The incorporation of rare earth-V (RE-V) semimetallic nanoparticles embedded in III-V compound semiconductors is of great interest for applications in solid-state devices including multijunction tandem solar cells, thermoelectric devices, and fast photoconductors for terahertz radiation sources and receivers. With regard to those nanoparticle roles in device applications and material itself, electrical and thermal properties of embedded RE-V nanoparticles, including nanoscale morphology, electronic structure, and electrical and thermal conductivity of such nanoparticles are essential to be understood to engineer their properties to optimize their influence on device performance. To understand embedded RE-V semimetallic nanostructures in III-V compound semiconductors, nanoscale characterization tools are essential for analysis their properties incorporated in compound semiconductors. In this dissertation, we used atomic force microscopy (AFM) with other secondary detection tools to investigate nanoscale material properties of semimetallic RE-V and GaAs heterostructures, grown by molecular beam epitaxy. We used scanning capacitance microscopy and conductive AFM techniques to understand electronic and electrical properties of ErAs/GaAs heterostructures. For the electrical properties, this thesis investigates details of statistical analysis of scanning capacitance and local conductivity images contrast to provide insights into (i) nanoparticle structure at length scales smaller than the nominal spatial resolution of the scanned probe measurement, and (ii) both lateral and vertical nanoparticle morphology at nanometer to atomic length scales, and their influence on electrical conductivity. To understand thermal properties of ErAs nanoparticles, in-plane and cross-sectional plane of ErAs/GaAs superlattice structure were investigated with a scanning probe microscopy technique implemented with 3[omega] method for thermal measurement. By performing detailed numerical modeling of thermal transport between thermal probe tip and employed samples, and estimation of additional phonon scattering induced by ErAs nanoparticles, we could understand influences of ErAs nanoparticles on the host GaAs thermal conductivity. Investigation of ErAs semimetallic nanostructure embedded in GaAs matrix with scanned probe microscopy provided detailed understanding of their electronic, electrical and thermal properties. In addition, this dissertation also demonstrates that an atomic force microscope with secondary detection techniques is promising apparatus to understand and investigate intrinsic properties of nanostructure materials, nanoscale charge transports, when the system is combined with detailed modeling and simulations. / text