Lithium ion batteries (LIBs) are key components of modern electronics and are regularly utilized as their primary power source. Understanding the electrical and mechanical properties of electrode materials plays a major role in the performance improvement of LIBs. In this article, we provide research using PinPoint™ scanning spreading resistance microscopy (SSRM) to effectively measure both electrical and mechanical properties of LIB electrode surfaces at a much higher quality in a high-vacuum environment than in ambient conditions. The data collected in this experiment demonstrate that this technique is an effective means for measuring the quantitative and qualitative topographical, electrical and mechanical data of advanced materials with improved image quality and data accuracy.