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Lecture I: Familiarization with XPS method and technique

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DOI: 10.13140/2.1.3354.9760

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Familirization with XPS
method and technique

by Dr. Dmitry A. Zatsepin*

Institute of Physics PAS, Al. Lotników 32/46

PL-02-668 Warsaw, POLAND

*on temporary leave from Institute of Metal Physics – Russian Academy of Sciences,
Laboratory of X-
X-ray Spectroscopy, S.Kovalevskoj Str. 18, 620990 Yekaterinburg

Sci.
Sci. Ed. made by Prof. Dr. Kurmaev E.Z., Russian Academy of Sciences
Sciences – Institute of Metal
Physics

Useful comments: Prof.Dr.

Prof.Dr. Krystyna Jablonska (IP-
(IP- PAS, Poland)
Poland) and Dr. Rolf Berger (Uppsala
Univ.,
Univ., Sweden)

Warsaw © 2014
 The scope :

1.What is inside XPS physics ? (the

description of physical phenomena used in
XPS)

2.Why X-ray Photoelectron

Spectroscopy ? (a brief review of XPS
method features)

3.XPS Instrumentation (Main parts and

XPS tricks for XPS beginners)
Part 1. What is inside XPS physics ?
1-1. What is inside XPS physics ?

 UPS-XPS-AES,
AES LEED and LEELS –
are the material science techniques
which belong to the Electron
Spectroscopy techniques →
electrons are carrying the information
about the material under study ;

 XPS is a technique that is using a

soft-x-rays in the range of about 150 –
2000 eV in order to examine solids ;

 Most important XPS-probe

characteristic: spatial and depth
resolution (depends on Spectrometer
construction)
 1-2. What is inside XPS physics ?

XPS Spatial and Depth resolution according to ThermoFisher Scientific Data

(reproduced from ThermoFisher Web Site © ThermoFisher Scientific)
 1-3. What is inside XPS physics ?

”Underwater rocks” in XPS :

 A lot of side-effects occur

while the sample is excited by
primary X-ray beam under XPS
study → strongly affect the
spectrometer resolution and
signal-to-noise ratio ;

 Auger side-process becomes a

problem in some cases due to ”
side-overlapping with some
XPS lines → the need to use Z n O :[ M n , C o ] 1 0
17
cm
-2
XPS: M n 2p
another X-ray source (i.e. Mg M n O (re fe re n c e )
Kα instead of Al Kα)

Normalized intensity (arb. units)

2 p 3 /2

 X-ray overheating of the Zn LM M

sample → XPS signal drop-
out
2 p 1 /2

The spectra were obtained by author at

ULVAC-
ULVAC-PHI XPS Versaprobe 500
630 640 650 660
B in d in g e n e r g y ( e V )
 1-4. What is inside XPS physics ?

Three-
Three-step XPS process model:
Based on numeric calculations made
by Scofield (ionization cross-
cross-sections
are in the frame of Hartree-
Hartree-Slater
approach).
approach).

In the frame of this model, the XPS

intencity at a normal incidence is:
where  tot  
nl
nl

because when more than one orbital is excited, then σtot is just the summation of partial
cross-sections σnl
photoionization cross-
Actually, an ionization cross-
cross-section σ is the probability per unit area and per unit time that a
photon of a given energy can be absorbed by an atom to excite the the photoelectrons.
P (h ) here P – are the absorbed photons per unit time and I – are the incident
 (h )  photons
I (h )
Gelius molecular orbital rule (by K.M.Ziegbahn and Geliuos) : the cross-sections for MO are
influenced by the nature of atomic orbital, from which this MO is „selected”.
 1-5. What is inside XPS physics ?
XPS process
 Ebinding = Ephoton – Ekinetic – Φ,
where Φ is a work-
work-function of XPS spectrometer
(usually this correction is made at the factory and
used automatically, the value of Φ is in the range of
2 - 5 eV and varies for different type of XPS
systems ) ;
E binding < E photon (XPS excitation rule)

 Binding Energies (BE) usually are measured with

respect to Fermi-
Fermi-level rather than to the level of
free electron (”
(”Vacuum”
Vacuum” level) – zero point for
the energy scale calibration of XPS
spectrometer : Φ = EF – EV ;

 Thus only Ekinetic value is measured directly in

order to detect Ebinding , because Ephoton and Φ are
known
 1-6. What is inside XPS physics ?
Particular values of work-function for different materials (according to recommendations
of Advanced Photonics Laboratory © 2004, Chang Gung University)

Physical meaning: it is a potential ”barrier” for electron emission

(Note: in the most modern XPS spectrometers it is selected automatically by Central
XPS Data Processing Unit while the test-spectrum acquiring is performed before ”clean”
measurements)
 1-7. What is inside XPS physics ?
XPS spectra – why Auger appears ?

