CHAPTER VI

CHARACTERIZATION TECHNIQUES
6.1 SCANNING ELECTRON MICROSCOPE (SEM):
It is an electron microscope that scans the surface of the sample
with the help of electrons. The interaction between the electrons and the atoms
in the surface of the sample produces many signals from which the topography,
morphology and the composition of the sample can be identified. The scan
pattern of the electron and the beam position helps to produce an image of the
sample. The SEM can give better resolution which is lesser than 1 nanometer.

The SEM test is carried out on the sample which is kept in high
vacuum conditions. In some cases, low vacuum or wet conditions are also used.

The signals used by a SEM to produce an image are because of the

interactions between electron beam and surface atoms of the sample. Signals
like secondary electrons, reflected electrons, characteristic X-rays and light
transmitted electrons are produced.

The secondary electrons are emitted from points that are closer to
the specimen surface. Thus the secondary electrons imaging can provide better
resolution of about 1 nm. Reflected electrons are beam electrons that are
reflected from the sample by elastic scattering. The resolution of BSE images is
lesser than SE images. Even though, the resolution of BSE is less, it is used in
many analytical SEM because of the signals of BSE are directly linked with the
atomic number of the specimen.

SEM images have a large depth of field yielding as the beam of

electron is very narrow. This is highly used for the identification of the structure
of the surface of the sample. The magnifications can vary from 10 times to
50,000 times of the original level of the lens.
 Fig 6.1: Scanning Electron Microscope (SEM)

6.2 ENERGY DISPERSIVE X-RAY SPECTROSCOPY (EDS):

Energy-dispersive X-ray spectroscopy is a technique used for

the elemental analysis or chemical characterization of a sample. It depends upon
the interaction of X- ray beam and a sample. This is mostly used since it is
based on the fact that each and every element has a separate, distinguished
atomic structure and the peaks vary in the electromagnetic spectra respectively.

Initially the beam of fast moving X-rays are initiated and made
to focus on the sample under study. Generally before excitation, the atom in the
sample contains ground state electrons. The incident beam of electrons will
excite the electron in inner shell and it moves up to higher levels after ejecting
from the initial position. Thus a hole is created in the initial position. The
electron of outer shell moves to fill the hole and thus X-ray is generated. The
energy of such X-ray is measured using energy dispersive spectrometer. Since
the energies of the X-rays are difference in energy between two different shells,
the atomic structure of the element which emits is found. Thus the element
composition is measured.
6.3 X-RAY DIFFRACTION (XRD):

X-ray powder diffraction (XRD) is used for phase identification

of crystalline materials and hence cell dimensions can be obtained. The material
is thoroughly grounded using grinder and homogenised to get the results.

X-ray diffraction is used mostly for studying the structure of

crystals.

X-ray diffraction is based on constructive interference

between monochromatic X-rays and a crystalline sample. The X-rays are
generated by a cathode ray tube. They are filtered to produce monochromatic
radiation, made to focus and directed towards the sample. The interaction of the
incident rays with the sample produces constructive interference through the
conditions of Bragg's Law.

This law relates the wavelength of radiation to the angle of

diffraction and the lattice spacing in a crystalline sample. These diffracted X-
rays are then detected, analysed and result is consolidated.
 Fig 6.2: X-Ray Diffractometer

6.4 TRIBOMETER:

Materials, coatings and lubricants often encounter situations

involving repeated back and forth (reciprocating) movements during operation.
Such situations are seen in various applications ranging from automotive to bio-
materials for implants. These contacts may see a range of operating conditions
from low amplitude, high frequency reciprocation to high amplitude and low
frequencies.
 The Linear Reciprocating Tribometer is designed to allow
users to characterize tribological performances of materials and lubricants in a
wide range of operating conditions ranging from fretting wear conditions to
large amplitude linear sliding conditions. If can effectively be used to study
bulk materials, coatings, lubricants and additives. The Linear Reciprocating
Tribometer can accommodate a variety of sample geometries to create point,
line and area contacts. Customized sample holders can also be provided for tests
requiring conformal contacts.

This system is computer controlled and includes a data

acquisition software that can be used to acquire, view and report results.

Fig 6.3: Linear Reciprocating Tribometer

6.5 PROFILOMETER:

A profilometer is a measuring instrument used to measure

a surface's profile, in order to quantify its roughness. Critical dimensions as
step, curvature, flatness are computed from the surface topography.

A surface profilometer (also known as a stylus profilometer) is an

instrument used for surface texture analysis as it measures the surface
topography of a sample to reveal a topographical image of the surface. Surface
profilometers are equipped with a diamond-tipped stylus used to move
vertically and laterally to scan across the surface of the sample. Stylus
profilometers can measure vertical displacement as a function of position. These
typical surface texture measuring systems can measure a vertical range from
10nm to 1mm. These contact profilometers can provide direct resolution as low
as 20nm for surface metrology applications.

Fig 6.4: Profilometer