CHEM-E5225 :Electron Microscopy Imaging I
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1 CHEM-E5225 :Electron Microscopy Imaging I Yanling Ge
2 Outline Amplitude Contrast Phase Contrast Images Thickness and Bending Effects
3 Amplitude Contrast Amplitude phase TEM STEM Incoherent elastic -> Mass-thickness contrast Coherent elastic -> Diffraction contrast
4 What is contrast? - Difference in intensity For eyes > 5-10%, 16 gray level
5 Amplitude Contrast BF and DF Images BF and DF interpretable amplitude contrast Objective Aperture: minimize lens aberrations, enhance diffraction contrast. Usage of it depends on what features of specimen cause scattering. For soft materials to form image without aperture will enhance mass-thickness contrast by losing diffraction contrast! First, view DP!
6 Mechanism of mass-thickness contrast Thicker or higher-z areas of the specimen will scatter more electrons off axis than thinner. Mass-thickness contrast arises from incoherent elastic (Rutherford scatter). The cross section for elastic scattering is a function of Z. Thickness increase, more elastic scattering because the mean free path remains fixed.
7 Mass-Thickness Contrast scattering (Rutherford scattering) of electrons, which is strong function of atomic number Z (hence the mass or the density r) and the thickness, t, of he specimen.) At low angles (< 5 ): mass-thickness contrast dominates but it also competes with Bragg-diffraction contrast; At high angles (>5 ): where Bragg scattering is usually negligible, the low-intensity scattered beams depends on atomic number (Z) only, - so called Z-contrast. Mass-thickness contrast is the critical contrast mechanism for biological materials. And it is usually taken without objective aperture to minimize diffraction contrast.
8 Mass-Thickness contrast TEM images (A) TEM BF image of latex particles on a carbon support film showing thickness contrast only. (B) Latex particles on a carbon film shadowed to reveal the shape of the particles through the addition of selective mass contrast (the edge of the shadow) to the image. (C) Reverse print of (B) exhibits a 3D appearance. TEM variables: objective aperture size and the kv Be careful when interpreting 2D images of 3D specimens.
9 Mass-Thickness Contrast STEM image In a STEM you have more flexibility than in a TEM because by varying L, you change the collection angle of your detector and create, in effect, a variable objective aperture. In summary, there are occasions when you might want to use STEM massthickness contrast images: The specimen is so thick that chromatic aberration limits the TEM resolution. The specimen is beam-sensitive. The specimen has inherently low contrast in TEM and you can t digitize your TEM image or negative. Your specimen is ideally suited for HRTEM by Z-contrast imaging. TEM BF STEM BF Image processed TEM BF
10 Mass-Thickness Contrast Specimens Showing Mass-Thickness Contrast Carbon Replica Thickness contrast Shadowed effect Thickness + Mass contrast Extraction replica Mass + Thickness contrast
11 Mass-Thickness Contrast Quantitative Mass-Thickness Contrast The probability that an electron scattered through greater than a given angle b. Higher-Z specimens scatter more, especially in higher β. Lowering E 0 increase scattering. Thicker specimen scattering more. Variable for control mass-thickness contrast: Z, t, β, E 0.
12 Z-Contrast high-resolution (atomic), mass-thickness, imaging technique Z-Contrast images are also termed as HAADF images. Bragg effects are avoided if the HAADF detector only gathers electrons scattered through an angle of > 50 mrad (~3 ). Imaging away from strong two-beam conditions and closer to zone-axis orientations is wise. The image resolution is determined by the probe size. STEM ADF detector collecting low angle elastically scattered electrons of single heavy atoms on low-z substrate. Inelastic scattering is removed by EELS, but diffraction contrast is preserved in the low angle EELS single.
13 TEM Diffraction Contrast - Coherent elastic scattering Good strong diffraction contrast in both BF and DF images need to be in two-beam condition, in which only one diffracted beam is strong. The direct beam is the other strong spot in the pattern. For crystalline bulk specimen, to study defects, BF and CDF must be done in two-beam condition, which is a time consuming and patient work! Two-beam condition: good contrast, simple interpretation. Deviation parameter: s must small and positive for best contrast from defects (The excess hkl Kikuchi line, just outside the hkl spot). Two-beam CDF, tilt weak h-k-l to center. Related DP to image, showing g vector in image.
14 Two-Beam Condition - CDF BF WBDF CDF
15 Tilt sample and beam guide by Kikuchi line
16 The incident beam must be coherent, i.e., the convergence angle must be very small. The specimen must be tilted to a tow-beam condition. Only the direct beam or the one strong diffracted beam must be collected by the objective aperture. In order to have same condition in STEM as in TEM: a T = a S β T = β S STEM Diffraction Contrast Or according principle of reciprocity: a S = β T a T = β S STEM images are rarely used to show diffraction-contrast images of crystal defects. This is solely the domain of TEM.