 Core-lines: of relativevly narrow shape,

results from 1s (K-shell), 2s (L1-shell), 2p
(L2,3-shell).
 Valence-band: much broader, usually
represents the total DOS near the Fermi
level energy region
Some of their spectral parameters (but
(but not the BE
position)
position) are affected by the X-
X-ray source energy !

 Auger-
Auger- lines:
lines: Kinetic enegy of electron does not
affected by the incident x-ray photon energy – it is a
”fingerprint”
fingerprint” of a concrete part of electronic structure of
material under study.
However,
However, the energy positions of Auger peaks in the
BE scale depend on incident x-ray photon energy
due to simultaneous coulombic re- re-arrangement of
electrons in the final state →

→ we can avoid Auger overlapping with XPS peaks

by CHANGING THE X-
X-RAY SOURCE TYPE !
 1-8. What is inside XPS physics ?

How it looks actually:

An example of XPS Survey
recordered under different
X-ray excitation sources –
Al Kα and Mg Kα.

Recorded at ThermoFisher XPS

EscaLab 250 Xi by ThermoFisher
analytical scientists © 2010
 1-9. What is inside XPS physics ?
XPS spectra – why chemical shift appears ?

Thus, for compounds with the dissimilar bonding majority the XPS peak position will
be also different → ”fingerprint” of chemical bonding type
Example : XPS Si 2p peak in ”pure”
pure” Si waffer BE = 99 eV, but (sic!)
XPS Si 2p peak in SiO2 BE = 102.3 eV
 1-10. What is inside XPS physics ?
XPS spectra – any other reasons for chemical shift ?
 1-11. What is inside XPS physics ?
Why we obtain sometimes single XPS peak and in other - double XPS peaks ?
 1-12. What is inside XPS physics ?
XPS satellites – what for they are ?

Arise when a core-electron is removed by a

photoionization (a sudden change in the
effective charge due to the loss of
screening electrons). This perturbation
induces a transition, in which, an electron
from a bonding orbital can be transferred to
an anti-bonding orbital simultaneously with
core-ionization).

 So, the major reason – relaxation in the final state and the loss of screening effect of the
core-
core-level

XPS Cu 2p were obtained by V.R.Galakhov in cooperation with the group of Prof. Manfred Neuman, © 1996,
University of Osnabrueck, Germany, using PHI XPS Mutitechnique 5600ci
1-13. What is inside XPS physics ?
XPS satellites – energy-level scheme
 1-14. What is inside XPS physics ?

Electron scattering effects in XPS:

 Can be recognized in XPS spectra ;

 Occur as a result of XPS electrons

interaction with the electron subsystem of
the material under study (collective
excitations) → electron transitions and
energy loss takes place → one can
observe discrete energy loss peaks or
plasmon peaks (PP) (can be of extrinsic
nature – the responce of the electronic
subsystem of material on the photoelectric
effect and of intinsic origin – screening
effect responce on the core-
core-hole creation);
creation);

 Mostly occur in „pure”

pure” surface materials →
why not to use as an additional criteria
of material characterization ???

The presented as an example XPS spectrum was obtained by Lois Scudiero © 2010,
Washington State University, USA
Part 2. Why X-ray Photoelectron Spectroscopy ?
 2-1. Why X-ray Photoelectron Spectroscopy (XPS) ?
Comparing with the other experimental methods, an XPS also has both ”Pro” and
”Contra” features. WHAT ARE THEY ?
The majority of XPS advantages:
 Relatively non-
non-destructive method of sample characterization (sample nature and
x-ray tube operation mode have to be taken into account) ;

 Covering by direct study all the elements from Periodic Table except H and He (in
some cases the indirect XPS study is possible) ;

