low vacuum scanning electron microscopy and … to low vacuum sem...principles and practice of...
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![Page 1: Low Vacuum Scanning Electron Microscopy and … to Low Vacuum SEM...Principles and Practice of Variable Pressure/Environmental Scanning Electron Microscopy (VP-ESEM), Debbie J Stokes,](https://reader034.vdocument.in/reader034/viewer/2022042811/5fa4ae5d8e1f4f7b7057a091/html5/thumbnails/1.jpg)
Low Vacuum Scanning Electron Microscopy and Microanalysis
Principles and Practice of Variable Pressure/Environmental Scanning Electron Microscopy (VP-ESEM), Debbie J Stokes, John Wiley&Sons 2008Several graphs courtesy of prof. Bradley Thiel
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• Conventional scanning electron microscopy (SEM) is a widely used as an analytical tool. However, there are several limitations on the type of samples, which may be observed.
• When a specimen consists of a non-conductive material, or not properly grounded to the specimen stub, charging occurs. Charging is the build-up of an excess of electrons on the surface of the specimen, which causes many undesirable artefacts. Both secondary and backscattered electrons utilised for SEM observations are significantly affected.
• The elimination of specimen charging is accomplished in the LowVac/ESEM scanning electron microscope by the introduction of a gas, water, nitrogen or air into the specimen chamber.
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Outline
Introduction to Variable Pressure (Environmental) Scanning Electron Microscopy
Image formation in VP-SEM
X-ray Microanalysis in VP-SEM
Variable pressure method
EBSD in VP-SEM
Conclusions
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LV-SEM – Low Vacuum Scanning Electron MicroscopyVacuum from 0 to 1 Torr (0 mbar – 1.33 mbar)
VP-SEM or Environmental Scanning Electron MicroscopyVacuum from 0 to 20 Torr (0 mbar – 26.6 mbar)
15
10
5
0
-10℃ 0℃ 10℃ 20℃
ESEM
Low
Vac
uu
m S
EM
Solid
phase
Liquid phase
Gaseous phase
Pre
ssu
re [
Torr
]
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Specimen Chamber1-20 Torr
Gun
Pressure limiting aperture 1
Pressure limiting aperture 2
Water vapor/gas
Vent
(Not to scale)
RP DP
IP
RP DP
RP
10-8 Torr
10-5 Torr
10-1 Torr
10-3 Torr
Variable Pressure Scanning Electron Microscope
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Pumping system of ESEM
PLA1
PLA2
Gas flow from chamber max. 20 Torr
Major gas flow(to rotary pump)
Minor gas flow(to ODP or TMP)
Emission area: min. 10-5 Torr
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E
Grounded Stub
Dielectric Specimen
Biased Anode
+ +
+ ++
+
+
+++
+++
+
+
+
Cascade Amplification
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Cascade Amplification
E
Grounded Stub
Dielectric Specimen
Biased Anode
The SEs collide with the gas molecules in the chamber and create further electrons which are also accelerated in the electric field: a cascade or avalanche promotes amplification
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SE Amplification
Specimen
Detector
Pop
ula
tio
n
EnergyV0
E
Second Generation
First Generation
Third Generation
Second Generation
First Generation
Fourth Generation
Third Generation
Second Generation
First Generation
Swarm Energy
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• The primary electron beam impinges on the sample, leading to the production of backscattered and secondary electrons.
• The electric field between the positively biased anode and the grounded specimen stage accelerates secondary electrons towards the anode.
• Secondary electrons collide with and ionise gas molecules in their path and amplify the secondary signal.
• Positive ions drift towards the sample surface to compensate negative charge build up.
A simplified schematic diagram of gaseous signal amplification via ionisation
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0 1 2 3 4 5 6 7 8 9 10Pressure (Torr)
Ca
scad
e A
mp
lific
atio
n (
a.u
.)
General Shape of Amplification Curve
If the pressure is too high (concentration of gas molecules is large), MFP is short and significant fraction of secondary
electrons is scattered before they acquire sufficient energy to cause ionisation
If the pressure is too small (concentration of gas molecules is
small too), MFP is large and amplification events are few and the
secondary electron signal is weak
The most efficientamplification
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Signal Components
Sign
alWater
0%
20%
40%
60%
80%
100%
0 1 2 3 4 5 6 7 8 9 10Pressure (Torr)
S.E.
