Preparation and Characterization of Zno هام
Preparation and Characterization of Zno هام
Preparation and Characterization of Zno هام
ABSTRACT
In this communication, preparation of Zinc Oxide nanoparticles using Moringa Oleifera aqueous extract from
leaf, flower and bark by green synthesis sol-gel method is done. Zinc Oxide Nanoparticles are analyzed by X-ray
diffraction (XRD), Scanning Electron Microscope (SEM), UV-Visible and Fourier Transform Infrared
spectroscopy (FTIR). From UV-Visible spectroscopy, higher band gap energy of 4.3eV is obtained in the near
visible region at the wavelength of 286.5 nm. Among these extract prepared from leaf, flower and bark of
Moringa Oleifera, ZnO nanoparticles using bark of the plant is shown sharp peaks in XRD confirming the
crystallinity of the particles.
KEYWORDS
Zinc Oxide Nanoparticles, Moringa Oleifera and Green Synthesis.
(2015) and various characterization studies were spectra and results of FESEM show spherical shape
done. From XRD spectra, it is observed that ZnO with average particle size of 32.58 nm6.
nanoparticles has hexagonal wurtzite structure and Biosynthesis of Zinc oxide nanoparticles was
antibacterial activity is shown maximum inhibition carried out with the different concentration of Zinc
zone for gram (+ve) bacteria and followed by Gram acetate and aqueous extract of Citrus aurantifolia
(-ve) bacteria for the concentration of 200 μg/ml1. by Nurul Ain Samat and Roslan Md Nor (2013).
Elumalai and Velmurugan (2015) synthesized ZnO The XRD result mentioned the orientation of
nanoparticles using aqueous leaf extract of reflection plane at (100) with hexagonal structure7.
Azadirachta indica (L) by sol-gel green synthesis Senthilkumar and Sivakumar (2014) synthesized
method. The antimicrobial activity of ZnO ZnO nanoparticles using the leaf extract of green
nanoparticles increased for the increase in tea (Camellia sinensis) and characterized by various
concentration of 50, 100 and 200 μg/ml. Also techniques. The results of the UV-Visible spectrum
concentration of ZnO nanoparticles increased with give the absorption peaks at 325 nm and by XRD
increase of H2O2 concentration from the surface of result, the average size of ZnO nanoparticles is
ZnO2. Anbuvannan et al. (2015) prepared ZnO found to be 16 nm. The antibacterial activity and
nanoparticles using Zinc nitrate and Phyllanthus antifungal activities are carried out using Agar well-
niruri leaf extract by biological method. ZnO diffusion method on pathogenic species8. Niranjan
nanoparticles are confirmed with the estimated band Bala et al. (2015) prepared ZnO nanoparticles using
gap energy of 3.51 eV and Photoluminescence (PL) Hibiscus subdariffa leaf extract and found that the
intensity observed at 402 nm in the visible region growth of the ZnO nanoparticles depend on the
and the intensity of the peak and band gap energy annealing temperature. It is confirmed that the
depends on the size of the nanoparticles and increase of temperature decreases the size of the
geometrical shape3. particle. Antibacterial activity of the particles is
The mediated bio reduction of ZnO nanoparticles analyzed using gram (+ve) positive and gram
using leaf extract of Solanum nigrum by green negative bacteria9. Sagar et al. (2015) investigated
biosynthesis method was prepared and various parameters of ZnO nanoparticles such as
characterized by Ramesh et al. (2014). The SEM physical properties; antibacterial property, high
results of the study reveal that the diameter of the piezoelectricity and binding energy. Larger
ZnO nanoparticles are in the range of 20-30 nm4. potential of Zinc Oxide nanoparticles in
Suresh et al. (2015) synthesized multifunctional pharmaceutical, textile, paint and rubber industries
ZnO nanoparticles from Zinc nitrate hexahydrate is highlighted10.
