A.E. GunnæsMENA3100 V08 Transmissions electron microscopy Basic principles Sample preparation...
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Transcript of A.E. GunnæsMENA3100 V08 Transmissions electron microscopy Basic principles Sample preparation...
A.E. Gunnæs MENA3100 V08
Transmissions electron microscopy
Basic principles
Sample preparation
Imaging
aberrations (Spherical, Chromatic, Astigmatism) contrast (Mass-thickness, Diffraction, Phase)
A.E. Gunnæs MENA3100 V08
Basic principles, first TEM
Wave length:
λ= h/(2meV)0.5 (NB non rel. expr.)
λ= h/(2m0eV(1+eV)/2m0c2)0.5 (relativistic expression)
200kV: λ= 0.00251 nm (v/c= 0.6953, m/m0= 1.3914)
Electrons are deflected by both electrostatic and magnetic fields
Force from an electrostatic field (in the gun)F= -e E
Force from a magnetic field (in the lenses)F= -e (v x B)
Nobel prize lecture: http://ernst.ruska.de/daten_e/library/documents/999.nobellecture/lecture.html
a) The first electron microscope built by Knoll and Ruska in 1933, b) The first commercial electron Microscope built by Siemens in 1939.
A.E. Gunnæs MENA3100 V08
Basic TEM
Electron gun
Vacuum requirements:
- Avoid scattering from residual gas in the column.- Thermal and chemical stability of the gun during operation.- Reduce beam-induced contamination of the sample.
LaB6: 10-7 torrFEG: 10-10 torr
Cold trap
Electron source:
●Tungsten, W
● LaB6
● FEG
Sample position
A.E. Gunnæs MENA3100 V08
The lenses in a TEM
Sample
Filament
Anode
1. and 2. condenser lenses
Objective lens
Intermediate lenses
Projector lens
Compared to the lenses in an optical microscope they are very poor!
The point resolution in a TEM is limited by the aberrations of the lenses.
The diffraction limit on resolution is given by the Raleigh criterion:
δd=0.61λ/μsinα, μ=1, sinα~ α
-Spherical - Chromatic-Astigmatism
A.E. Gunnæs MENA3100 V08
Spherical aberrations
• Spherical aberration coefficient
ds = 0.5MCsα3
M: magnificationCs :Spherical aberration coefficientα: angular aperture/ angular deviation from optical axis
2000FX: Cs= 2.3 mm2010F: Cs= 0.5 nm
r1
r2
Disk of least confusion
α
Cs corrected TEMs are now available
The diffraction and the spherical aberration limits on resolution have an opposite dependence on the angular aperture of the objective.
A.E. Gunnæs MENA3100 V08
Chromatic aberration
v
v - Δvdc = Cc α ((ΔU/U)2+ (2ΔI/I)2 + (ΔE/E)2)0.5
Cc: Chromatic aberration coefficientα: angular divergence of the beamU: acceleration voltageI: Current in the windings of the objective lensE: Energy of the electrons
2000FX: Cc= 2.2 mm2010F: Cc= 1.0 mm
Chromatic aberration coefficient:
Thermally emitted electrons:ΔE/E=KT/eV
Force from a magnetic field:F= -e (v x B)
Disk of least confusion
A.E. Gunnæs MENA3100 V08
Technical data of different sourcesTungsten LaB6 Cold
FEGSchottky Heated
FEG
Brightness (A/m2/sr)
(0.3-2)109 (0.3-2)109 1011-1014 1011-1014 1011-1014
Temperature (K)
2500-3000 1400-2000 300 1800 1800
Work function (eV)
4.6 2.7 4.6 2.8 4.6
Source size (μm)
20-50 10-20 <0.01 <0.01 <0.01
Energy spread (eV)
3.0 1.5 0.3 0.8 0.5
H.B. Groen et al., Phil. Mag. A, 79, p 2083, 1999http://dissertations.ub.rug.nl/FILES/faculties/science/1999/h.b.groen/c1.pdf
A.E. Gunnæs MENA3100 V08
Lens aberrations
• Lens astigmatism
Loss of axial asymmetry
y-focus
x-focusy
xThis astigmatism can not be
prevented, but it can be
corrected!
A.E. Gunnæs MENA3100 V08
Sample preparation for TEM• Crushing
• Cutting– saw, diamond pen, ultrasonic drill, FIB
• Mechanical thinning– Grinding, dimpling
• Electrochemical thinning
• Ion milling
• Coating
• Replica methods
Plane view or cross section sample?
Is your material brittle or ductile?
Is it a conductor or insulator?
Is it a multi layered material?
A.E. Gunnæs MENA3100 V08
Grind down/dimple
TEM sample preparation: Thin films
• Top view
• Cross section or
Cut out a cylinderand glue it in a Cu-tube
Grind down andglue on Cu-rings
Cut a slice of thecylinder and grindit down / dimple
Ione beam thinning
Cut out cylinder
Ione beam thinning
Cut out slices
Glue the interface of interest face to face together withsupport material
Cut off excessmaterial
• Focused Ion Beam (FIB)
A.E. Gunnæs MENA3100 V08
Imaging / microscopy
200 nm
Si
SiO2
TiO2
Pt
BiFeO3
Glue
TEM - High resolution (HREM) - Bright field (BF) - Dark field (DF) - Shadow imaging (SAD+DF+BF)
STEM - Z-contrast (HAADF) - Elemental mapping (EDS and EELS)
GIF - Energy filtering
Holography
A.E. Gunnæs MENA3100 V08
Simplified ray diagram
Objective lense
Diffraction plane(back focal plane)
Image plane
Sample
Parallel incoming electron beamSi
a
b
cPow
derCell 2.0
1,1 nm
3,8
Å
Objective aperture
Selected area aperture
A.E. Gunnæs MENA3100 V08
Apertures
Selected area aperture
Condenser aperture
Objective aperture
A.E. Gunnæs MENA3100 V08
Use of apertures
Condenser aperture: Limits the number of electrons hitting the sample (reducing the intensity), Reducing the diameter of the discs in the convergent electron diffraction pattern.
