microscopy: Fresnel fringes in the TEMregpot/winterschool2009/... · •best “reading”of the...
Transcript of microscopy: Fresnel fringes in the TEMregpot/winterschool2009/... · •best “reading”of the...
Phase microscopy: Fresnel fringes in the TEM
Interferences between waves not being in phase
overfocussed
Interferences between waves not being in phase
2 waves propagating through different media (sample, vacuum)
=> difference of mean inner potentialsp
=> difference of optical paths
=> phase differences
Transformed into intensity contrast by the objective lens j
underfocussed in focus
Phase TEM relies on coherency of incident beam (energy spread, point source) => FEG
underfocussed in focus
Phase microscopy: High Resolution Electron Microscopy
Multi‐beam mode image: transmitted + several diffracted beams interfereseveral diffracted beams interfere => contrast = f (phase relationships of these beams)
i “ ” h lliFT
‐ image “represents” the crystalline structure of the specimen => structural characterization at the atomic scale
FT‐1
‐ phase differences result from:(i) interactions between the e‐beam and the electrostatic potential in the object ( i di l f t l)FT 1 (periodical for a crystal)(ii) phase shift induced by the objective lens (transfer function)
specimen thin enough => beam amplitude variations can be neglected (“phase object”)=> phase shift proportional to the electrostatic potential at every point of the exit surface
High Resolution Electron Microscopy: WPO approx
• Transmission function of the sample:if small phase shift, Weak Phase Object (WPO) approximationq(x,y)= 1-iσΦ(x,y) Projected potentialq(x,y) 1 iσΦ(x,y)
• Image directly related to the projected potential of the object (atoms) after modification by the objective lens (filter)
Projected potential
y j ( )I(x,y)= |ψi(x,y)| 2 = |q (x, y)*t(x,y) |2
= 1+2σΦ(x,y) *s(x,y)
s(x,y)=TF{O (u, v)sin(χ(u, v)} is the imaginary part of t(x,y)
Projected potential (object)
Im. of t(x,y)(objective lens)
( ,y) F{ ( , ) (χ( , )} g y p ( ,y)
• best “reading” of the projected potential when‐largest possible frequency bandwith‐objective lens is underfocussed by Δf=-1.2(Csλ)1/2 (Scherzer condition)
High Resolution Electron Microscopy
• In all practical cases, WPO approximation is not valid=> comparison HREM images/numerical simulation of the images for ≠ Df is necessary to access to the real structure of the sample (ex: where are the atomic columns?)
• However, although non linear, information regarding the atomic structure can be directly obtained in some cases: stacking sequences, extra plane, orientation relationship presence of dislocationsrelationship, presence of dislocations…
• Good experimental conditions: thin specimen (10 nm range)‐thin specimen (10 nm range)‐ incident beam // to a simple (low index) direction of the crystal => diffraction= known plane of the RS‐ column perfectly alignedcolumn perfectly aligned‐ appropriate defocus of the objective lens (Schertzer condition)‐microscope resolution smaller than the distance between the atomic columns that you want to image!g
Never trust ONE image !Never trust ONE image !
Rod‐like defect in silicon Si « dumbells »B=[011]
High Resolution Electron Microscopy
Rod like defect in silicon Si « dumbells »
[-1-11] [-11-1][-200][-11-
1][-1-11]
B [011]
[ ]
[1-11] [11-1][200]
[ ]
0.14 nm
[1-13]
[ 3 3 2][-111][1-11]
0.543 nm
with Cs corrector
I f i i d f h id ifi i d f
[-3 3 2] with Cs corrector
Cherkashin 2005Houdellier 2005
Interfaces, precipitates, defects, phase identification, defects, strain, etc…
What else ?
