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Document 5398325
IOSR Journal of Applied Physics (IOSR-JAP)
e-ISSN: 2278-4861.Volume 8, Issue 3 Ver. I (May. - Jun. 2016), PP 16-22
www.iosrjournals.org
Synthesis and Antibacterial Investigation of
ZnO/CNPs Nanocomposite Powder by Hot Nickel Plate Assisted
Cost Effective Spray Pyrolysis Method and its Characterizations
1
1
2
3
4
D. Saravanakkumar , S. Sivaranjani , S. Karthi , S.Pandiarajan ,
5
B.Ravikumar
Research Scholar, Research and Development Centre,Bharathiar University, Coimbatore, Tamilnadu, India
Research guide, R&D centre, Bharathiar University, Coimbatore, India and Assistant Professor, Department
of Physics, SBM College of Engineering and Technology, Dindigul- 624 005, Tamilnadu, India
3, 4, 5
Department of Physics, Devanga Arts College (Autonomous), Aruppukottai, 626101, Tamilnadu, India
*Corresponding author Email: [email protected]
Abstract: Nanocomposite powder containing Zinc oxide and carbon nano particles (ZnO/CNPs) has been
synthesized by a cost effective hot nickel plate assisted simplified spray pyrolysis method using zinc acetate dihydrate
as host precursor source and sugar as carbon source. The structure, optical properties and morphologies of
ZnOnanoflakes have been characterized by X-ray diffraction (XRD), UV–Vis spectrophotometry, Fourier transform
infrared (FTIR), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX).The antibacterial
study against both gram positive and negative bacteria has been studied by well diffusion method. The SEM
analysisreveals the formation of ZnOnanoflakes. XRD shows the hexagonal structure of the ZnOnanoflakes. Strong
blue shift absorption is observed from the UV–vis spectrophotometry.
2
Keywords:Antibacterial study, Nano composite, Optical properties, Spray Pyrolysis, Structural Properties.
I.
Introduction
In current trends, countlessconcentration has been stimulated in the antibacterial studies for different
bacteria using ZnONPs of organic contamination by various experimental method. Zinc oxide (ZnO) is an ntype semiconductor with a wide direct band gap of 3.37 eV, which is a promising photocatalyst used extensively
for the photocatalytic degradation of different water pollutants because of its low cost, high activity, and
environment friendly features. ZnO has perhaps the richest family of nanostructures among all materials, both in
structures and properties. A variety of ZnO nanostructures, such as nanowires, nanotubes, nanofibers,
nanospheres and nano-tetrapods, nano-cabbage, nanocombs, nanowalls and nanoprisms have been successfully
grown by different methods including vapour-liquid-solid (VLS) technique, thermal evaporation, low
temperature aqueous chemical growth (ACG), electrodeposition, etcNano-scale particles of ZnO possess a high
surface area to volume ratio [1-4]. It possesses many importantapplications in electronic and optical devices.
Though ZnO is one of the vastly deliberated materials for solarcells, gas sensors, optoelectronic applications,
etc., owing to its excellent optical and electrical properties. A common low cost method to produce ZnO NPs are
to first produce chemically modified by using chemical routes and temperature annealing. ZnO NPs have
potential application in optoelectronic devices, such as in organic light emitting diodes and organic solar cells as
atransparent electrode material. The ZnO thin film crystal and its structural properties strongly depend on
growth technique and growth condition. Many fabrication methodologies and top–down approaches have been
applied to obtain high quality nano/micro structured ZnO NPs [5,6].
The emergence of carbon nanoparticle (CNPs) shows high potential in biological labeling, bioimaging and
other different optoelectronic device applications. Carbon nano particles/tubes/fibers are the most researched materials
of the 21st century with an international intention of growing industrial quantities due to their unique properties such
as good electrical/thermal conductivity, enhanced chemical/bio compatibility and excellent corrosion resistance for
wide range of applications which include polymer composites, electrochemical energy storage and conversion,
filtration, hydrogen storage, catalysis and biotechnology. Successful utilization of carbon nanoparticles in various
applications is strongly dependent on the development of simple, efficient and inexpensive technology for its
production [7-10].Common routes in making carbon nanoparticle includes high energy ion beam radiation based
creation of point defect in diamond particle followed by annealing laser ablation of graphite followed by oxidation
and functionalizationthermal decomposition of organic compound, electrooxidation of graphite and oxidation of
candle soot with nitric acid[11-14].
