Do Minh Nghiep

Materials Science Center

Electron Microscopy
and
d Diffraction
Diff i
2. Electron source
and Vacuum system
 Content
Content
Electron source
• Definition
• Classification
• Th
Thermionic
i i emission
i i gun
• Field emission gun
• Correction
• Selection
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 Content
Vacuum system
• Classification
• Vacuum system for EMs
• Application and selection of vacuum
• SEM with low vacuum

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 Electron source

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 Definitions and types
• Electron gun: where electrons are
generated LaB6
• Elements of the g gun:
- Emitter (cathode)
- Wehnelt cilynder or cap
- Anode
• Gun types:
FEG
- Thermionic emitter (W, LaB6) W
- Field emitter (W crystal)
• Filament:
Fil t tungsten,
t t LaB
L B6 wire
i or rod
d
• Cathode: negative electrode
• Anode: positive electrode

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 Electron gun
ƒ The filament/cathode:
- thermionic emission
(tungsten lanthanum boride)
(tungsten,
- field emission gun

ƒ Wehnelt cap:
negative bias

ƒ Anode:
positive bias

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Ch
Characteristics
t i ti

ƒ Filament current (FC)

(FC)/
heating current: currentt
running through the emitter
ƒ Beam current (BC)/
emission current: current
generated by
g y the emitter

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 FC--BC curve
FC
Increasing the filament current will increase the beam current but
only to the point of saturation at which point an increase in the
filament current will only shorten the life of the emitter.

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 Emission mechanism
Work function:
Ew = E - EF

ƒ Energy (or work) required to

withdraw an electron completely
from a metal surface.
ƒ This
Thi energy iis a measure off
how tightly a particular metal
holds its electrons.

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Power of electron light source
Optical brightness β
ƒ β is the
t current density per illumination angle
ƒ Described by equation:
β = (current) / [(area).( )] = 4ib/ (πd2α2)
[(area).(illumination angle)]
ƒ Maximal
M i lb brightness
i ht off th
thermionic
i i emission
i i att hihighh voltage
lt
βmax= JC.e.Vo/π.k.T
JC - current density on cathode surface T - absolute temperature
e - electron charge = 1.59 x 10-19 C d - beam diameter
Vo - accelerated voltage α- beam angle of coherence
k - Boltzmann constant = 8.6 x 10-5 eV/K ib - beam current

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 Two types of electron gun

Thermionic emitter Field emitter

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 Thermionic emitters
Thermionic emitters utilize heat to
overcome the work function of a materia

Tungsten filament (W) Lanthanum hexaboride (LaB6)

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Handouts-MSE4346-K51KHVL 12
 Thermionic emitters
W filament:
filament a wire of diameter
100 μm bent to V shape with a
sharp tip of diameter 100 μm
and emission area of 100 μm x
150 μm.
μ

Lanthanum Hexaboride (LaB6): a rod/single crystal LaB6 with sharp tip

of diameter 50 μm and length 0,5 mm is mounted and heated by
carbon/rhenium resistance, insensitive to LaB6.

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 Thermionic emitters
Tungsten filament

W wire bent into a loop of various dimensions (Tm=3410 degrees C)

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 Thermionic emitters
LaB6 filament

Heat is applied
pp by
y way
y of
separate resistance wires

or by ceramic mounts

and by ribbons: Filament

current is separate from
heating current

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Handouts-MSE4346-K51KHVL
 Thermionic emitters
LaB6 filament
Similar in design to a
tungsten filament

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 LaB6 filament

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 Field emitters
Definition and classification
Field emission: The emission of electrons that are
stripped from parent atoms by a
high electric field
Three types of field emitters
emitters::
FE - cold emitter ((byy electric field))
TE - thermal emitter (by electric field and heat)
SE- Schottky emisison (by electric field, heat,
coating (EW decreased)
Flashing the filament (FE vs. TE)
Filaments EW: W - 4,5 eV; LaB6 - 2,5 eV;
W/ZrO - 4,5÷2,8 eV
(
(coating
ti ZrO
Z O on <100> W)
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 Fi ld emitters
Field itt
Configuration
Sharp tip
ƒ Filament is single oriented
crystal of tungsten etched to a
ZrO coating
g fine tip of diameter 100 nm or
smaller,
ll spott welded
ld d on a W
wire and coated with ZrO.
ƒ Electric field is concentrated at
the tip.
tip Thus potential barrier is
reduced and electron emission
Tungsten wire will be easier to realized without
additional heating.

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 Fi ld emitters
Field i

Emission beam

A Field Emissiontip can be

“ ld” or thermally
“cold” th ll assisted
i t d
to help overcome the work
function, but ultimatelyy it is
a high voltage field of 3
keV that is needed.

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 A comparison

Other factors to consider ?

Cost: W= $15 LaB6 = $400 F.E. = $6000
Lifetime: 100 hr. 1000 hr ,
5-8,000 hr.