Selected area aperture: Allows only electrons going through an area on the sample that is limited by the SAD aperture to contribute to the diffraction pattern (SAD pattern).
Objective aperture: Allows certain reflections to contribute to the image. Increases the contrast in the image. Bright field imaging (central beam, 000), Dark field imaging (one reflection, g), High resolutionImages (several reflections from a zone axis).
A.E. Gunnæs MENA3100 V08
Objective aperture: Contrast enhancement
All electrons contributes to the image. A small aperture allows only electrons in the central spot in the back focal plane to contribute to the image.Intensity: Thickness and density
dependence
Mass-thickness contrast
Si Ag and Pb
glue(light elements)
hole
50 nmOne grain seen along a low index zone axis.
Diffraction contrast(Amplitude contrast)
A.E. Gunnæs MENA3100 V08
Diffraction contrast: Bright field (BF), dark field (DF) and weak-beam (WB)
BF image
Objectiveaperture
DF image Weak-beam
Dissociation of pure screw dislocationIn Ni3Al, Meng and Preston, J.Mater. Scicence, 35, p. 821-828, 2000.
A.E. Gunnæs MENA3100 V08
Bending contours
BF image
DF image
DF image
Obj. aperture
Obj. lens
sample
A.E. Gunnæs MENA3100 V08
Thickness fringes/contours
Sample (side view)
e
000 g
t
Ig=1- Io
In the two-beam situation the intensityof the diffracted and direct beamis periodic with thickness (Ig=1- Io)
Ig=(πt/ξg)2(sin2(πtseff)/(πtseff)2))
t = distance ”traveled” by the diffracted beam.ξg = extinction distance
Sample (top view)Hole
Positions with max Intensity in Ig
A.E. Gunnæs MENA3100 V08
Thickness fringes, bright and dark field images
Sample Sample
DF imageBF image
A.E. Gunnæs MENA3100 V08
Phase contrast: HREM and Moire’ fringes
2 nm
http://www.mathematik.com/Moire/
A Moiré pattern is an interference pattern created, for example, when two grids are overlaid at an angle, or when they have slightly different mesh sizes (rotational and parallel Moire’ patterns).HREM image
Long-Wei Yin et al., Materials Letters, 52, p.187-191
200-400 kV TEMs are most commonly used for HREM
Interference pattern
A.E. Gunnæs MENA3100 V08
Moire’ fringe spacing
Parallel Moire’ spacing dmoire’= 1 / IΔgI = 1 / Ig1-g2I = d1d2/Id1-d2I
Rotational Moire’ spacing dmoire’= 1 / IΔgI = 1 / Ig1-g2I ~1/gβ = d/β
Parallel and rotational Moire’ spacingdmoire’= d1d2/((d1-d2)2 + d1d2β2)0.5
β
g1
g2
Δg
g1g2 Δg
A.E. Gunnæs MENA3100 V08
Simulating HREM imagesContrast transfer function (CTF)
CTF (Contrast Transfer Function) is the function which modulates the amplitudes and phases of the electron diffraction pattern formed in the back focal plane of the objective lens. It can be represented as:
k = u
The curve depend on:•Cs (the quality of objective lens) (wave-length defined by accelerating voltage)f (the defocus value)u (spatial frequency)
In order to take into account the effect of the objective lens when calculating HREM images, the wave function Ψ(u) in reciprocal space has to be multiplied by a transfer function T(u).
In general we have:Ψ(r)= Σ Ψ(u) T(u) exp (2πiu.r)
T(u)= A(u) exp(iχ), A(u): aperture function 1 or 0
Χ(u)= πΔfλu2+1/2πCsλ3u4 : coherent transfer function
A.E. Gunnæs MENA3100 V08
Simulating HREM imagesContrast transfer function (CTF)
Effect of the envelope functions can be represented as:
where Ec is the temporal coherency envelope (caused by chromatic aberrations, focal and energy spread,instabilities in the high tension and objective lens current), and Ea is spatial coherency envelope (caused by the finite incident beam convergence).
http://www.maxsidorov.com/ctfexplorer/webhelp/background.htm
A.E. Gunnæs MENA3100 V08
Contrast transfer function (CTF)
http://dissertations.ub.rug.nl/FILES/faculties/science/2004/s.mogck/c2.pdf
Contrast transfer functions and damping envelopes of the JEOL 2010F at optimum defocus (analytical model).
The highly coherent electron source used in the 2010F, a FEG, is apparent from the many oscillations in the CTF of the 2010F
A.E. Gunnæs MENA3100 V08
Scherzer defocus
http://www.maxsidorov.com/ctfexplorer/webhelp/effect_of_defocus.htm
Δ f = - (Csλ)1/2Δ f = -1.2(Csλ)1/2
Scherzer condition Extended Scherzer condition
A.E. Gunnæs MENA3100 V08
HREM simulations
One possible model for which the simulated HREM images match rectangular region I
HREM simulation along [0 0 1] based on the above structures. The numbers before and after the slash symbol “/” represent the defocus and thickness (nm), respectively
”The assessment of GPB2/S′′ structures in Al–Cu–Mg alloys ”Wang and Starink, Mater. Sci. and Eng. A, 386, p 156-163, 2004.