Nanocalorimetry (NanoDSC) is applied to measure the melting characteristics of single layer silver pentadecanethiolate (AgSC15) crystals. Its attribute of high sensitivity enables the characterization of single layer species. The fast heating (similar to 50,000 K/s) and cooling (similar to 10(4) K/s) rates employed allow an in situ study of lamella layer evolution. By controlling the maximum temperature (T-max) achieved during heating/cooling cycles, the samples can be either melted or annealed. If T-max is larger than sample melting point (T-m), the first NanoDSC pulse shows the melting behavior of the as-synthesized crystal. The following rapid cooling (quenching) causes crystallinity loss. If T-max is smaller than T-m, electrical annealing takes place and partially recovers the quenched layered structure, but the melting enthalpy never reaches that of the first pulse. (C) 2014 Elsevier B.V. All rights reserved.