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Licensed Unlicensed Requires Authentication Published by De Gruyter (O) February 5, 2018

Single-crystal analysis of nanodomains by electron diffraction tomography: mineralogy at the order-disorder borderline

  • Enrico Mugnaioli EMAIL logo and Mauro Gemmi

Abstract

Electron diffraction tomography is a powerful emerging method for the structure characterization of materials available only as sub-micrometric grains. This technique can in fact deliver complete 3D information from a single crystal of few hundreds or few tens of nanometers, allowing the analysis of polyphasic or polytypic mixtures that generally cannot be fully addressed by X-ray methods. In this paper, we report and discuss three mineralogy-related study cases where electron diffraction tomography was the only way for achieving a proper description of the sample, by the identification and the structure determination of all the phases or all the polytypes within. We also show how electron diffraction tomography and dynamical refinement can be combined for finding accurate atomic positions and localizing hydrogen atoms at room conditions. Finally, we stress the future potential of this method in the fields of mineralogy and experimental petrology, where till now many samples cannot be properly described because nanocrystalline, polyphasic or disordered. Electron diffraction tomography can be used for detecting unexpected or unknown phases in high-pressure synthetic yields or for the characterization of fine rocks formed under extreme conditions, like impactites or meteorites. Eventually, this method allows the structure characterization of single domains that are ordered only at the scale of few cell repetitions, and therefore it makes possible investigating those materials at the borderline between crystalline and amorphous matter and delivers crucial and unique elements for the understanding of the first stages of solid matter organization.

Acknowledgements

Authors thank all people that cooperate with them in the analysis of the materials cited in this paper and Luca Bindi for inviting them to contribute to this special issue for Zeitschrift für Kristallographie.

References

[1] M. Knoll, E. Ruska, Z. Phys.1932, 78, 318.10.1007/BF01342199Search in Google Scholar

[2] C. Davisson, L. H. Germer, Phys. Rev.1927, 30, 705.10.1103/PhysRev.30.705Search in Google Scholar

[3] R. Rigamonti, Gazz. Chim. Ital.1936, 66, 174.Search in Google Scholar

[4] J. M. Cowley, Acta Crystallogr.1956, 9, 391.10.1107/S0365110X56001133Search in Google Scholar

[5] J. M. Cowley, A. F. Moodie, Acta Crystallogr.1957, 10, 609.10.1107/S0365110X57002194Search in Google Scholar

[6] H. Bethe, Ann. Phys.1928, 392, 55.10.1002/andp.19283921704Search in Google Scholar

[7] M. Blackman, Proc. R. Soc. Lond. A1939, 173, 68.10.1098/rspa.1939.0129Search in Google Scholar

[8] K. Gjønnes, Y. Cheng, B. S. Berg, V. Hansen, Acta Crystallogr. A1998, 54, 102.10.1107/S0108767397009963Search in Google Scholar

[9] T. E. Weirich, X. Zou, R. Ramlau, A. Simon, G. L. Cascarano, C. Giacovazzo, S. Hovmöller, Acta Crystallogr. A2000, 56, 29.10.1107/S0108767399009605Search in Google Scholar

[10] Z. G. Pinsker (eds.), Electron Diffraction, Butterworth, London, 1953.Search in Google Scholar

[11] B. K. Vainshtein, Structure Analysis by Electron Diffraction, Pergamon Press, Oxford, 1964.Search in Google Scholar

[12] A. P. Zhukhlistov, A. S. Avilov, D. Ferraris, B. B. Zvyagin, V. P. Plotnikov, Crystallogr. Rep.1997, 42, 774.Search in Google Scholar

[13] D. L. Dorset, H. A. Hauptman, Ultramicroscopy1976, 1, 195.10.1016/0304-3991(76)90034-6Search in Google Scholar

[14] D. L. Dorset, Acta Crystallogr. B1996, 52, 753.10.1107/S0108768196005599Search in Google Scholar PubMed

[15] T. E. Weirich, Acta Crystallogr. A2001, 57, 183.10.1107/S0108767300014070Search in Google Scholar

[16] S. Nicolopoulos, J. M. González-Calbet, M. Vallet-Regí, A. Corma, C. Corell, J. M. Guil, J. Pérez-Pariente, J. Am. Chem. Soc.1995, 117, 8947.10.1021/ja00140a008Search in Google Scholar

