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1. Biomaterial
characterization techniuqes
(XPS , MEB)
Abu Amro Abdelrahman
UMBB-Boumerdes
Faculté de technologie
Département Ingénierie des Systèmes Electriques
Spécialité : Instrumentation Biomédicale
3/22/2024
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2. OUTLINE
 XPS Defintion
 XPS Background
 Relevant Industries for XPS Analysis
 XPS Instrument
 How Does XPS Technology Work?
 Identification of XPS Peaks
 XPS Technology
 Advantages and Disadvantages
 microscopie électronique à balayage (MEB)
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3. XPS
 X-Ray Photoelectron Spectroscopy
 ESCA: electron spectroscopy for chemical
analysis
-elemental composition
-chemical formula
-chemical/electronic state of the element
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4. Introduction
 Biomaterials play an integral role in medicine today,
restoring function and facilitating healing for people after
injury or disease. Biomaterials may be natural or synthetic
and are used in medical applications to support, enhance,
or replace damaged tissue or a biological function .

5. X-ray photoelectron
spectroscopy (XPS)
 X-ray photoelectron spectroscopy (XPS) is a surface-
sensitive quantitative spectroscopic technique based on the
photoelectric effect that can identify the elements that
exist within a material (elemental composition) or are
covering its surface, as well as their chemical state, and the
overall electronic structure and density of the electronic
states in the material.

6. XPS Background
 In 1905, Einstein, photoelectric effect
 In 1960, Dr. Siegbahn and his research group, developed the
XPS technique and produce the first commercial
monochromatic XPS
 1981, Seighbahn, noble prize
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7. Photoelectric Effecct
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Fig: photoelectric effect
Electros
knock
away
from the
surface
with
definite
hν

8. XP SPECTROMETERS
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9. 3/22/2024
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10. XPS Instrument
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X-Ray Source
Ion Source
SIMS Analyzer
Sample introduction
Chamber

11. X-ray Photoelectron Spectrometer
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5 4 . 7
X-ray
Source
Electron
Optics
Hemispherical Energy Analyzer
Position Sensitive
Detector (PSD)
Magnetic Shield
Outer Sphere
Inner Sphere
Sample
Computer
System
Analyzer Control
Multi-Channel Plate
Electron Multiplier
Resistive Anode
Encoder
Lenses for Energy
Adjustment
(Retardation)
Lenses for Analysis
Area Definition
Position Computer
Position Address
Converter

12. How Does XPS Technology Work?
 A monoenergetic x-ray beam
emits photoelectrons from the
surface of the sample.
 The x-ray photons The
penetration about a micrometer of
the sample
 The XPS spectrum contains
information only about the top 10
- 100 Ǻ of the sample.
 Ultrahigh vacuum environment to
eliminate excessive surface
contamination.
 Cylindrical Mirror Analyzer
(CMA) measures the KE of
emitted e-s.
 The spectrum plotted by the
computer from the analyzer signal.
 The binding energies can be
determined from the peak
positions and the elements present
in the sample identified. 3/22/2024
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13. Which materials are analazıed?
 XPS is routinely used to analyze inorganic
compounds,metals,semiconductors,polymers,
ceramics,etc.
 Organic chemicals are not routinely analyzed by XPS
because they are readily degraded by either the energy
of the X-rays or the heat from non-monochromatic X-
ray sources
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14. The Atom and the X-Ray
Core electrons
Valence electrons
X-Ray
Free electron
proton
neutron
electron
electron vacancy
The core electrons
respond very well to
the X-Ray energy 3/22/2024
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15. Relevant Industries for
XPS Analysis
• Aerospace
• Automotive
• Biomedical/biotechnology
• Compound Semiconductor
• Data Storage Defense
• Displays
• Electronics
• Industrial Products
• Lighting
• Pharmaceutical
• Photonics
• Polymer
• Semiconductor
• Solar Photovoltaics
• Telecommunications
Figure 4: Pharmaceutical Industry
http://www.legaljuice.com/2010/12/salesman_calls_the_
cops_after.html
Figure 5: Solar Photovoltaics
http://www.fincher.org/Misc/AlternateE
nergy.shtml

16. Applications of
X-ray Photoelectron
Spectroscopy (XPS)

17. XPS Analysis of Pigment from Mummy Artwork
150 145 140 135 130
Binding Energy (eV)
PbO2
Pb3O4
500 400 300 200 100 0
Binding Energy (eV)
O
Pb Pb
Pb
N
Ca
C
Na
Cl
XPS analysis showed
that the pigment used
on the mummy
wrapping was Pb3O4
rather than Fe2O3
Egyptian Mummy
2nd Century AD
World Heritage Museum
University of Illinois

18. Analysis of Carbon Fiber- Polymer Composit
Material by XPS
Woven carbon
fiber composite
XPS analysis identifies the functional
groups present on composite surface.
Chemical nature of fiber-polymer
interface will influence its properties.
-C-C-
-C-O
-C=O
-300 -295 -290 -285 -280
Binding energy (eV)
N(E)/E

19. Analysis of Materials for Solar Energy Collection by
XPS Depth Profiling-
The amorphous-SiC/SnO2 Interface
The profile indicates a reduction of the SnO2
occurred at the interface during deposition.
Such a reduction would effect the collector’s
efficiency.
Photo-voltaic Collector
Conductive Oxide- SnO2
p-type a-SiC
a-Si
Solar Energy
SnO2
Sn
Depth
500 496 492 488 484 480
Binding Energy, eV
Data courtesy A. Nurrudin and J. Abelson, University of Illinois

21. microscopie électronique à
balayage (MEB)
 A scanning electron microscope (SEM) is a type of
electron microscope that produces images of a
sample by scanning the surface with a focused beam
of electrons. The electrons interact with atoms in the
sample, producing various signals that contain
information about the surface topography and
composition of the sample

22. SEM: background
 A SEM is a microscope that works
with electrons instead of photons
(optical microscope)
 The smaller wavelength of electrons
compared with photons allows to go
to higher resolutions

23. SEM: background
 Beam of electrons impact the
sample:
 A detector processes the outgoing
electrons and produces images
from them.
 Two types of outgoing electrons:
 Backscattered: (inelastic scattering
with the atoms). Z contrast
 Secondary electrons (elastic scattering
with the atoms). Topographic
contrast

24. INDEX
 Description of the technique
 Applications

25. Applications: FAAM BAe 146
inlet
To the filter
Sub-isokinetic
sampling
Bent
Inertial removing
of droplets (can be
kept off or on
through a bypass)
Theoretical calculations done by S. T. Parker and J.
Trembath
• Sub-isokinetic sampling: leads to an enhancement of
large aerosol particles
• Bent: adds a inertial cut-off for large aerosol particles
• Bypass: modifies the flow (less sub-isokinetic
sampling when it is on, therefore smaller
enhancement of large aerosol)
2 inlets

26. Applications: Mineral dust size
distribution
 Difficult to quantify the amount of mineral
dust in the atmosphere
 Large differences on dust evolution among
models
 Dust is one of the most efficient ice-
nucleating materials
 Single particle analysis SEM technique:
 Allows to estimate the size, number, surface
mass of atmospheric dust.
www.bsc.es

27. Conclusions
- X-ray Photoelectron Spectroscopy (XPS) and Microscopy Electron
Microscopy (MEB) serve as powerful allies in biomaterial analysis.
While XPS reveals surface chemical composition and bonding,
MEB offers detailed structural insights at microscopic scales.
Together, these techniques provide a comprehensive
understanding crucial for tailoring biomaterials in various fields like
medicine and biotechnology.

28. Thank you very much
Any Questions
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