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Dr Acha Hessler-Wyser
Bat. MXC 134, Station 12, EPFL+41.21.693.48.30.
Acha Hessler-Wyser
Outline
a. b. c. d. e. TEM principle A little about diffraction TEM contrasts Examples Structure analysis
Acha Hessler-Wyser
Acha Hessler-Wyser
Canon
Acha Hessler-Wyser
a. TEM principle
Acha Hessler-Wyser
a. TEM principle
Lenses, general principle of optical geometry
First approximation: thin lens
plan focal image plan focal objet
Fi Fi fi
F
o
Fo
fo
In particular, an image of the source placed at the object focal point F0 of the condensor 2 will give a parallel illumination onto the sample
Acha Hessler-Wyser
a. TEM principle
Parallel or converging illumination
Auger electrons
1-100 nm
absorbed electrons
Specimen
electron-hole pairs
direct beam
Acha Hessler-Wyser
Auger electrons
1-100 nm
Acha Hessler-Wyser
"=
QT
N 0# T $
The interaction cross section represents the chance of a particular electron to have any kind of interaction with an atom. ! The total scattering cross section is the sum of all elastic and inelastic scattering cross sections:
If a specimen contains N atoms/vol, it has then a thickness t, the probability of scattering from the specimen is given by QTt:
N" # QT = N" T = 0 T A
QT t =
N 0" T ( #t) A
with QT the total cross section for scattering from the specimen in units of cm-1, N0 the Avogadro's number (atoms/mole), A the atomic weight (g/mole) and ! the atomic density ! !
Intensive SEM/TEM training: TEM 10
Acha Hessler-Wyser
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Acha Hessler-Wyser
f(#) is a measure of the amplitude of an electron wave scattered from an isolated atom. ! $f(#)$2 is proportional to the scattered intensity. f(#) can be calculated from Schrdinger's equations, and we obtain the following description:
! E $ #1+ 0 2 & ! " m0 c % # ! f (! ) = # 8! 2 a0 # sin " " 2 $ & & ( Z ' fX ) & %
2
(sin#)/%& 0.1
1H 63Cu
118'000 29'900
Atomic scattering factors for neutrons (independent of #!), electrons and X rays, are a function of scattering angle and wave length % [].
fn : f fX = 1 : 104 : 10 Tir de L.H. Schwartz and J.B. Cohen, Diffraction from Materials
Intensive SEM/TEM training: TEM 14
Acha Hessler-Wyser
Amaille = 1 / r exp[2#ir]
with ri th position of an atom i: and K = g: K = h a* + k b* + l c*
i = atomes maille
! f ($ ) exp[2#iK " r ]
i i
ri = xi a + yi b + zi c
The structure factor is given by the sum of all scattering centres (the atoms) of the crystal that can scatter the incident wave:
Fhkl =
i = atomes maille
! f exp[2"i(hx + ky + lz )]
i i i i
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Acha Hessler-Wyser
Each point of the object re-emits a spherical wavelet. When all combined together, they are doing the resulting wave (transmitted, scattered or backscattered) If wavelets are coherent (phase relation well defined), resulting wave is the sum of the wavelets (interference) and the observed intensity Ic is the squared resulting wave modulus (usually called "diffraction").
objet
% ( ( *
If wavelet phases are not correlated (uncoherent), they cannot interfere and the observed intensity Iinc is the sum of the intensity of each wavelet (usually called "diffusion").
