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GI | Articles | Volume 8, issue 1
Geosci. Instrum. Method. Data Syst., 8, 97-111, 2019
https://doi.org/10.5194/gi-8-97-2019
© Author(s) 2019. This work is distributed under
the Creative Commons Attribution 4.0 License.
Geosci. Instrum. Method. Data Syst., 8, 97-111, 2019
https://doi.org/10.5194/gi-8-97-2019
© Author(s) 2019. This work is distributed under
the Creative Commons Attribution 4.0 License.

Research article 14 Mar 2019

Research article | 14 Mar 2019

Artifacts from manganese reduction in rock samples prepared by focused ion beam (FIB) slicing for X-ray microspectroscopy

Dorothea S. Macholdt et al.
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Balcells, L., Abad, L., Rojas, H., and Martínez, B.: Material damage induced by nanofabrication processes in manganite thin films, Nanotechnology, 19, 135307, https://doi.org/10.1088/0957-4484/19/13/135307, 2008. 
Barber, D. J.: Radiation damage in ion-milled specimens: characteristics, effects and methods of damage limitation, Ultramicroscopy, 52, 101–125, https://doi.org/10.1016/0304-3991(93)90025-S, 1993. 
Bargar, J., Tebo, B., K., P., McCubbery, D., Chiu, V., and B., T.: Manganese Oxide Biomineralization by Spores of the Marine Bacillus sp. Strain SG-1, AGU Fall Meeting Abstracts, 2001. 
Bassim, N. D., De Gregorio, B. T., Kilcoyne, A. L. D., Scott, K., Chou, T., Wirick, S., Cody, G., and Stroud, R. M.: Minimizing damage during FIB sample preparation of soft materials, J. Microsc., 245, 288–301, https://doi.org/10.1111/j.1365-2818.2011.03570.x, 2012. 
Betz, G. and Wehner, G. K.: Sputtering of multicomponent materials, in: Sputtering by Particle Bombardment II, Topics in Applied Physics, vol 52., edited by: Behrish, R., 11–90, Springer Berlin, Heidelberg, 1983. 
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Short summary
Focused ion beam (FIB) slicing is a widely used technique to prepare ultrathin slices for the microanalysis of geological and environmental samples. During our investigations of the manganese oxidation states in rock varnish slices, we found an FIB-related reduction of manganese(IV) to manganese(II) at the samples’ surfaces. This study characterizes the observed reduction artifacts and emphasizes that caution is needed in the analysis of transition metal oxidation states upon FIB preparation.
Focused ion beam (FIB) slicing is a widely used technique to prepare ultrathin slices for the...
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