and aqueous leaf extract of Arto carpus gomezianus Sagar Raut et al. (2015) explained green
by solution combustion method. The morphology of biosynthesis of zinc oxide nanoparticles using
the ZnO nanoparticles are highly porous and the aqueous Ocimum tenuiflorum plant extract. The
photocatalytic activity of ZnO nanoparticles is utilized plant is a reducing agent in the direct
shown the degradation of methylene blue dye chemical synthesis of ZnO nanoparticles. From the
exposed to sun light and UV light5. XRD result, the average particle size is found to be
Thirunavukkarasu santhoshkumar et al. (2014) 13.86 nm11. Green synthesis of zinc oxide
prepared and tested TiO2 nanoparticles using nanoparticles using aqueous Cassiafistula plant
Psidium guajava aqueous extract. The mediated extract was done by Suresh et al. (2015) and the
biosynthesis of titanium dioxide nanoparticles is leaf extract has reducing components such as
shown prominent peaks at 3410 cm-1, 1578 cm-1, polyphenols (11%) and flavonoids (12.5%).
1451 cm-1 and 1123 cm-1 respectively. Presence of Absorption peak is recorded at 370 nm in the UV-
alkynes, alkanes and C-O is confirmed by FT-IR Vis spectrum and TEM results give the average
crystalline size of 5-15 nm12. Ramesh et al. (2014)
prepared zinc oxide nanoparticles using Citrus and Figure No.1. Show the photograph of the
aurantifolia extract by biosynthesis method. drumstick tree.
Various characterization result reveals that the ZnO
nanoparticles are moderately stable, roughly MATERIAL AND METHODS
spherical and maximum particle has the size in the Materials
range from 9 to 10 nm in diameter13. Zinc nitrate hexahydrate (Zn(NO3)2. 6H2O), Zinc
Manokari et al. (2016) prepared ZnO nanoparticles acetate dehydrates ((CH3COO)2 Zn.2H2O), distilled
from zinc nitrate hexahydrate and aqueous extract water and leaf, bark and flower extracts of Moringa
of a medicinal plant (Micrococca mercurrialis) by Oleifera is used for the preparation ZnO
sol-gel biosynthesis method. The M. mercurialis nanoparticles.
plant is found to be high in primary and secondary Preparations of Aqueous Extract from Moringa
metabolites such as proteins, steroids and alkaloids. Oleifera Leaf
The UV-Visible result shows that the prepared ZnO Green leaves of Moringa Oleifera are collected and
nanoparticles from various parts extract such as washed with distilled water many times for the
leaves, stems, roots and fruits corresponding to the removal of dust particles. The leaves are then
absorbance peaks at 305 nm, 299 nm, 311 nm and grinded using mortar and pestle until the leaves are
302 nm respectively14. Rajesh kumar et al. (2015) grinded finely. Whatman Filter paper is used to
prepared zinc oxide nanoparticles using Camellia filter the grinded leaves to collect the leaf extract.
sinensis leaf extract by sol-gel heating method. The The extract is collected and kept at the room
antimicrobial activity of ZnO nanoparticles has the temperature.
maximum zone inhibition for Pseudomonas Preparation of Bark Extract
aeruginosa (32± 0.050) and minimum for The barks of the tree are collected and cut into
Staphylococcus aureus (25± 0.100)15. Ramesh et al. small pieces for the convenience. Distilled water is
(2014) investigated ZnO nanoparticles prepared used to wash the barks for many times and dried in
from 1 mM of zinc acetate using Cassia auriculata a shadow region for 5 days. The 150 grams of dried
flower extract by sol-gel method. Characterization bark is taken in a 250 mL beaker containing alcohol
results reveal the presence of Zinc oxide solution and kept for one day at the room
nanoparticles16. Bhumi and Savithramma (2014) temperature. The color of the solution turned into
studied ZnO nanoparticles prepared from zinc yellow and the solution is filtered using Whatman
acetate and sodium hydroxide using bio filter paper to get pure extract of the bark.
