Scanning probe microscopy (SPM) was utilized to study the thermal behavior of latex films dried under different conditions. Using the SPM probe resonance frequency method, the resonance frequency (ω) of the oscillating probe above the sample surface was followed as a function of temperature (T). Two different approaches for detecting thermal transitions were used and compared. In the heating-by-the-sample approach, the SPM probe acts as a thermal sensor detecting the heat dissipated by the heated sample. In the heating-by-the-probe approach, the SPM probe is utilized simultaneously as an actuator and a sensor: the heated probe both dissipates heat and detects the heat reflected from the sample surface. Thermal transitions in the polymer films could be observed in the Δω-T curves. The results were consistent with those observed by differential scanning calorimetry, but also additional information about the characteristics of the transitions was obtained. The heating-by-the-probe method showed higher surface sensitivity and more localized effects than the other approach. Furthermore, the progress of the latex film formation and the effect of the different drying conditions on film topography were studied by SPM imaging and roughness analysis. Skewness and local surface curvature are demonstrated to serve as useful numerical measures with which to distinguish different levels of particle deformation and the formation of a continuous film. Preannealing of the samples at high temperature influenced not only the topography (roughness) but also the characteristics of the thermal transitions.