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Contents
➢ Introduction
➢ Instrumentation
➢ Working Principle
➢ Case Study
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XPS Instrument
• The XPS is controlled by
using a computer system.
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XPS Instrument
• The instrument uses
different pump systems to
reach the goal of an Ultra
High Vacuum (UHV)
environment.
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XPS Instrument
X-Ray Source
Ion Source
SIMS Analyzer
Sample
introduction
Chamber
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Diagram of the Side View
of XPS System
X-Ray source
Ion source
Detector
SIMS
Analyz Axial Electron Gun
er
Sample
introduction
Chamber
Sample
Holder
sample
CM
A
Roughing Pump Sli
Ion Pump ts
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SCHEMATIC OF XPS
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WORKING PRINCIPLE OF X-RAY PHOTOELECTRON
SPECTROSCOPY (XPS)
• XPS technique is based on Einstein’s idea about Ejected Photoelectron
the photoelectric effect, developed around 1905
– The concept of photons was used to describe Incident X-ray
Free
the ejection of electrons from a surface when Electron
photons were impinged upon it Level
• The sample surface is irradiated with photons, Conduction Band
hitting the core electrons (e-) of the atoms Fermi
Level
• The X-Ray source produces photons with certain Valence Band
energies:
– MgK photon with an energy of 1253.6 eV 2p L2,L3
– AlK photon with an energy of 1486.6 eV
• Normally, the sample will be radiated with 2s L1
photons of a single energy (MgK or AlK),
known as a monoenergetic X-Ray beam
1s K
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WHY CORE ELECTRONS ?
Ejected Photoelectron
• An electron near the Fermi level is far from the
nucleus, moving in different directions and
does not carry information about any single Incident X-ray
atom. Free
Electron
– Fermi level is the highest energy level Level
occupied by an electron in a neutral solid
at absolute 0 temperature. Conduction Band
– Electron binding energy (BE) is calculated Fermi
with respect to the Fermi level. Level
Valence Band
• The core e-s are local close to the nucleus and
have binding energies characteristic of their
particular element. 2p L2,L3
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EQUATION
KE = hv – BE – Ø
• The equation will calculate the energy needed to get an e- out from the
surface of the solid.
KE Kinetic Energy (measure in the XPS spectrometer)
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X-RAYS ON THE SURFACE
• The X-Rays will penetrate to the core
e- of the atoms in the sample.
e- lower layer
e- top layer Outer surface
but no collisions
e- lower layer
• Some e-s are going to be released with collisions X-Rays Inner surface
without any problem giving the Kinetic
Energies (KE) characteristic of their
elements.
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X-RAYS AND THE ELECTRONS
Electron without collision X-Ray
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XPS SPECTRUM
1000 eV 0 eV
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INTERPRETING XPS SPECTRUM
# of electrons
• e- will collide with other e- from top
layers, decreasing its energy to N4
contribute to the noise, at lower kinetic
energy than the peak
N3
• The background noise increases with BE N2
because the sum of all noise is taken
from the beginning of the analysis. N1
Binding energy
Ntot= N1 + N2 + N3 + N4
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WHY DOES XPS NEED UHV?
• Ultra High Vacuum (10−9 mbar) is required
– To ensure the longest possible mean path of the photoelectrons
– To avoid the contamination of the sample surface.
• The ambient atmosphere that a sample is exposed to can change its properties.
– XPS is a surface sensitive technique
– Contaminates will produce an XPS signal and lead to incorrect analysis of the surface
of composition
– For example, at a pressure of 10-6 mbar, background gas constituents (O2, H2O, etc.)
can react with the surface of a sample in several seconds
• Removing contamination
– To remove the contamination the sample surface is bombarded with argon ions
(Ar+ = 3KeV).
– heat and oxygen can be used to remove hydrocarbons
• The XPS technique could cause damage to the surface, but it is negligible.
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THANK YOU
Any Queries?
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