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Powder X-ray diffraction (PXRD) measurements on rapid freezing samples of disaccharide (trehalose, sucrose, and maltose) solutions indicated that the crystalline phases in the sample were both hexagonal and cubic ice. The cubic ice existed at a higher ratio in the higher disaccharide concentration samples. The temperature ramping experiments revealed that the cubic ice was stable below 233 K, which was obviously higher than the temperature expected for a pure water system. The diffraction peak width of the hexagonal ice crystal was independent in the disaccharide concentrations. This indicated that the crystallite size of the hexagonal ice was more than several hundreds of nanometre, which coincided with the ice particle size previously observed in the freeze-fractured replica samples. The comparison of the present PXRD data with the replica observations by transmission electron microscope in an earlier study allows us to conclude that the cubic ice was formed at the grain boundary between the hexagonal ice and the coexisted non-crystalline disaccharide phase.

Powder X-ray diffraction observations of ice crystals formed from disaccharide solutions