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Transmission electron microscopy (TEM) of Earth and planetary materials: A review

  • M. R. Lee (a1)

Abstract

Using high intensity beams of fast electrons, the transmission electron microscope (TEM) and scanning transmission electron microscope (STEM) enable comprehensive characterization of rocks and minerals at micrometre to sub-nanometre scales. This review outlines the ways in which samples of Earth and planetary materials can be rendered sufficiently thin for TEM and STEM work, and highlights the significant advances in site-specific preparation enabled by the focused ion beam (FIB) technique. Descriptions of the various modes of TEM and STEM imaging, electron diffraction and X-ray and electron spectroscopy are outlined, with an emphasis on new technologies that are of particular relevance to geoscientists. These include atomic-resolution Z-contrast imaging by high-angle annular dark-field STEM, electron crystallography by precession electron diffraction, spectrum mapping using X-rays and electrons, chemical imaging by energy-filtered TEM and true atomic-resolution imaging with the new generation of aberration-corrected microscopes. Despite the sophistication of modern instruments, the spatial resolution of imaging, diffraction and X-ray and electron spectroscopy work on many natural materials is likely to remain limited by structural and chemical damage to the thin samples during TEM and STEM.

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Avilov, A., Kuligin, K., Nicolopoulos, S., Nickolskiy, M., Boulahya, K., Portillo, J., Lepeshov, G., Sobolev, B., Collette, J.P., Martin, N., Robins, A.C. and Fischione, P. (2007) Precession technique and electron diffractometry as new tools for crystal structure analysis and chemical bonding determination. Ultramicroscopy, 7, 431444.
Banfield, J.F. and Barker, W.W. (1994) Direct observation of reactant-product interfaces formed in natural weathering of exsolved, defective amphibole to smectite: Evidence for episodic, isovolumetric reactions involving structural inheritance. Geochimica et Cosmochimica Acta, 58, 14191429.
Barber, D.J. (1970) Thin foils of non-metals made for electron microscopy by sputter-etching. Journal of Materials Science, 5, 18.
Barber, D.J. (1981) Demountable polished extra-thin sections and their use in transmission electron microscopy. Mineralogical Magazine, 44, 357359.
Barber, D.J. (1993) Radiation damage in ion-milled specimens: Characteristics, effects and methods of damage limitation. Ultramicroscopy, 52, 101125.
Barber, D.J. and Wenk, H.-R. (1984) Microstructures in carbonates from the Alnö and Fen carbonatities. Contributions to Mineralogy and Petrology, 88, 233245.
Barker, W.W. and Banfield, J.F. (1996) Biologically versus inorganically mediated weathering reactions: Relationships between minerals and extracellular microbial polymers in lithobiontic communities. Chemical Geology, 132, 5569.
Beermann, T and Brockamp, O. (2005) Structure analysis of montmorillonite crystallites by convergent-beam electron diffraction. Clay Minerals, 40, 113.
Benzerara, K., Menguy, N., Guyot, F., Vanni, C. and Gillet, P. (2005) TEM study of a silicate-carbonate-microbe interface prepared by focused ion beam milling. Geochimica et Cosmochimica Acta, 69, 14131422.
Bland, P.A., Jackson, M.D., Coker, R.F., Cohen, B.A., Webber, J.B.W., Lee, M.R., Duffy, C.M, Chater, R.J., Ardakani, M.G., McPhail, D.S., McComb, D.W. and Benedix, G.K. (2009) Why aqueous alteration in asteroids was isochemical: High porosity ≠ high permeability. Earth and Planetary Science Letters, 287, 559568.
Bleloch, A. and Lupini, A. (2004) Imaging at the picoscale. Materials Today, 7, 42.
Bogner, A., Thollet, G., Basset, D., Jouneau, P.-H. and Gauthier, C. (2005) Wet STEM: A new development in environmental SEM for imaging nano-objects included in a liquid phase. Ultramicroscopy, 104, 290301.
