XII. Electron diffraction in TEM Newest TEM in MSE JEOL JEM-ARM200FTH Spherical-aberration Corrected Field Emission Transmission Electron Microscope Other TEM in MSE JEOL JEM-3000F JEOL JEM-2100 Simple sketch of the beam path of the electrons in a TEM Diffraction pattern: scattered in the same direction; containing information on the angular scattering distribution of the electrons Image plane (bottom) The diffraction pattern and the image are related through a Fourier transform. 12-1. Electron radiation (i) ~ hundreds Kev h p highly monochromatic than X-ray Typical TEM voltage: 100 – 400 KV Relativistic effect should be taken into account! SEM typically operated at a potential of 10 KV v ~ 20% c (speed of light) TEM operated at 200 kV v ~ 70% c. h E ( pc ) ( m 0 c ) 2 p E mc 2 2 KE m 0 c 2 2 ( KE m 0 c ) ( pc ) ( m 0 c ) 2 ( pc ) ( KE m 0 c ) ( m 0 c ) 2 2 2 2 2 2 KE pc 2 2 2 2 2 2 KEm 0 c m 0 c m 0 c 2 KE 2 KEm 0 c 2 2 4 2 2 Massless particle: p KE / c p 2 m 0 KE KE c 2 2 2 m 0 KE 1 KE 2m 0c 2 4 h p h 2 m 0 KE 1 KE 2m 0c 2 KE e voltage h = 6.62606957×10-34 m2kg/s m0 = 9.1093829110-31 Kg c = 299792458 m/s e = 1.60217657×10-19 coulombs 1eV = 1.60217656510-19 J (Kgm2/s2) For 200 KV electrons 14 KE 200 keV 3 . 204 10 1 KE 2 m 0c h 2 3 . 204 10 1 1 0 . 1956 1 . 0934 2 9 . 109 10 6 . 626 10 2 m 0 KE J(Kg m /s ) 2 31 34 31 2 14 ( 2 . 998 10 ) 8 2 2 m Kg/s 14 2 9 . 109 10 Kg 3 . 204 10 Kg m / s 34 2 6 . 626 10 m Kg/s 12 2 . 74 10 m 22 2 . 416 10 mKg/s h 2 m 0 KE 1 1 2 . 506 10 KE 2 m 0c 2 12 2 m 2 For 20 KV electrons KE 20 keV 3 . 20436 10 2 m 0c (eV ) 2 1 KE 2 m 0c h 2m0 2 2 9 . 109 10 31 15 J(Kg m /s ) 2 ( 2 . 998 10 ) 8 2 19 1 . 602 10 20000 1 6 1 . 022 10 6 . 626 10 2 9 . 109 10 1 . 22 10 1 . 22 10 KE 31 34 2 1 . 022 10 1 0 . 01957 1 . 00973 2 m Kg/s Kg 1 . 60217 10 19 9 9 1 . 22 10 20000 9 8 . 6 10 12 (m) J/eV 6 For X-ray h p E hc hc pc 6 . 626 10 E 34 2 8 2 10 15 19 1 . 2399 10 (m) 2 (m kg/s ) 1 . 288 10 E (eV) (m kg/s) 2 . 998 10 (m/s) 15 1 . 60217 10 hc E 1 . 542 10 1 . 288 10 E Wavelength = 1.542 Å (J) J 8 . 04 10 (eV) 3 (J/ e V) 6 (m) (eV/m) ~ 1240 (eV/nm) (nm) (ii) electrons can be focused c.f. x-ray is hard to focus (iii) easily scattered f e 10 f x 4 : form factor for electron and x-ray, respectively Form factor for electron includes nucleus scattering! f e and f x (iv) need thin crystals <1000Å, beam size m 12-2. Bragg angle is small 2 d hkl sin for 100 KeV 0 . 037 A Assume d = 2Å sin 0 . 0925 2 2 sin 0 . 037 0 . 0925 0 . 0925 180 0 . 53 o 0 . 025 A 180 o 0 . 0625 0 . 0625 0 . 34 for 200Kev 12-3. d spacing determination is not good 2 d hkl sin 2d sin (brevity) For fixed d cos d 2 2 sin 2 sin d cos d ( cot ) 2 sin sin d / d cot 90 ; cot 0 ; d 0 o we can get more accurate d at higher angle! o In TEM 0 . 5 Not good for d determination! 12-4. Electron diffraction pattern from a single crystalline material Example: epitaxial PtSi/p-Si(100) Ewald sphere construction: is very small k is very large compared to the lattice spacing in the reciprocal space (1) An electron beam is usually incident along the zone axis of the electron diffraction pattern. The sample can be tuned along another zone axis [xyz] . All the spots in the diffraction pattern belongs the zone axis [xyz]. 12-5. Electron diffraction pattern from a polycrystalline material Example: polycrystalline PtSi/p-Si(100) Ewald sphere constructions for powders and polycrystalline materials 12-6. diffraction and image (bright field, dark field) (a) Bright field image http://labs.mete.metu.ed u.tr/tem/TEMtext/TEMt ext.html (b) Dark filed image http://labs.mete.metu.edu.tr/tem/TEMtext/TEMtext.html Example: microcrystalline ZrO2 http://www.microscopy.ethz.ch/BFDF-TEM.htm Diffraction pattern Bright-Field Image Dark-Field Image BF image: some crystals appear with dark contrast since they are oriented (almost) parallel to a zone axis (Bragg contrast). DF image: some of the microcrystals appear with bright contrast, namely such whose diffracted beams partly pass the objective aperture.