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Electron Microscopy:

Fundamentals
Chemistry 445
Spring 2004
27 April 2004

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Basic principles in optical microscopy


M =

Si
So

1 1 1
+ =
S o Si f

So

Si

Magnification

Image type

So =

Si = f

M=0

real

2 f < So <

f < Si < 2 f

M<1

real

So = 2 f

Si = 2 f

M=1

real

f < So < 2 f

2 f < Si <

M>1

real

So = f

Si =

M => inf

So < f

Si > S o

M>1

virtual
http://www.matter.org.uk/tem/lenses/thin_lens_optics.htm

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Optical imaging system

Condenser lenses
Field diaphragm

Minimizes glare
Image is focused in object plane

Aperture diaphragm

Controls angle of cone of light entering


objective
Affects general level of illumination
Image is at rear focal plane of objective
lens
Back focal plane of condenser lens

Objective lens
Forms inverted image
Aperture improves contrast

Eye piece
Magnification source

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Angles in optical and electron microscopy


Optical microscopy

Electron microscopy
Oblique illumination

d min =

2 sin

Perpendicular illumination

d min =

Lmin =

2 (n sin )

sin

2 NA

Example: = 400 nm and NA = 0.95


Lmin = 210 nm
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

= 0.01 nm at 10 keV
= 0.004 nm at 100 keV

= 102 radians

Electron Microscopy
Transmission electron microscopy (TEM)

Scanning electron microscopy (SEM)

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

History of TEM
1926
H. Busch showed that electric and magnetic fields of
axial symmetry acted as lenses for electrons and other
charged particles

1928
E. Ruska began serious study of magnetic lenses

1932
First description of a crude electron microscope

1986
Nobel prize for electron microscopy give to Ruska
Nobel prize for scanning tunneling microscopy to
Binning and Rohrer

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Electron and optical microscopy

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Condenser System

http://www.matter.org.uk/tem/lenses/second_condenser_lens.htm

First condenser lens

Simulation of condenser system

Second condenser lens

Affects the beam convergence at the


sample
Controls diameter of the illuminated area

Aperture

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Creates a demagnified image of the gun


crossover
Controls minimum beam spot size

Controls the intensity of illumination

Objective Lens

Objective lens

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Forms an inverted initial image, which


is subsequently magnified
Forms a diffraction pattern in the back
focal plane

Objective Aperture

Objective aperture

Selects electrons that will contribute to


the image
Improves contrast of the final image
Placed in back focal plane of image

http://www.matter.org.uk/tem/lenses/objective_aperture_2.htm

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Intermediate and Projector Lenses

Intermediate lens
Magnifies the initial image formed
by objective lens
Focuses on initial image or
diffraction pattern formed in back
focal plane

Projector lenses
Magnifies size of image
Can have various strengths

diffraction pattern

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

image

Electrostatic lenses

Electrostatic lenses used to


Focus electrons in CRTs
Focus sources for electron
microscopes

Focusing is independent of
mass
Electrons and ions follow
same trajectory
Image is inverted

Converging lens: paraxial ray


approximation
Distances off axis are small
is small; tan ~
No skew of particle
trajectories

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Principle of least action


B

p i ds = 0
A

p ds + p ds = 0
sin 1 p1
=
sin 2 p2

Magnetic lenses

Magnetic lenses used for


Condenser lenses
Objective lenses

Focusing depends on
charge to mass ratio
103-105 less effective at
focusing ions
Image is inverted and
rotated
Focal length depends on
strength of magnetic field

Paraxial ray approximation

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Electrostatic and optical lenses


V1 < V0

V1 > V0

One problem: insulating films can build up on lens surfaces from


electron bombardment electrostatic charging
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Magnetic and Optical Lenses

Acts as convex lens

Image inverted and rotated relative to object


Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Summary of Electrostatic and Magnetic Lenses

All axially symmetric magnetic or electrostatic field


has the property of a lens for paraxial arrays

All such lenses are convergent

Focusing of a magnetic lens depends on q/m

Focusing of an electrostatic lens is independent of m

The image is inverted and rotated in the case of a


magnetic lens and merely inverted for an electrostatic
lens

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Resolution of the TEM

Spherical aberration
Object of extent with no aberration

d 0 ' = 12 Cs 3
For strong focusing

Cs = Ks f
Example: In a good magnetic lens design, Ks ~ 1; for an electrostatic lens, Ks > 1.
must be small (~ 10-2 rad)