$ ' e2 !ik"r +ai ' e#2 !ik"r +ai Iinc (r ) = + &i&i * = + ' A i (r ) A i (r ) ' r r i i )
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% 2 ( = + Ii (r ) ( i *
transmis
s diffu
Acha Hessler-Wyser
n Fres
me<<matom<<msample
!The energy transfer (loss) from the electron to the sample is usually negligible. !If electrons go through a thick sample: "Multiple interaction occur: dynamical effects "Diffraction patterns complex to interpret
Intensive SEM/TEM training: TEM 17
Acha Hessler-Wyser
Fresnel fringes can also be used to correct the astigmatism in the objective lens.
b) Irregular fringes, astigmatism. c) Underfocussed, uniform fringes d) Focussed, min of contrast, no fringes e) Overfocussed, uniform fringes
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Acha Hessler-Wyser
"
!
distance
Elastic diffraction
|k| = |k|
k k g = k-k
Periodic arrangement of atoms in the real space: g : vector in the reciprocal space
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Acha Hessler-Wyser
c. TEM contrasts
Imaging mode
Echantillon
Lentille objectif
Plan focal
Plan image
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Acha Hessler-Wyser
c. TEM contrasts
Diffraction mode
Echantillon
Lentille objectif
Plan focal
Plan image
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Acha Hessler-Wyser
c. TEM contrasts
Diffraction mode
Direct correlation between the back focal plane (first diffraction pattern formed in the microscope) of the objective lens and the screen
Imaging mode
Direct correlation between the image plane (first image formed in the microscope) of the objective lens and the screen
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Acha Hessler-Wyser
c. TEM contrasts
Diffraction: Zone axis
Several (hi ki li) planes intersect with a common direction [u v w] (zone axis) of the crystal. If electron beam is along [u v w ] direction, they all will be in Bragg condition. They satisfy the zone equation: hu+kv+lw=0 Each family of crystalline plane generates diffract in a single direction. This corresponds to a single spot the the focal plane.
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Acha Hessler-Wyser
c. TEM contrasts
Diffraction patterns for fcc
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Acha Hessler-Wyser
c. TEM contrasts
Different type of contrasts
Thickness contrast Z contrast HAADF (D)STEM
Obj. ap.! SA ap.!
Diffraction contrast => BF and DF Phase contrast The objective aperture allows to select a transmitted spot to increase the contrast in image mode The selected area aperture allows to select a region from which the diffraction pattern is considered
Intensive SEM/TEM training: TEM 27
Acha Hessler-Wyser
c. TEM contrasts
Bright field (BF), dark field (DF)
Bright fied (BF) : the image is formed with the transmitted beam only (0! Dark field (DF): the image is formed with one selected diffracted beam (hkl It gives information on regions from the sample that diffract in that particular direction. Note the particular case ot the DF mode: the incident beam is tilted.
Intensive SEM/TEM training: TEM 28
Acha Hessler-Wyser
c. TEM contrasts
Bright field (BF), dark field (DF)
100 nm
Bright field
Dark field
P.-A. Buffat!
Intensive SEM/TEM training: TEM 29
Acha Hessler-Wyser
c. TEM contrasts
Bright field (BF), dark field (DF)
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Acha Hessler-Wyser
c. TEM contrasts
Bright field (BF), dark field (DF)
Segregation of chemical species in OMCVD AlGaAs structures on patterned substrates
1.1 A B
1
III
c(Ga)normalized
0.9
0.8
0.7
0.6
I/1
II/1
II/2
0.5 0
I/2
50
100
150
200
250
300
distance/nm
Because of the Z dependence of the structure factor, we can observe a chemical contrast in dark field mode!
Intensive SEM/TEM training: TEM 31
Acha Hessler-Wyser
c. TEM contrasts
Thickness fringes
If we admit at this stage that a transmitted beam and a diffracted beam can interact in the material, we can calculate the intensity of each one. It varies periodically with the thickness t, resulting in equal thickness fringes.
Champ clair
Intensive SEM/TEM training: TEM
Champ sombre
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Acha Hessler-Wyser
c. TEM contrasts
Exctinction distance
This intensity depends on the extinction distance: #Ve cos$ B
"g = %Fg
)g [nm]
(111) (200) (220) Al 72 87 143 Ag 29 33 46 Au 23 25 35
and thus on the crystal orientation and the atomic number of the sample atoms. !
