This article presents the results of flow visualization studies of Novec refrigerants during condensation in minichannels. Experimental investigation of two-phase flow regimes was conducted in minichannels with internal diameter dh = 2.5, 2.0, 1.2, and 0.5 mm. Images of the two-phase flow structures were analyzed by using the MATLAB algorithm. To calculate void fraction, a two-dimensional areal quantitative stereology technique was used. Observation of flow structures formed during the process of condensation was the major aim of the investigations. The condensation studies were conducted over a wide range of mass flux densities (G = 80–5500 kg/m2s) and saturation temperatures (ts = 30–70 °C). Visualization results and image analysis methods are described in this paper. Based on the experimental results, a flow structure map was constructed and presented.