[17] I. G. Voigt-Martin, Z. X. Zhang, U. Kolb, C. Gilmore, Ultramicroscopy1997, 68, 43.10.1016/S0304-3991(97)00006-5Search in Google Scholar

[18] M. Gemmi, L. Righi, G. Calestani, A. Migliori, A. Speghini, M. Santarosa, M. Bettinelli, Ultramicroscopy2000, 84, 133.10.1016/S0304-3991(00)00007-3Search in Google Scholar

[19] R. Vincent, P. A. Midgley, Ultramicroscopy1994, 53, 271.10.1016/0304-3991(94)90039-6Search in Google Scholar

[20] M. Gemmi, X. Zou, S. Hovmöller, A. Migliori, M. Vennström, Y. Andersson, Acta Crystallogr. A2003, 59, 117.10.1107/S0108767302022559Search in Google Scholar PubMed

[21] D. L. Dorset, C. J. Gilmor, J. L. Jorda, S. Nicolopoulos, Ultramicroscopy2007, 107, 462.10.1016/j.ultramic.2006.05.013Search in Google Scholar PubMed

[22] M. Gemmi, S. Nicolopoulos, Ultramicroscopy2007, 107, 483.10.1016/j.ultramic.2006.03.010Search in Google Scholar PubMed

[23] U. Kolb, T. Gorelik, C. Kübel, M. T. Otten, D. Hubert, Ultramicroscopy2007, 107, 507.10.1016/j.ultramic.2006.10.007Search in Google Scholar PubMed

[24] U. Kolb, T. Gorelik, M. T. Otten, Ultramicroscopy2008, 108, 763.10.1016/j.ultramic.2007.12.002Search in Google Scholar PubMed

[25] E. Mugnaioli, T. Gorelik, U. Kolb, Ultramicroscopy2009, 109, 758.10.1016/j.ultramic.2009.01.011Search in Google Scholar PubMed

[26] U. Kolb, E. Mugnaioli, T. E. Gorelik, Cryst. Res. Technol.2011, 46, 542.10.1002/crat.201100036Search in Google Scholar

[27] E. Mugnaioli, Rend. Fis. Acc. Lincei2015, 26, 211.10.1007/s12210-014-0371-4Search in Google Scholar

[28] D. B. Williams, C. B. Carter, Transmission Electron Microscopy, Plenum Press, New York, 1996.10.1007/978-1-4757-2519-3Search in Google Scholar

[29] D. Zhang, P. Oleynikov, S. Hovmöller, X. Zou, Z. Kristallogr.2010, 225, 94.10.1524/zkri.2010.1202Search in Google Scholar

[30] B. L. Nannenga, D. Shi, A. G. W. Leslie, T. Gonen, Nat. Methods2014, 11, 927.10.1038/nmeth.3043Search in Google Scholar PubMed PubMed Central

[31] M. Gemmi, M. G. I. La Placa, A. S. Galanis, E. F. Rauch, S. Nicolopoulos, J. Appl. Crystallogr.2015, 48, 718.10.1107/S1600576715004604Search in Google Scholar

[32] I. V. Rozhdestvenskaya, E. Mugnaioli, M. Schowalter, M. U. Schmidt, M. Czank, W. Depmeier, A. Rosenauer, IUCrJ2017, 4, 223.10.1107/S2052252517002585Search in Google Scholar PubMed PubMed Central

[33] E. Mugnaioli, U. Kolb, Microp. Mesop. Mater.2014, 189, 107.10.1016/j.micromeso.2013.11.040Search in Google Scholar

[34] L. Palatinus, D. Jacob, P. Cuvillier, M. Klementová, W. Sinkler, L. D. Marks, Acta Crystallogr. A2013, 69, 171.10.1107/S010876731204946XSearch in Google Scholar PubMed

[35] L. Palatinus, V. Petříček, C. A. Corrêa, Acta Crystallogr. A2015, 71, 235.10.1107/S2053273315001266Search in Google Scholar PubMed

[36] L. Palatinus, C. A. Corrêa, G. Steciuk, D. Jacob, P. Roussel, P. Boullay, M. Klementová, M. Gemmi, J. Kopeček, M. C. Domeneghetti, F. Cámara, V. Petříček, Acta Crystallogr. B2015, 71, 740.10.1107/S2052520615017023Search in Google Scholar PubMed

