Current work dedicated for development of different material sample preparation methodology for research on field emission scanning electron microscopy (SEM) Mira/LMU (Tescan Czech Republic). Developed and experimentally approved the sequential sample preparation algorithm, what allows obtaining of high quality different metal, ceramic and biological origination surface structure microphotographs. During research of hard biological tissues, also dental samples, new simplified method for obtaining of tooth replica for further SEM investigations was developed. This method allows more accurately determine the changes in plugged material - tooth enamel boundary during the patient lifetime.