Bogner, A., Jouneau, P.-H., Thollet, G., Basset, D. and Gauthier, C. (2007) A history of scanning electron microscopy developments: Towards “wet-STEM” imaging. Micron, 38, 390401.
Bonneville, S., Smits, M.M., Brown, A., Harrington, J., Leake, J.R., Brydson, R. and Benning, L.G. (2009) Plant-driven fungal weathering: Early stages of mineral alteration at the nanometer scale. Geology, 37, 61 5618.
Bradley, J.P. and Brownlee, D.E. (1986) Cometary particles – thin sectioning and electron-beam analysis. Science, 231, 15421544.
Brown, W.L. and Parsons, I. (1984) Exsolution and coarsening mechanisms and kinetics in an ordered cryptoperthite series. Contributions to Mineralogy and Petrology, 86, 318.
Buseck, P.R., editor (1992) Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy. Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA, 516 pp.
Buseck, P.R. and Self, P. (1992) Electron energy-loss spectroscopy (EELS) and electron channeling (ALCHEMI). Pp 141180 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (Buseck, P.R., editor). Reviews in Mineralogy 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Casey, W.H., Westrich, H.R., Massis, T., Banfield, J.F. and Arnold, G.W. (1989) The surface of labradorite feldspar after acid hydrolysis. Chemical Geology, 78, 205218.
Cater, E.D. and Buseck, P.R. (1985) Mechanisms of decomposition of dolomite, Ca0.5Mg0.5CO3, in the electron microscope. Ultramicroscopy, 18, 241252.
Champness, P.E. (1977) Transmission Electron Microscopy in Earth Science. Annual Review of Earth and PlanetarySciences, 5, 203226.
Chizmadia, L.J. and Brearley, A.J. (2008) Mineralogy, aqueous alteration, and primitive textural characteristics of fine-grained rims in the Y-791198 CM2 carbonaceous chondrite: TEM observations and comparison to ALHA81002. Geochimica et Cosmochimica Acta, 72, 602625.
Chizmadia, L.J., Xu, Y., Schwappach, C. and Brearley, A.J. (2008) Characterization of micron-sized Fe,Ni metal grains in fine-grained rims in the Y-791198 CM2 carbonaceous chondrite: Implications for asteroidal and preaccretionary models of aqueous alteration. Meteoritics & Planetary Science, 43, 14191438.
Cliff, G. and Lorimer, G.W. (1975) Quantitative-analysis of thin specimens. Journal of Microscopy, 103, 203207.
Cowley, J.M. (2004) Applications of electron nanodiffraction. Micron, 35, 345360.
Egerton, R.F. (2009) Electron energy-loss spectroscopy in the TEM and SEM. Reports on Progress in Physics, 72, 016502.
Egerton, R.F., Li, P. and Malac, M. (2004) Radiation damage in the TEM and SEM. Micron, 35, 399409.
Feinberg, J.M., Harrison, R.J., Kasama, T., Dunin-Borkowski, R.E., Scott, G.R. and Renne, P.R. (2006) Effects of internal mineral structures on the magnetic remanence of silicate-hosted titanomagnetite inclusions: An electron holography study, Journal of Geophysical Research, 111, B12S15.
Fitz Gerald, J.D., Parsons, I. and Cayzer, N. (2006) Nanotunnels and pull-aparts: Defects of exsolution lamellae in alkali feldspars. American Mineralogist, 91, 772783.
Friedrich, H., McCartney, M.R. and Buseck, P.R. (2005) Comparison of intensity distributions in tomograms from BF TEM, ADF STEM, HAADF STEM, and calculated tilt series. Ultramicroscopy, 106, 1827.
Garvie, L.A.J. and Buseck, P.R. (1998) Ratios of ferrous to ferric iron from nanometre-sized areas in minerals. Nature, 396, 667670.
Garvie, L.A.J. and Buseck, P.R. (1999) Bonding in silicates: Investigation of the Si L2,3 edge by parallel electron energy-loss spectroscopy. American Mineralogist, 84, 946964.