The various synthesis routes have been reported for the preparation of ZnO nanoparticle. The notable
examples are simplifies spray pyrolysis method, copreparation method, sol-gel , solvothermal , microemulsion
physical methods including chemical vapor deposition, gel cumbution method, thermal decomposition of
DOI: 10.9790/4861-0803011622
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Synthesis And Antibacterial Investigation Of Zno/CnpsNanocomposite Powder By Hot Nickel Plate.
organometallic precursors, arc plasma, laser ablation, and levitation gas condensation reverse micelles process,
salt reduction, microwave dielectric heating reduction, ultrasonic irradiation, radiolysis, electrochemical
synthesis etc.,[15-21]
The presents work describes the synthesis of carbon nano particles doped ZnOnano particles using
simplified spray pyrolysis method with some modified experimental arrangement. Number of research work has
been reported using this method for preparing thin films only. In the present work, the title compound is
prepared in an slightly different from spray pyrolysis method which is cost effective and simple.
II.
Materials And Methods
Zinc acetate dihydrate (Sigma Aldrich, 99% purity) was taken as precursor. Zinc acetate of 0.05 M
precursor solution made of 50 ml of deionized water was used to synthesis ZnO nanoparticles. In the first step,
sugar (stevia sugar purity 99%) solution of 0.01 M is mixed with precursor solution. Then it is stirred for 2 hours
at 50˚C. In this case sugar mainly acts as carbon source. In second step the mixed solution is poured into the
perfume spray atomizer without any other impurity. In third step, the nickel plate in the dimension of
15cmx12cmx1mm is placed on the hot plate at 200˚C. In fourth step the mixed solution is sprayed nearly 100
times directly on the hot nickel plate with 5 seconds interval and then it is cooled for 30 minutes. Then,
deposited ZnO/CNPs nano composite powder removed by fine metal strip and collected in glass tube named as
sample A. The same procedure is followed for sample B having 0.02 Msugar solution where concentration of
precursor solution is constant.
After final preparation, the particles were dried at 80 °C and normal pressure and ground to a fine
powder with a pestle and mortar. Finally it is calcined at 150˚ for 8 hours in muffle furnace.
The structural characterization of both the ZnO/CNPs nano powder were carried out using X-ray
diffraction technique employing with Cu source. Absorption spectra were recorded on UV-Visible
spectrophotometer study (Shimadzu-1700 series) and the Fourier Transform Infrared (FTIR spectra Shimadzu
IR) studies were done for as prepared samples.
III. Result and Discussion
3.1 XRD Analysis
The X-ray diffraction (XRD) pattern of ZnO/CNPs nano particles powder is shown in Fig.3.1where
peaks at 2θ values are 24.0852, 31.7695, 34.4445, 36.2533, 47.5875, 56.6214, 62.9526, 67.9950 ,69.2302 for
sample A and 23.8050, 31.7622, 34.3898, 36.2361, 47.5547, 56.5902, 62.8360, 67.9780, 69.0242 Fig.3.1for
sample B can be associated with (100), (002), (101), (102), (110), (103), (200), (112) and (201) planes
respectively. The ZnO product shows hexagonal structure with primitive lattice, which are in good agreement
with other literatures [22].The patterns are in accord with the typical zincite structure ZnO diffraction where
hexagonal phase, spacegroup P63mc, with lattice constants a = 3.24982 Å, c = 1.6021 Å, Z = 2, JCPDS No. 36’
1451etc.The average particle size (D) was determined using the Scherer s equation D = 0.9λ / βcosϴ, where D is
the crystallite size, K is the shape factor, being equal to 0.9 , λ is the X-ray wavelength, β is the full width at half
maximum of the diffraction peak, and Ɵ is the Bragg diffraction angle in degree. The average particles size was
found to be in the range of 24-31nm [23]. The sharpness of peaks shows that ZnO NPs are highly crystalline
nature.
