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References
General References
Humphreys CJ (1979) Scattering of fast electrons by crystals. Rep Prog Phys 42:1825 (Useful as background to section 9.2.)
Reimer L (1984) Transmission Electron Microscopy. Springer Series in Optical Sciences, vol. 36. Springer, Berlin Heidelberg New York Tokio (Useful as background to section 9.2.)
Tillmann K, Thust A, Urban K (2004) Spherical aberration correction in tandem with exit-plane wave function reconstruction: interlocking tools for the atomic scale imaging of lattice defects in GaAs. Microsc Microanal 10:185–198 (Example of application)
Specific References
Bethe H (1928) Theorie der Beugung von Elektronen an Kristallen. Ann Phys 87:55–129 (For the Bethe–Bloch formalism)
Gerchberg RW, Saxton WO (1972) Practical algorithm for determination of phase from image and diffraction plane pictures. Optik 35:237
Kübel C, Thust A (2006) TrueImage – A software package for focal-series reconstruction in HRTEM. NATO Science Series, Series II. Math Phys Chem 211:373–392
Misell DL (1973) Examination of an iterative method for solution of phase problem in optics and electron optics. 1. Test calculations. J Phys D 6:2200–2216
Schiske P (2002) Image reconstruction by means of focus series. J Microsc 207:154–154 (Reprint of the original 1968 paper)
Diffraction, Imaging, and Cs-correction (i. e. ‘Forward’ Theory)
Bethe H (1928) Theorie der Beugung von Elektronen an Kristallen. Ann Phys 87:55–129 (The Bethe–Bloch formalism)
Cowley JM, Moodie AF (1957) The scattering of electrons by atoms and crystals. 1. A new theoretical approach. Acta Cryst 10:609–619 (The Multislice Approach)
Goodman P, Moodie AF (1974) Numerical evaluation of n-beam wave-functions in electron-scattering by multi-slice method. Acta Cryst A30:280–290 (More Multislice)
Haider M, Rose H, Uhlemann S, Schwan E, Kabius B, Urban (1998a) A spherical-aberration-corrected 200 kV transmission electron microscope. Ultramicroscopy 75:53–60 (Using the corrector in Sect. 9.3.3.)
Haider M, Uhlemann S, Schwan E, Rose H, Kabius B, Urban K (1998b) Electron microscopy image enhanced. Nature 392:768–769 (Using the corrector in Sect. 9.3.3.)
Humphreys CJ (1979) Scattering of fast electrons by crystals. Rep Prog Phys 42:1864 (For Bloch waves)
Jia CL, Lentzen M, Urban K (2003) Atomic-resolution imaging of oxygen in perovskite ceramics. Science 299:870–873 (Negative C S)
Jia CL, Lentzen M, Urban K (2004) High-resolution transmission electron microscopy using negative spherical aberration. Microsc Microanal 10(2):174–184 (Negative C S)
Lentzen M, Jahnen B, Jia CL, Thust A, Tillmann K, Urban K (2002) High-resolution imaging with an aberration-corrected transmission electron microscope. Ultramicroscopy 92:233–242 (First applications of C S correction)
Lichte H (1991) Optimum focus for taking electron holograms. Ultramicroscopy 38(1):13–22 (For his defocus Z opt)
Reimer L (1984) Transmission Electron Microscopy. Springer Series in Optical Sciences, vol. 36. Springer, Berlin Heidelberg New York Tokio
Rose H (1990) Outline of a spherically corrected semiaplanatic medium-voltage transmission electron-microscope. Optik 85:19–24 (Using the corrector in Sect. 9.3.3)
Scherzer O (1949) The theoretical resolution limit of the electron microscope. J Appl Phys 20:20–29 (For his defocus)
Linear FSR
Saxton WO in Advances in Electronics and Electron Physics. (1978). Academic Press, London, Suppl. 10, Ch. 9.7. When you are thinking about Eq. 9.30.
Saxton WO (1980) Correction of artifacts in linear and non-linear high-resolution electron-micrographs. J Microsc Spectrosc Electron 5:665–674 (When you are thinking about Eq. 9.30)
Saxton WO (1986). Proc. 11th Int. Congr. for Electron Microscopy, Kyoto, post deadline paper 1 (unpublished). When you are thinking about Eq. 9.30.
