Microstructural evolution in sintered ice particles containing NaCl observed by low-temperature scanning electron microscope

Ice particles containing NaCl were made by spraying 0.043 M salt solution into liquid nitrogen. The ice particles were packed into capsules and annealed at -8 °C for 168 h and -25 °C for 20 h. This material can be considered as a model material for sintered snow containing impurities. The capsules were fractured open inside the low-temperature scanning electron microscope, which minimized the artefacts caused by cryofixation. The morphology of the sintered structure was observed with low-temperature scanning electron microscope. The microstructure of the sintered material consists of ice grains with a liquid meniscus containing NaCl between the grains. This structure is similar to the equilibrium morphology of water-filled veins in polycrystalline ice and liquid phase sintered metallic materials. The combined effect of the surface energies between the solid, liquid, and vapour governs the morphology of the microstructure. A dihedral angle where the brine intersects a grain boundary in ice of 8.0 ± 2.6°, and a contact angle for brine on ice at the interface with vapour of 5.0 ± 1.3° were measured, for samples quenched from -8 °C. Using the dihedral angle measurement, a surface energy value for ice-brine of 32.6 ± 0.1 mJ/m2 was calculated.

[1]  A. Rango,et al.  Observations of snow crystals using low‐temperature scanning electron microscopy , 2006 .

[2]  E. Wolff,et al.  A technique for the examination of polar ice using the scanning electron microscope , 2002, Journal of microscopy.

[3]  R. German,et al.  Rearrangement densification in liquid-phase sintering , 2001 .

[4]  I. Baker,et al.  Observation of impurities in ice , 2001, Microscopy research and technique.

[5]  Yamaguchi,et al.  Thermodynamic Quantities of Surface Formation of Aqueous Electrolyte Solutions. , 1999, Journal of colloid and interface science.

[6]  Albert Rango,et al.  Snow crystal imaging using scanning electron microscopy: II. Metamorphosed snow , 1996 .

[7]  N. Read,et al.  Low‐temperature scanning electron microscopy in biology , 1991, Journal of microscopy.

[8]  S. Hardy A grain boundary groove measurement of the surface tension between ice and water , 1977 .

[9]  G. Chadwick,et al.  Experimental measurement of solid-liquid interfacial energies: The ice-water-sodium chloride system , 1971 .

[10]  P. Hobbs,et al.  An experimental determination of the surface energies of ice , 1969 .

[11]  J D Cross,et al.  Scanning Electron Microscopy of Evaporating Ice , 1969, Science.

[12]  W. Mullins Theory of Thermal Grooving , 1957 .

[13]  E. Wolff,et al.  Capture and scanning electron microscopy of individual snow crystals , 1994, Journal of Glaciology.

[14]  H. Mader Observations of the water-vein system in polycrystalline ice , 1992, Journal of Glaciology.

[15]  H. Mader The thermal behaviour of the water-vein system in polycrystalline ice , 1992, Journal of Glaciology.

[16]  J. Nye,et al.  Measuring the dihedral angle of water at a grain boundary in ice by an optical diffraction method , 1991, Journal of Glaciology.

[17]  N. Read,et al.  8 – Ambient- and Low-Temperature Scanning Electron Microscopy , 1991 .

[18]  J. F. Nye,et al.  The Geometry of Water Veins and Nodes in Polycrystalline Ice , 1989, Journal of Glaciology.

[19]  E. Wolff,et al.  Sulphuric acid at grain boundaries in Antarctic ice , 1988, Nature.

[20]  D. Roberts,et al.  Optical Measurements of Water Lenses in Ice , 1987, Journal of Glaciology.