Fig 3.1 XRD Spectrum OfZno/CnpsNanocomposites For Sample A (Red) And Sample B (Blue)
The analysis of carbon nano particles with ZnONPs was carried out to identify their crystal structure.
o
The XRD spectrum shows that there are two Bragg diffraction broad peaks at near 2θ = 23.68 It has been
o
reported that the XRD peak at near 2θ = 23.68 indexed as (002) is an indication of the presence of large
amounts of amorphous material in association with multi-walled carbon nano tubes [24, 25]. In the present
˚
study, the peaks at near 2θ = 23.80 and 24.08˚ were indexed as (002) plane which correspond to the presence of
DOI: 10.9790/4861-0803011622
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Synthesis And Antibacterial Investigation Of Zno/CnpsNanocomposite Powder By Hot Nickel Plate.
less amounts of amorphous MWCNT CNPs in association with hexagonal graphite lattice. The crystal structure
parameter such as crystallite size D, d - spacing, crystallites volume V, lattice parameter a & c, c/a ratio, cell
volume v,number of unit cells NU, bond length ιand dislocation density δ of ZnO/CNPs nanocompsite
calculated from XRD data are tabulated in the Table.1
3
-4
Sample 2Ɵ
D
d
V
Lattice Constant
v (Å)
NU
ι
δX 10
3
6
-2
(nm)
x10
nm
Nm
(Å)
(Å)
a (Å)
c (Å)
c/a
A
36.271
24.49
2.474
67.34
3.244
5.206
1.604
57.012
3.594
1.873
5.537
B
36.236
31.37
2.815
70.25
3.243
5.217
1.608
54.076
3.701
1.836
6.788
Table.1 Crystallite size, d - spacing, Crystallites volume, Lattice parameter, c/a ratio, cell volume,
Number of unit cell, Bond length and dislocation density of ZnO/CNPs nanocompsite calculated from
XRD data.
3.2 SEM Analysis
SEMmicrograph of ZnO/CNPs composite obtained from simplified spray pyrolysis withhot nickel plate
assistance method. The SEM analysis was used to determine the structure of the reaction products that were
formed. SEM image has showed carbon nanoparicles covered zinc oxide nano particles with more number of
aggregates as well. The SEM image showed relatively flake like nanoparticles shown in high magnification
SEM structure, with appearance some agglomerated grain groups. Figure 3.2 (a) shows SEM image of the NPs
from the solution of 5:1 volumetric ratio of Zinc acetate/sugar mixture S-A. Increasing the Zinc acetate/sugar
ratio to 5:2S-B, the agglomeration seems more pronounced and agglomerated groups are layered. However it is
clearly seen that the presence of MWCNTs yield a large number of ZnO nanoparticles mostly with irregular
shape and size Fig. 3.2 (b). Some particles display an appearance of hexagonal nanoplates, indicating uniform
growth of ZnO nanostructures.
Fig. 3.2 (a) SEM micrgraph of
Fig. 3.2 (b) SEM micrgraph of
ZnO/CNPs for S-A
ZnO/CNPs for S-B
The EDAX pattern in the fig 3.2 (c) reveals that only signals from O, Zn and C can be detected. In
addition, no trace of other element such as k, S, P, Cr detected in the EDX pattern, indicating that the nanowires
are pure ZnO/CNPs nano composite.
Fig 3.2 (c) EDAX spectrum of of ZnO/CNPs for S-B
DOI: 10.9790/4861-0803011622
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Synthesis And Antibacterial Investigation Of Zno/CnpsNanocomposite Powder By Hot Nickel Plate.
