04.11.13

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 1 CiMe

0. General introduction

Dr Aïcha Hessler-Wyser

Bat. MXC 134, Station 12, EPFL+41.21.693.48.30.

Centre Interdisciplinaire de Microscopie Electronique

CIME

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 2 CiMe

Outline

a.  History of microscopy b.  What can be done with a microscope? c.  General bibliography

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 3 CiMe

a. Little history

1665 2007

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 4 CiMe

a. Little history: optics

Optical microscopy Antiquity: first etch of convex lenses

XII-XIIIth centuries: magnification power of convex lenses, magnifier, glasses

1590 Janssen, first composed microscope

1609 Galilei: occhiolino

1665 Hooke: first cell image

1801 Young: wave nature of light

1872 (~) Abbe: the resolution limit is linked to wave length of the used beam

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 5 CiMe

a. Little history: electrons?

Electron microscopy 1923 De Broglie: concept of wavelength associated to

particles, confirmation by Young's experiment 1927 Busch: focalisation low for magnetic fields

Davisson, Germer, Thomson: electron diffraction 1931 Ruska, Knoll: first images by electron microscopy

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 6 CiMe

a. Little history: electrons?

Electron microscopy 1923 De Broglie: concept of wavelength associated to

particles, confirmation by Young's experiment 1927 Busch: focalisation low for magnetic fields

Davisson, Germer, Thomson: electron diffraction 1931 Ruska, Knoll: first images by electron microscopy

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 7 CiMe

a. Little history: electrons?

1936 Scherzer: main electromagnetic lens aberrations cannot be avoided

1938 Von Ardenne: first microprobe scanning electron microscope

1939 Siemens: first industrial electron microscopes

1948 Gabor: holography invention

1951 Castaing: first X-ray micro-analyser

1960 XX: first MV microscope, competition for resolution

1965 Crewe: first scanning transmission electron microscope

1982 Binnig et Rohrer: scanning tunnelling microscope

1986 Ruska, Binnig et Rohrer: Prix Nobel Physics

1990 Rose: proposes the Cs corrector principle

1995 Haider: first realisation of the Cs corrector

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 8 CiMe

a. Little history: resolution?

Resolution evolution with time and new technologies

0.0001

0.001

0.01

0.1

1

1800 1840 1880 1920 1960 2000 2040

Res

olut

ion

(An

g.-1)

Year

Electron Microscope

Light Microscope

Corrected EM

Ross

Amici

Abbe

Ruska

Marton

Dietrich(200keV)

Haider(200keV)

H. Rose, 1994 TEAM project, 2002

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 9 CiMe

a detector (eye, photographic plate,

video camera...

an illumination section (lenses, apertures...)

a magnification section (lenses, apertures...)

a sample (+ a "goniometer")

A "light" source

b. What can be done with an EM?

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 10 CiMe

b. What can be done with an EM?

And SEM techniques…

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 11 CiMe

b. What can be done with an EM?

Different signals Different detectors

= Different informations!

1. Interaction of electrons with matter

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 12 CiMe

b. What can be done with an EM?

Electron source

Lenses

Detectors

Pumping unit

2. Components of an electron microscope

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 13 CiMe

b. What can be done with an EM?

Topographical contrast

Z contrast

3. SEM basics

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 14 CiMe

b. What can be done with an EM?

Material deposition Ion imaging Nano-machining 3D reconstruction TEM sample preparation

4. FIB

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 15 CiMe

b. What can be done with an EM?

5. ESEM

Partial pressure Hydrated or charging samples

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 16 CiMe

b. What can be done with an EM?

Back-scattered + diffracted e-

Orientation map

6. EBSD

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 17 CiMe

b. What can be done with an EM?

7. Advanced SEM

Different detectors, different informations

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 18 CiMe

b. What can be done with an EM?

X-ray detection Chemical analysis Chemical mapping

8. EDS in SEM 15. EDS in TEM

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 19 CiMe

b. What can be done with an EM?

Conventional TEM BF, DF Basics of electron diffraction

9. TEM principles 13. Diffraction

contrast 14b. Bio TEM

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 20 CiMe

b. What can be done with an EM?

Electron diffraction

10. Basics of diffraction

11. Diffraction

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 21 CiMe

b. What can be done with an EM?

3mm m

ax.

2.4

mm

.

3mm.

12. Sample preparation

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 22 CiMe

b. What can be done with an EM?

Phase contrast Atomic column imaging High resolution

14a. HRTEM

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 23 CiMe

b. What can be done with an EM?

Inelastically scattered electrons Z contrast T contrast

16. STEM

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 24 CiMe

b. What can be done with an EM?

Energy lost by electrons Chemical information Electronic properties

17-18. EELS

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 25 CiMe

b. What can be done with an EM?

New technologies Aberration correction 3D tomography Cathodoluminescence

19. Next generation Bibliography

Cs corrector “On”; Cs = 0.05 mm

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 26 CiMe

b. What can be done with an EM?

Cs corrector “On”; Cs = 0.05 mm

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Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 27 CiMe

c. General bibliography

SEM J.I. Goldstein et al., Scanning Electron Microscopy and X-ray Microanalysis, Springer (2007), 3rd edition L. Reimer, Scanning Electron Microscopy, (Springer 1998), 2nd edition L. Reimer, Image Formation in Low-Voltage Scanning Electron Microscopy, Spie Press (1993)

J.I. Goldstein et al., Practical scanning electron microscopy, Plenum Press (1977) Lyman et al., Scanning electron microscopy, X-ray microanalysis, and analytical electron microscopy, Plenum Press (1990) D.E. Newbury, Advanced Scanning Electron Microscopy and X-ray Microanalysis, Plenum Press (1986) D.B Holt, D.C. Joy, SEM microcharacterization of semiconductors, Academic Press (1989) B.G. Yacobi, D.B. Holt, Cathodoluminescence microscopy of inorganic solids, Plenum Press (1990)

J. F. Bresse (ed.), Travaux pratiques de microscopie electronique à balayage et de microanalyse X, ANRT Paris (1994)

Intensive SEM/TEM training: Introduction Aïcha Hessler-Wyser 28 CiMe

c. General bibliography

TEM D.B. Williams and C.B. Carter, Transmission electron microscopy, Springer (2009)

J.W. Edington, Practical electron microscopy in material science, (1976)

Hirsch, Electron microscopy of thin crystals , (1977)

Multi-techniques R.W. Cahn et al., Materials Science and Technology, Characterization of Materials (vol. 1 and 2), VCH (1992)

S. Amelinckx et al., Handbook of Microscopy: Applications in Material Science, Solid State Physics and Chemistry (vol. 1 and 2), VCH (1997)

E. Fuchs, H. Oppolzer, H. Rehme, Particle Beam Microanalysis, VCH Verlag 1990)

J.P. Eberhart, Analyse structurale et chimique des matériaux, Dunod, (1989)

M. Amou éd., Microcaractérisation des Solides, Ecole CRAM (CRAM 1989, 541 p) D.K. Bowen, C.R. Hall, Microscopy of Materials, McMillan (1975)