Inernational Journal of Science Research Volume 01, Issue 04

Synthesis, Characterization and Antibacterial Activity of

Zinc Ferrite Nanopowder
R.S. Raveendraa*, P.A. Prashantha*, B. Daruka Prasadb, S. Chandra Nayakac, G.P. Sureshad, B.M. Nagabhushanae, H.
Nagabhushanaf, N.P. Bhagyaa.
a

Department of Chemistry, Sai Vidya Institute of Technology, Bangalore-560 064, India.

b

Department of Physics, Sai Vidya Institute of Technology, Bangalore-560 064, India.

Department of Studies in Biotechnology, University of Mysore, Mysore-570 006, India.

Department of medicinal chemistry, Dongguk University, Goyang(Seoul), South Korea.

Department of Chemistry, M.S.Ramaiah Institute of Technology, Bangalore-560 054, India.

f

Centre for Advanced Materials Research, Tumkur University, Tumkur-572 103, India.

*prsnthmysore@gmail.com, raveendrars@gmail.com

Abstract : Synthesis of nanosized particles with antibacterial properties are of immense attention in the development
of novel pharmaceutical products. Zinc ferrite nanopowder (ZnFe2O4) is known to have excellent bactericidal effects.
In this article we present the effectiveness of ZnFe2O4 nanopowder against few bacterial pathogens. ZnFe2O4 nanopowder
is prepared by facile solution combustion method from zinc nitrate and ferric nitrate using freshly prepared oxalyl
dihydrazide (ODH) as fuel. The structure and morphology of ensuing product was characterized by Powder X-ray
Diffraction (PXRD), Fourier Transform Infrared (FTIR) and Scanning Electron Microscopy (SEM) analysis. The PXRD
result confirms the formation of spinel cubic structure with Fd 3 m space group matches with JCPDS No. 22-1012. The
average particle size calculated by Debye Scherrer formula is 12 nm and the X-ray density of the powder is 2.398 g/cc3.
The FTIR spectrum confirms the purity of the sample. The SEM micrograph shows that the morphology of the sample
as agglomerated and flakes type of structure. The antibacterial activity of the synthesized ZnFe2O4 nanopowder was
done by Luria-Bertani broth (LB) method. ZnFe2O4 nanopowder was investigated with four different bacterial pathogens.
The observed result shows antibacterial activity against E.coli, S. aureus, B. tuberculosis and P. aeruginosa bacterial
pathogens. The concepts of fundamental molecular mechanism of antibacterial actions are responsible for these results.
For targeted drug delivery system, the magnetic nanoparticles of around 10 nm were preferred. Since the prepared
samples have these potentials, the magnetic properties of these samples are under investigation.
Keywords: Nano zinc ferrite, Antibacterial activity, Solution combustion synthesis, E.coli, S.aureus, LuriaBertani
broth..
Zn2+, Ni2+, Cu2+, Co2+ etc. The method of preparation of
nano ferrites with different metal ions modifies the
distribution of ions in the spinel structure. The ZF spinels
adopt normal spinel structure with Zn2+ cations occupy
tetrahedral sites. The various processing techniques,
which are used for the synthesis of spinel ZF nano
powders, include microwave refluxing, solution
combustion, hydrothermal, solgel, co-precipitation and
spray pyrolysis. The properties of ferrites are very sensitive
to the processing techniques [6-7].

1. INTRODUCTION
Nanoparticle-metal oxides represent a new class of
important materials that are increasingly being developed
for use in research and health related activities. In recent
years there has been growing interest in the preparation
and study of ferrite nanopowders [1- 3].
Nanosized spinel zinc ferrite (ZF) powders have engrossed
significant interest for their technical importance due to
their high electrical resistivity, high magnetization, high
permeability and low cost. ZF nanopowder with tailored
surface chemistry have been widely used experimentally
for biological applications like antibacterial, antifungal
activities, drug-delivery technology, catalysis, magnetic
resonance imaging (MRI) and fundamental understanding
of unusual properties of nanoparticles compared to those
of bulk materials [4-5]. The spinel structure of ferrite is
[M2+]tetra [Fe3+]octa O4 where M2+ is metal ion like Mn2+,

In the present work, we report on a synthesis procedure

of ZF by solution combustion method. The discussion on
the variation of antibacterial activity against E.coli, S.
aureus, B. tuberculosis and P. aeruginosa bacterial
pathogens are summarized. Different classes of bacteria
exhibit different susceptibilities to nanoparticles.
Although there are huge potentials of nanotechnology,

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Inernational Journal of Science Research Volume 01, Issue 04

the cytotoxicity of the nanoparticles remain a major
concern [8-10].

space group (JCPDS No. 22-1012). No diffraction peaks

of impurities were observed in the patterns. The powder
density was measured using Archimedes principle with a
pychometer with the help of xyleneas a medium. The
average crystallite size of sample was estimated by
employing the Debye-Scherrer formula.

