Assignment 01

MM-505: Electron Microscopy

Submitted by: - Maitreya Fulmali
Entry Number: - 2023MMZ0002
Q.1. What kind of characteristic X-Ray are there and how are they produced?
Ans. The generation of characteristic X-Rays begins with the generation of Secondary electrons (SE).
The incident beam or the primary electron beam when bombards the sample surface with high speed
electrons which are accelerated by tens or hundreds of kilovolts of potential, they would collide with
the electrons (inelastic collision) of another atom in the sample, knocking out electron from one of its
inner shell. This collision would cause the electron from the inner shell to get knocked off and create a
vacancy in the atom, this knocked out electron is the secondary electron.
For any electron to fill this vacancy has to come from a higher energy state, i.e. a shell that is further
from the nucleus. To make this jump the electron has to release some of its energy in the process, this
energy is released in the form of X-ray. This is characteristic X-Ray. The energy of the characteristic
X-Ray is equal to the energy difference between the two shells.
The classification of characteristic X-Ray would depend upon the shell from where the electron is
getting knocked out from. It could be any shell except for the most outermost shell. If the electron is
knocked from K shell it would give a Kα or Kꞵ radiation. This α and ꞵ would depend upon which shell
the electron is coming from. It can be better understood with an example,
Let’s say there is an atom with 3 shells, K, L and M. if the electron is knocked from the K shell, and an
electron from L shell jumps to fill it, it would generate an Kα radiation, as the electron is coming from
its closest shell. If the electron is coming from M shell it would generate a Kꞵ radiation. Same goes for
L shell whether the electron is coming from the nearest shell or the one next to it it would generate
either Lα or Lꞵ radiation.

Fig 1: - Generation of characteristic X-Rays. (https://www.wikipedia.org/)

Que 2. Any X-Ray other than characteristic ones produced by electron beam irradiation?
Ans.
(i) Continuous X-Ray: Another type of X-Ray produced due to electron irradiation are
Continuous X-Ray or Continuum X-Ray. They are formed, when a primary electron beam
is incident on the sample, due to its high speed the electron when it reaches near any atom,
its nucleus will start to attract it towards itself. As the electron is negatively charged and
the nucleus is positively charged there would be an attractive force between them, making
 the electron to change its direction and decelerate. Just like a comet would act like when it
in near any planet. This kind of interaction is called as elastic interaction. Although it is
termed as inelastic, there would still be some amount of energy that is being lost. This
energy is released in the form of an X-Ray. These X-Ray would be generated over a wide
range of spectrum. They have very low intensity and are often referred as background
radiation or noise in the data.

(a) (b)
Fig 2: - (a) Formation of Continuous X-ray; (b) Graph showing wavelength vs intensity for
Characteristic and Continuum X-Ray. [1]
(ii) Photoelectron X-Rays: These X-Rays are generated when an electron in the inner shell of
an atom would absorb any stray X-Ray. The X-Ray would provide enough energy to the
electron to overcome the binding energy of the nucleus that is holding it in the orbit. As the
excited electron now out of the shell, there is a vacancy. To fill the vacancy, any electron
from higher energy shells would jump to this lower energy shell and would release some
energy in the form of X-Ray. These X-Rays would also depend upon which shell is the
electron jumping from. These kind of X-Rays are termed as Photoelectron X-Rays.

Fig 3: - Photoelectron absorption of X-Ray. (https://www.wikipedia.org/)

Que 3. What should be done in order to improve accuracy of X-Ray analysis?
Ans. If the element we want to detect is a major element then it would not be difficult to obtain a
precision close to ±1%, but the complete analytical accuracy would be reduced, due to factors such as
uncertainty in the composition and presence of error in the corrections which are required to be applying
to raw data.
Another reason is due to the bombardment of electron on the specimen there would be generation of
Characteristic X-Rays, but with them there would also be generation of Continuous X-Rays. This
Continuous X-Ray would give very small peaks and is often referred to as background noise and can
be removed by using the background subtraction technique. Due to them being present as small peaks
in the analysis data they would often times overlap any elemental peaks that is smaller.
Strategies that could be used to improve the accuracy of X-Ray analysis would majorly be focused on
enhancing the signal to noise ratio, controlling sample contamination and optimizing instrumental
parameters.
1. Making sure that the sample is properly prepared and to have it gold coated if any non-
conducting element is present in the sample that can interfere with the correct X-Ray analysis.
2. The accelerating voltage as well as the beam current needs to be adjusted to optimize the signal
to noise ratio. Choice of X-Ray detector setting should be done in such a manner that ensures
the maximum sensitivity and resolution is obtained.
3. Achieving the desired spatial resolution by using appropriate working distance and spot size.
4. Using background subtraction technique to remove the noise from the background and improve
the accuracy of peaks identification.
5. Taking care to prevent the samples from surface contamination by using proper handling
technique and minimizing the sample exposure to the atmosphere.
6. When we are analyzing the data from X-Ray, the Kꞵ radiation is unwanted and Kα is the only
one that we want. Thin films of metals are used as filter material which would absorb the Kꞵ
radiation and only Kα would be considered.

References: -
[1] Black, Aine. (2019). An analytical solution of photon beam attenuation and energy downshift
via Compton Scattering.
[2] Hawkes, P. W., & Spence, J. C. (Eds.). (2007). Science of microscopy (Vol. 1, pp. 130-131). New
York: Springer.
[3] Stephen J.B. Reed (1995). Introduction to Energy Dispersive X-ray Spectrometry (EDS)
[4] https://cmrf.research.uiowa.edu/scanning-electron-microscopy