3.3 FTIR Analysis
Infrared (IR) spectroscopy is a popular characterization technique in which a sample is placed in the
path of an IR radiation source and its absorption of different IR frequencies is measured. Solid, liquid, and
gaseous samples can all be characterized by this technique. The FTIR spectrum of ZnO/CNPs nanostructure was
−1
recorded in the range 400-4000 cm , using FTIR spectrometer and is given in Figure 3.3 (a). The band between
-1
the 450-500 cm corelated to metal oxide bond (ZnO).
Fig 3.3 (a) FTIR spectrum of ZnO/CNPs Nanocomposites for sample A and B
The structural analysis of wurtziteZnO was further supported through FTIR investigation corresponds
-1
to the wurtzite oxide stretching frequencies of ZnO. The main absorption bands at ~ 450–500 cm are due to the
stretching mode of ZnO. From the FTIR spectrum, various functional groups and metal-oxide (MO) bond
-1,
-1
-1
present in the compound were analyzed, where absorption peak at 428 cm 442 cm and 666 cm are
attributed to stretching vibrations of Zn-O bonds. It confirms the presence of ZnOnano particles. Also the sharp
−1
−1
bands at 1015 cm and 1016 cm indicate the symmetric stretching of C-O group present in the extract [26].
The absorption band at 2920 cm-1 can be ascribed to the stretching mode of C-H bonds and its shift to 2936 cm
1
−1
−1
−1
and 2917 cm in synthesized ZnO NPs. The peaks at 3742 cm and 3756 cm indicate the presence of O-H
residue probably due to atmospheric moisture [27]. FTIR spectroscopy given further evidence of MWCNT-O–
−1
−1
C=O group that existed on the surface, and its characteristic weak absorption peak of 1728cm and 1756 cm
were observed for the samples A and B.Formation of ZnO/CNPs nanocomposite prepared by this method such
particles on the surface of disordered multi-walled CNTs (ZnO/MWCNTs) is possible from the sugar molecular
carbon source [28]. The SEM and EDAX results confirm the presence of noble CNPs and ZnO nanoparticles
3.4 UV-Vis Spectra Analysis
The electronic absorption spectrum of ZnO samples in the UV-vis range enables to characterize the
absorption edge related to semiconductor band structure. The direct band gap energy (Eg) for the ZnOnanocrystals is
n,
determined by fitting the reflection data tothe direct transition equation αhv=A (hv– Eg) whereαis the optical
absorption coefficient, hvis the photon energy, Egis the direct band gap and A is a constant and ‘n’ depends on the kind
of optical transition that prevails. Specifically, with n =1/2, a good linearity has been observed for the direct allowed
transition, the most preferable one in the system studied here by replacing n = 1/m which are n = 2 for allowed direct
transition, n = ½ for allowed indirect, n = 1/3 for forbidden indirect and n = 2/3 for forbidden direct of2 optical
transitions The exact value of the band gap is determined by extrapolating the straight line portion of (αhv) Vshvto
the x axis.Fig.3.4 (a)shows the absorption spectrumof the ZnO/CNPs composite with a sharp absorptionpeak at
349.393 nmwhich corresponds to a blue-shift of 15±2 nm compared to bulk ZnO [29, 30].
Fig 3.4 (a) UV-Vis Absorption spectrum of the ZnO/CNPs nanocomposite Sample A (black) & B (green)
DOI: 10.9790/4861-0803011622
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Synthesis And Antibacterial Investigation Of Zno/CnpsNanocomposite Powder By Hot Nickel Plate.
1/n
Fig.3.4 (b) shows the variation of (αhν) vs. photon energy, hνfor as synthesized ZnO/CNPs nano
particles with n values of 1/2. Allowed direct band gap of ZnOnano particles is calculated to be 3.3265 eV for SA and3.3905eV for S-B, which are closer to the reported value 3.37 eV [31].
Fig. 3.4 (b) Shows the variation of (αhν)
1/n
Vs photon energy, Sample A (black) & B (pink)
3.5 Antibacterial activity of ZnO/ CNPs (Sample B) against bacterial pathogens using
welldiffusion method
Antimicrobial activities of the synthesized Ag doped Bismuth oxide nanoparticles were performed
against both Gram-positive [Staphylococcus aureus] and Gram-negative [Pseudomonas aeruginosa] bacteria.
