High-Resolution Visualization Techniques: Structural Aspects

  • D. SchryversEmail author
  • S. Van Aert
Part of the Springer Series in Materials Science book series (SSMATERIALS, volume 148)


This chapter discusses a number of conventional and advanced techniques in transmission electron microscopy used for the visualization of structural aspects of disorder and strain-induced complexity in a selection of real materials. Most examples relate to shape memory materials such as \(\mathrm{Ni}\mbox{ \textendash }\mathrm{Al}\) and \(\mathrm{Ni}\mbox{ \textendash }\mathrm{Ti}(-\mathrm{X})\) and some to plasticity in bulk and thin films. The techniques are chosen in view of existing or potential quantitative output such as Geometric Phase Imaging based on atomic resolution images, statistical parameter estimation, tomography, and conical dark-field imaging. Clearly, this overview does not provide a complete list of present day methods for high-resolution imaging, but it should give the reader a flavour of the possibilities and potentials of transmission electron microscopy for the quantitative study of complex materials.The study of materials can be conducted on many length scales and by many different techniques and methods. For visualization techniques, despite efforts on multi-scale exercises, often the scale of the details aimed for relates closely to the dimensions of the device in mind or at most one order of magnitude smaller. A typical example of macroscopic imaging techniques is automated camera-assisted strain measurements using surface labelling techniques. Correlations between macroscopic properties and much smaller dimensions, e.g., at the nano-level, often still suffer from serious gaps in connecting results from different length scales. For functional materials, however, with properties sensitive to a change in the environment such as temperature, pressure, electric field, magnetic field, and chemical interactions, the working dimensions often immediately fall within the micro- or nano-scale so that no or little scale differences exist between the properties and the high-resolution imaging techniques. Moreover, the continuing evolution towards miniaturization of devices from functional materials even further calls for special imaging techniques with very high spatial resolution.In this chapter, the focus is on atomic or high-resolution transmission electron microscopy (HRTEM) used to collect data on a variety of real materials and problems, with the emphasis on shape memory materials. Some examples also include spectroscopic data from energy-dispersive X-ray analysis (EDX) or electron energy loss spectroscopy (EELS) and novel TEM techniques.


Habit Plane Electron Energy Loss Spectroscopy Shape Memory Material Twin Variant Statistical Parameter Estimation 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.



The authors thank S. Bals, W. Tirry, H. Idrissi, B. Wang, and Z.Q. Yang for support with the TEM observations. Part of this work was performed in the framework of a European FP6 project “Multi-scale modeling and characterization for phase transformations in advanced materials” \((\mathrm{MRTN}\mbox{ -}\mathrm{CT}\mbox{ -}2004\mbox{ \textendash }505226)\) and an IAP program of the Belgian State Federal Office for Scientific, Technical and Cultural Affairs (Belspo), under Contract No. P6/24. Support was also provided by FWO projects G.0465.05 “The functional properties of SMA: a fundamental approach”, G.0576.09 “3D characterization of precipitates in \(\mathrm{Ni}\mbox{ \textendash }\mathrm{Ti}\) SMA by slice-and-view in a FIB-SEM dual-beam microscope”, G.0188.08N “Optimal experimental design for quantitative electron microscopy”, G.0064.10N “Quantitative electron microscopy: from experimental measurements to precise numbers” and G.0180.08 “Optimization of Focused Ion Beam (FIB) sample preparation for transmission electron microscopy of alloys”.


