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

0555124 - ÚPT 2023 RIV US eng J - Journal Article
Závacká, Kamila - Neděla, Vilém - Tihlaříková, Eva - Šabacká, Pavla - Maxa, Jiří - Heger, D.
ESEM Methodology for the Study of Ice Samples at Environmentally Relevant Subzero Temperatures: “Subzero ESEM”.
Microscopy and Microanalysis. Roč. 28, č. 1 (2022), s. 196-209. ISSN 1431-9276. E-ISSN 1435-8115
R&D Projects: GA ČR(CZ) GA19-08239S; GA ČR(CZ) GA19-03909S; GA MPO(CZ) EG17_176/0015020
Institutional support: RVO:68081731
Keywords : morphological study * static observation * subzero ESEM * temperature simulation * thermodynamic equilibrium
OECD category: Physical chemistry
Impact factor: 2.8, year: 2022
Method of publishing: Limited access
https://www.cambridge.org/core/journals/microscopy-and-microanalysis/article/esem-methodology-for-the-study-of-ice-samples-at-environmentally-relevant-subzero-temperatures-subzero-esem/0145A6ED83A07396E5FA3E7655DEF66D

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.
Permanent Link: https://hdl.handle.net/11104/0333568