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Cryo-SEM method for the observation of entrapped bubbles and degree of water filling in large wet powder compacts
Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.ORCID iD: 0000-0003-4582-0902
Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
LKAB Research and Development.
2011 (English)In: Journal of Microscopy, ISSN 0022-2720, E-ISSN 1365-2818, Vol. 242, no 2, p. 189-196Article in journal (Refereed) Published
Abstract [en]

There are generally two problems associated with cryogenic scanning electron microscopy (cryo-SEM) observations of large wet powder compacts. First, because water cannot be vitrified in such samples, formation of artefacts is unavoidable. Second, large frozen samples are difficult to fracture but also to machine into regular pieces which fit in standard holders, especially if made of hard materials like ceramics. In this article, we first describe a simple method for planning hard cryo-samples and a low-cost technique for cryo-fracture and transfer of large specimens. Subsequently, after applying the entire procedure to green pellets of iron ore produced by balling, we compare the influence of plunge- and unidirectional freezing on large entrapped bubbles throughout the samples as well as the degree of water filling at the outer surface of the pellets. By carefully investigating the presence of artefacts in large areas of the samples and by controlling the orientation of the sample during freezing and preparation, we demonstrate that unidirectional freezing enables the observation of large entrapped bubbles with minimum formation of artefacts, whereas plunge freezing is preferable for the characterization of the degree of water filling at the outer surface of wet powder compacts. The minimum formation of artefacts was due to the high packing density of the iron ore particles in the matrix

Place, publisher, year, edition, pages
2011. Vol. 242, no 2, p. 189-196
National Category
Chemical Process Engineering
Research subject
Chemical Technology
Identifiers
URN: urn:nbn:se:ltu:diva-11896DOI: 10.1111/j.1365-2818.2010.03458.xISI: 000289163900009PubMedID: 21118249Scopus ID: 2-s2.0-79953302168Local ID: aec36dd0-f703-11df-8b95-000ea68e967bOAI: oai:DiVA.org:ltu-11896DiVA, id: diva2:984846
Note
Validerad; 2011; 20101123 (linste)Available from: 2016-09-29 Created: 2016-09-29 Last updated: 2018-07-10Bibliographically approved

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Mouzon, JohanneBhuiyan, Iftekhar UddinHedlund, Jonas

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