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SAED Patterns of Single Crystal, Polycrystalline and Amorphous Samples

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1 SAED Patterns of Single Crystal, Polycrystalline and Amorphous Samples
b c 020 110 200 r1 r2

2 Electron Diffraction Geometry for e-diffraction e- Bragg’s Law: l = 2dsin l=0.037Å (at 100kV) =0.26o if d=4Å dhkl Specimen foil l = 2d L 2 r/L=sin2 as   0 r/L = 2 r/L = l/d or r = lLx r T D Reciprocal lattice Due to short wavelength, diffraction angle in TEM is very small. Diffraction angle in diagram is exaggerated. Value of dhkl can be obtained by measuring rhkl. 1 d L -camera length r -distance between T and D spots 1/d -reciprocal of interplanar distance(Å-1) SAED –selected area electron diffraction hkl [hkl] SAED pattern

3 Ewald’s Sphere Ewald’s sphere is built for interpreting diffraction
lkl=1/ Ewald circle C incident beam diffracted beam 2 kd H ki g G 130 - Compare XRD (long wavelength) with SAED (short wavelength) To build the Ewald sphere 1. k has a magnitude of 1/ and points in the direction of the electron wave, 2. Construct a circle with radius 1/, i.e., lkl, which passes through 0, 3. The Ewald circle intersects the lattice point at G. CG-C0=0G or kd-ki=g Laue equation Wherever a reciprocal lattice point touches the circle, e.g., at G, Bragg's Law is obeyed and a diffracted beam will occur. At H, no diffraction.

4 Convergent Beam Electron Diffraction (CBED)
CBED uses a conver- gent beam of elec- trons to limit area of specimen which con- tributes to diffraction pattern. Each spot in SAED then becomes a disc within which variations in intensity can be seen. CBED patterns contain a wealth of information about symmetry and thickness of specimen. Big advantage of CBED is that the information is generated from small regions beyond reach of other techniques.

5 SAED vs CBED SAED CBED Parallel beam Convergent beam sample objective
Spatial resolution >0.5m Spatial resolution beam size Convergence angle sample objective lens spots disks T D T D SAED CBED

6 CBED-example 1

7 CBED-example 2 HOLZ HOLZ - High Order Laue Zone

8 Applications of CBED Phase identification
Symmetry determination-point and space group Phase fingerprinting Thickness measurement Strain and lattice parameter measurement Structure factor determination

9 Symmetry Deviations

10 Phase Identification in BaAl2Si2O8
Hexagonal Orthorhombic Hexagonal 6mm 6mm 2mm 800oC 200oC 400oC <0001>

11 Phase Fingerprinting By CBED
Orthorhombic AFE Cubic PE [001] CBED patterns of an antiferroelectric PbZrO3 single crystal specimen at (a) 20oC, (b) 280oC, (c)220oC. (d) [001] CBED pattern of a rhombohedral ferroelectric Pb(ZrTi)O3 Specimen at 20oC. Rhombohedral FE Rhombohedral FE

12 Symmetry and Lattice Parameter Determination
EDS CBED A BF A B 010 Nb A B 001 B [100] SAED 0.2m A B A [111] EDS can identify difference in chemical composition between the core and shell regions. Using CBED HOLZ line pattern accuracy of lattice parameter measurement is ~0.1%. [143] CBED-HOLZ B Lattice parameters Experimental simulated


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