B.S.E.
P.E.
Helium
0%
20%
40%
60%
80%
100%
0 1 3 5 7 9 11Pressure (Torr)
Sign
al
S.E.
B.S.E.
P.E.
PE – signal due to ionisation from primary electronsBSE – signal due to ionisation from backscatter electronsSE – signal due to ionisation from secondary electrons (most desired!)
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Alternative Gases
0
50
100
150
200
250
300
0 2 4 6 8 10 12Pressure (Torr)
Re
lati
ve A
mp
lific
atio
n
H2O
CO 2
N2O
N2
He
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H2O
4 torr 8 torr6 torr
He
2 torr 5 torr 12 torr
Copper grid on Carbon
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deG
0VBPd
APe
P – pressure, V0 – anode bias, A & B - gas specific constants
d
S
d
SexpII BSEPEd
oc
Ic – amplified gaseous electron current Io – primary beam current SPE – ionisation efficiency of primary electronsSBSE – ionisation efficiency of backscatter electronsδ – secondary electron coefficientη - backscatter electron coefficientα – ionisation efficiency of the gasd – sample-anode gap
The factor α is called Townsend’s first ionisation coefficient
Signal gain G is a function of the ionisation coefficient α and the specimen-anode distance d
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0 2 4 6 8 10Pressure (torr)
Re
lati
veC
on
trib
uti
on
to T
ota
l Sig
nal
Total
S.E.
PE
BSE
Graph of signal contributions as a function of chamber gas pressure (for water vapour). The maximum total amplification occurs at slightly higher pressure than the secondary electron maximum. At high pressures, the signal is dominated by
background signals such as ionisation of gas molecules by primary electrons
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Cascade Signal Components
The cascade signal is then composed of:
Amplified SE
BSE derived signal
PE derived signal
All of the above from the “skirt region”
Detector noise
Of these, only the first is desired!
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High vacuum versus low vacuum mode
SE image of Au coated Trich made in low vacuum mode (without charging)
SE images of Au coated Trich:despite the coating, the image still shows some charging effects
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Microstructure
E-SEM with W hair-pin filamentE-SEM with Shottky FEG
Natural HAp/bioglass compositeDiatomite(a powdery mineral composed of the fossilised
skeletal remains of microscopic single-celled aquatic plants called diatoms)
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The minimum pressure that can sustain water in the liquid phase is about 4.6 Torr at 0oC.Higher temperatures require higher pressures
To maintain a sample in its natural hydrated state it is necessary to drop the temperature below room temperature,
Peltier cooling stage -25°C to +50°C
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Hydrated sample orchid petal
1.4 Torr H2Ovapor at 6oC
dehydration is obvious
7 Torr H2O vapor at 6oC
H2O environment becomes saturated
and dehydration does not occur
before 2 min. exposure after 2 min. exposure
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ESEM ‘wet’ mode
Fresh bacteria
2 µm
Oil-in-water emulsion
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Matrix ice
Interfacial ice T = -120oC P = 0.7 Torr N2
x520
Stokes, Mugnier & Clarke (2004) J Microscopy 213(Pt 3)
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Microanalysisunder low vacuum conditions
Low vacuum SEM: charge is eliminated by a gas (water, air or N2)
Two major problems :
- beam damage (heating of sample)
- beam spread (skirt effect)
Beam spread
Electrons are scattered due to collisions with gas atoms
X-ray is generated outside the probe
X-ray information comes from up to 500 micron from central spot (skirt area)
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Pressure Limiting Aperture
High pressure region
Low pressure region
H2O= H2O+ + 1 e-
Non-conductive sample
_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _
+ + + + + + + + + + + + + + + + +
Elastic scattering – Skirt formation
Beam spread :
• X-rays from the probe spot (actualinformation)
• X-rays due to atmospheric effect (gas)
• X-rays information up to 500 micron from central spot (skirt)
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Fraction of electrons remaining in central probe:
where:
σ – scattering cross section
P – pressure
R – gas constant
d – gas path length
T – temperature
Electrons in the Skirt
RTPdef /σ-=
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Elastic Cross Sections
0.01
0.1
1
1 10 100
Energy (keV)
Cro
ss S
ect
ion
(Å
2) Nitrogen
Water
Helium
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Scattering out of the Probe
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0 500 1000 1500 2000 2500
Pressure Distance (GPL) (Pa-mm)
frac
tio
n in
pro
be
Air
2 keV
30 keV
10 keV5 keV
Use as low a pressure and as short a Gas Path Length as possible!