2. MATERIALS AND METHODS

Chemicals including zinc nitrate (Zn(NO3)2.6H2O) ferric
(III) nitrate (Fe(NO3)3.9H2O) were all purchased from
MERCK, and freshly prepared oxalyl dihydrazide (ODH)
(C2H6N4O2) used as starting materials without further
purification. Deionized water was used to prepare all
solutions.

Where d is the average crystalline dimension

perpendicular to the reflecting phases, 5 is the X-ray
wavelength, k is Schrrer constant varies from (0.880.92), the average value of 0.9 is taken for calculation.
57? and 5- ?? are measured from the PXRD graph as
shown in the Fig.1b, 57is the full width at half maximum
intensity of a Bragg reflection excluding instrumental
broadening and 5- ? is the Braggs angle. The crystal
size and the density of the ZF sample are summarized in
Table-1.

2.1 Synthesis of zinc ferrite

Zinc ferrites with stoichiometric composition were
prepared by solution combustion method. The
stoichiometric composition of the mixture was calculated
based on the total oxidizing and reducing valences of the
oxidizer and fuel necessary to release the maximum energy
for the reaction. In solution combustion method of
preparation, zinc nitrate hydrate, ferric nitrate hydrate and
freshly prepared oxalyl dihydrazide (ODH) mixture are
taken in a crystalline dish and dissolved in a minimum
amount of water. The solution was stirred with magnetic
stirrer for twenty minutes. The stirred solution was kept
in muffle furnace, preheated to 300 0 C, where the
smoldering type ignition took place, producing a zinc
ferrite in froth form.

Table. 1 Powder density and crystal size.

Sample
Code

Powder
Density
[gm/cc]

2
[deg]

ZF

1.60

35.32

FWHM Crystal
[radians] size
[nm]
0.011

12

X Ray
density
g/cc
2.398

2.2 Measurements
Powder X-ray diffraction (PXRD) analysis was conducted
on Philips analytical X-ray diffractometer using CuKa
radiation (5=1.5405Ao). Fourier transform infrared (FTIR) spectra were recorded in absorption mode with Perkin
Elmer FT-IR spectrometer (Spectrum 1000) along with
KBr pellets. FT-IR spectra in the range 300-4000 cm-1
were recorded in order to study the nature of the chemical
bonds formed. Morphologies of ZF were examined by
scanning electron microscope (SEM) JEOL (JSM-840A).
UV-Vis spectra of the samples were recorded with the
Specord S600 - 212C205 spectrometer and the samples
were obtained by dispersing the powder in liquid paraffin.
The antibacterial activity of the synthesized ZF
nanopowder was done by disc diffusion assay by using
standard medium.

Fig. 1a PXRD pattern of the prepared ZF sample.

3. RESULTS AND DISCUSSIONS

3.1 PXRD analysis
The PXRD pattern of the as formed sample for
combustion synthesis was shown in Fig.1a. All the
diffraction peaks confirmed the formation of the pure
single-phase ZF with cubic spinel phase and Fdm (227)

Fig. 1b PXRD pattern for (311) peak.

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Inernational Journal of Science Research Volume 01, Issue 04

3.2 FT-IR analysis

3.3 SEM analysis

In the range of 4000-310 cm-1, the FT-IR bands of solids

are usually assigned to vibration of ions in the crystal
lattice. Two main broad metal-oxygen bands are seen in
the FT-IR spectra of spinel ferrite in particular. The highest
one generally observed in the range of 600-540 cm-1,
corresponds to intrinsic stretching vibrations of the metal
at the tetrahedral site, whereas the lowest band observed
in the range of 450-375 cm-1 is assigned to octahedralmetal stretching. The highest wave number is for Zn2+,
which prefers tetrahedral sites because of its capability to
form covalent bonds involving sp3 hybrid orbitals. The
band at 540 cm-1 is corresponding to tetrahedral Zn2+
stretching whereas the band at 375 cm-1 is corresponding
to Fe3+ vibration at octahedral site. The bands observed
at 3428 cm-1 and 1621 cm-1 attribute to the stretching
modes and H-O-H bending vibration of the free or
absorbed water. The band at 1356 cm-1 is associated with
the antisymmetric NO3- stretching vibration occurring
from the residual nitrate groups of metal nitrates. The
absorption band at 2351 cm-1 corresponds to the vibrations
of CO2 trapped during combustion process. The spectra
of the as formed sample were shown in Fig.2a and 2b.

SEM analysis shown in Fig.3 reveals that the morphology

of ZF seems likely that the agglomeration of the product
composed of uniform nanoparticles of flakes type in the
sample. The resolution used in this study cannot detect
the individual crystallites. TEM analysis for the same is
under progress.

Fig.3 SEM image of ZF sample.