Garvie, L.A.J. and Buseck, P.R. (2004) Nanosized carbon-rich grains in carbonaceous chondrite meteorites. Earth and Planetary Science Letters, 224, 431439.
Garvie, L.A.J. and Craven, A.J. (1994) High-resolution parallel electron-energy-loss spectroscopy of Mn L(2,3)-edges in inorganic manganese compounds. Physics and Chemistry of Minerals, 21, 191206.
Garvie, L.A.J., Craven, A.J. and Brydson, R. (1994) Use of electron energy-loss near-edge fine-structure in the study of minerals. American Mineralogist, 79, 411425.
Garvie, L.A.J., Zega, T.J., Rez, P. and Buseck, P.R. (2004) Nanometer-scale measurements of Fe3+/ΣFe by electron energy-loss spectroscopy: A cautionary note. American Mineralogist, 89, 16101616.
Garvie, L.A.J., Burt, D.M. and Buseck, P.R. (2008) Nanometer-scale complexity, growth, and diagenesis in desert varnish. Geology, 36, 215218.
Grogger, W., Schaffer, B., Krishnan, K.M. and Hofer, F. (2003) Energy-filtering TEM at high magnification: spatial resolution and detection limits . Ultramicroscopy, 96, 481489.
Hay, D.C., Dempster, T.J., Lee, M.R. and Brown, D.J. (2010) Anatomy of a low temperature zircon outgrowth. Contributions to Mineralogyand Petrology, 159, 8192.
Heaney, P.J., Vicenzi, E.P., Giannuzzi, L.A. and Livi, K.J.T. (2001) Focused ion beam milling: A method of site-specific sample extraction for microanalysis of Earth and planetary materials. American Mineralogist, 86, 10941099.
Herd, C.D.K., Papike, J.J. and Brearley, A.J. (2001) Oxygen fugacity of martian basalts from electron microprobe oxygen and TEM-EELS analyses of Fe-Ti oxides. American Mineralogist, 86, 10151024.
Hetherington, C. (2004) Aberration correction for TEM. Materials Today, 7, 5055.
Hochella, M.F. Jr, Moore, J.N., Golla, U. and Putnis, A. (1999) A TEM study of samples from acid mine drainage systems: Metal-mineral association with implications for transport. Geochimica et Cosmochimica Acta, 63, 33953406.
Houben, L., Thust, A. and Urban, K. (2006) Ultramicroscopy, 106, 200214.
Jacob, D., Cordier, P., Morniroli, J.P. and Schertl, H.P. (2009) Application of precession electron diffraction to the characterization of (021) twinning in pseudo-hexagonal coesite. American Mineralogist, 94, 684692.
Janney, D.E. and Wenk, H.-R. (1999) Peristerite exsolution in metamorphic plagioclase from the Lepontine Alps: An analytical and transmission electron microscope study. American Mineralogist, 84, 517527.
Janney, D.E., Cowley, J.M. and Buseck, P.R. (2000) Structure of synthetic 2-line ferrihydrite by electron nanodiffraction. American Mineralogist, 85, 11801187.
Janney, D.E., Cowley, J.M. and Buseck, P.R. (2001) Structure of synthetic 6-line ferrihydrite by electron nanodiffraction. American Mineralogist, 86, 327335.
Kirkland, A.I. and Meyer, R.R. (2004) ‘Indirect’ high-resolution transmission electron microscopy: Aberration measurement and wavefunction reconstruction. Microscopy and Microanalysis, 10, 401413.
Kirkland, A., Chang, L.-U., Haigh, S. and Hetherington, C. (2008) Transmission electron microscopy without aberrations: Applications to materials science. Current and Applied Physics, 8, 425428.
Lee, M.R. (1993) The petrography, mineralogy and origins of calcium sulphate within the Cold Bokkeveld CM carbonaceous chondrite. Meteoritics, 28, 5362.
Lee, M.R. and Ellen, R. (2008) Aragonite in the Murray (CM2) carbonaceous chondrite: implications for parent body compaction and aqueous alteration. Meteoritics & Planetary Science, 43, 12191231.
