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High-resolution imaging of biotite using focal series exit wavefunction restoration and the graphene mechanical exfoliation method

Published online by Cambridge University Press:  02 January 2018

W. Bower ,
W. Head ,
G. T. R. Droop ,
R. Zan ,
R. A. D. Pattrick ,
P. Wincott  and
S. J. Haigh
W. Bower
Affiliation:
School of Earth, Atmospheric and Environmental Sciences and the Williamson Research Centre, The University of Manchester, Manchester M13 9PL, UK
W. Head
Affiliation:
School of Earth, Atmospheric and Environmental Sciences and the Williamson Research Centre, The University of Manchester, Manchester M13 9PL, UK
G. T. R. Droop
Affiliation:
School of Earth, Atmospheric and Environmental Sciences and the Williamson Research Centre, The University of Manchester, Manchester M13 9PL, UK
R. Zan
Affiliation:
School of Materials, The University of Manchester, Manchester M13 9PL, UK
R. A. D. Pattrick
Affiliation:
School of Earth, Atmospheric and Environmental Sciences and the Williamson Research Centre, The University of Manchester, Manchester M13 9PL, UK
P. Wincott
Affiliation:
School of Earth, Atmospheric and Environmental Sciences and the Williamson Research Centre, The University of Manchester, Manchester M13 9PL, UK
S. J. Haigh*
Affiliation:
School of Materials, The University of Manchester, Manchester M13 9PL, UK
*
*E-mail: sarah.haigh@manchester.ac.uk
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Abstract

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We have applied mechanical exfoliation for the preparation of ultra-thin samples of the phyllosilicate mineral biotite. We demonstrate that the 'scotch tape' approach, which was made famous as an early method for production of single-atom-thick graphene, can be used for production of sheet-silicate specimens that are sufficiently thin to allow high-resolution transmission electron microscope (HRTEM) imaging to be achieved successfully while also being free from the specimen preparation artefacts that are often caused by ion-beam milling techniques. Exfoliation of the biotite parallel to the (001) planes has produced layers as thin as two structural TOT units thick (∼2 nm). The minimal specimen thickness enabled not only HRTEM imaging but also the application of subsequent exit wavefunction restoration to reveal the pristine biotite lattice. Exit wavefunction restoration recovers the full complex electron wave from a focal series of HRTEM images, removing the effects of coherent lens aberrations. This combination of methods therefore produces images in which the observed features are readily interpreted to obtain atomic resolution structural information.

Keywords

biotiteexfoliationfocal serieshigh-resolution transmission electron microscopygraphene
Type
Research Article
Information
Mineralogical Magazine , Volume 79 , Issue 2 , April 2015 , pp. 337 - 344
Creative Commons
Creative Common License - CCCreative Common License - BY
Copyright © The Mineralogical Society of Great Britain and Ireland 2015 This is an Open Access article, distributed under the terms of the Creative Commons Attribution license. (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted re-use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2015

Footnotes

†

Present address: Department of Physics, Faculty of Arts and Sciences, Nig˘de University, 51000 Nig˘de, Turkey

