making a uhv sealfizz.phys.dal.ca/~ihill/phyc_6250_files/phyc6250_2014_lect2.ppt.pdf · practical...
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![Page 1: Making a UHV sealfizz.phys.dal.ca/~ihill/Phyc_6250_files/PHYC6250_2014_Lect2.ppt.pdf · Practical Surface Analysis - Auger and X-ray Photoelectron Spectroscopy D. Briggs and M. P](https://reader034.vdocument.in/reader034/viewer/2022052013/602a7dfe943d756a1763ccfc/html5/thumbnails/1.jpg)
Making a UHV seal
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Rotary Vane Pump a) Without gas ballast a) Pump is connected to the vessel, which is already almost empty of air (70 mbar) – it must thus transport mostly vapor particles b) Pump chamber is separated from the vessel – compression begins c) Content of pump chamber is already so far compressed that the vapor condenses to form droplets – overpressure is not yet reached d) Residual air only now produces the required overpressure and opens the discharge valve, but the vapor has already condensed and the droplets are precipitated in the pump.
Fundamental of Vacuum Technology, Leybold catalogue
a b
c d
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Turbo Pump
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Fundamental of Vacuum Technology, Leybold catalogue
Ion Pump
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Finite Line Width of X-ray source …
Mg Kα1,2 x-ray energy 1253.6 eV ± 0.75 eV
Al Kα1,2 x-ray energy 1486.7 eV ± 0.85 eV
Mg Al Kα’ 4.5 eV (1%) 5.6 eV (1%) Kα3 8.4 eV (9.2%) 9.6 eV (7.8%) Kα4 10.0 eV (5.1%) 11.5 eV (3.3%)
D. Briggs and M. P. Seah “Practical Surface Analysis”
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X-ray Satellites in XPS
X-ray satellites observed in carbon 1s spectrum
D. Briggs and M. P. Seah “Practical Surface Analysis”
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Aperture Determines Region of Analysis
Aperture settings ! Large Area 4mm diameter ! Small Area:
! 100µm ! 200µm ! 350µm ! 600µm
! Angular resolved
aperture
deceleration sector
electron path
entrance slit
detector
sample
exit slit
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Pass Energy and Slit Width Determine Resolution
V
V0
entrance/exit slits:
0.5 mm 1 mm 2 mm 5 mm
detector
Pass Energy Ep =eV0 Resolution ΔE:
⎟⎟⎠
⎞⎜⎜⎝
⎛≅Δ
02RwEE p
380 375 370 365
870 875 880
Cou
nts
/ sec
Binding Energy (eV)
Kinetic Energy (eV)
Ag 3d3/2
Ag 3d5/2
R0=150mm
For 5mm slit, the analyzer resolution is ~1.5% of pass energy
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Resolution vs Count Rate
1 100.7
0.8
0.9
1
Al Kα (15kV, 26mA)
Mg Kα (15kV, 20mA)
Res
olut
ion
(ΔEm
, eV
)
Pass Energy (Ep, eV)
Slit Width = 0.5mm Slit Width = 2.0mm Slit Width = 5.0mm
0.8 1 2 4 6 8 10 20 40 60102
103
104
105
106
107
nPEI ∝
1.841.741.55
1.571.77
1.90
Slit Width = 0.5mm Slit Width = 2.0mm Slit Width = 5.0mm
Mg Kα (15kV, 20mA)
Al Kα (15kV, 26mA)C
ount
s / S
ec
Pass Energy, Ep (eV)
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BE
Metallic Samples & Analyzer Work Function
E
vac φs analyzer
work function
KE = hν – BE – φΑ
0
KE
BE
φA= 4.6V
BE Z
Sample Analyzer
Fermi Energy
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BE
Metallic Samples & Analyzer Work Function
E
vac φs
KE = hν – BE – φΑ - V
0
KE
BE
BE
V
Z
Sample Analyzer V
analyzer work function
φA= 4.6V
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BE
Insulating Samples
E
vac φs
KE = hν – BE – ?
0
KE
BE
φA
BE
V ?
Z
Sample Analyzer Charging V ?
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Ways of Reducing Charging ! Reduce insulator thickness ! Decrease resistivity (doping) ! Lower x-ray power ! Use metal grid over sample ! Evaporate Au overlayer ! Electron flood gun
Ways of Accounting for the charging ! Estimate Vs by measuring shift in the C 1s peak from
hydrocarbon contamination BE(C 1s) = 285.0 eV ± 0.2 eV ! Not valid for inhomogeneous sample
! Compare Auger and XPS peaks
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Line Width Measured by XPS ! Factors contributing to measured photoelectron line width:
! Natural line width: Lorentzian ! X-ray line width 0.75 - 0.85 eV ! Analyzer (example: Ep = 50eV, 5mm slit → 0.8eV resolution) ! Measured line-width ∆Emeasured
2 ≈ ∆Enat
2 + ∆Ex-ray2 + ∆Espec
2
! Voigt function is a more accurate account of the correlation of the natural line width with the x-ray & analyzer
! Phenomenological Gaussian-Lorentzian product more commonly used
( ) ⎟⎟⎠
⎞⎜⎜⎝
⎛
Δ
−−−
Δ+−
Δ= )2ln()(1exp
)()( 2
20
220
2
EEEM
EEEMEEf
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XPS Measurement of Overlayer Thickness
⎟⎟⎠
⎞⎜⎜⎝
⎛⎟⎟⎠
⎞⎜⎜⎝
⎛−−=
⎟⎟⎠
⎞⎜⎜⎝
⎛−=
∞
∞
θλ
θλ
cos)(exp1
cos)(exp
AA
AAA
BA
ABB
EdII
EdII
! Overlayer thickness can be determined by: ! Measuring IB as a function of angle θ ! Measuring the ratio of IB / IA
B
A
z
θ dA
Practical Surface Analysis - Auger and X-ray Photoelectron Spectroscopy D. Briggs and M. P. Seah (Editors), Wiley Interscience, 1990 (2nd ed.)
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Angular Dependent XPS
708090100110
Inte
nsity
(Arb
. Uni
ts)
Binding Energy (eV)
θ=40
708090100110
Inte
nsity
(Arb
. Uni
ts)
Binding Energy (eV)
θ=55
708090100110
Inte
nsity
(Arb
. Uni
ts)
Binding Energy (eV)
θ=70
Si
Au
z
θ dAu
708090100110
Inte
nsity
(Arb
. Uni
ts)
Binding Energy (eV)
θ=0
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Shake-up Satellites
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Siegbahn, Rev. Mod. Phys. 54, 709–728 (1982)
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Electron Scattering Effects Plasmon Loss Peak
a
A=15.3 eV
a a aAl 2s
Metal