STKK 6104 Laboratory Skill

Practices
Ions Scattering

Spectroscopy (ISS)
Norfarhana Abdul Samad
Nur Khairul Nabila
Kamarudin
Mohd Razali Shamsuddin
Serawati Jafirin
Siti Zarina Zakwan

P59341
P59342
P61352
P62181
P62981

General
Principles

a) Classical binary collisions

In a first approximation, ion
scattering can be described by
elastic binary hard-sphere
collisions

Due to the law of conservation

of
energy and momentum one
obtains the following relations
for the scattered atom (E1) and
2
the recoiled atom (E
):
m cos m 2 2 m 2 sin 2
1
2
1
1
E1 E0 1

m1 m2

4m1m2 cos 2 2
E 2 E0
(m1 m2 ) 2

In the case of 90 or 180 scattering detection the equation for E1

2
simplifies to:
m2 m1

m
2
1
E1 E0

E
1
0
m m
m2 m1
2
1
180:
90:

Shadowing and
blocking

When a parallel ion beam impinges

on a target atom, the trajectories
are bent due to the repulsive
forces, leading to so called shadow
cones. These cones depend on the
primary energy and the electronic
charge of the involved particles
2 There is a critical angle c
above which the scattered
projectile can hit a second
atom.

An additional phenomenon of 3
shadowing is the blocking. A
blocking cone is formed behind
blocking atoms.

This blocking can be nicely seen

in the experiment,
e.g. backscattering of 150 keV
protons from a W(100) crystal

Channeling
When an ion beam is aligned along a high
symmetry of a single crystal, most of the ions can
penetrate deep into the crystal (thousands of ).
This is due to the fact that the shadow cones are
small for high energetic and light ions (e.g. 1MeV
He+).
During their way through the crystal electronic
interaction leads to a continuous energy loss:
electronic stopping power. For 1 MeV He+ in Si it
is Sputtering
about 60 eV per monolayer.
Impinging ions may produce a number of
recoiling atoms and in form of a cascade process
some sample atoms may be ejected from the
surfaces: sputtering

Sputter yield
The number of sputtered atoms
per impinging ions depends on the
primary energy, the mass of the
ions and the target atoms and the
angle of incidence.
The maximum yield is at about 30
keV.
At higher energies ion implantation
is prevalent.
The sputter yield also increases
The application
with increasing
angle of sputtering is manifold:
a) Detection and identification of ions in the SIMS
technique
b) Combined sputtering and surface analysis by AES or XPS
for depth profiling
c) Sputtering for thin film production
d) Sputtering for surface etching

Ion Scattering
Spectroscopies
LEIS

(Low Energy Ion Scattering) spectroscopy is

referred to primary energies in the range of 100 eV to
10k eV.

Medium

Energy Ion Scattering (MEIS) to a range from

100 to 200k eV.

High

Energy Ion Scattering (HEIS) to energies between

1 and several MeV.

HEIS

technique is best known as Rutherford

Backscattering Spectroscopy (RBS).

Low-energy ion
scattering (LEIS)

Low-energy ion scattering (LEIS)

is an analytical tool that provides
information on the atomic
composition of the outer surface,
when noble gas ions are used as
projectiles.
quantitative composition analysis
is currently done on a huge
variety of materials, including
catalysts and organic materials.
LEIS (Low Energy Ion Scattering)
spectroscopy is referred to
primary energies in the range of
100 eV to 10 keV
Often the LEIS technique is called
Ion Scattering Spectroscopy (ISS)

Instrumentation

LEIS is based on simple

principles: the laws of
mechanics. The surface
under investigation is
targeted by light noble
gas ions (often He+).
When
such
an
ion
collides with a surface
atom, momentum and
energy are transferred,
depending on the mass
of the surface atom and
the collision angle.

