Abstract. An environmental scanning electron microscope (ESEM) was used for the first time to obtain well-resolved images, in both temporal and spatial dimensions, of labprepared frost flowers (FFs) under evaporation within the chamber temperature range from −5 to −18 • C and pressures above 500 Pa. Our scanning shows temperature-dependent NaCl speciation: the brine covering the ice was observed at all conditions, whereas the NaCl crystals were formed at temperatures below −10 • C as the brine oversaturation was achieved. Finger-like ice structures covered by the brine, with a diameter of several micrometres and length of tens to 100 µm, are exposed to the ambient air. The brine-covered fingers are highly flexible and cohesive. The exposure of the liquid brine on the micrometric fingers indicates a significant increase in the brine surface area compared to that of the flat ice surface at high temperatures; the NaCl crystals formed can become sites of heterogeneous reactivity at lower temperatures. There is no evidence that, without external forces, salty FFs could automatically fall apart to create a number of sub-particles at the scale of micrometres as the exposed brine fingers seem cohesive and hard to break in the middle. The fingers tend to combine together to form large spheres and then join back to the mother body, eventually forming a large chunk of salt after complete dehydration. The present microscopic observation rationalizes several previously unexplained observations, namely, that FFs are not a direct source of sea-salt aerosols and that saline ice crystals under evaporation could accelerate the heterogeneous reactions of bromine liberation.
Observation of a uranyl-salt brine layer on an ice surface using backscattered electron detection and ice surface morphology using secondary-electron detection under equilibrium conditions was facilitated using an environmental scanning electron microscope (ESEM) at temperatures above 250 K and pressures of hundreds of Pa. The micrographs of a brine layer over ice grains prepared by either slow or shock freezing provided a complementary picture of the contaminated ice grain boundaries. Fluorescence spectroscopy of the uranyl ions in the brine layer confirmed that the species exists predominately in the solvated state under experimental conditions of ESEM.
Key words. Scintillation detector, secondary electrons detection, variable pressure scanning electron microscope.
SummaryWe present results obtained with a new scintillation detector of secondary electrons for the variable pressure scanning electron microscope. A detector design is based on the positioning of a single crystal scintillator within a scintillator chamber separated from the specimen chamber by two apertures. This solution enables us to decrease the pressure to several Pa in the scintillator chamber while the pressure in the specimen chamber reaches values of about 1000 Pa (7.5 Torr). Due to decreased pressure, we can apply a potential of the order of several kV to the scintillator, which is necessary for the detection of secondary electrons. Simultaneously, the two apertures at appropriate potentials of the order of several hundreds of volts create an electrostatic lens that allows electrons to pass from the specimen chamber to the scintillator chamber. Results indicate a promising utilization of this detector for a wide range of specimen observations.
Abstract. The microstructure of polycrystalline ice with a threading solution of brine
controls its numerous characteristics, including the ice mechanical
properties, ice–atmosphere interactions, sea ice albedo, and (photo)chemical
behavior in and on the ice. Ice samples were previously prepared in laboratories
in order to study various facets of ice–impurity interactions and (photo)reactions
to model natural ice–impurity behavior. We examine the impact of the
freezing conditions and solute (CsCl used as a proxy for naturally occurring
salts) concentrations on the microscopic structure of ice samples via an
environmental scanning electron microscope. The method allows us to observe
the ice surfaces in detail, namely, the free ice, brine puddles,
brine-containing grain boundary grooves, individual ice crystals, and
imprints left by entrapped air bubbles at temperatures higher than
−25 ∘C. The amount of brine on the external surface is found
proportional to the solute concentration and is strongly dependent on the
sample preparation method. Time-lapse images in the condition of slight
sublimation reveal subsurface association of air bubbles with brine. With
rising temperatures (up to −14 ∘C), the brine surface coverage
increases to remain enhanced during the subsequent cooling and until the
final crystallization below the eutectic temperature. The ice
recrystallization dynamics identify the role of surface spikes in retarding
the ice boundaries' propagation (Zener pinning). The findings thus quantify
the amounts of brine exposed to incoming radiation, available for the gas
exchange, and influencing other mechanical and optical properties of ice.
The results have straightforward and indirect implications for artificially
prepared and naturally occurring salty ice, respectively.
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