  1. 1.
    I.M. Robertson, C.M. Wayman, Tweed microstructures I. Characterization in β-NiAl. Phil. Mag. A 48, 421 (1983)Google Scholar
  2. 2.
    D. Schryvers, D. Holland-Moritz, Austenite and martensite microstructures in splat-cooled Ni-Al. Intermetallics 6, 427 (1998)CrossRefGoogle Scholar
  3. 3.
    D. Schryvers, L.E. Tanner, On the interpretation of high-resolution electron microscopy images of premartensitic microstuctures in the Ni-Al B2 phase. Ultramicroscopy 32, 241 (1990)CrossRefGoogle Scholar
  4. 4.
    S. Shapiro, B. Yang, Y. Noda, L. Tanner, D. Schryvers, Neutron-scattering and electron-microscopy studies of the premartensitic phenomena in NixAl100-x alloys. Phys. Rev. B 44, 9301 (1991)CrossRefGoogle Scholar
  5. 5.
    B.I. Halperin, C.M. Varma, Defects and the central peak near structural phase transitions. Phys. Rev. B 14, 4030 (1976)CrossRefGoogle Scholar
  6. 6.
    Y. Yamada, Y. Noda, M. Takimoto, ‘Modulated lattice relaxation’ in β-based premartensitic phase. Sol. St. Comm. 55, 1003 (1985)CrossRefGoogle Scholar
  7. 7.
    R. Gooding, J. Krumhansl, Symmetry-restricted anharmonicities and the CsCl-to-7R martensitic structural phase transformation of the NixAl1-x system, Phys. Rev. B 39, 1535 (1989)CrossRefGoogle Scholar
  8. 8.
    W. Cao, J. Krumhansl, R. Gooding, Defect-induced heterogeneous transformations and thermal growth in athermal martensite. Phys. Rev. B 41, 11319 (1990)CrossRefGoogle Scholar
  9. 9.
    W. Zhang, Y.M. Jin, A.G. Khachaturyan, Phase field microelasticity modeling of heterogeneous nucleation and growth in martensitic alloys. Acta. Mat. 55, 565 (2007)CrossRefGoogle Scholar
  10. 10.
    P. Lloveras, T. Castán, M. Porta, A. Planes, A. Saxena, Influence of elastic anisotropy on structural nanoscale textures. Phys. Rev. Lett. 100, 165707 (2008)CrossRefGoogle Scholar
  11. 11.
    Y. Wang, A.G. Khachaturyan, Three-dimensional field model and computer modeling of martensitic transformations. Acta. Mat. 45, 759 (1997)CrossRefGoogle Scholar
  12. 12.
    T. Tadaki, Y. Nakata, K.I. Shimizu, K. Otsuka, Crystal structure, composition and morphology of a precipitate in an aged Ti-51 at.% Ni shape memory alloy. Trans. JIM. 27, 731 (1986)Google Scholar
  13. 13.
    W. Tirry, D. Schryvers, K. Jorissen, D. Lamoen, Electron-diffraction structure refinement of Ni4Ti3 precipitates in Ni52Ti48. Acta. Cryst. B 62, 966 (2006)CrossRefGoogle Scholar
  14. 14.
    W. Tirry, D. Schryvers, Quantitative determination of strain fields around Ni4Ti3 precipitates in NiTi. Acta. Mat. 53, 1041 (2005)CrossRefGoogle Scholar
  15. 15.
    Z. Yang, W. Tirry, D. Schryvers, Analytical TEM investigations on concentration gradients surrounding Ni4Ti3 precipitates in Ni-Ti shape memory material. Scripta. Mat. 52, 1129 (2005)CrossRefGoogle Scholar
  16. 16.
    Z. Yang, W. Tirry, D. Lamoen, S. Kulkova, D. Schryvers, Electron energy-loss spectroscopy and first-principles calculation studies on a Ni-Ti shape memory alloy. Acta. Mat. 56, 395 (2008)CrossRefGoogle Scholar
  17. 17.
    W. Tirry, D. Schryvers, Linking a completely three-dimensional nanostrain to a structural transformation eigenstrain. Nat. Mater. 8, 752 (2009)CrossRefGoogle Scholar
  18. 18.
    M. Hÿtch, E. Snoeck, R. Kilaas, Quantitative measurement of displacement and strain fields from HRTEM micrographs. Ultramicroscopy 57, 131 (1998)CrossRefGoogle Scholar
  19. 19.
    L. Bataillard, J.E. Bidaux, R. Gotthardt, Interaction between microstructure and multiple-step transformation in binary NiTi alloys using in-situ transmission electron microscopy observations. Phil. Mag. A 78, 327 (1998)CrossRefGoogle Scholar
  20. 20.
    J. Verbeeck, G. Bertoni, Model-based quantification of EELS spectra: Treating the effect of correlated noise, Ultramicroscopy 108, 74 (2008)CrossRefGoogle Scholar
  21. 21.
    J. Cui, Y.S. Chu, O.O. Famodu, Y. Furuya, J. Hattrick-Simpers, R.D. James, A. Ludwig, S. Thienhaus, M. Wuttig, Z. Zhang, I. Takeuchi, Combinatorial search of thermoelastic shape-memory alloys with extremely small hysteresis width. Nat. Mater. 5, 286 (2006)CrossRefGoogle Scholar
  22. 22.
    Z. Zhang, R.D. James, S. Müller, Energy barriers and hysteresis in martensitic phase transformations. Acta. Mat. 57, 4332 (2009)CrossRefGoogle Scholar
