The efficiency of low voltage scanning electron microscopy, which presents near-surface information, has been well known for a long time. However, it is not widely known that the high resolution capability can only be achieved when the surface reveals the original characteristics of the materials without any deterioration due contamination. Therefore, initial attention in this study is directed at clarifying the efficient use of the ultra high resolution, low voltage SEM (UHRLV SEM), (Ultra55, Zeiss). The SEM images and the selected electrons for detection, and damage that occurs through UHRVL SEM observation are also researched. Subsequently, the most efficient specimen preparation technique, which is appropriate for the characteristics of the individual materials, is investigated for galvanized steel, ultrasonically welded alloys of Al6111 and AZ31 alloy, Ti6Al4V alloy honeycomb structure and a ceramic sensor. The outcomes of appropriate specimen preparation technique and use of the extremely Low-Voltage below 2.0 kV, are presented in the results section. The study also presented the challenge of improving the low compositional contrast for the dissimilar materials of aluminium and magnesium, and to reduce charging effects in an insulating material comprising a ceramic sensor. As an application of the surface prepared by the process in this study, 3D tomography is also introduced.