MATERIALS CHARACTERIZATION (MST613)

LAB REPORT (PART B)

SUBMITTED TO:
DR NUR AIMI BINTI JANI

NAME:
NUR SYUHADA BINTI AHMAD TERMIZI

STUDENT ID:
2019813952

GROUP:
AS2404M2

DATE OF SUBMISSION:
4th of JULY 2021
 EXPERIMENT 1
X-RAY DIFFRACTION (XRD) TECHNIQUE

Objectives:
1. To observe the operational and function of the X-ray diffraction.
2. To understand the characteristic of each materials concerning to their position and
crystallite size.

Introduction:

X-Ray Diffraction or also known as XRD is non-destructive test and a technique

used to analyze the structure of crystalline materials and determining their structure as well as
lattice parameter thereby reveal chemical composition of the components present. This
information can be used to characterize the material because every metallic element in the
periodic table consists of a combination of lattice structure and parameter. Furthermore, using
x-ray diffraction, it is easier to determine the size and shape of the unit cell for any
compound.

This kind of technique is performed by directing an x-ray beam at a sample and

measuring the scattered intensity as a function of the outgoing direction. Once the beam is
separated, the scatter, also called a diffraction pattern, indicates the sample’s crystalline
structure. Bragg’s Law is applied in determining a crystal parameter from its characteristics
x-ray pattern. It describes the relationship for constructive interference, where x-rays of
wavelength, λ incident on the material at angle, θ are diffracted by crystal planes separated by
distance, d and n represents an integer.

2dsinθ = nλ

Because of the constructive interference, an x-ray signal peak will be observed.

These peaks are then used to determine crystal directions and lattice parameters. For cubic
systems, the interplanar spacing, d, can be calculated using the crystal geometry equation,
where a is the lattice parameter and h, k, and l are the Miller indices. The equation as follows:
 a
d hkl =
√ h +k 2+l2
2

Summary finding:

The X-ray diffraction requires an X-ray source, the sample that will undergo
investigation and a detector to collect the diffracted x-rays. Firstly, x-rays are generated in a
cathode ray tube through heated filament which release electrons and accelerates the
electrons toward the sample. Electrons with sufficient energy will remove the sample’s inner
shell electrons, resulting in the characteristic of X-ray spectra. Bragg’s Law is significance
that are used to determine the structure of a crystalline. When an incident wave, x-ray of a
known λ was scanned over a range of angle value, θ range, on a sample and diffraction occurs
at a specific θ, and the structure parameter (d) of the specimen. By using the Bragg’s Law
from the known values of λ and the diffracted θ, the unit cell “a” of the element of the
specimen can be determined from equation. Basically, the parameters of crystal structure,
lattice parameters, miller indices and particle size also can be determined. In addition, based
on the pattern of h, k, l, we can determine the types of crystal structure of the samples.

Figure 1 shows the characterized of zinc oxide with nano particles by XRD. The
peaks at 2θ = 31.67°, 34.31°, 36.14°, 47.40°, 56.52°, 62.73°, 66.28°, 67.91°, 69.03°, and
72.48° were assigned to (100), (002), (101), (102), (110), (103), (200), (112), (201), and
(004). There were no characteristic peaks of any impurities were detected and initially proved
that the successful synthesis of ZnO NPs which are in well accordance with the standard
pattern of JCPDS No.5-0664.
 Figure 2: XRD patterns of ZnO NPs.

Figure 2 shows the phase and purity of the as prepared SnO 2 nanoparticles with
cinnamon were determined by XRD. From the observation, all the diffraction peaks are
assigned to tetragonal phase of tin dioxide (JCPDS No. 41-1455). The average crystallite size
of SnO2, which were indexed as (1 1 0), (1 0 1), (2 0 0), (2 1 1), and (2 2 0) are different due
to the variation of calcination temperatures and molecular weight of polyethylene glycol,
PEG. The SnO2 sample calcined at lower temperature (450 °C) with addition of high
molecular weight of PEG (PEG 4000) revealed had the smallest crystallite size as increasing
in calcination temperatures caused the peaks to be stronger and narrower.