17 BF STEM BF STEM βs smaller BF TEM
18 Phase-Contrast Images
19 Introduction Phase contrast arise due to the difference in the phase of electron waves scattered through a thin specimen. A phase-contrast image requires the selection of more than one beam. In general, the more beams collected, the higher the resolution of the image. Phase-contrast is very sensitive to many factors: the appearance of the image varies with small changes in the thickness, orientation, or scattering factor of the specimen, and variations in the focus or astigmatism of the objective lens.
20 The Origin of Lattice Fringes Two beam condition, interference of direction beam and diffracted beam. The intensity of phase contrast is a sinusoidal oscillation normal to g, with a periodicity that depends on s and t. This simple analysis shows that the location of a fringe does not necessarily correspond to the location of a lattice plane.
21 Some Practical Aspects of Lattice Fringes s = 0, hkl // optic axis s 0; hkl edge on If s 0 If s is not zero, then the fringes will shift by an amount which depends on both the magnitude of s and the value of t, but the periodicity will not change noticeably. The fringe periodicity is the same as the spacing of the planes which give rise to g. This result holds wherever s = 0 no matter how 0 and g are located relative to the optic axis, even if the diffraction planes are not parallel to the optic axis. We expect this s dependence to affect the image when the foil bends slightly, as is often the case for thin specimens. We also expect to see thickness variations in many-beam images, since s may be non-zero for all of the beams; s may also vary from beam to beam.
22 The image real structure! In general, this array of spots bears no direct relationship to the position of atoms in the crystal. Fringes are not direct images of the structure, but just give you information on lattice spacing and orientation. There is cases that these images can only be interpreted using extensive computer simulation.
23 Moiré Patterns General Moiré Fringes Translational Moiré Fringes Rotational Moiré Fringes
24 Experimental Observations of Moiré Fringes Translational Moiré Patterns We know that the top of an inclined island is not in contact with the substrate yet it shows fringes; so this reminds us that moiré fringes do not tell us about the interface structure! Rotational Moiré Patterns
25 Dislocations and Moiré Fringes
26 Fresnel Contrast magnetic domain wall In any situation where the inner potential changes abruptly, we can produce Fresnel fringes if we image that region out of focus. Magnetic-Domain Walls
27 Fresnel Contrast from Voids or Gas Bubbles By orienting the region of interest so that s = 0; the cavity then reduces the thickness of material locally. By using Fresnel contrast Caution: Small particles can give similar contrast to small voids, the Fresnel contrast can easily be misinterpreted as a core-shell structure! In the Fresnel technique, the image shows contrast whenever the objective lens is not focused on the bottom surface of the specimen. A dark fringe at under focus and a bright fringe at over focus.
28 Fresnel Contrast from Lattice Defects When you use the Fresnel-fringe technique to study grain boundaries or analyze intergranular films, you must orient the boundary in the edge-on position so that you can probe the potential at the boundary. Using the Fresnel-fringe technique to image end-on low angle grain boundaries assume there is a change in the mean inner potential at the core of the dislocation.
29 Thickness and Bending Effects
30 Thickness and Bending effects - Diffraction contrast All TEM specimens are thin but their thickness invariably changes. Because the specimens are so thin they also bend elastically, i.e., the lattice planes physically rotate. The planes also bend when lattice defects are introduced.
31 The Origin of Thickness Fringes and Bend Contours two beam condition s eff effective excitation error x g extinction distance The diffracted intensity is periodic in the two independent quantities, t and s eff. If we imaging the situation where t remains constant but s (and hence s eff ) varies locally, then we produce bend contours. Similarly, if s remains constant while t varies, then thickness fringes will result.
32 Thickness Fringes Intensity of both the 0 and g beams oscillate as t varies. Furthermore, these oscillations are complementary for the DF and BF images. As a rule of thumb, when other diffracted beams are present the effective extinction distance is reduced. At greater thicknesses, absorption occurs and the contrast is reduced.
33 Thickness Fringes and DP A general rule in TEM is that, whenever we see a periodicity in real space (i.e., in the image), there must be a corresponding array of spots in reciprocal space; the converse is also true.
34 Bend Contours (Annoying Artifact, Useful Tool, Invaluable Insight)
35 ZAPs and Real-Space Crystallography Although the ZAP is distorted, the symmetry of the zone axis is clear and such patterns have been used as a tool for real-space crystallographic analysis. Each contour is uniquely related to a particular set of diffraction panes, so the ZAP does not automatically introduce the twofold rotation axis that we are used to in SAD patterns. Also in this case, a small g in the DP gives a small spacing in the image, contrary to the usual inverse relationship between image and DP.
36 Summary: We can define a parameter x g which is usually about 10 x g and is really a fudge factor which modifies the Howie-Whelan equations to fit the experimental observations. The different Bloch waves are scattered differently. If they don t contribute to the image, we say that they were absorbed. We thus have anomalous absorption which quite normal! Usable thicknesses are limited to about 5x g, but you can optimize this if you channel the less-absorbed Bloch wave. Absorption Effects
37 homework Question based home work: T23.2; T23.11; T23.16
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