 Usual probing depth range is from 4 nm up to 10 nm (standard portable Al Kα and Mg

Kα X-ray sources) and in extended mode up to 20 nm (portable Zr Lα and ….. X-ray
sources) → surface and ”near surface” layers sensitive technique ;

 Element traces analysis – concentration sensitivity limit at about 1% of atomic

fraction (guaranteed sencitivity – if lower, then additional XPS technique is needed);
needed

 Direct chemichal bonding information (core-

core-levels & Valence Band)
Band) in the case of
qualification of multi-
multi-component compounds – i.e. triple-components or more ;

 Qualitative and quantitative analysis as well as strong theory support

support for XPS-
XPS-data
interpretation (both by ”hand-made” interpretation and with special software).
 2-2. Why X-ray Photoelectron Spectroscopy (XPS) ?
The most common XPS disadvantages:
Hi-vacuum system is needed (usually up to 10-8 Pa in the ”Idle Mode” and not
worth than 10-6 Pa in the ”Measuring Mode” of XPS-spectrometer) → no stable hi-
hi-
vacuum = no precise XPS experiment (1st XPS rule);
rule)

Strong local charging of the insulating wide-gap materials under study → energy
calibration and correct XPS data processing and interpretation could be a problem →
no proper charge neutralizing = no precise XPS experiment (2nd XPS rule); rule)

Relatively complicated sample preparation for precise XPS study (the removing of
gaseous fractures, cleaving in vacuum, ion-gun sputtering, the use of vacuum-
transfer-vessel, …. ) → improper sample manipulation = no precise XPS
experiment (3nd XPS rule);
rule)

As result – XPS systems are complicated to operate them correctly and costly
(~ 800 000 USD per the basis XPS configuration) and needs a hi-qualified training as
well as strong education background.

But, anyway, it is really poweful experimental tool for material

science !
 2-3. Why X-ray Photoelectron Spectroscopy (XPS) ?

The possibilities of XPS (ESCA) analysis in comparance

with other experimental techniques.
(according to the data of Advanced Photonic Laboratory, Chang Gung
Gung University © 2004)
 2-4. Why X-ray Photoelectron Spectroscopy (XPS) ?

The standard X-ray sources that are applied in XPS material science are :

Al Kα = 1486.6 eV (0.85 eV line-width) and Mg Kα = 1253.6 eV (0.7 eV

line-width) which are more or less enough for the common XPS tasks
because of their relatively narrow line-width, but additional X-ray
sources can be used for some particular and special XPS study:
Zr Lα = 2042.4 eV (1.7 eV),
eV) Ti Kα = 4510 eV (2.0 eV),
eV) Cr Kα = 5417 eV (2.1 eV),
eV)
Cu Kα = 8048 eV (2.8 eV)

Note: It is the need to use monochromator in order to filter out the n earest satellites-
lines as well as so-called Bremsstrahlung Isochromat (continious radiation) and, as
a result, to obtain the ”clean excitation line”.

Also He (I) = 21.2 eV ( ~ 1.8 meV, the so-called ”neutral” He-line) and He (II) =
40.8 eV( ~ 2 meV, ”singly ionised” He-line) are used for XPS-UPS study.

 The use of different X-ray sources definitely extends the range of XPS application
 2-5. Why X-ray Photoelectron Spectroscopy (XPS) ?

350000
ZnO (reference)
17 -2
XPS: Survey
ZnO:(Mn,Co) (10 cm )
What tasks can be solved by 300000
Zn 2p
XPS technique

Intensity [Arbitrary Units]

in material science : 250000
O1s
LMM
200000
1. Element analysis in a simple
form via XPS Survey LMM Zn 3p
Spectrum (element 150000 C1s Zn 3s Zn 3d

identification in material, the

presence of contaminations, 100000
oxidation, …..)
Co 2p Mn 2p
50000

0
1100 1000 900 800 700 600 500 400 300 200 100 0
Binding Energy [eV]

An example of XPS Survey recorded by author at Ulvac-PHI XPS Versaprobe 500

 2-6. Why X-ray Photoelectron Spectroscopy (XPS) ?

