MSE-632 Characterization of Materials Raman Spectroscopy: A Term Paper On

MSE-632
CHARACTERIZATION OF MATERIALS
A TERM PAPER ON
RAMAN SPECTROSCOPY
Presented by, Presented to,

Jenis Samuel (21310014), Prof. Emila Panda,
Ph.D. Scholar, Associate Professor,
Materials Engineering Discipline, Materials Engineering Discipline,
IIT- Gandhinagar. IIT- Gandhinagar.
1
Vibrational Spectroscopy for Molecular Analysis- Introduction
● This technique analyzes the structure of the molecules by examining the
interaction between the electromagnetic radiation and the nuclear vibrations in
molecules.
● Vibrational spectroscopy uses electromagnetic waves with longer wavelengths of
order 10-6 m as compared to the X-Rays.
● Typical electromagnetic radiation used is Infrared radiation and Visible light.
● This detects the absorption of the light or the inelastic scattering of light by
molecule.
● This can be used to study solids, liquids and gases.
● Raman spectroscopy is one of the vibrational spectroscopy techniques widely
used by scientists and engineers for materials characterization.
2
Raman Scattering
● Raman Spectroscopy is based on the phenomenon of Raman Scattering of

electromagnetic radiation by molecules.
● When monochromatic radiation is incident on the sample, the light will be
scattered both elastically and inelastically.
● Elastic scattering is known as Rayleigh Scattering.
● Inelastic scattering is known as Raman Scattering.
● Both elastic and inelastic scattering can be understood in terms of energy
transfer between photons and molecules.
3
Fig.1. Elastic and inelastic scattering of incident light by molecules
Ref: Materials Characterization, Yang Leng, [pp. 288]

4
Raman Activity
● Among different vibration modes of a molecule, only some can be identified by the Raman
spectroscopy.
● Such vibration modes are called as Raman active.
● Only active modes can be seen as the vibration modes in their respective Raman spectra.
● To be Raman active, a vibration mode must cause polarizability changes in a molecule.
● When a molecule is placed in an electric field, it generates an induced dipole because its
positively charged nuclei are attracted toward the negative pole of the field and its
electrons are attracted toward the positive pole of the field.
● Polarizability (α) is a measure of the capability of inducing a dipole moment (μ) by an
electric field. It is defined in the following equation
μ = αE (1)
● Vibrations of covalent bond is stronger in Raman spectroscopy (C=C).
5
Raman Spectroscopy
● Raman spectra are acquired by irradiating a sample with a nearly monochromatic laser
source in the visible or near-IR spectra region.
● During irradiation, the spectrum of the scattered radiation is measured at some angle
(often 90°) with a suitable spectrometer.
Fig. 2. Block diagram of Raman spectrometer
Ref: Principles of Instrumental Analysis, Douglas A skoog, 7E, [pp. 443]

6
Instrumentation
Raman spectroscope consists of following elements.
● Laser Source
● Sample illumination and collection system
● Spectral analyzer
● Detection and control system
● Processing system
Fig. 3. Optical Diagram of Raman spectroscopy
Ref: Materials Characterization, Yang Leng

7
Laser source
● Lasers are mostly used as the source in Raman spectrometry as laser have high intensity. It
is necessary to produce Raman scattering of sufficient intensity to be measured with a
reasonable signal-to-noise ratio.
● The mostly used laser type here is Argon and Krypton.
● Intensity of Raman Scattering is 𝛂 𝜈4.
Laser Type Wavelength nm
Ar 488 or 514.5
Kr 413.1, 530.9, 647.1
He- Ne 632.8
Diode 660-880
Nd-YAG 1064
Table 1. Common Laser sources Ref.Principles of Instrumental Analysis, Douglas A skoog, 7E, [pp. 443]
8
Sample illumination system
● The beam from the laser source is first filtered to obtain a monochromatic wavelength.
● Then, a pinhole spatial filter is used to remove the appearance of the diffraction rings so as to
obtain a clean point laser beam.
● The clean laser beam is reflected by the beam splitter and goes through the objective lens to
illuminate the sample.
Fig. 4. Sample illumination system

9
Collection system
● The Raman scattered light is collected by spatial filter through an objective
lens placed in the other side of the microscope.
● This arrangement ensures only the light from the area illuminated on the
sample is passed to the spectral analyzer and detector.
● The scattered light from the microscope must be passed through special
filters before reaching the spectral analyzer in order to remove elastically
scattered light.
● The Raman light cannot be seen without the filters, because the elastically
scattered light has much higher intensity than the inelastically scattered
Raman light.
10
Spectral Analyzer
● The main component of the spectral analyzer is the diffraction grating.
● It disperses the Raman scattering light with respect to its wave numbers.
● The light dispersion is based on Bragg’s law of diffraction and initial
wavelength.
Fig. 5. Diffraction grating

11
Detector system and processing system
● The Raman scattered light separated according to wavelength is recorded by
a detector that is made from photoelectric materials.
● The detector converts photon signals of the scattered Raman radiation to
electric signals.
● The charged-coupled device (CCD) is the most commonly used detector.
● A CCD is a silicon-based semiconductor arranged as an array of
photosensitive elements.
● The Raman shift (mainly Stokes scattering) is calculated and plotted versus
wave number in the Raman spectrum by computer processing.
12
Raman Imaging
● It is a technique used to obtain spatial distribution of the molecules present in a sample.
● This is similar to elemental mapping in X-Ray and electron microscopy.
● Raman Imaging is difficult to obtain as compared to the X-Ray and electron microscopy.
● Raman imaging can be obtained by scanning or direct imaging method.
Fig. 6. Raman Imaging Fig. 7. Raman Image of rubber particles in epoxy film
(Ref. Materials Characterization, Yang Leng) 13
Applications
● Phase identification of polymorphic solids
● Polymer identification
● Composition determination
● Determination of residual strain
● Determination of crystallographic orientation
Fig. 8. Raman Spectra of (a) Graphite (b) polycrystalline graphite (c) a C (d) DLC
(Ref. Materials Characterization, Yang Leng)
14

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MSE-632

Presented by, Presented to,

● Raman Spectroscopy is based on the phenomenon of Raman Scattering of

Ref: Materials Characterization, Yang Leng, [pp. 288]

● Vibrations of covalent bond is stronger in Raman spectroscopy (C=C).

Fig. 2. Block diagram of Raman spectrometer

Ref: Principles of Instrumental Analysis, Douglas A skoog, 7E, [pp. 443]

Fig. 3. Optical Diagram of Raman spectroscopy

Ref: Materials Characterization, Yang Leng

Kr 413.1, 530.9, 647.1

Fig. 4. Sample illumination system

Fig. 5. Diffraction grating

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