Transmissions electron microscopy

Sample preparation Basic principles Imaging

aberrations (Spherical, Chromatic, Astigmatism)

contrast (Mass-thickness, Diffraction, Phase)

A.E. Gunns

MENA3100 V10

Sample preparation for TEM

Crushing
Plane view or cross section sample? Cutting
saw, diamond pen, ultrasonic drill, FIB

Is your material brittle or ductile?

Is it a conductor or insulator? Is it a multi layered material?

Mechanical thinning
Grinding, dimpling

Electrochemical thinning Ion milling Coating Replica methods FIB

A.E. Gunns

MENA3100 V10

TEM sample preparation: Thin films

Cut out cylinder

Grind down/ dimple

Top view
Cut out slices Cut out a cylinder and glue it in a Cu-tube

Ione beam thinning

Grind down and glue on Cu-rings

Cross section

Glue the interface of interest face to face together with support material

or

Focused Ion Beam (FIB)

Cut a slice of the cylinder and grind it down / dimple

Cut off excess material

Ione beam thinning

A.E. Gunns

MENA3100 V10

Basic principles, first TEM

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) Wave length: = h/(2meV)0.5 (NB non rel. expr.) = h/(2m0eV(1+eV)/2m0c2)0.5 (relativistic expression) 200kV: = 0.00251 nm (v/c= 0.6953, m/m0= 1.3914) a) The first electron microscope built by Knoll and Ruska in 1933, b) The first commercial electron Microscope built by Siemens in 1939.

Nobel prize lecture: http://ernst.ruska.de/daten_e/library/documents/999.nobellecture/lecture.html A.E. Gunns MENA3100 V10

Basic TEM
Electron gun
Electron source: Tungsten, W LaB6 FEG

A.E. Gunns

MENA3100 V10

Electron guns
Thermionic gun Field emission gun (FEG)

A.E. Gunns

MENA3100 V10

Technical data of different sources

Tungsten Brightness (A/m2/sr) Temperature (K) Work function (eV) Source size (m) Energy spread (eV) (0.3-2)109 LaB6 (0.3-2)109 Cold FEG 1011-1014 Schottky 1011-1014 Heated FEG 1011-1014

2500-3000

1400-2000

300

1800

1800

4.6

2.7

4.6

2.8

4.6

20-50

10-20

<0.01

<0.01

<0.01

3.0

1.5

0.3

0.8

0.5

Monochromator: Energy spread less than 0.15 ev

http://dissertations.ub.rug.nl/FILES/faculties/science/1999/h.b.groen/c1.pdf H.B. Groen et al., Phil. Mag. A, 79, p 2083, 1999

A.E. Gunns

MENA3100 V10

Basic TEM
Electron gun
Electron source: Tungsten, W LaB6

Cold trap Sample position

FEG

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 torr FEG: 10-10 torr

A.E. Gunns

MENA3100 V10

The lenses in a TEM

Filament

Anode

The diffraction limit on resolution is given by the Raleigh criterion:

1. and 2. condenser lenses

d=0.61/sin, =1, sin~

Sample

Objective lens

Compared to the lenses in an optical microscope they are very poor!

Intermediate lenses

The point resolution in a TEM is limited by the aberrations of the lenses.

Projector lens

-Spherical - Chromatic -Astigmatism

A.E. Gunns

MENA3100 V10

Spherical aberrations
Spherical aberration coefficient
ds = 0.5MCs3
M: magnification Cs :Spherical aberration coefficient : angular aperture/ angular deviation from optical axis 2000FX: Cs= 2.3 mm 2010F: Cs= 0.5 nm

Cs corrected TEMs are now available

r2 r1

Disk of least confusion

The diffraction and the spherical aberration limits on resolution have an opposite dependence on the angular aperture of the objective.

A.E. Gunns

MENA3100 V10

Aberrations in a nutshell
Before Cs correction

After Cs correction

Core of the M100 galaxy seen through Hubble (source: NASA) A.E. Gunns MENA3100 V10

Q.M. Ramasse

Resolution limit
Year 1940s 1950s 1960s Resolution ~10nm ~0.5-2nm 0.3nm (transmission) ~15-20nm (scanning) 0.2nm (transmission) 7nm (standard scanning) 0.15nm (transmission) 5nm (scanning at 1kV) 0.1nm (transmission) 3nm (scanning at 1kV) <0.1 nm (Cs correctors)

1970s
1980s 1990s 2000s

http://www.sfc.fr/Material/hrst.mit.edu/hrs/materials/public/ElecMicr.htm

A.E. Gunns

MENA3100 V10

Chromatic aberration
Disk of least confusion Chromatic aberration coefficient: dc = Cc ((U/U)2+ (2I/I)2 + (E/E)2)0.5
Cc: Chromatic aberration coefficient : angular divergence of the beam U: acceleration voltage I: Current in the windings of the objective lens E: Energy of the electrons 2000FX: Cc= 2.2 mm 2010F: Cc= 1.0 mm

v - v v

Thermally emitted electrons:

E/E=KT/eV

Force from a magnetic field:

F= -e (v x B)

A.E. Gunns

MENA3100 V10

Lens aberrations
Lens astigmatism
Loss of axial asymmetry This astigmatism can not be prevented, but it can be corrected!
x

y-focus

x-focus

A.E. Gunns

MENA3100 V10

Operating modes
Convergent beam Parallel beam

Can be scanned (STEM mode)