17 -2
ZnO:(Mn,Co) (10 cm ) XPS: Co 2p
CoO (reference)
Co3O4 (reference)
What tasks can be solved by
2p3/2
XPS technique in material

Intensity [Arbitrary Units]

science:

2p1/2
2. The information about chemical
bonding nature in the surface
and near surface region (via
chemical shifts of core-level
spectra and XPS satellites
shape transformation)

770 775 780 785 790 795 800 805 810

Binding Energy [eV]

An example of XPS Co 2p core-level recorded by author at Ulvac-PHI XPS Versaprobe 500

 2-7. Why X-ray Photoelectron Spectroscopy (XPS) ?

What tasks can be solved by

XPS technique in
material science :

3. The classification of Valence

Band nature as well as the
considerations about origin
and hybridization between
partial densities of states
near Fermi level → XPS VB
Overlay Mapping method.

XPS VB Overlay Mapping method - obtained by author at ThermoFisher XPS EscaLab 250 Xi
 2-8. Why X-ray Photoelectron Spectroscopy (XPS) ?

What tasks can be solved by

XPS technique in material
science :

4. To control the sampling depth

by changing the emission angle
and qualification of contribution
for different components at
different probing depth → Angle
Resolved X-ray Photoelectron
Spectroscopy (ARXPS
technique) of thin films

ARXPS example of Ti/SiO2 interface, reproduced after N.Benito, C.Palasio © University of

Madrid, Spain, 2014, recorded at SPECS Phobios XPS 100MDC-5
 2-9. Why X-ray Photoelectron Spectroscopy (XPS) ?

What tasks can be solved by

XPS technique in material science :

5. To study the appearance and origin of

Metal-Insulator-Transition (MIT) → Hi-
Resolution Photoelectron
Spectroscopy near Fermi level
under different temperatures and He I
– He II excitation sources (UPS-XPS
technique)

Hi-resolution XPS-UPS example of MIT appearance in Valence Band of CuIr2S4,

obtained in cooperation with J.Matsuno, T.Misokawa, A. Fujimori et al. © 1998
University of Tokyo, Russian Academy of Sciences and Muroran Institute of
Technology (Japan). Spectra were recorded with PHI XPS Multitechnique 5600 ci
system.
 2-10. Why X-ray Photoelectron Spectroscopy (XPS) ?

What tasks can be solved by

XPS technique in material science:

6. To study the appearance and

origin of mid-gap-states in
functionalized materials → Hi-
Resolution Photoelectron
Spectroscopy near Fermi level
under convenient excitation and
temperatures (Hi-ResXPS
technique)

Hi-ResXPS technique for ZnO:Fe system recorded by author at Ulvac-PHI XPS

Versaprobe 500
 2-11. Why X-ray Photoelectron Spectroscopy (XPS) ?
What tasks can be solved by XPS technique in material science:

7. Micro-area XPS-imaging material analysis → microXPS imaging,

chemical state mapping and micro-area XPS technique)

The data obtained at Ulvac-PHI XPS Versaprobe 500 by ULAVC-PHI analytical

scientists © 2009, ULVAC-PHI USA, Inc.
 2-12. Why X-ray Photoelectron Spectroscopy (XPS) ?

What tasks can be solved by XPS technique in material science:

8. XPS sputtering and depth profiling

Attention, sample destructive method !!!

The data reproduced from ThermoFisher web-site as an example © ThermoFisher Inc.

 2-13. Why X-ray Photoelectron Spectroscopy (XPS) ?
What tasks can be solved by XPS technique in material science:

9. XPS analysis by cleaving sample ”in situ”

situ” or diamond funneling (presented at figure)
(XPS simple cross-section and hemisphere cross-section analysis)

Attention, sample destructive method !!!

Schematic figure of diamond-funneled hemispherical crater after drilling

 2-14. Why X-ray Photoelectron Spectroscopy (XPS) ?

What other tasks can be solved by XPS technique in material science:

10. Sample XPS pre-experiment procedures allow to perform ”clean”

experiment:

• Vacuum cleaning of the sample in the Intro Chamber → allows to avoid

accidental surface absorption and touch-prints contaminations for solids ;
• Vacuum-transfer-vessel allow to study ”just” sintered samples or samples that
are not suitable to face with the atmosphere → extends the range of the
samples under study ;
• Most modern XPS systems have automatic temperature stabilizing systems
for sample-holders during XPS experiment → stable photoelectron emission
from the sample even under High-Power modes (HP) of X-ray spot and, thus,
no distortion of the signal occurs (HP mode = more than 300-350 Watts,
actual application of HP value depends on the sample nature !) ;
• Magnetic shielding to compensate magnetic influence and magnetic
deviations while obtaining XPS data.
 2-15. Why X-ray Photoelectron Spectroscopy (XPS) ?

