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SEM

Scanning Electron Microscopy


construction, operation
and application
:

Prof. dr habil. ing. Wodzimierz Dudziski

Types of microscopes: LM,TEM, SEM

Electron microscopes
First electron microscope 1931 Ernst Ruska and Maks Knoll
First project of SEM - 1938
First construction of SEM Cambridge, England, 1960-1961.

SEM How it works?


Wave-particle duality de Broglie wavelength
Electron wavelength in electrostatic field
Resolution of the
microscope
(Abbys formula)

Comparison of radiation types


wiato widzialne

Fala elektronowa

Promieniowanie
rentgenowskie

400-800nm

0,007nm (30 kV)

0,1nm

rdo
promieniowania

arwka, laser

emisja termiczna (W,


LaB6), zimna emisja
polowa

lampa rentgenowska

Soczewki

optyczne

elektromagnetyczne

brak

Dugo fali

Tworzenie
obrazu

bona fotograficzna,
matwka, matryce
CCD i CMOS

matryce CCD i CMOS

bona fotograficzna,
matwka, matryce
CCD i CMOS, ekrany
fluorescencyjne

SEM construction and operation

SEM sources of electrons

Role of electrons source:

Formation of electron beam with stable and sufficent current density and as
small as possible diameter

Types of electron guns:


- Directly heated cathode W (Tungsten)
- Indirectly heated cathode LaB6
- Field emision guns - FEG
Cold emision Cold FEG
Hot emision - Shotky FEG
Cathode
Wehnelt cylinder
Anode
Electron beam

Electron gun with directly heated


cathode - Tungsten

Cathode from tungsten wire


Wehnelt cylinder
Equipotential lines
Aperture angle of electron beam

Electron gun with directly heated


cathode Tungsten filament

Electron gun with indirectly heated


cathode LaB6 filament

Cooled cathode holder


Heating coil
Tantalium thermal screen
Cathode, single crystal LaB6 or CeB6
Wehnelt cylinder
Anode

Electron gun with indirectly heated


cathode LaB6 filament

Field emision gun cold FEG cathode

Cathode single crystal of tungsten


Insulator

Influence of beam current

rednica - Beam diameter, Prd - Beam current,


Cathodes: Tungsten, LaB6, FEG

Influence of beam current - details

Ceramic , Acceleration voltage 10 kV, magnification 5400x

Influence of acceleration voltage

Influence of acceleration voltage


High Acc. Voltage:
high resolution, lack of surface transparency,
strong effect of edge, influence of surface charge
collection, strong degradation of specimen structure

Low Acc. Voltage:


low resolution, transparent surface structure,
low influence of surface charge collection,
low effect of edge,

Influence of beam current - details

Principle of magnetic lens operation

Effect of Lorencs Force on electron moved inside


magnetic field

Inside magnetic field, electron is moved on helical path

Magnetic lens - construction

ferromagnetic coat
gap
windings

Types of Magnetic Lens


with opened cover (I)
with closed cover (II)
with pole pieces (III)

electron beam

magnetic induction distribution

Superconducted magnetic lenses

liquid helium tank


electron beam

pole pieces prepared


from holm or dyspros

superconducted winding
iron cover

Aperture
Aperture in plane of the lenses eliminate electrons maximally up
away from lens axis, but density of current is decrised
Aperture has direct influence on depth of field and image resolution

Plane of optimum focus, depth of field region

Scanning coils

Electron beam
Scanning coils
Detector
Investigated object
Amplifier
Screen

Main types of radiation

direction of electron beam, X-ray radiation, BSE electrons,


SE electrons, volume of interaction

Types of radiations
Informations carried by different types of radiation

*rozdzielczo zaley od napicia przyspieszajcego oraz liczy atomowej

Back Scattered Electrons - BSE


Electrons are dispersed with angles from 0 up to 180.
Electrons dispersed under a large angles are named
Back Scatteres Electrons - BSE

Direction of the beam


Back scattered electron
Nucleus particles

Comparison between SE and BSE


images

Absorbed Electrons - AE
Regions richer with heavy elements looks like dark
Regions contained light elements looks like brighter

X-ray radiation
X-ray radiation forms the image with lower quality then
electrons image. The reason is much higher surface of
X-rays what causes weak resolution
Presence impulses of Xray reflexes characteristic for
elements, gives possibilities for their detection

Cathodoluminescence
Emission of the visible light emited by solids/rocks
caused by electron beam excitation
With the aid of this phenomen it is possible to make
observations of rocks properties which are not visible
under ordinary petrographic/polarised microscope

Impact area

Primary electrons beam


Characteristic X-ray radiation
Low atomic number
High atomic number
High acc. voltage
Low acc. voltage

Detector of Secondary Electrons - SE

Mesh, scintillator covered by Al layer, fiber, photocathode, electric field,


dynodes of photomultiplayer

Detector of BSE radiation

Au layer
production of electron-hole pairs
p-n junction

Detectors of X-ray radiation

Image defects
abberation
spherical
chromatic
astygmatism
leak of focus and contrast
image instability
noisy image
frayed specimen images edges
over contrasted images
deformed images

Main possibilities of SEM microscope


Resolution much higher then application by light
microscope (up to 5nm with magnification 105 times)
Possibilities investigation of specimen with very different
topography
From the reason of small angle aperture, depth of focus
it is up to 300 times higher compared with light
microscopes working with identical magnification
Possibility to install detectors EDS or WDS for chemical
analyse or EBSD detectors for crystallographic analyse

Main types of materials investigated


by SEM methods
Insulators - materials non conducted electrical
current
Conductors materials conducted electrical
current
Semi conductors

Rules of specimens preparation for


SEM investigation
Adjustement of specimen size corresponding to the
microscope holder/or specimen table dimension
Cleaning of specimen surface/ultrasonic washing
Covering of non conductive specimen surface, by
vaporized or sputered elements like: C, Au, Pt, Cu.

Types of investigated specimens

metal (metal alloys)


composites
polymers
ceramic
powders
specimens in nano scale
biological specimens
geological specimens

Non conductive specimens


Biological specimens

Crystals of sugar x350

Farine/storch on potato cross-section,


x1000

Non conductive specimens


Biological Specimens

Housefly. x400

Head of bean insect. x400

Non conductive specimens

Mites. x150

Non conductive specimens

Non conductive specimens

Non conductive specimens

Different types of pollen flowers

Non conductive specimens

Non conductive specimens


Ceramics

Ceramics powder covered by Cu layer: a) nanopowder of Al 2O3 b) powder of Al2O3 , medium size of grain
is 30 m, spherical particles of Cu are visible

Non conductive specimens


Composites

Structure of composite Al-WO3-SnO

Coper layer disposed on polymer foil


with ceramic powder. x10000

Bibliography

Reimer Scaning electron microscopy


http://www.kgmip.wnoz.us.edu.pl/
http://www.sgml.pwr.wroc.pl/
http://www.biolog.pl/
http://www.chemia.uj.edu.pl/
http://pl.wikipedia.org/wiki/

Thank You for Your attention

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