The document discusses various surface spectroscopy techniques including electron spectroscopy and ion spectroscopy. Electron spectroscopy techniques covered are electron spectroscopy for chemical analysis (ESCA) and Auger electron spectroscopy (AES). Ion spectroscopy techniques discussed are secondary ion mass spectroscopy (SIMS) and ion scattering spectroscopy (ISS). The document provides details on the principles, instrumentation and applications of these surface analysis techniques.

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ELECTRO ION
SPECTROSOCPY
C r e a t e d B y
N i s h a n t C h a u d h a r i ( P R N : 1 8 2 2 2 0 7 )
H r u s h i k e s h P a t i l ( P R N : 1 7 2 1 0 1 4 )
T Y I n s t r u m e n t a t i o n ( B T E C H )
G o v e r n m e n t C o l l e g e o f E n g i n e e r i n g , J a l g a o n

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1 - S u r f a c e S p e c t r o s c o p y Te c h n i q u e s
2 - P r i n c i p l e
3 - E l e c t r o n S p e c t r o s c o p y f o r C h e m i c a l A n a l y s i s
4 - A u g e r S p e c t r o s c o p y
5 - S e c o n d a r y i o n m a s s s p e c t r o s c o p y
6 - I o n s c a t t e r i n g s p e c t r o s c o p y
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Content

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Surface Spectroscopic
Techniques
T h e s e a r e c l a s s i f i e d a s f o l l o w s
1 - E l e c t r o n S p e c t r o s c o p y
a ) E l e c t r o n I o n s p e c t r o s c o p y f o r c h e m i c a l a n a l y s i s
( E S C A )
b ) A u g e r s p e c t r o s c o p y ( A E S )
2 - I o n S p e c t r o s c o p y
a ) S e c o n d a r y - i o n m a s s s p e c t r o s c o p y ( S I M S )
b ) I o n s c a t t e r i n g s p e c t r o s c o p y ( I S S )
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Principle of Electron and Ion spectroscopy
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Electron and ion spectroscopy techniques find
application for surface analysis.
They can provide chemical information, which
the classical methods like microscopy,
reflectivity and adsorption isotherms cannot.
With electron and ion spectroscopy, one can
obtain elemental analyses either as elemental
ratio or oxidation sate ratio.

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When a beam is incident on the surface, it
penetrates to some depth within the surface
layer.
A second beam exits from the surface, which
can be analyzed by a spectrometer.
The beam may be photons, electrons and
ions.
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Electron Ion spectroscopy for chemical analysis
(ESCA)
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 Electron Ion spectroscopy for chemical analysis (ESCA), also known as x-
ray photoelectron spectroscopy (XPS) is an effective technique for detecting
the element and their bonding states on the surface of solids.
 The methods use soft X-ray to eject electrons from inner-shell orbitals.
 The kinetic energy of these photoelectron energies are dependent upon the
chemical environment of the atom, it makes XPS useful to obtain the oxide
state and ligands of an atom.
• In XPS, we are concerned with the ejection of an electron from one of the
tightly bound core or weakly bound valence shells of an atom or molecule
(usually a core level for analytical purposes, as we will see later) under the
influence of a monochromatic source of X-rays.

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Figure 1: Schematic diagram of a typical electron spectrometer
showing the necessary components. A hemispherical electrostatic electron energy analyzer is depicted.

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Auger Electron Spectroscopy (AES)
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 Other electron spectroscopic technique which is used for
the surface analysis.
 It is a analytical technique for determining the composition
of surface layer.
 It is the most common technique for surface analysis used
for determining the composition of the surface layers of the
sample.
 The characterization can be achieved up to a depth of 1nm
and smallest surface that can be characterized is a few nm
wide.
 Qualitative chemical analysis is performed by this
technique.
Fig. Block diagram of Auger Electron
spectroscope.

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Auger Electron Spectroscopy(AES)
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 The technique include three main steps:
i. Emission of photoelectron or atomic ionization.
ii. Transition of valence electron or electron emission.
iii. Emission of auger electron.
 The process has an involvement of three electrons.
 Kinetic energy of auger electron is given by,
K.E. = hv – B.E. – Work function.
 Kinetic energy can be estimated from binding energies of various levels involved.
 Auger transition is characterized primarily by,
i. Location of initial hole.
ii. Location of final hole.
 Auger electron fail to emerge with their characteristic energies if they start from deeper than 0.5 to
5nm into the surface.
 Highly sensitive for all elements for all atoms but H and He.

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Auger Electron Spectroscopy(AES)
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Auger Electron Spectroscopy(AES)
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Features Limitations
• High Resolution, spatially resolved chemical
analysis.
• Quantitative compositional analysis of surface
region specimen by comparison with standard
samples
• Highly versatile sensitive (0.1% atom) : standard
analytical tools in lab
• Stronger KLL transition in lower atomic number and
stronger MNN transition in higher atomic number
elements.
• It can’t be used to detect hydrogen and helium.
• It does not include non-destructive depth profiles.
• It requires sample to be compatible with high
vacuum.
• Non conducting samples gets charged under
electron beam bombardment and simply can’t be
analyzed.

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Auger Electron Spectroscopy(AES)
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• Instrumentation:
i. Ultra high vacuum : 10e-7 pascal or
10e-9 torr
ii. Mean free path of the electron should
be approximately 40km.
iii. Ion source: Ar+ Ions (Energy 1-5 keV)
iv. Primary Beam: focused electron beam
v. Detected: Auger electrons, Secondary
electrons
vi. Elements Detected: Li-U; Chemical
bonding information
vii. Resolution: 2 – 3 nm (Profiling mode)
viii. Detection Limits: 0.1-1% at sub-
monolayer
• Applications :
i. Surface analysis.
ii. Particle analysis.
iii. Depth profiling.
iv. Thin film composition analysis.

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Ion mass spectroscopy.
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• Technique used to analyze the composition of solid surfaces and thin film by sputtering the surface of the
specimen with a focused primary ion beam and collecting analyzing ejected secondary ions.
• This technique is used to measure up to a depth of 1 to 2nm.
• Most sensitive surface analyzing technique with elemental detection limits ranging from parts per million to
parts per billion.
• Ion mass spectroscopy is divided into two parts:
i. Secondary ion mass spectroscopy.
ii. Ion scattering spectroscopy.

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Ion mass spectroscopy.
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• An inert gas ion having kinetic energy 0.3 to 5 keV is incident on the
surface of sample.
• The ion is penetrated into the surface of the solid and cause
considerable disruption by transfer of momentum to lattice atoms or
molecules this is called sputtering.
• This results in expelling atomic and molecular fragments, these
fragments can be neutral or ions.
• These ions are referred to as secondary ions and thus termed as
secondary ion mass spectroscopy.

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