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 A comparison
p

Operating temperature: 2700 K 1800 K 1800 K

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 Thermionic
Th i i vs field
fi ld emitter
itt
Thermionic emitter Field emitter
Pros: Pros:
- direct and rapid heating - narrow electron beam from
- chip technology source
CONS:
- good brightness
- big depth of field (DOF)
- relative low brightness
CONS:
- evaporation of cathode - ultra high
g vacuum ((UHV >10-
materials 9 torr)
- thermal drift during - high gradient of electric field
operation - tip sensitive to shape,
- broad
b d electron
l t b
beam ffrom surface,
f erosion,
i dirt
di t
source
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Electron source comparison for TEM

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 Adj t
Adjustment
t off electron
l t gun

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Adjustment of electron gun
Filament centering

Gun horizontal

Gun tilt

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 Vacuum system

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 Why vacuum in EM column ?
ƒ In SEM the pressure P must be < (10-4) Pa ( ≈ 10-6 torr)
- for thermionic W emitter: P < 10-4 Pa (10-6 torr)
- for more sensitive LaB6 emitter: P < 10-5 Pa (10-7 torr)
ƒ Reasons
Reasons::
- Elimination of interaction between electron beam and gas
molecules, which reduce intensity of primary beam and scatter it
- If the pressure over 1 Pa (10-2 torr) may be a discharge between
scintilating crystal (+10.000 V) and Faraday cup (+250 V)
- To reduce specific pressure of the hydrocacbon compound
(dissociation of hydrocacbon compound dirties sample)
ƒ Limitations
Limitations:: escape of gas impossible
impossible; drying and freezing of
biosamples coating of non-conductive
biosamples, non conductive samples required
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 Why vacuum in EM column ?
ƒ In order to allow passage of the electron
beam through g the microscopep without
interference from gas molecules, the
pressure within the instrument has to be
reduced
d d to
t the
th point,
i t where
h th
there i very
is
small probability, that an electron will
encounter a gas molecule.
molecule
ƒ Pressure should be lower than 10-5 torr.

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 Classification
• Vacuum system
system:
y : low → veryy high
g ((1 Pa = 10-2 torr))
Rough vacuum: 105-102 Pa (103-1 torr)
Medium vacuum: 101-10-1 Pa (10-1-10-3 torr)
High vacuum: 10-1-10-5 Pa (10-3-10-7 torr)
Ultra-high vacuum: < 10-5 Pa (10-7 torr)
• Pump types
types:: rotary pump, diffusion pump, turbo-pump
- Rotary pump: for rough to medium vacuum (from air
pressure to 2 x 10-22 torr)
- Diffusion pump: for high vacuum (10-2 to < 10-9 torr)
- Turbo
Turbo-pump:
pump: for ultra
ultra-high
high vacuum (10-3 to < 10-10 torr)
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 Rotary pump

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 Diffusion pump

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 Vacuum in EMs
Vacuum system is
devided into various
regions of EM

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 Application and selection

(Pa) 10-5 10-1 102 105

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 Environmental SEM

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 Vacuum is variable
ƒ Different names: Environmental (E)/
Low Voltage (LV)/ Variable Pressure (VP)/
Elevated Pressure (EP) SEM
ƒ Vacuum: (100-1000)
(100 1000) Pa (≈1
(≈1-10
10 torr)
ƒ Various pumps: for sample stage, column
and electron gun
ƒ Media: O2, Ar, N, H2O, air

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 Vacuum regions in ESEM

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 Operating principles of ESEM

ƒ SE ionizes gas molecules in

sample chamber (only about
1% BSE take part in
ionization).
ƒ Formed ions will neutralize
anyy electric charge
g built upp
above the surface of non-
conductive sample.
ƒ Specific SE detectors are
used for ESEM because of
high pressure nearby sample
surface.

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 Operating
p g principles
p p of ESEM

VPSE detectors of LEO allow measurement

of SE in both cases of low and high vacuum.

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 Pros of ESEM
ƒ Imaging off wet samples
- by replacing air with water vapour in sample
chamber
ƒ Following of hydration and dehydration process
- thanks to a medium super
super-saturated
saturated by water
- change of sample state and structure in the process
- condensation/evaporation of water on sample
surface

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 Cons of ESEM

ƒ Max resolution only 2 nm, much lower than that

of SEM (0,5
(0 5 nm)
ƒ Low density of incident electrons because of
scattering
ƒ Background artefacts caused by electron
scattering
ƒ Low contrast

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 Application of ESEM

ƒ ESEM overcomes limitation of SEM: coating is required in the case of

electric charge on non-conductive sample surface, moist
/hydrated/liquid samples must be dried.
ƒ ESEM allows to see samples (solid/liquid) in its original state: media
may be water, argon, nitrogen, oxigen, air.
ƒ ESEM allows to analyze moist/wet samples at high pressure (50 torr),
without vacuum.
ƒ In-situ study
y of specimen
p with video-capture
p of dissociation, hydration,
y
dehydration, crystallization, melting, absorbtion, corrosion processes
(agglomeration of polymer colloids; expansion, dissolvation, separation
mechanism of medicine; kinetic physico-chemical behavior )

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 Illustrations: crystallization

0 min. 15 min.

10 min.
20 min.

VPSE detector of LEO used

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 Illustrations: metal melting

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 Illustrations: charge reduction

In presence of air and under controlled pressure

of sample chamber, the charged region doesn’t
exist and quality of image is better

Charged region on surface of

CaCO3 sample under high vacuum

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 Illustrations: water loss
(structural collapse)

Image of dehydrated (link, bottom) and hydrated

(right, top) samples observed in vacuum and
without
ith t vacuum

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