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Combined Focused Ion Beam-Ultramicrotomy Method for TEM Specimen Preparation of Porous Fine-Grained Materials

Published online by Cambridge University Press:  20 December 2019

Kenta K. Ohtaki Open the ORCID record for Kenta K. Ohtaki [Opens in a new window] ,
Hope A. Ishii  and
John P. Bradley
Kenta K. Ohtaki
Affiliation:
Advanced Electron Microscopy Center, Hawai‘i Institute of Geophysics and Planetology, University of Hawai‘i at Mānoa, 1680 East-West Road, Honolulu, HI96822, USA
Hope A. Ishii*
Affiliation:
Advanced Electron Microscopy Center, Hawai‘i Institute of Geophysics and Planetology, University of Hawai‘i at Mānoa, 1680 East-West Road, Honolulu, HI96822, USA
John P. Bradley
Affiliation:
Advanced Electron Microscopy Center, Hawai‘i Institute of Geophysics and Planetology, University of Hawai‘i at Mānoa, 1680 East-West Road, Honolulu, HI96822, USA
*
*Author for correspondence: Hope A. Ishii, E-mail: [email protected]
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Abstract

A new transmission electron microscopy (TEM) specimen preparation method that utilizes a combination of focused ion beam (FIB) methods and ultramicrotomy is demonstrated. This combined method retains the benefit of site-specific sampling by FIB but eliminates ion beam-induced damage except at specimen edges and allows recovery of many consecutive sections. It is best applied to porous and/or fine-grained materials that are amenable to ultramicrotomy but are located in bulk samples that are not. The method is ideal for unique samples from which every specimen is precious, and we demonstrate its utility on fine-grained material from the one-of-a-kind Paris meteorite. Compared with a specimen prepared by conventional FIB methods, the final sections are uniformly thin and free from re-deposition and curtaining artifacts common in FIB specimens prepared from porous, heterogeneous samples.

Keywords

fine grainfocused ion beamion beam damage and sample preparationporoustransmission electron microscopyultramicrotomy
Type
Software and Instrumentation
Information
Microscopy and Microanalysis , Volume 26 , Issue 1 , February 2020 , pp. 120 - 125
Copyright
Copyright © Microscopy Society of America 2019

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References

Berger, EL & Keller, LP (2015). A hybrid ultramicrotomy-FIB technique for preparing serial electron transparent thin sections from particulate samples. Microsc Today 23, 18–23.CrossRefGoogle Scholar
Engelmann, HJ, Volkmann, B, Ritz, Y, Saage, H, Stegmann, H, de Robiliard, Q & Zschech, E (2003). TEM sample preparation using focused ion beam—capabilities and limits. Microsc Today 11, 22–25.CrossRefGoogle Scholar
Graham, GA, Teslich, NE, Kearsley, AT, Stadermann, FJ, Stroud, RM, Dai, Z, Ishii, HA, Hutcheon, ID, Bajt, S, Snead, CJ, Weber, PK & Bradley, JP (2008). Applied focused ion beam techniques for sample preparation of astromaterials for integrated analysis. Meteorit Planet Sci 43, 561–569.CrossRefGoogle Scholar
Heaney, PJ, Vicenzi, EP, Giannuzzi, LA & Livi, KJT (2001). Focused ion beam milling: A method of site-specific sample extraction for microanalysis of Earth and planetary materials. Am Miner 86, 1094–1099.CrossRefGoogle Scholar
Hewins, RH, Bourot-Denise, M, Zanda, B, Leroux, H, Barrat, J-A, Humayun, M, Goepel, C, Greenwood, RC, Franchi, IA, Pont, S, Lorand, J-P, Cournéde, C, Gattacceca, J, Rochette, P, Kuga, M, Marrocchi, Y & Marty, B (2014). The Paris meteorite, the least altered CM chondrite so far. Geochim Cosmochim Acta 124, 190–222.CrossRefGoogle Scholar
Ishitani, T, Umemura, K, Ohnishi, T, Yaguchi, T & Kamino, T (2004). Improvements in performance of focused ion beam cross-sectioning: Aspects of ion-sample interaction. J Electron Microsc 53, 443–449.CrossRefGoogle ScholarPubMed
Kakizaki, Y, Koyama, J, Yamaguchi, A, Umegai, S, Ayukawa, S & Kitano, H (2017). Transmission electron microscopy study of focused ion beam damage in small intrinsic Josephson junctions of single crystalline Bi2Sr2CaCu2O y. Jpn J Appl Phys 56, 043101.CrossRefGoogle Scholar
Lee, L-H, Yu, C-H, Wei, C-Y, Lee, P-C, Huang, J-S & Wen, C-Y (2019). Plan-view transmission electron microscopy specimen preparation for atomic layer materials using a focused ion beam approach. Ultramicroscopy 197, 95–99.CrossRefGoogle ScholarPubMed
Lee, MR, Bland, PA & Graham, G (2003). Preparation of TEM samples by focused ion beam (FIB) techniques: Applications to the study of clays and phyllosilicates in meteorites. Mineral Mag 67, 581–592.CrossRefGoogle Scholar
Leroux, H, Cuvillier, P, Zanda, B & Hewins, RH (2015). GEMS-like material in the matrix of the Paris meteorite and the early stages of alteration of CM chondrites. Geochim Cosmochim Acta 170, 247–265.CrossRefGoogle Scholar
Mayer, J, Giannuzzi, LA, Kamino, T & Michael, J (2007). TEM sample preparation and FIB-induced damage. MRS Bull 32, 400–407.CrossRefGoogle Scholar
McCaffrey, JP, Phaneuf, MW & Madsen, LD (2001). Surface damage formation during ion-beam thinning of samples for transmission electron microscopy. Ultramicroscopy 87, 97–104.CrossRefGoogle ScholarPubMed
Melo, LAG, Hitchcock, AP, Berejnov, V, Susac, D, Stumper, J & Botton, GA (2016). Evaluating focused ion beam and ultramicrotome sample preparation for analytical microscopies of the cathode layer of a polymer electrolyte membrane fuel cell. J Power Sources 312, 23–35.CrossRefGoogle Scholar
Montoya, E, Bals, S, Rossell, MD, Schryvers, D & Tendeloo, GV (2007). Evaluation of top, angle, and side cleaned FIB samples for TEM analysis. Microsc Res Tech 70, 1060–1071.CrossRefGoogle ScholarPubMed
Schaffer, M, Schaffer, B & Ramasse, Q (2012). Sample preparation for atomic-resolution STEM at low voltages by FIB. Ultramicroscopy 114, 62–71.CrossRefGoogle ScholarPubMed
Wirth, R (2004). Focused Ion Beam (FIB): A novel technology for advanced application of micro- and nanoanalysis in geosciences and applied mineralogy. Eur J Miner 16, 863–876.CrossRefGoogle Scholar
Xu, Y, Gu, L, Li, Y, Mo, B & Lin, Y (2018). Combination of focused ion beam (FIB) and microtome by ultrathin slice preparation for transmission electron microscopy (TEM) observation. Earth Planets Space 70, 150.CrossRefGoogle Scholar
Zega, TJ, Nittler, LR, Busemann, H, Hoppe, P & Stroud, RM (2007). Coordinated isotopic and mineralogic analyses of planetary materials enabled by in situ lift-out with a focused ion beam scanning electron microscope. Meteorit Planet Sci 42, 1373–1386.CrossRefGoogle Scholar
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