 So argumentally it was shown the power of XPS technique possibilites

offered for material science. Please, note, that the XPS systems are in
permanent further development and upgrading process of their construction,
prescision, durability and spectroscopy features. Thus, we can say that the
story only had started …..

All the XPS users and material scientists should be

very pleased for the appearing and development of
XPS method to Prof. Kai M. B. Siegbahn, who got
the Nobel Prize in Physics in the Year of 1981 for the
valuable contribution to the development of electron
spectroscopy (was born in 1918, died in 2007).
 2-16. Why X-ray Photoelectron Spectroscopy (XPS) ?

What about XPS-UPS technique ???

Here we should mention the

contribution of Dr. David Warren
Turner – the so-called ”Sir Siegbahn”
of ultraviolet-photoelectron
spectroscopy technique (UPS),
discovered at Imperial College,
London, Great Britain, 1962. In the
Year of 1973 he was elected for a
Fellow of Royal Society of Great
Britain.
2-17. Why X-ray Photoelectron Spectroscopy (XPS) ?

Some history: the pictures of XPS zero

generation systems, hand-made in Russian
Academy of Sciences – Siberian Division,
1970 (left) and in Research Laboratory of
Kratos Inc. - SHIMADZU Group, 1969 (right)
 2-18. Why X-ray Photoelectron Spectroscopy (XPS) ?
Some modern XPS systems: ThermoFisher XPS ESCALAB 250 Xi (the model
model of 2010,
left), ULVAC-
ULVAC-PHI XPS VersaPROBE 500 (known as VersaProbe I, the model of 2011,
2011,
center) and SPECS XPS (2009, right)

Please, note the different type of hemispherical analyser positions:

positions: vertical, under some
angle,
angle, and horisontal – affects overall specifications value of XPS system (signal-
(signal-to-
to-
noise ratio, CPS value, ….. under other equal conditions.

The photos are reproduced from official User Operating Manuals, supported by
appropriate manufacturing companies © (2010)ThermoFisher Scientific,
© (2011) ULVAC-PHI, and © (2009) SPECS Inc. – from left to the right
Part 3. XPS Instrumentation
 3-1. XPS Instrumentation – Main Parts

Typical X-ray photoelectron spectromemter - simplified scheme

Based on ThermoFisher Scientific XPS EscaLab 250 Xi © 2010 ThermoFisher Scientific

 3-2. XPS Instrumentation – Main Parts
Typical X-ray Source Scheme for photoelectron spectromemter

• XPS tricks for the X-ray Source:

 Stable vacuum
 Stable coolant flow
 At least 10 min. of idle-cycle before XPS
 Stable filament current and accelerating
voltage
 Avoid long-time previously used e--target
zone
 Always use the most possible „soft”
source power mode for X-rays

 Stable X-
X-ray Source = Precise XPS Data
 3-3. XPS Instrumentation – Main Parts
X-ray Source Monochromator

Different types of monochromators : Czerny-

Czerny-Turner type
(plane multilayers) and Rowland type (curved
multilayers).
multilayers). The latter can be build using different X-
X-ray
„focusing”
focusing” schemes. Hi- Hi-End XPS systems have
adjustable dispersers or multiplying dispersers for
obtaining high-
high-brilliance X-
X-ray Source.

XPS tricks for the X-

X-ray Monochromator :
 Avoid X-X-ray Source intencity decrease or/and distortion due to improper monochromatization while
using different X-
X-ray sources (Al, Mg, Zr, . . . )

 Perfect X-ray Source Monochromatization = Precise XPS Data !

 3-4. XPS Instrumentation – Main Parts
Hemispherical Energy Analyser – main idea

There two principally different types of Energy

Analysers in electron spectroscopy : hemispherical
(HA-
(HA-type) and cylindrical (CA-
(CA-type) energy analyser.
Actually for XPS the HA-
HA-type is used, because of
adequate brilliance within the different electron energy
range, no BE position distortion (high-
(high-prescision),
possibility to made ARXPS.