Lee, M.R. and Parsons, I. (2003) Microtextures of authigenic Or-rich feldspar in the Upper Jurassic Humber Group, UK North Sea. Sedimentology, 50, 597608.
Lee, M.R. and Smith, C.L. (2006) Scanning transmission electron microscopy using a SEM: applications to mineralogy and petrology. Mineralogical Magazine, 70, 561572.
Lee, M.R., Russell, S.S., Arden, J.W. and Pillinger, C.T. (1995) Nierite (Si3N4), a new mineral from ordinary and enstatite chondrites. Meteoritics, 30, 387–98.
Lee, M.R., Bland, P.A. and Graham, G. (2003) Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites. Mineralogical Magazine, 67, 581592.
Lee, M.R., Brown, D.J., Smith, C.L., Hodson, M.E., MacKenzie, M. and Hellmann R. (2007) Characterization of mineral surfaces using FIB and TEM: A case study of naturally-weathered alkali feldspars. American Mineralogist, 92, 13831394.
Lee, M.R., Hodson, M.E., Brown, D.J., MacKenzie, M. and Smith, C.L. (2008 a) The composition and crystallinity of the near-surface regions of weathered alkali feldspars. Geochimica et Cosmochimica Acta, 72, 49624975.
Lee, M.R., Brown, D.J., Hodson, M.E., MacKenzie, M. and Smith, C.L. (2008 b) Weathering microenvironments on feldspar surfaces: implications for understanding fluid-mineral reactions in soils. Mineralogical Magazine, 72, 13191328.
Lee, S., Kim, Y.-M. and Kim, Y.-J. (2007) Formation of crystalline silicon in kaolinite by electron beam irradiation and in situ heating in the HVEM. Journal of Electron Microscopy, 56, 153155.
Leppard, G.G. (2008) Nanoparticles in the environment as revealed by transmission electron microscopy: Detection, characterisation and activities. Current Nanoscience, 4, 278301.
Leroux, H. (2001) Microstructural shock signatures of major minerals in meteorites. European Journal of Mineralogy, 13, 253272.
Leroux, H., Rietmeijer, F.J.M., Velbel, M.A., Brearley, A.J., Jacob, D., Langenhorst, F., Bridges, J.C., Zega, T.J., Stroud, R.M., Cordier, P., Harvey, R.P., Lee, M., Gounelle, M. and Zolensky, M.E. (2008). A TEM study of thermally modified comet 81P/Wild 2 dust particles by interactions with the aerogel matrix during the Stardust capture process. Meteoritics & PlanetaryScience, 43, 124.
Loomer, D.B., Al, T.A., Weaver, L. and Cogswell, S. (2007) Manganese valence imaging in Mn minerals at the nanoscale using STEM-EELS. American Mineralogist, 92, 7279.
Loretto, M.H. (1994) Electron Beam Analysis of Materials. 2nd edition, Chapman and Hall, London, 272 pp.
Ma, C., Goreva, J.S. and Rossman, G.R. (2002) Fibrous nanoinclusions in massive rose quartz: HRTEM and AEM investigations. American Mineralogist, 87, 269276.
McLaren, A.C. (1991) Transmission Electron Microscopy of Minerals and Rocks. Cambridge University Press, Cambridge, UK, 399 pp.
Midgley, P.A. and Weyland, M. (2003) 3D electron microscopy in the physical sciences: the development of Z-contrast and EFTEM tomography. Ultramicroscopy, 96, 413431.
Midgley, P.A. and Dunin-Borkowski, R.E. (2009) Electron tomography and holography in materials science. Nature Materials, 8, 271280.
Mikouchi, T., Zolensky, M., Ivanova, M., Tachikawa, O., Komatsu, M., Le, L. and Gounelle, M. (2009) Dmitryivanovite: A new high-pressure calcium aluminium oxide from the Northwest Africa 470 CH3 chondrite characterized using electron backscatter diffraction analysis. American Mineralogist, 94, 746750.