Figure 2: XRD pattern of SnO2 nanoparticles after calcination at 600 °C with addition of (a) PEG 300
and (b) PEG 4000 & SnO2 after calcinations at 450 °C addition of (c) PEG 300 and (d) PEG 4000.
 Besides that, analysis of Polyvinyl pyrrolidone/Chitosan (PVP/CS) blend with pure
ZnS nanoparticles (ZnS-NPs) been investigated by the XRD. The wide-angle XRD results of
the ZnS nanoparticles reveal the (100), (002), (112), (103), and (112) planes corresponding to
26.9°, 28.5°, 30.5°, 47.6°, and 56.4°, This indicate indicating the hexagonal zinc wurtzite
phase according to the (JCPDS 05-0566).

Figure 3: XRD pattern for ZnS-NPs.

Figure 4 shows XRD pattern of TiO2 nanoparticle and the PVA-PEG/TiO2 composite
to study their morphology and elemental analysis, the crystal structures. The diffraction
planes (101), (004), (200), (105), (211), (204) showed that the anatase phase of TiO2 (JCPDS
No: 21-1272) was successfully synthesized and compatible with diffraction peaks.

Figure 4: XRD analysis of TiO2 nanoparticle and the PVA-PEG/TiO2 composite.

 EXPERIMENT 2

MICROSTRUCTURE OBSERVATION BY FIELD EMISSION SCANNING

ELECTRON MICROSCOPY (FESEM)

Objectives:

1. To observe the process and function of FESEM.

2. To understand the basic principle of FESEM including sample preparation and
analysis of images.

Introduction:

Field Emission Electron Microscope (FESEM) is an electron microscope that capture

the surface of the sample using a high-energy beam of electrons in a raster scan pattern. It
works with electrons (particles with a negative charge) to visualize very small topographic
details on the surface or entire or fractioned objects with higher resolution at magnifications
of 10x to 300,000x, with virtually unlimited depth of field. The detector gathers these X-rays,
backscattered electrons, and secondary electrons and produces into an electronic This signal
is amplified and transformed into a video scan-image that can be viewed on a monitor or a
digital image that can be saved and processed further. The electron interactions with the
atoms in the signal sample contain information about the sample's surface topography,
composition, and other properties.

The difference between FESEM and SEM is their electron generation system. FESEM
produces clearer, less electrostatically distorted images with spatial resolution down to 1 1/2
nm three to six times better than SEM. FESEM produces high resolution and quality imaging
with very low accelerating voltages. This enhances the observation of very fine surface
features, electron beam sensitive materials, and non-conductive materials. FESEM is very
ideal for imaging polymer samples and thin films.
Summary finding:
Before conducting the observation under FESEM, the sample must be made
conductive for current by coating them with an extremely thin layer (1.5-3.0 nm) of gold or
gold palladium. For powder samples, the minimum quantity of sample required is 10 mg.
Chemically fixed material needs first to be washed and dried below the critical point to avoid
damage of the fine structures due to surface tension then performed the coating in a separate
device. The sample holder that holds the sample was then inserted into the SEM for
characterization and imaging.

Figure 3 shows the FESEM analysis been made for the synthesis of silver
nanoparticles (AgNPs) from cinnamon against bacterial pathogens. It has shown that the
particles size lies between the 50 and 70 nm in diameter. From the FESEM micrograph, it
revealed that a uniform alignment of silver nanoparticles having size in the range of 50–70
nm and mono dispersed, spherical in shape. Thus, the presence of silver nanoparticles the
synthesized particles can be confirmed through FESEM.

Figure 5: FESEM analysis of silver nanoparticles on cinnamon.

Another observation from FESEM analysis to study the morphology and particle size
of the prepared SnO2 samples by using sol-gel method. The analysis is to investigate
relationship between the temperature, molecular weight of Polyethylene glycol, PEG and
particle size. It revealed that lowering the temperature with an increase in molecular weight
of PEG caused the reduction of particle size.
 Figure 6: FESEM micrograph of SnO2 nanoparticles calcined at 450°C with addition of (a) PEG 300
and (b) PEG 4000 & SnO2 calcined at 600 °C addition of (c) PEG 300 and (d) PEG 4000.

From the FESEM micrograph, it revealed the average particle sizes of SnO 2
calcined at lower temperature with PEG 300 (a) and PEG 4000 (b) were 22–31 nm and 14–17
nm respectively. On the For SnO2 after calcination at 600 °C, the average particle size was
29–36 nm (c) (PEG 300) and 26–29 nm (d) (PEG 4000). The samples with addition of PEG
4000 demonstrate a very small size but less uniform while the SnO2 sample with PEG 300
exhibits more uniform and narrow size distribution, while near-spherical particles were
observed for the SnO2–PEG rich-sample.
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