[37] D. Jacob, L. Palatinus, P. Cuvillier, H. Leroux, C. Domeneghetti, F. Cámara, Am. Mineral.2013, 98, 1526.10.2138/am.2013.4296Search in Google Scholar

[38] M. Gemmi, M. Merlini, L. Palatinus, P. Fumagalli, M. Hanfland, Am. Mineral.2016, 101, 2645.10.2138/am-2016-5722Search in Google Scholar

[39] L. Palatinus, P. Brázda, P. Boullay, O. Perez, M. Klementová, S. Petit, V. Eigner, M. Zaarour, S. Mintova, Science2017, 355, 166.10.1126/science.aak9652Search in Google Scholar PubMed

[40] I. Rozhdestvenskaya, E. Mugnaioli, M. Czank, W. Depmeier, U. Kolb, A. Reinholdt, T. Weirich, Mineral. Mag.2010, 74, 159.10.1180/minmag.2010.074.1.159Search in Google Scholar

[41] I. V. Rozhdestvenskaya, T. Kogure, E. Abe, V. A. Drits, Mineral. Mag.2009, 73, 883.10.1180/minmag.2009.073.2.883Search in Google Scholar

[42] I. Rozhdestvenskaya, U. Kolb, E. Mugnaioli, A. Reinholdt, T. Weirich, W. Depmeier, M. Czank, Z. Kristallogr. Suppl.2009, 29, 103.Search in Google Scholar

[43] I. Rozhdestvenskaya, E. Mugnaioli, M. Czank, W. Depmeier, U. Kolb, S. Merlino, Mineral. Mag.2011, 75, 2833.10.1180/minmag.2011.075.6.2833Search in Google Scholar

[44] M. Gemmi, I. Campostrini, F. Demartin, T. E. Gorelik, C. M. Gramaccioli, Acta Crystallogr. B2012, 68, 15.10.1107/S010876811104688XSearch in Google Scholar PubMed

[45] J. Plášil, L. Palatinus, J. Rohlíček, L. Houdková, M. Klementová, V. Goliáš, P. Škácha, Am. Mineral.2014, 99, 276.10.2138/am.2014.4671Search in Google Scholar

[46] F. Colombo, E. Mugnaioli, O. Vallcorba, A. Garcia, A. R. Goñi, J. Rius, Mineral. Mag.2017, 81, 1191.10.1180/minmag.2016.080.159Search in Google Scholar

[47] G. C. Capitani, E. Mugnaioli, J. Rius, P. Gentile, T. Catelani, A. Lucotti, U. Kolb, Am. Mineral.2014, 99, 500.10.2138/am.2014.4446Search in Google Scholar

[48] G. Ventruti, E. Mugnaioli, G, Capitani, F, Scordari, D. Pinto, A. Lausi, Phys. Chem. Miner.2015, 42, 651.10.1007/s00269-015-0751-zSearch in Google Scholar

[49] J. Majzlan, L. Palatinus, J. Plášil, Eur. J. Mineral.2016, 28, 63.10.1127/ejm/2015/0027-2495Search in Google Scholar

[50] E. Mugnaioli, I. Andrusenko, T. Schüler, N. Loges, R. E. Dinnebier, M. Panthöfer, W. Tremel, U. Kolb, Angew. Chem. Int. Ed.2012, 51, 7041.10.1002/anie.201200845Search in Google Scholar PubMed

[51] E. Makovicky, Am. Mineral.2016, 101, 1636.10.2138/am-2016-5324Search in Google Scholar

[52] A. G. Christy, Cryst. Growth Des.2017, 17, 3567.10.1021/acs.cgd.7b00481Search in Google Scholar

[53] L. Palatinus, M. Klementová, V. Dřínek, M. Jarošová, V. Petříček, Inorg. Chem.2011, 50, 3743.10.1021/ic200102zSearch in Google Scholar PubMed

[54] P. Boullay, L. Palatinus, N. Barrier, Inorg. Chem.2013, 52, 6127.10.1021/ic400529sSearch in Google Scholar PubMed