We usually admit that kinematic (400) 237 75 55 theory is valid as long as the diffracted beam intensity/incident beam intensity is lower than 10%. Thus, the thickness limit is )g calculated for $g $g
t < t max " #
"
10
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metals at 300 kV
Acha Hessler-Wyser
c. TEM contrasts
Thickness fringes and chemical contrast
Fast assessment of thicknesses of complex multilayer structures by TEM, in collaboration with Dr. E. Gini, IQE-ETHZ, Prof. K.Melchior
TEM: contrastes
Thickness fringes and chemical contrast
Quanum wires InP/GaInAs. Cleaved wedge method The bending of the fringes indicates clearly the presence of a chemical concentration gradient close to the interfaces.
P.-A. Buffat
Intensive SEM/TEM training: TEM 35
Acha Hessler-Wyser
TEM: contrastes
Bended samples
When a sample is deformed, the diffraction conditions are not the same in two different regions. In bright field, the diffracting area appears in dark. It is then possible to observe lines with a different contrast: they are called bend contour.
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Acha Hessler-Wyser
TEM: contrastes
Bended samples
When a sample is deformed, the diffraction conditions are not the same in two different regions. In bright field, the diffracting area appear in dark. It is then possible to observe lines with a different contrast: they are called bend contour. Each line can be associated with a family of diffracting planes.
d. Structure analysis
Zone axis
Each diffraction spot corresponds to a well defined familly of atomic planes. On a diffraction pattern, the distances between the diffracted spots depend on the lattice parameter, but their ratio is constant for each Bravais lattice. Quick structure identification, manual or computer assisted.
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d. Structure analysis
Diffraction pattern indexing
Simulation: Software JEMS (P. Stadelmann) If we propose possible crystal, it calulates its electron diffraction for all orientations and compares with experimental diffraction pattern.
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Acha Hessler-Wyser
d. Structure analysis
Camera length
Diffraction spots are supposed to converge at infinity. The projective lenses allow us to get this focal plane into our microscope: The magnification of the diffraction pattern is represented by the camera length CL.
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Acha Hessler-Wyser
d. Structure analysis
Camera length
Diffraction spots are supposed to converge at infinity. The projective lenses allow us to get this focal plane into our microscope: The magnification of the diffraction pattern is represented by the camera length CL. tg(2#hkl) = R/CL For small angles, # ! sin# ! tg# and with the Bragg's law 2dhklsin#hkl=n% we have: dhklR= %CL (=cte)
Intensive SEM/TEM training: TEM 41
Acha Hessler-Wyser
dhkl
2#hkl CL
d. Structure analysis
Phase identification
The detailed analysis of the diffrated spots gives us the crystalline structure of the sample. If the microscope is perfectly calibrated, it is then possible to get the crystal interplanar distance, and thus its lattice parameter. However, usually, we have possible strucures and diffraction allows us to choose between the candidates.
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Acha Hessler-Wyser
d. Structure analysis
Phase identification
0-13 1-2-2
[831]
Hexagonal %-(AlFeSi)
40-3
0-20
FIB lamella of ! 50 nm thickness, GJS600 treated Bright Field micrograph, 2750x (Philips CM20) Simulated diffraction on JEMS software
Intensive SEM/TEM training: TEM
[304]
Monoclinic Al3Fe
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d. Structure analysis
Powder diagram
Polycrystaline TiCl All reflexions (i.e. all atomic planes with structure facteur) are present They are also called "ring pattern" Angular relations between the atomic planes are lost.
222 311 220 200 111
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c. TEM contrasts
High resolution contrast (HRTEM)
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Acha Hessler-Wyser
c. TEM contrasts
Scanning transmission (STEM)
High angle thermal diffuse scattering ~z2 = z-contrast incoherent imaging: no interference effects dedicated STEM: beam size ~0.1-0.2nm Limitation: beam formation by magnetic lens: Cs !!!
HRTEM
Acha Hessler-Wyser
HAADF-STEM
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Acha Hessler-Wyser