  23. 23.
    R. Delville, D. Schryvers, Z. Zhang, R.D. James, Transmission electron microscopy investigation of microstructures in low-hysteresis alloys with special lattice. Scripta. Mat. 60, 293 (2009)CrossRefGoogle Scholar
  24. 24.
    R. Delville, S. Kasinathan, Z. Zhang, J. Van Humbeeck, R.D. James, D. Schryvers, Transmission electron microscopy study of phase compatibility in low hysteresis shape memory alloys. Phil. Mag. 90, 177 (2010)CrossRefGoogle Scholar
  25. 25.
    R. Delville, From functional properties to micro/nano-structures: a TEM study of TiNi(X) shape memory alloys (Antwerp, 2010)Google Scholar
  26. 26.
    Y. Watanabe, T. Saburi, Y. Nakagawa, S. Nenno, Jpn. Inst. Met. 54, 861 (1990)Google Scholar
  27. 27.
    R. Delville, B. Malard, J. Pilch, P. Sittner, D. Schryvers, Microstructure changes during non-conventional heat treatment of thin Ni-Ti wires by pulsed electric current studied by TEM. Acta. Mat. 58, 4503 (2010)CrossRefGoogle Scholar
  28. 28.
    R. Delville, B. Malard, J. Pilch, P. Sittner, D. Schryvers, Transmission electron microscopy investigation of dislocation slip during superelastic cycling of Ni-Ti wires. Int. J. Plast. 27, 282 (2011)CrossRefGoogle Scholar
  29. 29.
    M.A. Haque, M.T.A. Saif, Strain gradient effect in nanoscale thin films. Acta. Mat. 51, 3053 (2003)CrossRefGoogle Scholar
  30. 30.
    M. Coulombier, A. Boe, C. Brugger, J.P. Raskin, T. Pardoen, Imperfection sensitive ductility of aluminium thin films. Scripta. Mat. 62, 742 (2010)CrossRefGoogle Scholar
  31. 31.
    S. Gravier, M. Coulombier, A. Safi, N. André, A. Boé, J.P. Raskin, T. Pardoen, J. Microelectromech. Syst. 18, 555 (2009)CrossRefGoogle Scholar
  32. 32.
    A. Boé, A. Safi, M. Coulombier, D. Fabrègue, T. Pardoen, J.-P. Raskin, MEMS-based microstructures for nanomechanical characterization of thin films. Smart. Mat. Struct. 18, 115018 (2009)CrossRefGoogle Scholar
  33. 33.
    A. Boé, A. Safi, M. Coulombier, T. Pardoen, J.P. Raskin, Internal stress relaxation based method for elastic stiffness characterization of very thin films. Thin Solid Films 518, 260 (2009)CrossRefGoogle Scholar
  34. 34.
    H. Idrissi, B. Wang, M.S. Colla, J.P. Raskin, D. Schryvers, T. Pardoen, Ultrahigh Strain Hardening in Thin Palladium Films with Nanoscale Twins. Advanced Materials 23, 2119 (2011)CrossRefGoogle Scholar
  35. 35.
  36. 36.
    A. Van den Bos, Parameter estimation for scientists and engineers (Wiley-Interscience, 2007)Google Scholar
  37. 37.
    A.J. den Dekker, S. Van Aert, A. van den Bos, D. Van Dyck, Maximum likelihood estimation of structure parameters from high resolution electron microscopy images. Part I: a theoretical framework. Ultramicroscopy 104, 83 (2005)Google Scholar
  38. 38.
    S. Bals, S. Van Aert, G. Van Tendeloo, D. Avila-Brande, Statistical estimation of atomic positions from exit wave reconstruction with a precision in the picometer range. Phys. Rev. Lett. 96, 096106 (2006)CrossRefGoogle Scholar
  39. 39.
    S. Van Aert, J. Verbeeck, R. Erni, S. Bals, M. Luysberg, D. Van Dyck, G. Van Tendeloo, Quantitative atomic resolution mapping using high-angle annular dark field scanning transmission electron microscopy. Ultramicroscopy 109, 1236 (2009)CrossRefGoogle Scholar
  40. 40.
    J. Jansen, D. Tang, H.W. Zandbergen, H. Schenk, MSLS, a least-squares procedure for accurate crystal structure refinement from dynamical electron diffraction patterns. Acta. Cryst. A 54, 91 (1998)CrossRefGoogle Scholar
  41. 41.
    J. Jansen, H.W. Zandbergen, Determination of absolute configurations of crystal structures using electron diffraction patterns by means of least-squares refinement. Ultramicroscopy 90, 291 (2002)CrossRefGoogle Scholar
  42. 42.
    P.M. Voyles, J.M. Gibson, M.M. Treacy, Fluctuation microscopy: a probe of atomic correlations in disordered materials. J. Elect. Microsc. 49, 259 (2000)Google Scholar
  43. 43.
    G. Wu, S. Zaefferer, Advances in TEM orientation microscopy by combination of dark-field conical scanning and improved image matching. Ultramicroscopy 109, 1317 (2009)CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2012

Authors and Affiliations

  1. 1.EMAT, University of AntwerpAntwerpBelgium

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