Fluctuation Electron Microscopy Study of Medium-Range Packing Order in Ultrastable Indomethacin Glass Thin Films

Abstract

ABSTRACTWe have used fluctuation electron microscopy (FEM) to measure the medium range order in the molecular packing of 40 nm thick indomethacin glass films. Vapor deposition of indomethacin can create glasses with extraordinary kinetic stability and high density. We find peaks in the FEM variance at diffraction vector magnitudes between 0.03 and 0.09 Å-1, corresponding to intermolecular packing distances of 1-3 nm. FEM experiments were performed with a 13 nm diameter electron probe, so these data are sensitive to medium-range order in intermolecular packing. The FEM variance from an indomethacin glass with normal stability cooled from the liquid is significantly smaller than the variance from the ultrastable glass, suggesting that ultrastable glass is more structurally heterogeneous at a 13 nm length scale. A dose of ∼7×105 e-/nm2 with a very low beam current of ∼ 2.5 pA at 200 kV was used to minimize electron beam damage to the sample, and the average electron diffraction from the sample is unchanged at total electron doses fourteen times larger than required for a FEM experiment. These preliminary results on medium-range order in molecular glasses suggest that we may be able to provide insight into the structural differences between the remarkable ultrastable thin films and ordinary glasses.