Staphylococcus aureus is a gram-positive cocal bacterium that is a member of the Firmicutes, and is frequently
found in the nose,respiratory tract, and on the skin. It is often positive for catalase and nitrate reduction.
Although S. aureus is
not always pathogenic, it
is a
common cause of skin infections such
as abscesses, respiratory infections such as sinusitis,
and food poisoning. Pathogenic
strains often
promote infections by producing potent protein toxins, and expressing cell-surface proteins that bind and
inactivate antibodies.Antibacterial activities of the ethanolic extract of the compounds Sample B were
determined using well diffusion method. It is performed by sterilizing Mueller Hinton agar media. After
solidification, wells were cut on the Mueller Hinton agar using cork borer. The test bacterial pathogens such as
Staphylococcus aureus and Pseudomonas aeruginosa were swabbed onto the surface of Mueller Hinton agar
plates. Wells were impregnated with 25 µl of the test samples (ethanolic extract of the compounds). The plates
were incubated for 30 min to allow the extract to diffuse into the medium. The plates were then incubated at
o
37 C for 24 hours, and then the diameters of the zone of inhibition were measured in millimetres.
Fig.3.5 (c) Antimicrobial activity of
ZnO/ CNPs (Sample B)against
Staphylococcus aureus
Fig.3.5 (d) Antimicrobial activity
of ZnO/ CNPs (Sample B)against
Pseudomonas aeruginosa
Each antibacterial assay was performed in triplicate and mean values were reported and the
photographs showing the inhibition zones around the disks are shown in Fig. 3.5 (c) and (d). The histogram
chart representing the zone of inhibition are shown in Fig. 3.5 (e). Antibacterial activity of metal compounds
against bacterial pathogens was tabulated in Table.2. From these results, it is found that ZnO/CNPs composite
powder exhibits antibacterial nature and its efficiency is higher for gram positive bacteria [Staphylococcus
aureus] than Gram-negative [Pseudomonas aeruginosa] bacteria.
DOI: 10.9790/4861-0803011622
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Synthesis And Antibacterial Investigation Of Zno/CnpsNanocomposite Powder By Hot Nickel Plate.
Test bacterial pathogens
Zone of inhibition in millimeter (in diameter)
ZnO/ CNPs (Sample B)
33
21
Staphylococcus aureus
Pseudomonas aeruginosa
Table. 2. Antibacterial activity of metal compounds against bacterial pathogens
Solvent used: Ethanol, Standard used: Ampicillin 10 µg
Staphylococcus aureus
Zone of inhibition for Amp 10 µg - 17 mm
Pseudomonas aeruginosa
Zone of inhibition for Amp 10 µg - 12 mm
Fig. 3.5 (e) Antibacterial activity of ZnO/CNPs composite(S-B) against bacterial pathogens
IV.
Conclusion
In the present work, we first report an eco-friendly and simple method for the synthesis of ZnO/CNPs
composite using sugar solution.The formation of ZnO/CNPs nanocomposite confirmed by XRD, SEM and
EDAX methods. XRD analysis reveals that the average grain size of the nanoparticles was found to be 24-31 nm
which was calculated by Debye-Scherrer equation. The formation of ZnO/CNPs nanocomposite was also
confirmed by Fourier transform infrared spectroscopy (FTIR). From the FTIR spectrum, the stretching and
bending frequencies of the molecular functional groups in the sample were studied. The optical bandgap of as
prepared Nano composite were obtained from optical absorption spectra by UV-Vis absorption spectroscopy.
Upon increasing the concentration of the sugar solution the optical band gap decreases from 3.39 eV to 3.29 eV.
From the antibacterial study the inhibition zone is larger for gram positive bacteria than gram negative
bacteria.The method of the present study offers several important advantageous features. The synthesis route is
economical and environment friendly, because it involves inexpensive and non-toxic materials for second, large
scale synthesis.
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