Techniques EDX, EELS et HAADF en TEM: possibilités d analyse et applications

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1 Techniques EDX, EELS et HAADF en TEM: possibilités d analyse et applications Thomas Neisius Université Paul Cézanne

2 Plan Imaging modes HAADF Example: supported Pt nanoparticles Electron sample interaction EELS Example: AlN/Si interface EFTEM Example: embedded Al nanoparticles EDX in S/TEM Préparé par: T. Neisius 30 novembre

3 Imaging modes Scanning Transmission Electron Microscope STEM k 0 k -g k g Specimen Objective lens Back focal plane Objective aperture Detector plane

4 Imaging modes Scanning Transimission Electron Microscope STEM High Angle Annular Dark Field At large collection angles the signal is mainly due to incoherent scattering. Z- contrast Illumination aperture Objective lens pre-field Si (110) Specimen Detector plane BF ADF HAADF

5 HAADF Example: NOx conversion catalyst Pt particles supported by LaCo 1-y Fe y O 3 - Perovskite C. Lancelot UCCS Lille TEM 300kV Exposure time: 0.5 s low particle contrast beam damage Difficult to identify the Pt-particles

6 HAADF Example: NOx conversion catalyst Pt particles supported by LaCo 1-y Fe y O 3 - Perovskite C. Lancelot UCCS Lille STEM HAADF 300kV Exposure time: 60 s chemical contrast reduced beam damage during scan Easy to identify the Pt-particles

7 HAADF Example: NOx conversion catalyst Pt particles supported by LaCo 1-y Fe y O 3 - Perovskite C. Lancelot UCCS Lille

8 Electron Sample Interaction incoming electrons E in thin specimen

9 Electron Sample Interaction Elastic Interaction No energy transfer incoming electrons E in thin specimen: mostly elastic Scattering events elastically scattered electrons E out = E in Ideal for imaging: high coherence between the scattered electrons

10 Inelastic Interaction Energy transfer from electron to the sample Electron Sample Interaction incoming electrons thin specimen E in elastically scattered electrons E out < E in

11 Inelastic Interaction Energy transfer from electron to the sample Electron Sample Interaction incoming electrons thin specimen E in

12 Inelastic Interaction Energy transfer from electron to the sample Electron Sample Interaction incoming electrons Collective Excitations E in Phonon: E ~ 0.01eV Plasmon: E ~ 10eV

13 Inelastic Interaction Energy transfer from electron to the sample Electron Sample Interaction Core level Excitation E ~ 50eV 10keV

14 Inelastic Interaction Energy transfer from electron to the sample Electron Sample Interaction «Knock-on» effect E ~ E in C Si Cu Au E 0 [kev]

15 Spectroscopy: how to exploit the inelastic electron sample interaction measuring the electron energy behind the sample ( EELS ) measuring the energy release during the sample relaxation ( EDX, Auger )

16

17 «Primary» Spectroscopy: Electron Energy Loss Spectroscopy EELS: Intensity of a certain energy loss has be measured I( E) is detemined by electronic structure

18 EELS Scheme from Botton 2007

19 EELS Spectrum from Sauer

20 Making the sample as thin as possible is the most important part of EELS

21 Making the sample as thin as possible is the most important part of EELS

22 Instrumentation GIF

23 AlN/ structure and chemistry of the interface G. Radtke IM2NP AlN buffer grown by 735 C (Cambridge University) AlN <11-20> Si <110>

24 AlN buffer grown by 1040 C (Cambridge University) AlN <11-20> Si <110>

25 EFTEM- Al nanoparticles embedded in Al 2 O 3 M. Cheynet SIMAP Grenoble

26 EFTEM- Al nanoparticles embedded in Al 2 O 3 M. Cheynet SIMAP Grenoble

27 EFTEM- Al nanoparticles embedded in Al 2 O 3 M. Cheynet SIMAP Grenoble

28 «Secondary» Spectroscopy: X-ray fluorescence ( EDS, WDS ) For a certain moment system stays in an excited state (electron hole pair).

29 «Secondary» Spectroscopy: X-ray fluorescence ( EDS, WDS ) hν Relaxation of the sample via emission of a characteristic photon

30 EDX in SEM versus TEM from Fulz et al Beam broadening (empirical): b ~ ZE -1 t 3/2 broadening of the beam less important loss of signal easier to correct

31 Typical geometry for EDX in TEM Only 1% of the signal detected Sample damage Drift problems Ω = 0.13sr from Otten 1998 The way to the optimal EDX in TEM Best lateral resolution at shortest acquisition times Thin sample Maximum solid angle Brighter electron source

32 Newest geometry for EDX in TEM FEI ChemiSTEM probe corrected high brilliance optics 4 symmetrical arranged SDD detectors Ω = 0.9sr Fe Au Pt Acquisition time < 4min

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