components of Catharanthus roseus leaves extract Preparation of Flower Extract
by biological synthesis method. ZnO Nanoparticles The flowers of the tree are collected and washed for
are found to be spherical in shape and the average many time using distilled water. Washed flowers
size of the particles in the range of 23-57 nm17. are dried in a shadow region for 3 days. The flower
In the present study, an attempt is made to becomes dried and 100 grams of the flower is taken
synthesize ZnO nanoparticles using leaf, bark and in a 250 mL beaker containing 150 mL distilled
flower extract of Moringe Oleifera as the plant has water and boiled for 20 minutes at 90˚C. The flower
traditional and medicinal values since 200 years by extract turns yellow kept inside the refrigerator for
ancient Tamil Siddhas’ and used for various 3h. Finally the extract is filtered for many times
diseases. Moreover, the plant grows in all climatic using Whatman filter paper.
conditions and specific medicinal value of boosting Green Synthesis of ZnO Nanoparticles Using
libido. Moringa Oleifera Leaf Extract
Green synthesis of zinc oxide nanoparticles using Zinc nitrate of 0.2M with the prepared leaf extract
leaf, bark and flower extract of Moringa Oleifera of the plant is taken in a beaker and using magnetic
stirred, the solution is continuously stirred at 80˚C.
The stirring is continued until, a colloid of the O-amino, C-O stretching and C-Cl stretching
solution is obtained. The colloidal solution is dried vibrations respectively. Table No.1 represents the
in hot air oven in the range of 120-130˚C for 1h and energy band and its corresponding functional group
annealed at 300˚C for 1h in Muffle furnace. The identified using FTIR spectra.
yellow color particles obtained is crushed in XRD Analysis
ceramic mortar pestle to get ZnO nanoparticles. XRD spectrums of ZnO nanoparticles using the
Similarly, ZnO nanoparticles are prepared using the leaf, bark and flower extract of Moringa oleifera
leaf and flower extract of Moringa Oleifera. are shown in the Table No.2, Figure No.5 (a), 5 (b)
Various characterization studies are carried out for and 5 (c). The diffraction peaks are obtained for 2θ
the structural, morphological and physical values viz., 31.85, 34.32, 36.47, 47.61 and
properties of the prepared ZnO particles. Figure 56.62correspond to the lattice planes (100), (002),
No.2 shows the graphical flow-chart for synthesis (101), (102) and (110). The XRD spectrum reflects
of ZnO nanoparticle using Moringa Oleifera hexagonal wurtzite structure and it is in agreement
extract. with JCPDS data No: 89-7102 and also the
diffraction peaks indicate the crystallinity of the
RESULTS AND DISCUSSION particles. The crystallite average size is calculated
UV-Visible spectra analysis using Scherrer equation
ZnO nanoparticles prepared using the extract D = Kλ/ (2)
obtained from the leaf, flower and bark of Moringa Where D is the mean size of crystallites (nm), K is
Oleifera is subjected to record UV-Vis crystallite shape factor a good approximation is 0.9,
spectroscopy. Figure No.3 (a), 3 (b) and 3 (c) shows λ is x-ray wavelength (1.540Å), B is full width at
the photograph of the UV-Vis spectra of ZnO half the maximum (FWHM) in radians of the X-ray
nanoparticles prepared from the extracts of Moringa diffraction peak and θ is the Bragg angle. The
Oleifera. The absorption peaks is obtained at the lattice parameters can be calculated by using the
wavelength 286.5, 285.89 and 289.93nm for ZnO following relation.