The light ion is scattered

backwards with a
high energy after a collision with
a heavy surface atom and with a
low energy after a collision with a
light atom.
By measuring the energy of the
backscattered ions in an energy
spectrum while keeping the angle
fixed the mass of the surface
atoms can be determined and this
leads to the elucidation of the
atomic composition of the
surface.

Figure 3 shows an example of an application of LEIS

in catalysis. It shows how platinum in an automotive
exhaust catalyst is covered with coke during use.
This deteriorates the performance of the catalyst.
The coke can be removed in a regeneration step and
the platinum is
available for the reaction.

Medium Energy Ion Scattering (MEIS)

E0= 100 keV -200 keV
MEIS more surface sensitive and more complex
instrument
High depth resolution of the atomic composition in MEIS
is useful for studies of all solids
1) crystalline,
2) nanocrystalline
3) semiconducting
4) insulating

MEISInstrumentation

POSCHENRIEDER ELECTROSTATIC
DEFLECTOR

COLLIMATOR

ACCELERATION

X-Y STEERER

TUBE
CHOPPING

BENDING

ELECTRODE

MAGNET

Q-LENS

CHOPPING

EINZEL LENS

(a)

APERTURE

(b)

X-Y

PULSE
GENERATOR

(d)

STEERER
DUOPLASMATRON

(c)
MCP

ION SOURCE

SAMPLE

SCATTERED-ION
DECELERATION TUBE

DELAY
TIME

AMPLIFIER

CFD

DELAY

ANALYZER

a) Ion beam source in combination with a 100 k eV

accelator
b) Beam chopping system
c) Target on a 3-axis goniometer
d) TOF energy analyzer located at scattering angle of 180o

High Energy Ion Scattering

Rutherford Backscattering
Spectroscopy (RBS)
E0=1 and several MeV
Usually protons, 4He, and sometimes lithium
ions are used as projectiles at backscattering
angles of typically 150 170.
Different angles or different projectiles are
used in special cases.

RBSINSTRUMENTATION

1. An ion source, usually alpha particles (He2+ ions) or, less

commonly, protons.
2. A linear particle accelerator capable of accelerating incident
ions to high energies, usually in the range 1-3 MeV.
3. A detector capable of measuring the energies of backscattered
ions over some range of angles.

ISS Application
Coatings LEIS can be used to:
Detection and quantification of pinholes
Root cause analysis of adhesion failure
Quantification of initial growth
Cleaning
Surface modification

Example:
Detection of bad wetting of coated
surface
With

a normal ion beam

the surface composition
of the coating is
determined.
With a microbeam in the
line scan mode the
composition of the outer
surface inside the
pinholes and the
distribution of the
pinholes is determined.

ISS Application
Oxygen membranes and Solid Oxide Fuel Cells (SOFC)
The

performance of oxygen membranes and Solid

Oxide Fuel Cells (SOFC) relies on the oxygen
transport through an electrolyte.
A popular electrolyte is yttria stabilized zirconia
(YSZ).
Using LEIS it has been found that at the operation
temperature trace impurities in the YSZ segregate to
the surface and block the oxygen diffusion. This
impurity segregation was found to be typical for YSZ
samples heated in oxygen at temperatures of 700C
or higher.

YSZ after
calcination

The main surface constituents

are calcium- and
hafniumoxide.
Since there is no Y or Zr peak,
these elements are not
present in the outer surface.
The strong increase in the
background at energies below
2700 eV demonstrates that
the 2nd and deeper layers do
consist of yttria and zirconia.

ADVANTAGES
Non-destructive depth profiling

Quantitative determination of amorphization and defect

density without standards
Whole wafer analysis (150, 200, 300 mm) as well as
irregular and large samples
Conductor and insulator analysis

DISADVANTAGE
S
Large

analysis area (~2 mm)

Useful information limited to top ~1
m of samples

APPLICATI
ONS
ideal use for:
Crystallographic analysis of thin films
Crystal damage/defect profiling
Determining percent amorphization
Determining thickness of amorphous layers
Relevant industries
Defense
Semiconductor
Telecommunications