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This document contains a tutorial on instrumentation with 8 questions and answers about various topics in instrumentation including Raman spectroscopy, Auger electron spectroscopy, and X-ray photoelectron spectroscopy. It includes diagrams to illustrate key concepts such as Raman scattering processes, how Auger electrons are produced, why AES is surface sensitive, the typical process for Auger depth profiling, and how chemical shifts are resolved with XPS. Formulas are provided for calculating kinetic energies of Auger electrons and concentrations measured by XPS.

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Nur Alisya Hasnul Hadi
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25 views

Instru Tuto4 Solved

This document contains a tutorial on instrumentation with 8 questions and answers about various topics in instrumentation including Raman spectroscopy, Auger electron spectroscopy, and X-ray photoelectron spectroscopy. It includes diagrams to illustrate key concepts such as Raman scattering processes, how Auger electrons are produced, why AES is surface sensitive, the typical process for Auger depth profiling, and how chemical shifts are resolved with XPS. Formulas are provided for calculating kinetic energies of Auger electrons and concentrations measured by XPS.

Uploaded by

Nur Alisya Hasnul Hadi
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
You are on page 1/ 9

Isntrumentation (SIF20038)

Tutorial 4
Abdul Rahman bin Mohd @ Mohamed
17177739 / SIF180002
June 10, 2020

1
Contents
1 Q1 3

2 Q2 4

3 Q3 4

4 Q4 5

5 Q5 6

6 Q6 6

7 Q7 7

8 Q8 9

2
1 Q1
Explain in detail the Raman effect with an aid of diagram. (Your explanation
should include: Rayleigh, Stokes and Anti-Stokes Scattering).

Figure 1: Energy level diagram for Rayleigh, Stokes and Anti-Stokes Scattering

Raman effect is the phenomena where a sample irradiated by an intense monochro-


matic light usually laser light scatters the light in 3 types of scattering. As we can see in
Figure 1, the 1st type of scattering with highest amount of scattering is the Rayleigh scat-
tering where the scattered light have the same frequency as the incoming light. The next
type of scattering is the Stokes scattering where the scattered light have lower frequency
than original incoming frequency. The last one is the Anti-Stokes scattering where the
scattered light have higher frequency than the incoming light’s frequency.

In Stokes scatering, the incoming light gives energy to the sample in form of a phonon,
causing the scattered light to have lower energy/frequency and higher wavelength than
the original incoming light.

While in Anti-Stokes scattering, the incident light absorbs energy from the sample
in form of a phonon. Causing the scattered light to have higher energy/frequency and
shorter wavelength compared to the incident light’s.

3
2 Q2
How are Auger electrons produced?

Figure 2: Diagram of how an Auger electron is produced.

Auger electron is a type of backscattered/reflected electron. It is produced when a


sample is bombarded usually by an electron beam causing an inner shell (1s) electron to
be removed. This vacancy is then filled by an outer shell (2s) electron. This outer shell
electron fills the vacancy and releases an energy that is transferred to an outer electron
(2p) making this electron able to be ejected from the atom. This ejected electron is what
is known as an Auger electron.

3 Q3
Why is AES surface sensitive?

Figure 3: AES spectrum for Paladium (Pd)

Auger electron is surface sensitive because Auger electron that is emitted in the
solid/sample, not from the surface will undergo inelastic scattering causing it to lose
some energy in the process of going from inside the sample to the surface. These Auger
electron that have lost some of its energy will become the ”background” electron in the
lower energy region of an Auger peaks as shown in Figure 3. Some of the electrons could
also lose all energy and not able to escape the surface to be analyzed for AES. That’s
why AES is surface sensitive because only Auger electron emitted from the surface of the
sample that will be able to be analyzed in AES.