[55] L. Bindi, J. M. Eiler, Y. Guan, L. S. Hollister, G. MacPherson, P. J. Steinhardt, N. Yao, Proc. Natl. Acad. Sci. USA2012, 109, 1396.10.1073/pnas.1111115109Search in Google Scholar PubMed PubMed Central

[56] M. Koch-Müller, E. Mugnaioli, D. Rhede, S. Speziale, U. Kolb, R. Wirth, Am. Mineral.2014, 99, 2405.10.2138/am-2014-4944Search in Google Scholar

[57] E. F. Rauch, J. Portillo, S. Nicolopoulos, D. Bultreys, S. Rouvimov, P. Moeck, Z. Kristallogr.2010, 225, 103.10.1524/zkri.2010.1205Search in Google Scholar

[58] C. Viti, A. Brogi, D. Liotta, E. Mugnaioli, R. Spiess, A. Dini, M. Zucchi, G. Vannuccini, J. Struct. Geol.2016, 86, 1.10.1016/j.jsg.2016.02.013Search in Google Scholar

[59] I. Pignatelli, Y. Marrocchi, E. Mugnaioli, F. Bourdelle, M. Gounelle, Geochim. Cosmochim. Acta2017, 209, 106.10.1016/j.gca.2017.04.017Search in Google Scholar

[60] I. Pignatelli, E. Mugnaioli, J. Hybler, R. Mosser-Ruck, M. Cathelineau, N. Michau, Clays Clay Miner.2013, 61, 277.10.1346/CCMN.2013.0610408Search in Google Scholar

[61] I. Pignatelli, E. Mugnaioli, R. Mosser-Ruck, O. Barres, U. Kolb, N. Michau, Eur. J. Mineral.2014, 26, 221.10.1127/0935-1221/2014/0026-2370Search in Google Scholar

[62] M. Gemmi, J. Fischer, M. Merlini, S. Poli, P. Fumagalli, E. Mugnaioli, U. Kolb, Earth Planet. Sci. Lett.2011, 310, 422.10.1016/j.epsl.2011.08.019Search in Google Scholar

[63] S. Bhat, L. Wiehl, L. Molina-Luna, E. Mugnaioli, S. Lauterbach, S. Sicolo, P. Kroll, M. Duerrschnabel, N. Nishiyama, U. Kolb, K. Albe, H.-J. Kleebe, R. Riedel, Chem. Mater.2015, 27, 5907.10.1021/acs.chemmater.5b01706Search in Google Scholar

[64] G. C. Capitani, E. Mugnaioli, A. Guastoni, Am. Mineral.2016, 101, 1679.10.2138/am-2016-5605Search in Google Scholar

[65] A. Baraldi, E. Buffagni, R. Capelletti, M. Mazzera, M. Fasoli, A. Lauria, F. Moretti, A. Vedda, M. Gemmi, J. Phys. Chem. C2013, 117, 26831.10.1021/jp4101174Search in Google Scholar

[66] L. Palatinus, PETS – Program for Analysis of Electron Diffraction Data, Institute of Physics of the AS CR, Prague, 2011.Search in Google Scholar

[67] M. C. Burla, R. Caliandro, B. Carrozzini, G. L. Cascarano, C. Cuocci, C. Giacovazzo, M. Mallamo, A. Mazzone, G. Polidori, J. Appl. Crystallogr.2015, 48, 306.10.1107/S1600576715001132Search in Google Scholar

[68] G. M. Sheldrick, Acta Crystallogr. A2008, 64, 112.10.1107/S0108767307043930Search in Google Scholar PubMed

[69] P. Fumagalli, S. Poli, J. Petrol.2005, 46, 555.10.1093/petrology/egh088Search in Google Scholar

[70] P. Fumagalli, S. Poli, J. Fischer, M. Merlini, M. Gemmi, Contrib. Mineral. Petrol.2014, 167, 979.10.1007/s00410-014-0979-5Search in Google Scholar

[71] K. Momma, F. Izumi, J. Appl. Crystallogr.2011, 44, 1272.10.1107/S0021889811038970Search in Google Scholar

[72] V. Petříček, M. Dušek, L. Palatinus, Z. Kristallogr.2014, 229, 345.10.1515/zkri-2014-1737Search in Google Scholar

