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ESEM Methodology for the Study of Ice Samples at Environmentally Relevant Subzero Temperatures: “Subzero ESEM”

Published online by Cambridge University Press:  23 December 2021

Kamila Závacká Open the ORCID record for Kamila Závacká [Opens in a new window] ,
Vilém Neděla ,
Eva Tihlaříková ,
Pavla Šabacká ,
Jiří Maxa  and
Dominik Heger
Kamila Závacká*
Affiliation:
Environmental Electron Microscopy Group, Institute of Scientific Instruments of the Czech Academy of Sciences, Královopolská 147, 61264Brno, Czech Republic
Vilém Neděla
Affiliation:
Environmental Electron Microscopy Group, Institute of Scientific Instruments of the Czech Academy of Sciences, Královopolská 147, 61264Brno, Czech Republic
Eva Tihlaříková
Affiliation:
Environmental Electron Microscopy Group, Institute of Scientific Instruments of the Czech Academy of Sciences, Královopolská 147, 61264Brno, Czech Republic
Pavla Šabacká
Affiliation:
Environmental Electron Microscopy Group, Institute of Scientific Instruments of the Czech Academy of Sciences, Královopolská 147, 61264Brno, Czech Republic
Jiří Maxa
Affiliation:
Environmental Electron Microscopy Group, Institute of Scientific Instruments of the Czech Academy of Sciences, Královopolská 147, 61264Brno, Czech Republic
Dominik Heger
Affiliation:
Department of Chemistry, Faculty of Science, Masaryk University, Kamenice 5, 62500Brno, Czech Republic
*
*Corresponding author: Kamila Závacká, E-mail: zavacka@isibrno.cz
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Abstract

Frozen aqueous solutions are an important subject of study in numerous scientific branches including the pharmaceutical and food industry, atmospheric chemistry, biology, and medicine. Here, we present an advanced environmental scanning electron microscope methodology for research of ice samples at environmentally relevant subzero temperatures, thus under conditions in which it is extremely challenging to maintain the thermodynamic equilibrium of the specimen. The methodology opens possibilities to observe intact ice samples at close to natural conditions. Based on the results of ANSYS software simulations of the surface temperature of a frozen sample, and knowledge of the partial pressure of water vapor in the gas mixture near the sample, we monitored static ice samples over several minutes. We also discuss possible artifacts that can arise from unwanted surface ice formation on, or ice sublimation from, the sample, as a consequence of shifting conditions away from thermodynamic equilibrium in the specimen chamber. To demonstrate the applicability of the methodology, we characterized how the true morphology of ice spheres containing salt changed upon aging and the morphology of ice spheres containing bovine serum albumin. After combining static observations with the dynamic process of ice sublimation from the sample, we can attain images with nanometer resolution.

Keywords

morphological studystatic observation“subzero ESEM”temperature simulationthermodynamic equilibrium
Type
Software and Instrumentation
Information
Microscopy and Microanalysis , Volume 28 , Issue 1 , February 2022 , pp. 196 - 209
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Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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