XPS tricks for the hemispherical Energy Analyser :

 The lower pass energy E0 – usually the better resolution of XPS, but improper values
of pass energy and input-
input-output slits result in spectrum shape distortion
 Made test XPS recording for well-
well-known material and verify the obtained spectral
parameters with published data

 Accurate Manipulation with Energy Analyser settings and XPS DATA verification = Precise XPS Data !
 3-5. XPS Instrumentation – Main Parts
Hemispherical Energy Analyser – how it is inside XPS system ?
 3-6. XPS Instrumentation – Main Parts
Cylindrical Energy Analyser – main idea

XPS tricks for the Cylindrical Energy

Analyser :
 Pass energy – the same trick as for
HA systems
 Acceptance and Entrance Angles
add one more additional limitation to
XPS with CMA: no ARPS is possible 
Highly suitable to collect Auger data

 Correct choise of Energy Analysing System = Extended possibilities for XPS !

 3-7. XPS Instrumentation – Main Parts
Energy Analysers – example of Pass Energy Influence
 3-8. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – XPS Signal Intensity (theory)
 3-9. XPS Instrumentation – Main Parts
XPS Data Acquisition – XPS Signal Attenuation Effect
Dual type of XPS electron release from the sample:
sample: X-Ray Flux
Interacting electrons
„clean”
clean” (without collisions) – actual XPS data ;
interacted with energy loss – XPS background.
background „Clean”
Clean” electrons

Interactions are elastic and inelastic → attenuation → IFMP curve

XPS tricks :

 Better to record spectrum under X-

X-ray LPM (i.e
(i.e.. 50 W instead of 200 W), but to collect XPS data from
multiple points of the surface sample with summation,
summation, than to use only 1 XPS scan under HPM
 ALWAYS use Background Removal Software to remove inelastic contribution from XPS Data
 Correct XPS Data Acquisition = Precise XPS Data !
 3-10. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – Multipoint Aquizition

e- top layer e- lower layer Outer surface

but no collisions
e- lower layer X-Rays Inner surface
with collisions

Atoms layers

XPS tricks :

 Multipoint and relatively not high PM of X-

X-ray Source Modes allow also to control the
homogeneity of the sample under strudy
 Multiple experimental data selection ALWAYS reduce experimental error contribution

 XPS Data Collecting = Precise XPS Data !

 3-11. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – Charge Neutralization with a Flood Gun
XPS tricks for Charge Neutralization :

 Try to reduce the actual acquisition time for

wide-
wide-gap insulators as well as the Power
Mode of X-X-ray source, the longer acquisition
and higher Power of the X- X-ray Source – the
stronger surface charge ;
 Better to apply short time-
time-range but
multipoint XPS Data collection way instead of
X-ray HP Mode and short time-
time-range
acquisition → avoidance of Neutralizer Limit
(depends on Neutralizer model)
 Always made 10- 10-15 min. Idle Cycle for
Charge Neutralizing Unit before XPS
acquisition → stable charge compensation
parameters
 Always control FWHM of the XPS
obtained (especially for core-
core-level XPS)
XPS) →
FWHM broadening may be a signature of
improper neutralizing mode
 Sometimes it is possible to apply Carbon or
Gold spray onto the frame of the wide-
wide-gap
insulator sample for stable charge leaking

 Correct Charge Compensation = Precise Chemical-shift XPS Data !

 3-12. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – Flood Gun types

1. Steady-
Steady-state One-
One-channel and Dual-
Dual-channel Charge Compensators (no dynamic charge-
charge-neutralising)
neutralising)

2. Dynamic Charge Compensators (the value of surface-

surface-charge is the time-
time-range controlled and automatically
compensated by dinamically varying the electon flux density, electron energy, …. of the flood gun)
gun)
 3-13. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – XPS FWHM dependence on DATA accumulation
The higher CPS – the better ???