Effects of diffraction
For perpendicular illumination

d=

sin

In TEM, resolution estimated by objective lens

d min =

= Cs 3

d min = Cs1/ 4 3/ 4

Example: = 0.037 A (100 keV electron) and Cs = 1 mm (for TEM objective lens)
dmin = 4.74 A
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Contrast in TEM

Inelastic scattering
Absorption
Occurs in all materials

Incoherent, elastic
scattering
Amorphous materials

Coherent scattering
Diffraction from singlecrystal regions

eik ' r el
(r ) =
f
r

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Examples of TEM images

Samples must be thin


Light elements, t < 1 m
Heavy elements, t < 0.1 m
Lattice imaging, t ~ 10 nm

50 nm

D.A. Muller (IBM), Nature 416, 826 (2002)


F. Caruso (Max Planck Institute), Adv. Mat. 14, 908 (2002)
H. Lichte, Ultramicroscopy 38, 13 (1991)
P. Yang (UC Berkeley), Nano Lett. 2, 83 (2002)
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Electron Microscopy
Transmission electron microscopy (TEM)

Scanning electron microscopy (SEM)

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

History of the SEM


1935
Knoll built an SEM with 100 m beam diameter

1938
Von Ardenne built the first true SEM with 50-100 nm
resolution. Destroyed in 1944 Berlin air raid.

1953
McMullan and Oatley at Cambridge U. Used electron
multiplier and collected backscattered electrons from
inclined samples.

1961
First commercial instruments

1965
R.F. W. Pease and W. Nixon achieved 10 nm resolution
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

SEM imaging

Electron gun

Condenser lens

Electron source
Anode
Positive accelerating voltage
0.5 to 30 kV

Anode

Condenser lenses
De-magnify beam
Control probe size and current

Condenser lens

Objective aperture

Minimizes lens aberrations


Controls final probe current
Determines convergence angle

Scanning coils
Stigmators

Objective lens
Sample

Objective aperture

Stigmators
Corrects astigmatism

Objective lens
Final focusing

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Electron sources

Source
size (nm)

B @ 25 kV
(A/cm2/Sr)

E
(eV)

10

30000

2 x 105

2000

100

5000

5 x 106

300

>1000

<5

5 x 108

0.22

>1000

<5

5 x 107

Source

Temp
(K)

2900

LaB6
W, cold FE tip
Zr/O/W thermal FE

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Lifetime
(hrs)

Electron emission

Electron emission

J 0 = AT 2 e / kT

Review of solid angles

= A / L2

Aberration-free beam
diameter
eV
J = J0 +1 sin2
kT

For small angles,

J =B

J eV

+ 1
B= 0
kT
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

4i 1
d0 =
2B

2
i=

d02
4

J=

d02
4

B 2

Resolution of the SEM

Aberration-free beam diameter


d0 =

4i 1
2B

Spherical aberration
Uncertainty in focusing the electrons as a function of how far their trajectory is
from the center of the lens.
1
3
5 nm

d s = Cs
2

Chromatic aberration
Uncertainty in focus due to the energy spread and speed of electrons

E
d c = Cc
E

Diffraction

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

df =

10 nm
< 1 nm for FE tip

< 1 nm

Electrons emitted from surfaces


Secondary

Backscattered
Auger

Secondary electrons
0 < E < 50 eV

Backscattered electrons
50 eV < E < E0

Auger electrons
150 eV < E < 800 eV

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Current at the sample


ibeam - iemitted

Detectors for electron collection


Secondary electrons

Backscattered electrons

www.jeol.com
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Appearance of an SEM image

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

Contrast in SEM

Backscattered electrons
Substrate atomic number
(Z)
Angle of beam incidence
Occurs in all materials

ibackscatt . = ibeam

Secondary electrons
Angle of beam incidence
Energy of beam incidence
Work function and surface
condition

isecondary = total ibeam

total = in + out

Chemistry 445: Science and Technology at the Nanoscale


Teri W. Odom

total ( ) =

total (0)
cos

Different signals collected by detector


Backscattered image

Secondary electron image

www.jeol.com
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Minimizing sample charging


Reduce the accelerating voltage
Coat sample with conducting film
Tilt the sample

10 keV

Material

4 keV
Chemistry 445: Science and Technology at the Nanoscale
Teri W. Odom

Escape depth
(Ls, nm)

Pt

MgO

23

Al

5-8

Au

3-4

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