements of electrical and mechanical behaviour. In this work, a novel form of carbon, so-called glassy-carbon, is used as standard to calibrate the electrical response of the NanoECR^® system. The properties of four different glassy-carbon from two different manufacturers are characterised.  One glassy-carbon material was shown to display significantly different mechanical properties compared to the other three materials. This correlated with a higher level of impurities as measured using Rutherford Backscattering Spectroscopy and this sample was not selected as a calibration standard for the NanoECR^® system.  Three novel bulk piezoelectric materials were studied using nanoindentation and NanoECR. A piezoelectric response was detected on a bulk material using these systems for the first time