Saxton WO (1994) What is the focus variation method – is it new – is it direct. Ultramicroscopy 55:171–181 (When you are thinking about Eq. 9.30)
Schiske P (1968). Proc 4th Reg Congr Electron Microscopy, Rome, 1, 145. If you can find it when you are thinking about Eq. 9.30.
Schiske P (2002) Image reconstruction by means of focus series. J Microscopy 207:154–154 (When you are thinking about Eq. 9.30. Reprint of Schiske P (1968))
Nonlinear FSR
Allen LJ, Oxley MP (2001) Phase retrieval from series of images obtained by defocus variation. Optics Commun 199:65–75 (The transport-of-intensity formalism)
Coene WMJ, Thust A, de Beeck MO, Van Dyck D (1996) Maximum-likelihood method for focus-variation image reconstruction in high resolution transmission electron microscopy. Ultramicroscopy 64:109–135 (Using general least-squares)
Gerchberg RW, Saxton WO (1972) Practical algorithm for determination of phase from image and diffraction plane pictures. Optik 35(2):237 (The Gerchberg-Saxton algorithm)
Kirkland EJ (1984) Improved high-resolution image-processing of bright field electron-micrographs. 1. Theory. Ultramicroscopy 15:151–172 (Using general least-squares)
Kirkland EJ, Siegel BM, Uyeda N, Fujiyoshi Y (1985) Improved high-resolution image-processing of bright field electron-micrographs. 2. Experiment. Ultramicroscopy 17:87–103 (Using general least-squares)
Kübel C, Thust A (2006) TrueImage – A software package for focal-series reconstruction in HRTEM. NATO Science Series, Series II. Math Phys Chem 211:373–392
Misell DL (1973) Examination of an iterative method for solution of phase problem in optics and electron optics.1. Test calculations. J Phys D 6:2200–2216 (The Misell algorithm)
Thust A, Lentzen M, Urban K (1994) Nonlinear reconstruction of the exit plane-wave function from periodic high-resolution electron-microscopy images. Ultramicroscopy 53:101–120 (Use of stochastic algorithms)
Thust A, Coene WMJ, de Beeck MO, Van Dyck D (1996) Focal-series reconstruction in HRTEM: Simulation studies on non-periodic objects. Ultramicroscopy 64:211–230 (Using general least-squares)
Thust A, Lentzen M, Urban K (2000) Scanning Microscopy Suppl 1:435 (Use of stochastic algorithms)
Numerical Aberration Correction
Thust A, Overwijk MHF, Coene WMJ, Lentzen M (1996) Numerical correction of lens aberrations in phase-retrieval HRTEM. Ultramicroscopy 64:249–264 (Numerical aberration correction; dislocation core)
Materials Science Applications of FSR
Barthel J, Weirich TE, Cox G, Hibst H, Thust A (2010) Structure of Cs-0.5[Nb2.5W2.5O14] analysed by focal-series reconstruction and crystallographic image processing. Acta Mater 58:3764–3772 (Catalyst)
Van Dyck D, Jinschek JR, Chen FR (2012) ‘Big Bang’ tomography as a new route to atomic-resolution electron tomography. Nature 486:243–246 (and 489, 460. Graphene)
Houben L, Thust A, Urban K (2006) Atomic-precision determination of the reconstruction of a 90 degrees tilt boundary in YBa2CU3O7-delta by aberration corrected HRTEM. Ultramicroscopy 106:200–214 (Near-picometre-precision)
Jia CL, Thust A (1999) Investigation of atomic displacements at a Sigma 3 {111} twin boundary in BaTiO3 by means of phase-retrieval electron microscopy. Phys Rev Lett 82(25):5052–5055 (Near-picometre-precision)
Jia CL, Thust A, Urban K (2005) Atomic-scale analysis of the oxygen configuration at a SrTiO3 dislocation core. Phys Rev Lett 95:article #225506 (Dislocation core)
Jia CL, Rosenfeld R, Thust A, Urban K (1999) Atomic structure of a Sigma=3, {111} twin-boundary junction in a BaTiO3 thin film. Phil Mag Lett 79(3):99 (Twin arrangement in barium titanate)
Jinschek JR, Yucelen E, Calderon H, Freitag B (2011) Quantitative atomic 3-D imaging of single/double sheet graphene structure. Carbon 49:556–562 (Graphene)
Kisielowski C, Hetherington CJD, Wang YC, Kilaas R, O’Keefe MA, Thust A (2001) Imaging columns of the light elements carbon, nitrogen and oxygen with sub Angstrom resolution. Ultramicroscopy 89:243–263 (Applications include e.g. the first reconstruction of light atoms)
Mahalingam K, Eyink KG, Brown GJ, Dorsey DL, Kisielowski CF, Thust A (2006) Quantifying stoichiometry of mixed-cation-anion III–V semiconductor interfaces at atomic resolution. Appl Phys Lett 88(9):article #091904 (Semiconductor heterostructures)