Incident beam
specimen
2ΘDiffracted l t
Transmitted electrons
EELSelectrons Energy loss
electrons
BCEV intensity jumps
Electron Energy Loss Spectroscopy
BC
BVEF
M
intensity jumpsionization energy levels
=> edges =core level distributions
ML
K
Im(-1/ε) = ε2 / (ε1 2 +ε2
2 )
Low-losses (the first few ten eV)Core-losses (up to a few thousand eV)
El m nt l ntit ti n l i
Valence electrons (VEELS)
Collective excitation : PlasmonIndividual excitation :Interband Transition
Core losses (up to a few thousand eV)
Inelastic interactions with inner or core level electrons
Elemental quantitative analysis
Electronic structureI~Im(-1/ε) = ε2 ∝ unoccupied DOS
Thickness: It/Izl=t/λpDielectric function
ε = ε1 + i ε2 I~Im(-1/ε) = ε2 ∝ unoccupied DOSEnergy Loss Near Edge fine Structure
ELNES
1 2Optical parametersn, k, μ, R = f (ε1, ε2)
Electronic structure JDOSε2 ∝ JDOS
Electron Energy Loss Spectroscopy
Electron Energy Loss Spectroscopy
. Electron Energy Loss Spectroscopy
Energy filtered TEMEnergy filtered TEM
TEM/EELS
EELS adds one dimension to TEM imaging
B bi th it ti f l t b d d t th lid ith th l t fBy probing the excitations of electrons bounded to the solid with the electrons from the incident beam
Gives information on: ‐specimen thickness‐elemental chemical composition and spatial distribution of elements‐spatial distribution of first neighbors relative to an atomic site‐chemical bonding‐electronic band structure‐dielectric function
with an energy resolution ranging between 1 eV and 0.3 eV
with a spatial resolution ranging between 10 nm and 1 nmwith a spatial resolution ranging between 10 nm and 1 nm
Concept of holography
ϕiAe=ΨComplex wave : amplitude and phase Take a picture :
²² AI =Ψ=You loose the phase !!! ϕ
AeΨWe want to retrieve the phase !
Coherent photon wave
Object
Object wave
Reference wave
)2cos(2²²² 0 refobjectobjectrefobjectrefobjectref xRAAAAI ϕϕπ −+++=Ψ+Ψ=
Information in the phase
∫ dE )()(φ ∫= dzzxVE ),(C)x( Eφ
∫∫= dxdz)zx,(- )x( nBeM
hφ
EMT φφφ +=
Electron Holography in a TEM
Sample
)exp(o K.ri=ψ ))((exp)(s r.rr ss KiA ϕ+=ψ
Objective lens
Focal plane
V+
Image plane
V+
Projector lensesProjector lenses
IHolo=⏐Ψo Ψs*⏐
2)yx(2A= 1 +Holo ⏐ o s ⏐ )yx,(sA= 1 +
)]yx,(s.xR2cos[)yx,(sA2 0 ϕ+π+
GPA analysis of the hologram
FT MaskFT
FT‐1FT
−π < ϕ < π
d
)yx,(sAImage d’amplitude
)yx,(sϕImage de phase
2π jumps unwrapped
Experimental aspects
• Coherent Electron Beam
Field Emission Gun
Fresnel fringesd t th hi hdue to the high coherence of the beam
• Elliptic illumination to increase the spatial coherence biprism
meilleure cohérence
Reference hologram
(without object)
Hologram with the object
FT FT
20 nm
FT-1FT-1
siesAsϕ=Ι RRR
ieA ϕ=Ι
)s(ieA
sAs RRR
ϕ−ϕ=ΙΙ
20 nmDérivée de la phase
ϕΔ=ϕ−ϕ RsNR
AA
sA=Normalised Amplitude Phase shift due to the object only
Non magnetic sample (B = 0)
∫∫∫ −= dxdzzyxBedzzyxV )()(C)yx(ϕ
∫ dV )(C)(
∫∫∫ dxdzzyxBdzzyxV ),,(),,(C)yx,( nEh
ϕ
∫= dzzyxVelect ),,(C )yx,( Eϕ⎟⎟⎠
⎞⎜⎜⎝
⎛++
⎟⎠⎞
⎜⎝⎛=
)2EE(EEE
λπ2C :with
0
0E
V( ) V ( ) V ( )V(x,y,z) = Vi (x,y,z) + V (x,y,z)
• Vi (x,y,z) = Mean Inner Potential (MIP)
V • V (x,y,z) = Local electric potential (junctions, CMOS, diode ..)
• if Vi et V are constants along the e-beam direction « z » :
ϕelect = CE (Vi + V ) t t = sample thickness
Need to perfectly know the sample thickness (sphere, cleaved sample, CBED hi k ) if V d Vthickness measurement...) to quantify Vi and V
ϕelect = CE Vi tMean Inner Potential (MIP) measurement
F NiFe0.5Ni0.5
10 nm
10 nm
10Fe Ni 910nmFe0.3Ni0.7
6
7
8
s FeNi theory
3
4
5
6
Pha
se/ra
dian
s yFeNi exp
tVEc 0=φ1
2
3P tVEc 0φ
00 5 10 15 20 25 30 35 40 45 50 55 60
Position/nm
• MIP measurement
• Composition analysis
• Morphological studies
∫∫∫ −=ϕ dxdz)z,x(Bedz)z,x(VC )x( nEh
Magnetic samples
Pb. 1: The objective must be witched off. => use of Lorentz lens to get sufficient resolution
• Object in a magnetic field free area
• Field of view up to 1µm
f = 30 mm
Cs = 7430 mm (!!)Cs = 7430 mm (!!)