[73] M. C. Burla, R. Caliandro, M. Camalli, B. Carrozzini, G. L. Cascarano, L. De Caro, C. Giacovazzo, G. Polidori, D. Siliqi, R. Spagna, J. Appl. Crystallogr.2007, 40, 609.10.1107/S0021889807010941Search in Google Scholar

[74] L. Akselrud, Y. Grin, J. Appl. Crystallogr.2014, 47, 803.10.1107/S1600576714001058Search in Google Scholar

[75] L. Palatinus, G. Chapuis, J. Appl. Crystallogr.2007, 40, 451.Search in Google Scholar

[76] J. Felsche, J. Appl. Crystallogr.1969, 2, 303.10.1107/S0021889869007266Search in Google Scholar

[77] A. N. Christensen, A. F. Jensen, B. K. Themsen, R. G. Hazell, M. Hanfland, E. Dooryhee, Acta Chem. Scand.1997, 51, 1178.10.3891/acta.chem.scand.51-1178Search in Google Scholar

[78] V. P. Rogova, Y. P. Rogov, V. A. Drits, N. N. Kuznetsova, Zapiski Vsesoyuznogo Mineralogicheskogo Obshchestva1978, 107, 94.Search in Google Scholar

[79] Y. P. Menshikov, Zapiski Vsesoyuznogo Mineralogicheskogo Obshchestva1984, 113, 718.Search in Google Scholar

[80] K. Dornberger-Schiff, K. Fichtner, Krist. Techn.1972, 7, 1035.10.1002/crat.19720070907Search in Google Scholar

[81] G. Ferraris, E. Makovicky, S. Merlino, Crystallography of Modular Materials, IUCr Monographs on Crystallography 15, Oxford University Press, Oxford, 2004.Search in Google Scholar

[82] S. V. Krivovichev, Mineral. Mag.2013, 77, 275.10.1180/minmag.2013.077.3.05Search in Google Scholar

[83] E. Mugnaioli, Acta Crystallogr. B2015, 71, 737.10.1107/S2052520615022441Search in Google Scholar PubMed

[84] C. A. Corrêa, M. Klementová, V. Dřínek, J. Kopeček, L. Palatinus, J. Alloys Compd.2016, 672, 505.10.1016/j.jallcom.2016.02.190Search in Google Scholar

[85] M. Colmont, L. Palatinus, M. Huvé, H. Kabbour, S. Saitzek, N. Djelal, P. Roussel, Inorg. Chem.2016, 55, 2252.10.1021/acs.inorgchem.5b02663Search in Google Scholar PubMed

[86] M. Klementová, M. Karlík, P. Novák, L. Palatinus, Intermetallics2017, 85, 110.10.1016/j.intermet.2017.02.003Search in Google Scholar

[87] E. Mugnaioli, M. Gemmi, M. Merlini, M. Gregorkiewitz, Acta Crystallogr. B2016, 72, 893.10.1107/S2052520616015651Search in Google Scholar PubMed PubMed Central

[88] R. M. Hazen, J. H. Ausubel, Am. Mineral.2016, 101, 1245.10.2138/am-2016-5601CCBYSearch in Google Scholar

[89] R. M. Hazen, E. S. Grew, R. T. Downs, J. Golden, G. Hystad, Can. Mineral.2015, 53, 295.10.3749/canmin.1400086Search in Google Scholar

[90] R. M. Hazen, G. Hystad, R. T. Downs, J. J. Golden, A. J. Pires, E. S. Grew, Am. Mineral.2015, 100, 2344.10.2138/am-2015-5417Search in Google Scholar

[91] R. M. Hazen, D. R. Hummer, G. Hystad, R. T. Downs, J. J. Golden, Am. Mineral.2016, 101, 889.10.2138/am-2016-5546Search in Google Scholar

[92] I. Nederlof, E. van Genderen, Y.-W. Li, J. P. Abrahams, Acta Crystallogr. D2013, 69, 1223.10.1107/S0907444913009700Search in Google Scholar PubMed PubMed Central


Supplemental Material:

The online version of this article offers supplementary material (https://doi.org/10.1515/zkri-2017-2130).


Received: 2017-11-9
Accepted: 2018-1-2
Published Online: 2018-2-5
Published in Print: 2018-3-28

©2018 Walter de Gruyter GmbH, Berlin/Boston

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