Mahalingam K, Eyink KG, Brown GJ, Dorsey DL, Kisielowski CF, Thust A (2008) Compositional analysis of mixed-cation-anion III–V semiconductor interfaces using phase retrieval high-resolution transmission electron microscopy. J Microscopy 230:372–381 (Semiconductor heterostructures)
Thust A, Rosenfeld R (1998) State of the art of focal-series reconstruction in HRTEM Proc ICEM 14, Cancun, Mexico. vol. 1., pp 119–120 (Use N images to reduce noise)
Tillmann A, Thust K, Urban K (2005) Spherical aberration correction in tandem with exit-plane wave function reconstruction: interlocking tools for the atomic scale imaging of lattice defects in GaAs. Microsc Microanal 10(2):185–198 (A structural analysis of the stacking fault in GaAs)
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Appendix
Appendix
9.1.1 People
The development of the FSR method in electron microscopy began roughly in the 1970s. Over time, generations of scientists contributed to the evolvement of various mathematical variants, numerical implementations, and actual applications of FSR. For this reason, developing an only rudimentarily fair genealogical table of important contributors would simply require too much space. Instead, we name here only one person, who was frequently ignored in the scientific literature and who is barely known: Peter Schiske. He is the guy who invented the FSR principle! Peter Schiske (1924–2012) was an Austrian physicist, mathematician and early computer expert. In the early 1950s he collaborated with the well-known Austrian physicist and electron optician Walter Glaser, who was a strong proponent of the wave optical view of image formation based on the Schrödinger equation. Not surprisingly, we also made strong use of the wave optical view throughout this chapter. It was finally Peter Schiske who published in 1968 for the first time the idea of focal-series reconstruction in electron microscopy. The original paper was a short conference abstract written in German. Fortunately, due to its fundamental importance, Schiske’s original paper has meanwhile been translated to English and re-printed (see References).
9.1.2 Self-Assessment Questions
- Q9.1:
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Why is it favorable to have the object wavefunction available compared to a single HRTEM image?
- Q9.2:
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Are you aware of a TEM technique, where the object wavefunction can be obtained without requiring a multitude of images?
- Q9.3:
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State at least two reasons why it is advisable to perform HRTEM experiments in thin-object regions. How many nanometers are roughly considered as ‘thin’?
- Q9.4:
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How is the thickness dependence of a wavefunction related to the atomic charge number?
- Q9.5:
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What kind of artifacts are introduced even by a ‘neutral’ microscope, which just produces a magnified image of the object wavefunction?
- Q9.6:
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What would you expect to see in images of a thin object made with a ‘neutral’ microscope?
- Q9.7:
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If a constant-phase-shift microscope was available (Zernike phase plate), how many images would be required to restore the object wavefunction?
- Q9.8:
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How do the projection surfaces in the 3D (Re, Im, g) space of a constant-phase-shift microscope differ from those of a real microscope?
- Q9.9:
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How are the projection surfaces in the 3D (Re, Im, g) space related to the well-known contrast transfer function (CTF)?
- Q9.10:
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How large roughly is the minimum contrast delocalization obtainable with a non-corrected field emission microscope? What minimum contrast delocalization can be obtained with a C S -corrected version?