Cc = 39 mm
Point resolution # 2 nmPoint resolution # 2 nm
Pb. 2: How to separate the magnetic and electrostatic contributions B and CEVit ?
Magnetic samples
Phase shift induced bt the local electrostatic potential:potential:
∫= dzzxVelect ),(C )x( Eϕ
Phase shift induced by the local magnetic
∫
y gfield :
∫∫ d d)()( Be∫∫= dxdz)zx,(-)x( nBmag
hϕ
Total phase shift
)x()x()x( ϕϕϕ += )x()x()x( magelectTot ϕϕϕ +=
Pb. 2: How to separate the magnetic and electrostatic contributions B and CEVit ?
1/ Taking two holograms (4 with the reference holograms) switching upside down the sample => The sign of the magnetic contribution is reversed and the electrostatic one remains.
VBt Vi BVi
∫∫−= dsBetVi nE .C 1 h
ϕ ∫∫+= dsBetVi nE2 .C h
ϕh
∫∫= dsBen2-
12 hϕϕ tVC iE2
12=+ϕϕ
Problem : finding back the same area of interest
2/ Taking two holograms with two different high voltages⎟⎟⎞
⎜⎜⎛ +
⎟⎞
⎜⎛= 0EEπ2
EC2/ Taking two holograms with two different high voltages
∫∫−= dsBetVi nE .C 11 h
ϕ)(
- 12
CCtVi =
ϕϕ
⎟⎟⎠
⎜⎜⎝ +
⎟⎠
⎜⎝
=)02EE(EλEC
)(12
EE CC −
P bl k i th i iti diti ( ifi ti
∫∫−= dsBetVi nE .C 22 h
ϕ
Problem : keeping the same acquisition conditions (magnification, alignment…) when changing the high voltage.
3/ Using the high magnetic field of the objective (~2 Tesla) to saturate the magnetic sample in two opposite directionstwo opposite directions
HObjectiveHObjectiveHObjective
+Θ -Θ
Back to Θ = 0 – objective switch off
∫−=ϕ dx).x(B.t.et.VC niE1h ∫+=ϕ dx).x(B.t.et.VC niE2
h
t
-d)(Bte 12 ϕϕ∫ tVC 12 ϕ+ϕ
∫h ∫h
2dx).x(B.t.e 12n
ϕϕ=∫h 2tVC iEϕϕ=
Magnetic contribution to the Electrostatic contribution to the phase shift phase shift
x1
∫∫=
−=−=Δ dzdzyBeyxyx nx
ξξϕϕϕξ
),,(),(),(1
2
12h
txBexx
n ).()(h
=∂
∂ϕ • The gradient of the phase is proportional to the in‐plane component of the magnetic induction Bn
• The equiphase contour gives the direction of the magnetic induction B
Magnetic Configuration of an isolated Fe Nanocube42
982)
, pp
4293
–4t.,
200
8, 8
(12
al.,
Nan
o Le
ttS
noec
ket
a
(a) TEM image, (b) Magnetic contribution to the phase shift, (c) Magnetic induction mapping, (d) micromagnetic simulation (OOMMF)
Magnetic Configuration of two neighbouring Fe Nanocubes
(a) TEM image, (b) Magnetic contribution to the phase shift, (c) Magnetic induction ( ) g , ( ) g p , ( ) gmapping, (d) micromagnetic simulation (OOMMF)
Magnetic Configuration of four neighbouring Fe Nanocubes
(a) TEM image, (b) Magnetic contribution to the phase shift, (c) Magnetic induction mapping, (d) micromagnetic simulation (OOMMF)
φ(x) = e/ħ ∫ B┴(x) t(x) dx
Magnetic multilayers
φ ∫
dφ(x)/dx = (e / ħ) . t . B┴(x)
E. Snoeck, P. Baules, G. BenAssayag, C. Tiusan, F. Greullet, M. Hehn, A. Schuhl
J. Phys.: Condens. Matter 20 (2008) 055219.
Sample preparation
Cross Section
specimen 1 t t
glue
specimen 1st cut
Ar+ ionsspecimen
electrons
2nd cutReady for TEMMechanical grinding
(abrasive papers + dimpler)(abrasive papers dimpler)
‐> 10‐20 µm
+ ion milling ‐> hole
Sample preparation
Plan view
electronsAr+ ions
20 µm
specimen mechanical grinding+ dimpling
ion milling ‐> hole Ready for TEM
Sample preparation
Sample preparation
Sample preparation
Sample preparation: FIB
Sample preparation: FIB
Summary
d l fGood TEM results from
50% specimen preparation,
20% TEM’s price
30% ’ i30% guy’s experience…