Moore, K.T., Elbert, D.C. and Veblen, D.R. (2001) Energy-filtered transmission electron microscopy (EFTEM) of intergrown pyroxenes. American Mineralogist, 86, 814825.
Mugnaioli, E., Capitani, G., Nieto, F. and Mellini, M. (2009) Accurate and precise lattice parameters by selected-area electron diffraction in the transmission electron microscope. American Mineralogist, 94, 793800.
Muller, D.A. (2009) Structure and bonding at the atomic scale by scanning transmission electron microscopy. Nature Materials, 8, 263270.
O'Keefe, M.A. (2008) Seeing atoms with aberration-corrected sub-Angstrom electron microscopy. Ultramicroscopy, 108, 1 96209.
Obst, M., Gasser, P., Mavrocordatos, D. and Dittrich, M. (2005) TEM-specimen preparation of cell/mineral interfaces by Focused Ion Beam milling. American Mineralogist, 90, 12701277.
Palenik, C.S., Utsunomiya, S., Reich, M., Kesler, S.E., Wang, L. and Ewing, R.C. (2004) ‘Invisible’ gold revealed: Direct imaging of gold nanoparticles in a Carlin-type deposit. American Mineralogist, 89, 13591366.
Peacor, D.R. (1992 a) Diagenesis and low grade metamorphism of shales and slates. Pp 335380 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (Buseck, P.R., editor). Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Peacor, D.R. (1992 b) Analytical electron microscopy: X-ray analysis. Pp 113140 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (Buseck, P.R., editor). Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Prior, D.J., Boyle, A.P., Brenker, F., Cheadle, M.C., Day, A., Lopez, G., Peruzzo, L., Potts, G.J., Reddy, S., Spiess, R., Timms, N.E., Trimby, P., Wheeler, J. and Zetterstrom, L. (1999) The application of electron backscatter diffraction and orientation contrast imaging in the SEM to textural problems in rocks. American Mineralogist, 84, 17411759.
Putnis, A. (1992) Introduction to Mineral Sciences. Cambridge University Press, Cambridge, UK, 457 pp.
Reddy, S.M., Timms, N.E., Trimby, P., Kinny, P.D., Buchan, C. and Blake, K. (2006) Crystal-plastic deformation of zircon: A defect in the assumption of chemical robustness. Geology, 34, 257260.
Reeder, R.J. (1992) Carbonates: Growth and alteration microstructures. Pp 381424 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Miroscopy (Buseck, P.R., editor). Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Seydoux-Guillaume, A.M., Goncalves, P., Wirth, R. and Deutsch, A. (2003) Transmission electron microscope study of polyphase and discordant monazites: Site-specific specimen preparation using the focused ion beam technique. Geology, 31, 973976.
Self, P. (1992) High-resolution image simulation and analysis. Pp 85112 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (Buseck, P.R., editor). Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Smith, D.J. (2008) Ultimate resolution in the electron microscope? Materials Today, 11 supp. 1, 3038.
Steeds, J.W. and Morniroli, J.-P. (1992) Selected area electron diffraction (SAED) and convergent beam electron diffraction (CBED). Pp 3784 in: Minerals and Reactions at the Atomic Scale: Transmission Electron Microscopy (Buseck, P.R., editor). Reviews in Mineralogy, 27, Mineralogical Society of America, Chantilly, Virginia, USA.
Stephan, T., Jessberger, E.K.,Klöck, W., Rulle, H. and Zehnpfenning, J. (1994) TOF-SIMS analysis of interplanetary dust. Earth and Planetary Science Letters, 128, 453467.
Stroud, R.M., Alexander, C.M.O'D. and MacPherson, G.J. (2000) A precise new method of microsampling chondritic material for transmission electron microscope analysis: preliminary application to calcium-aluminium-rich inclusions and associated matrix material in the Vigarano CV3 meteorite. Meteoritics & Planetary Sciences Supplement, 35, A153154.
Urban, K.W. (2008) Studying atomic structures by aberration-corrected transmission electron microscopy. Science, 321, 506510.