particles prepared from leaf, bark and flower of 1/d2 = 4/3 [h2+hk+l2/a2] +l2/c2 (3)
Moringa Oleifera. From the UV-Vis graphs, energy SEM Analysis
band gap is obtained as 4.3, 4.3 and 4.2eV using the SEM photograph is taken for ZnO nanoparticles in
formula different resolutions and depicted in the Figure
Eg =1240 /λmaxeV (1) No.6-8. Figure No.6 shows the SEM result of ZnO
FTIR spectra analysis nanoparticles obtained from the leaf extract of
To identify the functional groups involved in the Moringa Oleifera. It is observed that the particles
ZnO particles prepared from the leaf, bark and show flakes like structure and there are no pores.
flower extract of Moringa Oleifera, FTIR- spectra Figure No.7 represents the SEM image of ZnO
is recorded in the wavelength from 400cm-1 to 4000 nanoparticles synthesized using bark extract and it
cm-1. is observed that the flakes formed are clinged
The Figure No.4 shows FTIR analysis for ZnO together and it reveals that the particle size
nanoparticles using Moringa Oleifera aqueous decreases with increase in annealing temperature.
extract and measured absorption band is carried out Similarly, SEM photographs of ZnO nanoparticles
in the wave number range from 400 cm-1 to 4000 from the flower extract are shown in the Figure
cm-1. Figure No.4 (a), 4 (b) and 4 (c) shows the No.8. From the figure, it is clear that the particles
photograph of the FTIR spectroscopy recorded for are granular nanosized and size of the particle
the prepared samples. From the Figure No.4 (a), it ranges from 14-21nm.
is observed that, Energy band at 3517.99, 1652.93,
1010.77 and 828.85 cm-1 corresponds to the O-H,
Table No.2: Shows XRD results grain size and lattice parameter of ZnO nanoparticles
Sample Grain Size(nm) Lattice Parameter Å
S.No
(Moringa Oleifera) a c
1 ZnO NPs (leaf extract) 16.63 3.2870 3.4534
2 ZnO NPs (bark extract) 11.10 3.2461 5.2121
3 ZnO NPs (flower extract) 11.73 3.2313 3.3162
50ml Leaves extract + 50ml bark extract + 0.2M Zinc 30ml Flower extract +
0.2 M Zinc nitrate acetate + 100ml Distilled water 0.2M Zinc nitrate
Light yellow ZnO paste Reddish ZnO paste Light yellow ZnO paste
To obtain ZnO
Nanoparticles
(a) (b)
(c)
Figure No.3: (a) Leaf Extract (b) Inner Bark Extract (c) Flower Extract
(a)
(b)
(c)
Figure No.4: (a) Leaf Extract (ZnO NPs) (b) Inner Bark Extract (ZnO NPs) (c) Flower Extract (ZnO NPs)
Available online: www.uptodateresearchpublication.com July - September 128
Thirunavukkarasu C. et al. / Asian Journal of Phytomedicine and Clinical Research. 4(3), 2016, 121 - 132.
Z n + M L
2 5 0 0
(101)
2 0 0 0
(110)
(002)
Intensity
1 5 0 0
(102)
1 0 0 0
5 0 0
2 0 4 0 6 0 8 0
2 T h e ta ( d e g r e e )
2 5 0 0
(101)
Z n + M B
2 0 0 0
(100)
(002)
(110)
1 5 0 0
Intensity (a.u)
(102)
(112)
1 0 0 0
5 0 0
0
2 0 4 0 6 0 8 0
2 T h e ta ( d e g r e e )
Z n + M F
1 6 0 0
1 4 0 0
(002)
(110)
Intensity(a.u)
(103)
(102)
1 2 0 0
(112)
1 0 0 0
8 0 0
6 0 0
2 0 4 0 6 0 8 0
2 T h e ta ( d e g r e e )
Please cite this article in press as: Thirunavukkarasu C et al. Preparation and characterization of ZnO nanoparticles
using moringa oleifera extract by green synthesis method, Asian Journal of Phytomedicine and Clinical Research,
4(3), 2016, 121 - 132.
Available online: www.uptodateresearchpublication.com July - September 132