This paper reports on visualisation of a phase separation in Agx(As0.33So.67)100-x and Agx(Aso.33So.335Seo.335)100-x chalcogenide glasses by means of atomic force microscopy (AFM). Sufficient topographical contrast (~20nm) was achieved by selective polishing of a phase-separated sample (Ag-poor, Ag-rich regions) and phase separation occurred within 0.5-20 at.% Ag and 2-18 at.% Ag in Agx(Aso.33So.67)100-x and Agx(As0.33So.335Seo.335)100-x systems, respectively. Homogeneous regions were observed below and above the phase sepration lower and upper limits. Direct comparison of scanning electron microscopy and atomic force microscopy sensitivity of phase separation detection is shown. In addition, concentration of silver in particular phases of AgAsS system was evaluated by NanoSIMS and very similar concentration of silver was detected in the phases at boundaries of immiscibility region.
