Electron microscopy II
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1 Electron microscopy II Nanomaterials characterization I RNDr. Věra Vodičková, PhD.
2 Interaction ction: electrons solid matter Signal types SE.secondary e - AE Auger s e - BSE back scattered e - X-ray photons, and others TE transmitted e - DE diffracted e - Scanning electron microscopy (SEM) Transmission electron microscopy (TEM) Interactive area 2
3 Transmission electron microscopy- information provided by transmitted e- (TE, DE) TEM makes possible studying of the internal material structure (dislocations, stacking faults) specimens must be transparent thickness cca nm foils or replicas special preparation TEM better resolution than REM (usually) 3
4 Transmission microskope scheme, constructive elements Construction is similar to SEM (only specimen location is different) Source of e - cathode (heated or autoemitting) Imaging system electromagnetic lenses (condenser and projector lenses) Image is visible on fluorescent screen 4
5 Image generation and interpretation EM difractograph TEM Pattern rises in back focal plane Pattern rises in image plane Either diffraction pattern or specimen image is projected on screen SAD selected area diffraction diffraction from selected part of specimen (realization selected area aperture) Accuracy of SAD decreases with diffraction angle 5
6 Image generation and interpretation Specimen image Diffraction pattern 6
7 Image formation and interpretation CAMERA CONSTANT K describes the magnification of diffraction pattern For small diffraction angles (2θ 2 sinθ tg 2θ) is R = Ltg2θ = L2θ (R - distance between primary and diffracted beam) From Brag s law: K = Rdhkl = λl 7
8 Image formation and interpretation Basic ways of imaging delimitation of beams that create image on screen delimitation of straight beam only bright field image (BF) delimitation of one of diffracted beams only dark field image (DF) deflection of primary e - beam (one of those diffracted beams must pass through the optical axis of the microscope) centered dark field (CDF) TEM Contrast : Mass-thickness contrast in image mode, due to differences in intensity of scattering diffraction contrast in diffraction mode 8
9 Scattering contrast formation Aproximation of exponential absorption law Total intensity of transmitted beam σ s t σ a σ 0ρ I = I e 0 s Ar Condition for thickness of TEM specimen 0,5 σ t s so: contrast is given as partial variation of scattered e - density, defined by parameters σ s and t 1 = N 9
10 Electron diffraction Diffraction pattern concentric circles polycrystalic specimen point patterns (dot diagram) thin monocrystals Kikuchi lines more massive monocrystals 10
11 Diffraction on polycrystals - circular TEM diffractograms dot density is proportional to - number of grains in unit volume - size of selected area aperture circles indexing: sequence of diameters must be corresponding to sequence of specimen d hkl Diffraction on monocrystals - dot TEM diffractograms pattern image of reciprocal lattice plane k every spot (dot) represents one system of lattice planes Indexing assign of Miller indices hkl to every spot according to distance from central spot (by means of camera constant, Burgers vectors and angles) simplification of indexing via Kikuchi lines 11
12 Kikuchi lines parallel bright and dark lines change of position at specimen tilt formation is connected with nonelastic scattering of e - system of Kikuchi line defines of specimen crystalography lines from crystal planes split of distance between corresponding lines maps of Kikuchi lines fast orientation in specimen crystalography 12
13 Extraordinary diffraction spots finer structure of diffraction pattern broadening, elongation of spots, satellite or extraordinary spots Formation factors: shape of particles deformation and faults Examples: Double diffraction extraordinary spots Long range ordering forbidden reflections Planar defects splitting of spots Thermal oscillation Point defects Satellite spots Bending (from periodic and modulated structure) Spinodal decomposition 13
14 Methods of electron diffraction Selected area diffraction (SAD) metals, minerals (d<2,5-4 nm). Selected area aperture using maximalization of image, better delimitation of diffraction area Diffra raction with high resolution specimen location under projector imaging aberration suppression, higher resolution Small-angle angle dif Reflective diffra Diffra raction with too much diffraction thickness d=2 200 nm raction surface layers (oxides) with scanning specimens that heat up 14
15 TEM specimen preparation Foils for internal structure study, thin transparent specimens - thinning of material: polishing - final thinning: electrolytic polishing or ion bombardment Replicas prints of surface for study of surface details - material of replicas must copy the surface perfectly (carbon or polymers ) - by proceeding produce of replicas: one-step, two-step or extraction replicas 15
16 TEM foils preparation 16
17 TEM foils preparation Electolytic jet polisher 17
18 Examples of foils using Study of dislocation structure Phase identification Study of grain boundaries 18
19 TEM replicas preparation FIB preparation Two-step replica 19
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