Specimen
Spectroscopy and mapping (EDS and EELS)

Imaging mode
or

Diffraction mode
A.E. Gunns MENA3100 V10

Image or diffraction mode

Filament

Anode

1. and 2. condenser lenses

Spesimen

Objective lens

Objective aperture Selected area aperture

Diffraction plane Image plane

Bi-prism
Intermediate lenses

Projector lens Viewing screen

STEM detectors (BF and HAADF) Image or diffraction pattern

A.E. Gunns

MENA3100 V10

Advanced nanotool

JEOL 2010F FEGTEM

Ultra high resolution version with analytical possibilities
A.E. Gunns MENA3100 V10

Imaging / microscopy
TEM - High resolution (HREM) - Bright field (BF) - Dark field (DF) - Shadow imaging (SAD+DF+BF) SiO2 STEM - Z-contrast (HAADF) - Elemental mapping (EDS and EELS) GIF - Energy filtering Holography Si 200 nm

BiFeO3 Pt TiO2 Glue

A.E. Gunns

MENA3100 V10

Simplified ray diagram

Si
3,8

A.E. Gunns

c b a

Parallel incoming electron beam

Sample

1,1 nm
PowderCell 2.0

Objective lense

Diffraction plane Objective aperture (back focal plane)

Image plane MENA3100 V10

Selected area aperture

Apertures

Condenser aperture

Objective aperture Selected area aperture

A.E. Gunns

MENA3100 V10

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 resolution Images (several reflections from a zone axis).

A.E. Gunns

MENA3100 V10

Objective aperture: Contrast enhancement

Si Ag and Pb hole

glue
(light elements)

All electrons contributes to the image. Intensity: Thickness and density dependence

A small aperture allows only electrons in the central spot in the back focal plane to contribute to the image.

Diffraction contrast Mass-thickness contrast

(Amplitude contrast)

One grain seen along a 50 nm low index zone axis.

A.E. Gunns

MENA3100 V10

Diffraction contrast: Bright field (BF),

dark field (DF) and weak-beam (WB)

Objective aperture

BF image

DF image

Weak-beam

Dissociation of pure screw dislocation In Ni3Al, Meng and Preston, J. Mater. Scicence, 35, p. 821-828, 2000.

A.E. Gunns

MENA3100 V10

Bending contours

sample

Obj. lens Obj. aperture

BF image DF image DF image

A.E. Gunns

MENA3100 V10

Thickness fringes/contours
In the two-beam situation the intensity of the diffracted and direct beam is periodic with thickness (Ig=1- Io) 000 g Ig=1- Io e

Sample (side view)

Hole
Ig=(t/g)2(sin2(tseff)/(tseff)2)) t = distance traveled by the diffracted beam. g = extinction distance

Sample (top view)

Positions with max Intensity in Ig A.E. Gunns MENA3100 V10

Thickness fringes, bright and dark field images

Sample Sample

BF image A.E. Gunns MENA3100 V10

DF image

Phase contrast: HREM and Moire fringes

Long-Wei Yin et al., Materials Letters, 52, p.187-191

HREM image
2 nm

A Moir 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). http://www.mathematik.com/Moire/

Interference pattern 200-400 kV TEMs are most commonly used for HREM

A.E. Gunns

MENA3100 V10

Moire fringe spacing

Parallel Moire spacing dmoire= 1 / IgI = 1 / Ig1-g2I = d1d2/Id1-d2I
g2 g1 g

Rotational Moire spacing dmoire= 1 / IgI = 1 / Ig1-g2I ~1/g = d/

g1 g2 g

Parallel and rotational Moire spacing dmoire= d1d2/((d1-d2)2 + d1d22)0.5

A.E. Gunns

MENA3100 V10

Simulating HREM images

Contrast 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:

In order to take into account the effect of the objective lens when calculating HREM images, the wave function (u) in reciprocal space has to be multiplied by a transfer function T(u).
In general we have: (r)= (u) T(u) exp (2iu.r) T(u)= A(u) exp(i), A(u): aperture function 1 or 0

k=u The curve depend on: Cs (the quality of objective lens) l (wave-length defined by accelerating voltage) Df (the defocus value) u (spatial frequency)

(u)= fu2+1/2Cs3u4 : coherent transfer function

A.E. Gunns

MENA3100 V10

Simulating HREM images Contrast 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. Gunns

MENA3100 V10

Scherzer defocus

f = - (Cs)1/2 Scherzer condition

f = -1.2(Cs)1/2 Extended Scherzer condition

http://www.maxsidorov.com/ctfexplorer/webhelp/effect_of_defocus.htm

A.E. Gunns

MENA3100 V10

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 AlCuMg alloys Wang and Starink, Mater. Sci. and Eng. A, 386, p 156-163, 2004.

A.E. Gunns

MENA3100 V10

Combined HAADF and EELS

HAADF image of an icosahedral FePt particle (false colors): thanks to the small probe size, it is possible to probe precisely the chemical structure of samples at the atomic level, revealing here a small crystalline layer of iron oxide surrounding the outermost shell of the particle.
A.E. Gunns MENA3100 V10

Energy filtering

A. Thgersen et al., Collaboration with Prof. T. Finnstad, UiO, S. Diplas, SINTEF and UniS, UK and NIMS, Japan
A.E. Gunns MENA3100 V10