- Q9.11:
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By which feature of the projection surfaces in the 3D (Re, Im, g) space can one observe the function ∇χ(g)?
- Q9.12:
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Is there an analytical solution to the linear reconstruction problem? Is there an analytical solution to the nonlinear reconstruction problem?
- Q9.13:
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At which defocus value should one approximately place the midpoint of a focal series?
- Q9.14:
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Is there a substantial difference in the defocus value Z opt between an uncorrected microscope and a C S-corrected microscope? State typical values.
- Q9.15:
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Does the choice of the classical Scherzer defocus instead of Z opt make any sense for FSR with an uncorrected field emission microscope?
- Q9.16:
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Which single parameter apart from the wavelength determines the lowest reconstructible frequency g min?
- Q9.17:
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Which single parameter apart from the wavelength determines the resonance frequency g res in the high-frequency regime?
- Q9.18:
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Which single parameter apart from the wavelength determines the optimum focal step size δ opt?
- Q9.19:
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Would it be efficient from a mathematical point of view to decrease the lowest reconstructible frequency g min by increasing the number of recorded images? Additionally, what physical effect related to the object hampers such an attempt?
- Q9.20:
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Is it a good idea to try a reconstruction using only a small number of images (e.g., less than five)? What exactly is sacrificed when reducing the number of images?
- Q9.21:
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Is there an advantage of recording an equidistant focal series over recording an irregularly spaced series?
- Q9.22:
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State three reasons why the application of FSR can yield an advantage over taking just one C S-corrected image at the optimum defocus?
- Q9.23:
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Would it be a good idea to apply FSR to amorphous materials or to nanoparticles lying loosely on a support film?
- Q9.24:
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Who is the third Austrian named in the “People” section at the end of the chapter? Which view in physics/optics do they share?
9.1.3 Text-Specific Questions
- T9.1:
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Derive the fundamental Eq. 9.12, which is one possible definition of the Scherzer defocus Z S , by requiring that χ(g *, Z S) = −2 π/3, where g * is the position of the local minimum of χ.
- T9.2:
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The local minimum of the aberration function g * can be easily recognized as a dip in the plateau of the Scherzer CTF displayed in Fig. 9.6d. What property of the respective helical surface of Fig. 9.8a, d changes at the specific frequency g *?
- T9.3:
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Derive the fundamental Eq. 9.16, which defines the optimum defocus Z opt, by setting ∇χ(g int, Z opt) = −∇χ(g max, Z opt), and by solving the resulting third-order equation. Take care with the signs! It might be helpful to use |Z| in combination with compensating signs.
- T9.4:
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Derive the optimum value of the spherical aberration C S and the thereby resulting minimal achievable radius R min of the point-spread function for a C S-corrected microscope by demanding that Z S of Eq. 9.12 equals Z opt of Eq. 9.16.
- T9.5:
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What is the purpose of the first and the second terms in the enumerator of the linear filter function of Eq. 9.30?
- T9.6:
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What important property is reflected by the denominator of the linear filter function of Eq. 9.30?
- T9.7:
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Explain why the titanium atom columns produce stronger phase peaks in the image of Fig. 9.15 (right-hand side) than the barium atom columns, although titanium is the lighter and therefore also the weaker scattering element.
- T9.8:
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In the reconstructed phase of Fig. 9.16 it can be observed that the two polygonal structure units stacked above each other are absolutely identical. However, in both input images of Fig. 9.14 one can observe clear differences between the upper and the lower units. How can one and the same image exhibit different contrast for identical object features?
- T9.9:
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When comparing the number of intensity maxima in the C S-corrected Scherzer image of Fig. 9.18c with the number phase maxima in Fig. 9.18d one finds that there are many more intensity maxima than phase maxima. Whereas the phase maxima are all located at Ga or As atomic column positions as is expected, some of the intensity maxima are located at empty crystal positions and are thus artifacts. Which mechanism can be responsible for the ‘ghost’ atoms in the C S-corrected Scherzer image?
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Thust, A. (2016). Focal-Series Reconstruction. In: Carter, C., Williams, D. (eds) Transmission Electron Microscopy. Springer, Cham. https://doi.org/10.1007/978-3-319-26651-0_9
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