Surface characteristics of particles; such as structure, morphology, and chemical composition of surface have a major effect on its response to metallurgical processing operations. In order to understand the characteristics and reactivity of the system, information on the physical topography, the chemical composition, the chemical structure, the atomic structure, the electronic state, and a detailed description of bonding of molecules at the surface are required. Most of the instrumental techniques used for identification of major/minor and bulk/surface characteristics of substances now can be easily utilized as well for the characterization of mechanically activated minerals. This article is concerned with several representative identification techniques which are currently used for characterization of the materials prepared by mechanochemical processes. Fundamental aspects of spectroscopic (Infrared, Raman, and X-ray photoelectron), electron microscopic (Scanning electron microscopy and Transmission electron microscopy), and probe microscopic (Scanning tunneling microscopy and Atomic force microscopy) techniques used for surface characterization of mechanically activated minerals are overviewed.