In situ temperature-modulated microscopy observation of two-phase co-existing states of coumarin and coumarin derivative in melting

Abstract

Coumarin (C9H6O2) and coumarin derivative, coumarin 6H (C15H15NO2) samples were observed with a polarizing microscope at and around the melting points. The states of the two samples are crystalline at room temperature. When the temperature of the Coumarin sample was raised and a part was melted, the crystalline phases coexisted with the liquid phase. The crystal surface coexisting with the liquid phase went through a repetition of melting and crystallization on slightly modulating the sample temperature. The two-phase coexisting state was observed with a digital camera attached to a microscope. The changes in the number of pixels in the crystal part of the photographed image showed Debye relaxation with temperature change. It was found that the relaxation time was 4.9 s when the number of pixels decreased due to surface melting or increased due to surface crystallization. This relaxation time was in good agreement with that of the dynamic-specific heat measured by AC calorimetry. The coumarin 6H microcrystal also coexisted with the melt in a temperature range at and around the melting point. The change in the number of pixels of the coumarin 6H crystal part showed Debye relaxation with respect to the temperature, and the relaxation time was 15 s, which was the same as the relaxation time of the dynamic-specific heat measured in the melting temperature range of coumarin 6H.