Urban, K.W. (2009) Is science prepared for atomic resolution electron microscopy? Nature Materials, 8, 260262.
Utsunomiya, S. and Ewing, R.C. (2003) Application of high-angle annular dark field scanning transmission electron microscopy, scanning transmission electron microscopy-energy dispersive X-ray spectrometry, and energy-filtered transmission electron microscopy to the characterisation of nanoparticles in the environment. Environmental Science and Technology, 37, 786791.
Utsunomiya, S., Palenik, C.S., Valley, J.W., Cavosie, A.J., Wilde, S.A. and Ewing, R.C. (2004) Nanoscale occurrence of Pb in an Archean zircon. Geochimica et Cosmochimica Acta, 68, 46794686.
Utsunomiya, S., Valley, J.W., Cavosie, A.J., Wilde, S.A. and Ewing, R.C. (2007) radiation damage and alteration of zircon from a 3.3 Ga porphyritic granite from the Jack Hills, Western Australia. Chemical Geology, 236, 91111.
Utsunomiya, S., Kersting, A.B. and Ewing, R.C. (2009) Groundwater nanoparticles in the far-field of the Nevada test site: Mechanism for radionuclide transport. Environmental Science and Technology, 43, 12931298.
Van Ngo, V., Hernandez, M., Roth, B. and Joy, D.C. (2007) STEM imaging of lattice fringes and beyond in a UHR in-lens field-emission SEM. Microscopy Today, 15(2) 1216.
Watt, L.E., Bland, P.A., Prior, D.J. and Russell, S.S. (2006) Fabric analysis of Allende matrix using EBSD. Meteoritics & Planetary Science, 41, 9891001.
Williams, D.B. and Carter, C.B. (1996) Transmission Electron Microscopy – A Textbook for Materials Science. Plenum Press, New York and London, 729 pp.
Wirth, R. (2004) Focused ion beam (FIB): A novel technology for advanced application of micro- and nanoanalysis in geosciences and applied mineralogy. European Journal of Mineralogy, 16, 863876.
Wirth, R. (2009) Focused ion beam combined with SEM and TEM: Advanced analytical tools for studies of chemical composition, microstructure and crystal structure in geomaterials on a nanometer scale. Chemical Geology, 261, 217229.
Xin, H.-J., Intaraprasonk, V. and Muller, D.A. (2008) Depth sectioning of individual dopant atoms with aberration-corrected scanning transmission electron microscopy. Applied Physics Letters, 92, 013125.
Zega, T.J., Garvie, L.A.J. and Buseck, P.R. (2003) Nanometer-scale measurements of iron oxidation states of cronstedtite from primitive meteorites. American Mineralogist, 88, 11691172.
Zega, T.J., Nittler, L.R., Busemann, H., Hoppe, P. and Stroud, R.M. (2007) Coordinated isotopic and mineralogical analyses of planetary materials enabled by in situ lift-out with a focused ion beam scanning electron microscope. Meteoritics & PlanetaryScience, 42, 13731386.
Zhang, S. and Veblen, D.R. (2007) Chemical and structural variations at augite (100) deformation twin boundaries. American Mineralogist, 92, 18331837.
Zhu, C., Veblen, D.R., Blum, A.E. and Chipera, S.J. (2006) Naturally weathered feldspar surfaces in the Navajo Sandstone aquifer, Black Mesa, Arizona: Electron microscopic characterization. Geochimica et Cosmochimica Acta, 65, 34593474.
Ziegler, J.F. (2003) The stopping and range of ions in matter (SRIM-2003). Annapolis, Maryland. http://www.srim.org
Zolensky, M., Nakamura-Messenger, K., Fletcher, L. and See, T. (2008) Curation, spacecraft recovery, and preliminary examination for the Stardust mission: A perspective from the curational facility. Meteoritics & Planetary Science, 43, 521.

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Transmission electron microscopy (TEM) of Earth and planetary materials: A review

  • M. R. Lee (a1)

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