SEM IMAGES OF SS316L

CHAPTER 5

RESULT AND DISCUSSION

WE HAVE CONDUCTED THE FOLLOWING TESTS TO MEASURE THE MECHANICAL PROPERTIES AND

 FTIR ANALYSIS
 CYCLIC VOLTOMETRY
 SEM WITH EDAX
 ELECTRO CHEMICAL TEST
 HARDNESS TEST

FOLLOWING RESULTS ARE OBTAINED

5.1 FTIR(FORIER TRANSFORM INFRARED SPECTROSCOPY) ANALYSIS

Fourier-transform infrared spectroscopy (FTIR)[1] is a technique used to obtain
an infrared spectrum of absorption or emission of a solid, liquid or gas. An FTIR spectrometer
simultaneously collects high-spectral-resolution data over a wide spectral range. This confers a
significant advantage over a dispersive spectrometer, which measures intensity over a narrow
range of wavelengths at a time.
The goal of any absorption spectroscopy (FTIR, ultraviolet-visible ("UV-Vis") spectroscopy, etc.)
is to measure how well a sample absorbs light at each wavelength. The most straightforward way
to do this, the "dispersive spectroscopy" technique, is to shine a monochromatic light beam at a
sample, measure how much of the light is absorbed, and repeat for each different wavelength.
(This is how some UV–vis spectrometers work, for example.)
Fourier-transform spectroscopy is a less intuitive way to obtain the same information. Rather
than shining a monochromatic beam of light (a beam composed of only a single wavelength) at
the sample, this technique shines a beam containing many frequencies of light at once and
measures how much of that beam is absorbed by the sample. Next, the beam is modified to
contain a different combination of frequencies, giving a second data point. This process is
repeated many times. Afterwards, a computer takes all this data and works backward to infer
what the absorption is at each wavelength.
As mentioned, computer processing is required to turn the raw data (light absorption for each
mirror position) into the desired result (light absorption for each wavelength). The processing
required turns out to be a common algorithm called the Fourier transform (hence the name
"Fourier-transform spectroscopy"). The raw data is sometimes called an "interferogram"
The interferogram is converted to a spectrum by Fourier transformation. This requires it to be
stored in digital form as a series of values at equal intervals of the path difference between the
two beams. To measure the path difference a laser beam is sent through the interferometer,
generating a sinusoidal signal where the separation between successive maxima is equal to the
wavelength. This can trigger an analog-to digital converter to measure the IR signal each time
the laser signal passes through zero. Alternatively the laser and IR signals can be measured
synchronously at smaller intervals with the IR signal at points corresponding to the laser signal
zero crossing being determined by interpolation.[6] This approach allows the use of analog-to-
digital converters that are more accurate and precise than converters that can be triggered,
resulting in lower noise.

When a chemical sample is exposed to the action of IR LIGHT, it can absorb some frequencies and
transmit the rest. Some of the light can also be reflected back to the source.
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CLASSIFICATION OF IR BANDS IR bands can be classified as strong (s), medium (m), or weak (w),
depending on their relative intensities in the infrared spectrum. A strong band covers most of the y-
axis. A medium band falls to about half of the y-axis, and a weak band falls to about one third or less
of the y-axis.

RESULT
C:\Users\Admin\Documents\Bruker\OPUS_7.5.18\DATA\MEAS\SS3162.0 3/18/2019 6:58:33 PM
100.0
99.8
99.6
99.4
Transmittance [%]

99.2
99.0
98.8
98.6

3779.60
3704.02
3650.21

3161.29
3037.18

2882.55
2753.15

2562.54
2483.53
2358.40

1592.87
1481.17
1432.98
1363.77

675.50
98.4

3500 3000 2500 2000 1500 1000

Wavenumber cm-1

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C:\Users\Admin\Documents\Bruker\OPUS_7.5.18\DATA\MEAS\SS3162 - 1.0 3/18/2019 6:59:46 PM

100.0
99.8
99.6
Transmittance [%]