4
That’s why, in executing AES, we need to properly clean the surface of the sample
before performing AES. The difference between AES performed on cleaned sample surface
and adsorbed sample surface can be seen in Figure 4 below;

Figure 4: AES spectrum of nickel (Ni) surface a) After argon sputter-cleaning and b)
After Adsorbed by carbon and oxygen

4 Q4
How is depth profiling in AES performed?

Figure 5: Typical Auger depth profiling process

As can be seen from Figure 5 above, depth profiling in AES is performed by incorpo-
rating ion beam sputtering to remove materials from the sample surface sequentially and
then performing AES. Usually, in a cycle of depth profiling process, it involves sputtering
small amount of ion to the sample, stopping, measuring the Auger spectrum and then
performing elemental quantification.

5
5 Q5
dN
Why AES uses dE
instead of N(E) directly?

Figure 6: AES spectrum of copper.

The reason why AES uses dN dE


is to accentuate the Auger signal by suppressing the
background noise due to secondary and backscattered electrons. As we can see from
Figure 6 above, using the direct spectrum (N(E) vs E), the Auger signal is not really
prominent while when using the differential spectrum ( dN
dE
vs E), the Auger signal is
more prominent making the detection sensitivity of Auger signal more enhanced.

6 Q6
Which method is used to resolve chemical shift and why?

The method that is used to resolve chemical shift is by XPS. This is because the
chemical shift of a sample can be known from the change in its binding energy. This is
based on the formula;

EBE = hf − EKE − φ (1)


Where;
EBE is the binding energy
h is Planck’s constant
f is the frequency of incident photon
EKE is kinetic energy of emitted photoelectron
φ is work function of spectrometer

6
Figure 7: Chemical shift of Ti 2p in TiO2

So, for example, looking at Figure 7, from XPS, we can know that a sample have
shifted chemically (e.g. oxidized) by analyzing its binding energy EBE spectrum before
and after a chemical reaction. We can see in Figure 7, when a sample is oxidized, its
binding energy will increase. This is because of stronger Coulombic interaction between
the emitted photoelectron and the ion core.

7 Q7
Determine the Auger transitions that produced electrons with the provided
information. The binding energy information for Mg is:

Figure 8: Binding energy based on subshell.

Based on the atomic number of magnesium, Mg, the dominant type of Auger transition
is KLL type. So, based on magnesium’s electronic configuration, we can get a collection
of its Auger transition as shown below;

1. KL1 L1

2. KL1 L2

3. KL1 L3

4. KL2 L2

5. KL2 L1

6. KL2 L3

7. KL3 L3

8. KL3 L1

9. KL3 L2

7
Next, using Equation 2 below, we can calculate the emitted Auger electron’s kinetic
energy, EKE .

EKE = EA − EB − EC (2)
Where the subscript A, B, and C depends on the type of the Auger transition. For
example, for a KLL Auger Transition, EKE = EK − EL − EL . So, for this particular
magnesium atom, EK = 1407eV , EL1 = 98eV and EL2 = EL3 = 45eV . its Auger
electron kinetic energy is;

1. 1211eV

2. 1264eV

3. 1264eV

4. 1317eV

5. 1264eV

6. 1317eV

7. 1317eV

8. 1264eV

9. 1317eV

8
8 Q8
I1 , I2 , I3 are the measured intensities and S1 , S2 and S3 are the corresponding
sensitivity in an XPS spectra. Determine the concentration of element 2.

Supposing that I1 , I2 , I3 are the measured intensities of element 1, 2 and 3 respectively


and S1 , S2 , S3 are the sensitivity of element 1, 2 and 3 respectively for a XPS spectra,
we can calculate the concentration, ηi of any of the element using the formula below;

Ii0
ηi = (3)
Itotal
Where;
Ii0 is the corrected intensities
Itotal is the total intensities

Ii0 can be expressed as;


Ii
Ii0 = (4)
Si
and Itotal can be expressed as;

Itotal = I10 + I20 + I30 (5)


So, the concentration of element 2, η2 can be expressed as;
I2
I20 S2
η2 = = (6)
Itotal I10 + I20 + I30

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