CHAPTER 5

5. RESULTS AND DISCUSSIONS

➢ X-Ray diffraction patterns (XRD) are generally used to determine the mean size of
nanoparticles by using Scherer’s equation.

➢ FTIR confirms the presence of functional group present in the Nanoparticles.

➢ SEM is used to study the three dimensional image of the specimen. SEM results
illustrated that using precursors affected the size and shape of the nanoparticles.

➢ The microstructure was studied by transmission electron microscopy (TEM) is the

selected Area Electron Diffraction (SAED) pattern of ZnO nanostructures further
confirms the crystalline nature of the sample.

➢ The Energy Dispersive X-Ray Analysis (EDX), referred to as EDS or EDAX, is an X-ray
technique used to identify the elemental composition of materials.

➢ The optical transmittance of ZnO nanoparticles were studied through UV-Vis

spectroscope

35
5.1 POWDER XRD ANALYSIS
Synthesized particles were subjected to X-Ray diffraction studies, for confirming the size and
structure of Nanoparticles. Figure (5.1) reveal the XRD pattern of zinc oxide nanoparticles. The
Intensity of peak (101) was observed to be very strong in comparison with other peaks in Fig
(5.1). The location of the peaks was compared to the literature values and the presence of ZnO
was confirmed. Number of Bragg reflections for ZnO NPs at 2θ = 31.87, 34.54, 36.35, 47.65,
56.73, 62.98 and 68.07 can be indexed to the (100), (002), (101), (102), (110), (103) and (112)
that are good agreement with the JCPDS file (JCPDS: 80-0075 card), which elucidates the
hexagonal wurtzite structure which corresponds to pure zinc oxide nanoparticles [22, 23].

Fig.5.1 X-ray diffraction analysis of ZnO

The average crystalline size was calculated using Debye-Scherre's Formula [24]
D = K λ \β cosθ
Where D is the crystal size of zincoxide Nanoparticlesk is the Scherre's Constant 0.9
λ is the wavelength of the X-Rays (1.5406Å)
β is the full width half Maximum
θ is the Bragg diffraction angle.

By using Debey-Scherre’s equation the average particle size of synthesized particles was
calculated to be as 9nm.

36
5.2 FOURIER TRANSFORM INFRA-RED SPECTROSCOPY

To classify functional groups in the leaf extract and zinc oxide nanoparticles, we perform FTIR
spectroscopy in the range of 4000−400cm-1. The FTIR spectrum of ZnO nanoparticles is shown
in the given Fig. (5.2). The FT-IR spectrum showed the presence of bonds due to O–H stretching
(around 3407 cm-1) and aldehydic C–H stretching (around 2992 cm-1 and 2104 cm-1) [28]. The
intense bands observed at 1391.51 cm-1 have been assigned to C–N stretching vibrations of
aliphatic and aromatic amines [56], respectively. The band at 1044.55 cm-1 corresponds to C–N
stretching vibration of amine [31]. Then the peaks at 648.71 cm-1 and 601.39 cm-1 indicates the
stretching vibrations of ZnO nano particle which is consistent with that reported before [20].

Fig.5.2 Fourier Transforms Infra-Red Spectroscopy of ZnO

37
5.3 SCANNING ELECTRON MICROSCOPE

Fig. 5.3 Scanning Electron Microscope of ZnO

SEM analysis was carried out to find the surface morphology of zincoxide nanoparticles. The
SEM magnification images indicated that the ZnO nanoparticles are spherical shape with
irregular morphology and aggregated nanoparticles. SEM results illustrated that using precursors
affected the size and shape of the nanoparticles. From the Fig.(5.3) it was confirmed that the

38
synthesized ZnO nanoparticles were well in agreement with the result obtained from XRD. The
average crystallite size was obtained by drawing histogram for the SEM image. From the
Fig(5.4) most particles were having size of the order of 561nm. There is difference in the average
particle size obtained by PXRD (9nm) and SEM result (561nm). This is because SEM image
taken was for very small portion of the sample. Probably, the part of the sample for which SEM
image taken was large in size.

Fig.5.4 Histogram Image of SEM

39
5.4 ENERGY DISPERSIVE SPECTRUM (EDS)

The EDS Micrograph showed purity of the ZnO compound. No other elements other than Zinc
and Oxide were found in the sample. The EDX result Fig. (5.5) showed the presence of Zinc and
Oxide by the appearance of Zn and O peaks. According to the EDS report the weight percentage
and atomicity of Zn and O were found to be 75.32%, 24.68%and 55.51%, 44.49% respectively
which is close to bulk ZnO weight percentage (80 for Zn and 20 for O). Fig.(5.5) Exhibits Zn
spectrum with high intense peaks and single small peak which are associated with O atom
respectively.

Fig. 5.5 EDS Analysis of ZnO

40
5.5TRANSMISSION ELECTRON MICROSCOPE

Fig.5.6.TEM image of ZnO

The particle size and nanostructure of ZnO nanoparticles have been examined through TEM are
shown in fig (5.6). The particle size of the zincoxide sample are consistent with the results of
XRD analysis. The SAED pattern further confirms the polycrystalline nature of the sample. The
average crystallite size was obtained by drawing histogram fig.(5.7) for the TEM image. The

41
particles were roughly spherical with a size of about 20nm. From the Fig.(5.6) shows an electron
diffraction pattern representing well-defined quanticontinuous diffraction rings. It was also
confirmed that the synthesized ZnO nanoparticles were well in agreement with the result
obtained from XRD.

Fig.5.7 Histogram Image of TEM

42
5.6 OPTICAL ANALYSIS

Fig.5.8.UV absorbtion spectra of ZnO

The optical characterization of the sample was recorded on UV-Vis absorption spectrum. Fig.5.8.
represents the UV absorbtion spectrum of ZnO. The absorption spectrum of ZnO NP’s sample
was studied in the range between 200 and 800nm. The UV higher cut off wavelength of zinc
oxide lies near 328nm. The band gap of is found using the relation E=hc/λ and is found to be
3.7eV.

43