99.4
99.2
99.0

1811.36
1769.13
1724.15

1661.41

1592.11

1482.40
1433.86

1366.29

852.77

672.98
624.06
98.8

1800 1600 1400 1200 1000 800 600

Wavenumber cm-1

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The X-Axis: The Infrared Spectrum

The x-axis—or horizontal axis—represents the infrared spectrum, which
plots the intensity of infrared spectra. The peaks, which are also called
absorbance bands, correspond with the various vibrations of the sample’s
atoms when it’s exposed to the infrared region of the electromagnetic
spectrum. For mid-range IR, the wave number on the infrared spectrum is
plotted between 4,000 to 400 cm-1.

The Y-Axis: Absorbance or Frequency

The y-axis—or vertical axis—represents the amount of infrared light
absorbed or transmitted by the material being analyzed.

The Absorbance Bands

Typically, absorbance bands are grouped within two types: Group
frequencies and fingerprint frequencies.

Group frequencies are characteristic of small groups of atoms or functional

groups such as CH₂, OH, and C=O. These types of bands are typically
seen above 1,500cm-1 in the infrared spectrum (See top spectrum in the
graph below) and they’re usually unique to a specific functional group,
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making them a reliable means of identifying functional groups in a

molecule.

As for fingerprint frequencies, these are highly characteristic of the

molecule as a whole; they tell what is going on within the molecule. These
types of absorbances are typically seen below 1500cm-1 in the infrared
spectrum (See bottom graph of figure below); however, some functional
groups will absorb in this region as well. As a result, this region of the
spectrum is less reliable for identification, but the absence of a band is
often more indicative than the presence of a band in this region.
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CYCLIC VOLTOMETRY

Cyclic voltammetry (CV) is a powerful and popular electrochemical technique commonly employed
to investigate the reduction and oxidation processes of molecular species. CV is also invaluable to
study electron transfer-initiated chemical reactions, which includes catalysis

Experimental setup
CV experiments are conducted on a solution in a cell fitted with electrodes. The solution consists
of the solvent, in which is dissolved electrolyte and the species to be studied.
A standard CV experiment employs a cell fitted with three electrodes: reference
electrode, working electrode, and counter electrode. This combination is sometimes referred to
as a three-electrode setup. Electrolyte is usually added to the sample solution to ensure sufficient
conductivity. The solvent, electrolyte, and material composition of the working electrode will
determine the potential range that can be accessed during the experiment.
The electrodes are immobile and sit in unstirred solutions during cyclic voltammetry. This "still"
solution method gives rise to cyclic voltammetry's characteristic diffusion-controlled peaks. This
method also allows a portion of the analyte to remain after reduction or oxidation so that it may
display further redox activity. Stirring the solution between cyclic voltammetry traces is important
in order to supply the electrode surface with fresh analyte for each new experiment. The solubility
of an analyte can change drastically with its overall charge; as such it is common for reduced or
oxidized analyte species to precipitate out onto the electrode. This layering of analyte can
insulate the electrode surface, display its own redox activity in subsequent scans, or otherwise
alter the electrode surface in a way that affects the CV measurements. For this reason it is often
necessary to clean the electrodes between scans.
Common materials for the working electrode include glassy carbon, platinum, and gold. These
electrodes are generally encased in a rod of inert insulator with a disk exposed at one end. A
regular working electrode has a radius within an order of magnitude of 1 mm. Having a controlled
surface area with a well-defined shape is necessary for being able to interpret cyclic voltammetry
results.
To run cyclic voltammetry experiments at very high scan rates a regular working electrode is
insufficient. High scan rates create peaks with large currents and increased resistances, which
result in distortions. Ultramicroelectrodes can be used to minimize the current and resistance.
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The counter electrode, also known as the auxiliary or second electrode, can be any material that
conducts current easily and will not react with the bulk solution. Reactions occurring at the
counter electrode surface are unimportant as long as it continues to conduct current well. To
maintain the observed current the counter electrode will often oxidize or reduce the solvent or
bulk electrolyte.