References

Binning, G., Quate, C.F. and Gerber, C. (1986) Atomic force microscope. Physical Review Letters, 56, 930–933.CrossRefGoogle Scholar
Blake, P., Hill, E.W., Castro Neto, A.H., Novoselov, K.S. and Jiang, D. (2007) Making graphene visible. Applied Physics Letters, 91, 063124. Brigatti, M.F., Guidotti, C.V., Malferrari, D. and Sassi, F.P. (2008) Single-crystal X-ray studies of trioctahedral micas coexisting with dioctahedral micas in metamorphic sequences from western Maine. American Mineralogist, 93, 396–408.Google Scholar
Coene, W., Janssen, G., Op de Beeck, M. and Van Dyck, D. (1992) Phase retrieval through focus variation for ultra-resolution in field-emission transmission electron-microscopy. Physical Review Letters, 69, 3743–3746.CrossRefGoogle ScholarPubMed
Coene, W.M.J., Thust, A., Op de Beeck, M. and Van Dyck, D. (1996) Maximum-likelihood method for focus-variation image reconstruction in high resolution t r ansmission electron microscopy. Ultramicroscopy, 64, 109–135.CrossRefGoogle Scholar
Cruciani, G. and Zanazzi, P.F. (1994) Cation partitioning and substitution mechanisms in 1M-phlogopite: a crystal chemical study. American Mineralogist, 78, 289–301.Google Scholar
Goodman, P. and Moodie, A.F. (1974) Numerical evaluation of N-Beam wave function in electron scattering by the multislice method. Acta Crystallograhica, A30, 280–290.CrossRefGoogle Scholar
Ewing, R.C., Meldrum, A., Wang, L.M. and Wang, S.X. (2000) Radiation-induced amorphization. Transformation Processes in Minerals, 39, 319–361.CrossRefGoogle Scholar
Fleet, M.E. (2003) Rock-Forming Minerals, Volume 3A Sheet Silicates: Micas. The Geological Society, London, 758 pp. Geim, A.K. and Grigorieva, I.V. (2013) Van der Waals heterostructures. Nature, 499, 419–425.Google Scholar
Lynch, D.F. and O’Keefe, M.A. (1972) N-Beam lattice images. 2. Methods of calculation. Acta Crystallographica, A28, 536–548.CrossRefGoogle Scholar
Ma, C. Fitzgerald, J.D., Eggleton, R.A. and Llewellyn, D.J. (1998) Analytical electron microscopy in clays and other phyllosilicates: Loss of elements from a 90-nm stationary beam of 300-keV electrons. Clays and Clay Minerals, 46, 301–316.CrossRefGoogle Scholar
McCaffrey, J.P., Phaneuf, M.W. and Madsen, L.D. (2001) Surface damage formation during ion-beam thinning of samples for transmission electron microscopy. Ultramicroscopy, 87, 97–104.CrossRefGoogle ScholarPubMed
Meyer, J.C., Girit, C.O., Crommie, M.F. and Zettl, A. (2008) Imaging and dynamics of light atoms and molecules on graphene. Nature, 454, 319–322.CrossRefGoogle Scholar
Meyer, R.R., Kirkland, A.I., Dunin-Borkowski, R.E. and Hutchison, J.L. (2000) Experimental characterisation of CCD cameras for HREM at 300 kV. Ultramicroscopy, 85, 9–13.CrossRefGoogle ScholarPubMed
Meyer, R.R., Kirkland, A.I. and Saxton, W.O. (2002) A new method for the determination of the wave aberration function for high resolution TEM 1. Measurement of the symmetric aberrations. Ultramicroscopy, 92, 89–109.CrossRefGoogle Scholar
Meyer, R.R., Kirkland, A.I. and Saxton, W.O. (2004) A new method for the determination of the wave aberration function for high-resolution TEM. 2. Measurement of the antisymmetric aberrations. Ultramicroscopy, 99, 115–123.CrossRefGoogle ScholarPubMed
Novoselov, K.S., Geim, A.K., Morozov, S.V., Jiang, D., Zhang, Y., Dubonos, S.V., Grigorieva, I. V. and Firsov, A.A. (2004) Electric field effect in atomically thin carbon films. Science, 306, 666–669.CrossRefGoogle ScholarPubMed
Pattrick, R.A.D., Charnock, J.M., Geraki, T., Mosselmans, J.F.W., Pearce, C.I., Pimblott, S. and Droop, G.T.R. (2013) Alpha particle damage in biotite characterized by microfocus X-ray diffraction and Fe K-edge X-ray absorption spectroscopy. Mineralogical Magazine, 77, 2867–2882.CrossRefGoogle Scholar
Reed, S.J.B. (2010) Electron Microprobe Analysis and Scanning Electron Microscopy in Geology. Cambridge University Press, Cambridge, UK. Saxton, W.O. (1988) Accurate atom positions from focal and tilted beam series of high-resolution electronmicrographs. Scanning Microscopy, 2, 213–224.Google Scholar
Takeda, H. and Ross, M. (1975) Mica polytypism: Dissimilarities in the crystal structures of coexisting 1M and 2M1 biotite. American Mineralogist, 60, 1030–1040.Google Scholar
Urban, K.W. (2008) Studying atomic structures by aberration-corrected transmission electron microscopy. Science, 321(58), 506–510.CrossRefGoogle Scholar