XPS tricks for DATA Accumulation (! hardware limits !) :

 Avoid the saturation limit of XPS DATA Acquisition Unit, it is different

different for particular X-
X-ray Spot Size and is
individual for each XPS system ;
 Wanna get higher CPS ? Just do the multipoint XPS and made spectra summation

 Using Linear-
Linear-range of Data Acquisition Unit Specifications = Precise XPS Data !
3-14. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – ARXPS (theory)
 3-15. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – ARXPS

XPS tricks for ARXPS :

 Take an additional care for sample preparation and mounting on
sample-holder for ARXPS → possibility for shift-skewness for the
”zero-point” of normal Take-off angle → distorted XPS Data
dependence on Take-off Angle
 3-16. XPS Instrumentation – Main Parts
XPS Data Acquisition Unit – Core-level and VB Calibration Algorithm
 3-17. XPS Instrumentation – Main Parts
XPS Sample Manipulation Unit – Sample holder and Intro-Chamber

XPS tricks :

 Control the sample mounting onto the sample-holder before placing it into the Intro Chamber ;

 In some cases the cleaning with 99% purity alkohol can be applied before installing sample for
TMP-pumping ;

 Leave the sample at least 12 hours in the Intro Chamber under TMP-pumping for gaseous fraction
removing → stable hi-vacuum in the Main Vacuum Chamber Unit during measurement ;

 Avoid studying powder-fraction samples if no Powder Trap System → use pressed pellets instead

 Proper sample preparation and mounting = Precise XPS Data !

 3-18. XPS Instrumentation – Main Parts
XPS Media Support Unit – Hi-
Hi-Vacuum System

• Hi-
Hi-Vac Systems widely used for XPS:
XPS
1. ion-
ion-getter pumps with automatic „cut-
cut-off”
off” system (IGP
IGP type + IGP controller);
controller
2. titanium sublimation pumps with automatic „cut-cut-off”
off” system (TSP
TSP type + TSP controller);
controller
3. Titan TM ion-getter pumps with automatic „cut-
cut-off”
off” system (TGP
TGP type + IGP controller);
controller
4. Combined TSP-IGP pumps
Most importatnt charachteristics of a Hi-
Hi-Vac Pump:
Pump

1. Pumping speed ;
2. Saturation effect for absorbing plates ;
3. Pumping stability ;
4. Starting and Drop-
Drop-down pressures ;
5. Bakeability ;
6. Contamination influence on above mentioned characteristics.
Additional information about XPS Pumping systems can be obtained at www.vacom-
www.vacom-vacuum.com
 3-19. XPS Instrumentation – Main Parts
XPS specifications

Comparance made by Advanced Photonics Laboratory © 2004, Chang Gung University

Part 4. UPS Technique
 4-1. UPS Technique – Main Parts
UPS Data Acquisition Unit – UPS
Relatively small UPS spot-
spot-size:
size: < 1mm; High- flux: ~ 1.5 x 1012 phs/sec
High-photon flux: phs/sec

High-
High-Voltage plasma ignition system
 4-2. UPS Technique – Main Parts
UPS Data Acquisition Unit – UPS theory
 4-3. UPS Technique – Main Parts
UPS Data Acquisition Unit – UPS examples
 The author would like to acknowledge the following persons, who made
an essential contribution to the field of X-ray Photoelectron
Spectroscopy and with whom it was a great honour to collaborate:
• Academician Vladimir I. Nefedov, Russian Academy of Sciences, Russia

• Prof. Dr. Ernst Z. Kurmaev, Russian Academy of Sciences - Ural Division, Russia

• Prof. Dr. Atsushi Fujimori, Tokyo University, Japan

• Prof. Dr. Koichi Kitazawa, The Graduate School of Science, Tokyo (now the Executive Director of the Japan
Science and Technology Agency, Japan)

• Prof. Dr. Vladimir I. Anisimov, Russian Academy of Sciences - Ural Division, Russia

• Prof. Manfred Neumann, University of Osnabrueck, Germany

• Dr. Vadim R. Galakhov, Russian Academy of Sciences - Ural Division, Russia

• Prof. Dr. Joseph E. Nordgren, University of Uppsala, Sweden

• Dr. Rolf Berger, University of Uppsala, Sweden

• Prof. Dr. Hans-J. Fitting, University of Rostok, Germany

• Dr. Wolfgang Betz, ULVAC-PHI Inc., USA

 Thanks a lot to all of them and to the others for their dedicated work in the field
of XPS science and to You, for Your attention and patience!

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