Solvents
CV can be conducted using a variety of solutions. Using typical electrodes, solvents dissolve not
only the analyte, often at mM levels, but also electrolyte, generally at much higher
concentrations. For aqueous solutions, these requirements are trivial, but for nonaqueous
solutions, the choices of suitable solvents are fewer.[8]

Electrolyte
The electrolyte ensures good electrical conductivity and minimizes iR drop such that the
recorded potentials correspond to actual potentials. For aqueous solutions, many electrolytes are
available, but typical ones are alkali metal salts of perchlorate and nitrate. In nonaqueous
solvents, the range of electrolytes is more limited, and a popular choice is tetrabutylammonium
hexafluorophosphate.
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SEM (SCANNING ELECTRON MICROSCOPY) ANALYSIS

A scanning electron microscope (SEM) is a type of electron microscope that
produces images of a sample by scanning the surface with a focused beam
of electrons. The electrons interact with atoms in the sample, producing various
signals that contain information about the surface topography and composition of the
sample. The electron beam is scanned in a raster scan pattern, and the position of
the beam is combined with the intensity of the detected signal to produce an image.
In the most common SEM mode, secondary electrons emitted by atoms excited by
the electron beam are detected using an Everhart-Thornley detector. The number of
secondary electrons that can be detected, and thus the signal intensity, depends,
among other things, on specimen topography. SEM can achieve resolution better
than 1 nanometer.
SEM ANALYSIS APPLICATIONS
The signals generated during SEM analysis produce a two-dimensional image and
reveal information about the sample, including external morphology (texture),
chemical composition, when used with the EDS feature, and orientation of materials
making up the sample.
The EDS component of the system is applied in conjunction with SEM analysis to
determine elements in or on the surface of the sample for qualitative information. It
also measures elemental composition for semi-quantitative results and identifies
foreign substances that are not organic in nature and coatings on metal.
THE SEM ANALYSIS PROCESS
Scanning Electron Microscopy uses a focused beam of high-energy electrons to
generate a variety of signals at the surface of solid specimens. In most SEM
microscopy applications, data is collected over a selected area of the surface of the
sample and a two-dimensional image is generated that displays spatial variations in
properties including chemical characterization, texture and orientation of materials.
The SEM is also capable of performing analyses of selected point locations on the
sample. This approach is especially useful in qualitatively or semi-quantitatively
determining chemical compositions, crystalline structure and crystal orientations.
The EDS detector separates the characteristic X-rays of different elements into an
energy spectrum and EDS system software is used to analyze the energy spectrum
in order to determine the abundance of specific elements. A typical EDS spectrum is
portrayed as a plot of X-ray counts vs. energy (in keV). Energy peaks correspond to
the various elements in the sample. Energy Dispersive X-ray Spectroscopy can be
used to find the chemical composition of materials down to a spot size of a few
microns and to create element composition maps over a much broader raster area.
Together, these capabilities provide fundamental compositional information for a
wide variety of materials, including polymers and metals.
Scanning electron microscopes (SEMs) employ electron beams in order to get
information from a sample at the nanoscale. The main type of signals that are
detected are the backscattered (BSE) and secondary electrons (SE), which generate
a grayscale image of the sample at very high magnifications. However, there are
many other signals which can be a product of the electron-matter interaction, and
these can provide additional information about the sample. In this blog we will
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describe how energy-dispersive X-ray (EDX or EDS) analysis works on a SEM.

Electron – matter interaction

The electron beam-matter interaction generates a variety of signals that carry

different information about the sample (Figure1). For example, backscattered
electrons produce images with contrast that carries information on the differences in
atomic number; secondary electrons give topographic information (you can read
more about it here); cathodoluminescence can give information on the electronic
structure and the chemical composition of materials; and transmitted electrons can
describe the sample’s inner structure and crystallography. Another type of signal that
is widely used in SEMs is X-rays.

Figure 1: Illustration of the electron-matter interaction depicting its different products.

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