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Influence of atomic number on primary electron mean free path λ as a function of primary beam
energy
Influence of atomic number on skirt radius rs as a function of primary beam energy
Which gas?
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Influence of atomic number on the percentage of primary electrons remaining in the focused probe as a function of primary beam energy
Helium –theoretically the best gas.However it is the most difficult gas to ionize and the small size of helium atoms makes this gas notoriously difficult to handle with a typical vacuum pump. Prolonged use of helium is definitely not recommended.
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Helium
Nitrogen
Argon
Exploring the Gas Path Length
The general trends can be seen in all cases: there is a sharp rise in the radius of the skirt as the primary beam energy decreases below about 5 keV and almost two orders of magnitude difference between radii for GPL = 1 mm compared to 15 = mm
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Exploring the Gas Path LengthWith the exception of helium, the percentage of electrons remaining in the focused probe falls sharply as the GPL increases. That brings with it a reduction in electron beam current.For argon, it would be advisable to maintain gas path length of a millimeter or two.For nitrogen and oxygen the GPL of the order a few millimeters is advisable.
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Influence of energy on elastic mean free path λ as a function of pressure for nitrogen
How much gas?
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How much gas?
Influence of atomic number on skirt radius rs as a function of pressure
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Influence of pressure on skirt radius rs for several GPLs for nitrogen
p = 100 PaRs = 2.4 μm for GPL = 1 mmrs = 26 μm for GPL = 5 mm
p = 2.8 kPars = 12.5 μm for GPL = 1 mmrs = 139 μm for GPL = 5 mm
How much gas?
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Percentage of electron remaining in the focused probe as a function of pressure and atomic
number
GPL = 2 mm, E0 = 20 keV
Percentage of electron remaining in the focused probe as a function of pressure and a range of
primary beam energy
GPL = 1 mm, nitrogen
How much gas?
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Microanalysisunder low vacuum conditions
• Low vacuum SEM: charge is eliminated by a gas (water, air or N2)
• Two major problems :
- beam damage (heating of sample)
- beam spread (skirt effect)
Beam spread
• Electrons are scattered due to collisions with gas atoms
• X-ray is generated outside the probe
• X-ray information comes from up to 500 micron from central spot (skirt area)
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X-ray Skirt
Electron beam
Precipitates
Matrix
„Skirt”
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Sample : Jadeite NaAlSi2O6
Matrix 1 : polymer
Matrix 2 : Cu/Zn block
Distance between the spot position (centre of mineral)and the Cu/Zn block is more than 500 micron
Large sample in homogeneous matrix
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High-vacuum spectrum - Jadeite 25kV
Cu and Zn peaks are not visible
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Microanalysisunder low vacuum conditions
To reduce the skirt effect:• use short gas path (a special cone attached
to pole piece)• use high acceleration voltage (25kV)• use low pressure (0.1 - 0.3 mbar)
VP gas compensated technique(with 2 spectra measured at different pressures)
developed by Wernisch and Dijkstra
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A pressure variation methodinvolves collecting spectra at two different pressures (with other parameters constant)
and uses the difference spectrum to extrapolate back to zero-scattering case.
This method assumes that the composition does not change with pressure!!!
It is only X-ray intensity that changes!
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Pressure variation method
More pressure: more X-rays from B, less from A
AB
pressure
Intensity
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Pressure variation methodTake 2 measurementsat 2 different pressures
Extrapolate the intensitiesto pressure 0
Apply matrix correction to extrapolated intensities
to get compositionpressure
Intensity
Charging
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Low-vacuum spectrum0.4 mbar 25kV
Contribution of the matrix (brass holder) is clearly visible
Low-vacuum spectrum0.8 mbar 25kV
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Results
High Vac
Low Vac results (gas compensated) are close to those of the HVanalysis.
Low Vac
(0.2 - 0.4 mbar)
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X-ray Mapping: Curing cement
Dry Wet
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Summary - Skirt Effect
Imaging: No problem; skirt adds a nearly uniform backgroundResolution is defined by central probe
X-ray analysis:quantification is difficult but possiblemapping stillz possible
Trade-offs between variables: Pressure
Working distance
Type of gas
Energy of primary electrons
Resolution
Charge control
To reduce skirt effect:use short gas path (a special
cone attached to pole piece)
use high acceleration voltage
use low pressure (0.3 - 0.4 torr)
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Hi-vac
Lo-vac
ESEM
Imaging: No problem; skirt adds a nearly uniform backgroundResolution is defined by central probe
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Charge control by Duane –Hunt limit
Electron beam energy 3 keV
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EBSD from non-conductive samples
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Orientation maps acquired from non-conductive smaple (cubic ZrO2)
50 μm 10 μm
a) C-SEM – electric charge non compensated
All Euler map
b) VP-SEM – electric charge compensated
All Euler map
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Rule of thumb: Use as low pressure and small polepiece-specimen
distance as possible!
Trade-offs between several variables:
Pressure
Working distance
Type of gas
Energy of primary electrons
Resolution
Charge control
Elastic Cross Section
Scattering out of the Probe
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0 500 1000 1500 2000 2500
Pressure Distance (Pa-mm)
frac
tio
n in
pro
be
Air
2 keV
30 keV
10 keV5 keV
0.01
0.1
1
1 10 100
Energy (keV)
Cro
ss S
ect
ion
(Å2
)
Nitrogen
Water
Helium
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PLZT as a ferroelectric ceramics reveals spontaneous polarization within the grains.
The polarization direction differs from grain to grain and depends on crystallographic orientation.
Applied electric field changes the polarization direction leading to mechanical stresses within the grains.
If the applied electric field is too strong, it can produce such large mechanical stress and corresponding strain within the grains that they can be pulled out and cracks are formed.
What happens when the charge is not compensated
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Effect of coating on diffraction pattern from NiO monocrystala) no coating, b) carbon coating, c) gold coating
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Gas inlet
Variable Pressure SEM seems to be a good solution to overcome
charging problems!
Courtesy of EDAX
Effect of coating on diffraction patter qualitya) no coating – VP-SEM, b) carbon coating, c) gold coating
Low backscatter yield of the ceramics due to low average atomic number !!!
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Effect of vacuum in SEM chamber on diffraction pattern from Pta) 0.05 Torr, b) 0.5 Torr, c) 1.0 Torr
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EBSD pattern recorded from the PLZT ceramics in FEGSEM at different pressures:a) 50 Pa, b) 70 Pa, c) 90, d) 130 Pa
FEGSEM• a huge electrical charging
due high beam current• mechanical and electron
beam drift
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In order to achieve the best electron backscatterdiffraction quality in low vacuum conditions, there aresome parameters in the SEM which need to beadjusted, mainly:• beam energy and current,• gas path length,• gas pressure,• dwell time.
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Inverse pole figure shows randomly oriented grains
91% of diffraction patterns solved!!! All Euler map
PLZT ceramicsPb1-3x/2LaxZr0.65Ti0.35O3 for x = 0.08
(denoted as PLZT 8/65/35)
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Misorientation Distribution Function (Al2O3/WC )
32
32
O]2231[]1000[
O)0101()0101(
AlWC
AlWC
32
32
O]2594[]1000[
O)0101()0101(
AlWC
AlWC
32
32
O]0110[]1000[
O)0112()0112(
AlWC
AlWC
32
32
O]1891[]12110[
O)0213()0213(
AlWC
AlWC
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Misorientation Distribution Function (Al2O3/ WC )
The crystallographic relationships correspond respectively to: 12%, 5%, 2%, 7% and 4% of the total Al2O3/WCinterphase boundary length.
0
2
4
6
8
10
12
14
1 2 3 4 5
Serie1
32
32
O]2231[]1000[
O)0101()0101(
AlWC
AlWC
32
32
O]2594[]1000[
O)0101()0101(
AlWC
AlWC
32
32
O]0110[]1000[
O)0112()0112(
AlWC
AlWC
32
32
O]1891[]12110[
O)0213()0213(
AlWC
AlWC
32
32
O]0101[]0211[
O)1000()1000(
AlWC
AlWC
% o
f th
e to
tal in
terp
ha
se b
oun
dary
len
gth
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Al2O3 (H2O pressure - 0.4 mbar) Al2O3 (pressure H2O - 1.33 mbar)
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Coarse grained Al2O3 Fine grained Al2O3
When the pressure is too low…
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Thank you for attention