3.4 UV-Vis spectra analysis and evaluation of Energy
gap (Eg)
The energy gap (Eg) has been evaluated for ZF prepared
by solution combustion method, by fitting reflection data
to the direct transition equation
Where?545 ?5 is the wavelength, A is a constant and
n can have values 1/2, 3/2, 2 and 3 depending on the
mode of inter-band transition, i.e., direct allowed and
direct forbidden, indirect allowed and indirect forbidden
transition, respectively. Plotting (ahc/5)2 as a function of
photon energy (hc/5), and extrapolating the linear portion
of the curve to absorption equal to zero as shown in Fig.
4, gives the value of the direct band gap (Eg). The inset
of Figs. 4 show the UV-Vis absorption spectrum is taken
in the range of 200 to 1020 nm.

Fig.2a FTIR spectra of ZF sample.

Fig.4 UV-Vis spectra of ZF.

Fig.2b Main metal-oxygen bands of FTIR spectra.

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Inernational Journal of Science Research Volume 01, Issue 04

4. ANTIBACTERIAL STUDIES

Table. 2a Antibacterial activity of ZF by Luria-Bertani

broth method.

The antibacterial activity of the prepared ZF nanopowder

was tested using four common bacterial pathogens:
Escherichia coli, Pseudomonas aeruginosa (Gram
negative), Mycobacterium tuberculosis, Staphylococcus
aureus (Gram positive). In brief, 105 cells/ml in LuriaBertani broth (LB) were shaken (250 rpm) in light with
zinc ferrite nanopowder (0.3%) for 24 h at 370 C. The
number of feasible bacteria was determined by plotting
successive dilutions on LB agar plates and determining
number of colony forming units (CFU). Each fragment
of this compound i.e., zinc nitrate and ferric nitrate were
as such tested for antibacterial activity and found inactive.
The concentration used for test compound and that of
standard remains the same. The results are summarized
in Fig.5a, Fig.5b and tables 2a, 2b. The ZF nanopowder
show variable activity on the bacterial pathogens and
significantly increased antibacterial activity by nearly two
fold on all the four bacterial pathogens when compared
to conventional antibiotics viz., streptomycin and
tetracycline.

Sl.
No.

Bacterial
pathogens

Zone of inhibition in
diameter (mm)

Controle

80

E.coli

18

P.aeruginosa

17

M. tuberculosis

15

S. aureus

16

Table.2b Antibacterial activity of conventional

antibiotics.
Sl.
No.

Conventional
antibiotics

Zone of inhibition in
diameter (mm)

Streptomycin

35

Tetracycline

40

Fig.5a Efficacy of ZF nanopowder on various bacterial

pathogens. Controle refers to bacteria incubated
without ZF nanopowder.

The observed enhancement in antibacterial activity of the

synthesized ZF nanopowder may be due to the presence
of both zinc oxide and iron oxide in the synthesized
compound. The fallowing factor may be responsible for
the enhancement of antibacterial activity viz., (i) the
improved colloidal aqueous stability of magnetic
composite nanoparticles from the combination of zinc
oxide with iron oxide. (ii) the ionic size of ZF and (iii)
reactive oxygen species (ROS) formation. The
antibacterial effect of this ZF nanopowder seems to be
governed by the presence of ionic and bulky structural
motifs which is in good agreement with the
pharmacophore. The presence of these helps the
compound to interact or penetrate more with cell
membrane of the microorganisms and there by inactivating
them.

Fig.5b Comparison of efficacy of convetional

antibiotics and ZF nanopowder.

Overall it is clear that the gram positive bacteria

(Mycobacterium tuberculosis, Staphylococcus aureus) are
more sensitive to nanoparticles than gram negative
bacteria (Escherichia coli, Pseudomonas aeruginosa) [1112]. This may be due to the distance between the positively
charged groups and the nanoparticles. Another widely
postulated mechanism is that of the self-promoted
uptake of the antibiotic across the outer membranes of
bacteria which consist of lipopolysaccaride surface. This
suggests that the nanoparticles interact with the charged
outer membrane and subsequent channel formation in the
cytoplasmic membrane via either Barrel-Stave or
Carpet mechanism resulting in cell death.

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5. CONCLUSION
The present study demonstrates the facile synthesis of
ZnFe2O 4 nanopowder of sizes 12 nm, by nucleation
followed by controlled growth of ZnFe2O4 nanopowder.
The prepared ZnFe2O4 nanopowder is more sensitive than
the conventional antibiotics due to the reactive oxygen
species formation and lesser ionic size of the ZnFe2O4
nanopowder. Further, ZnFe2O4 nanopowder, applied at
higher concentrations, may also be used as antibacterial
agents. In the future, the study of the antibacterial activity
of the ZnFe2O4 nanopowder will be extended to include
other bacterial pathogens, and the utilization of this
nanopowder for targeted drug delivery system will also
be investigated.

3.

G.Nocoara, D. Fratiloiu, MNogues et al Ni-Zn-ferrite nanoparticles prepared by ball milling Materials science forum,
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R.Qiao, C.Yang, and M. Gao, Superparamagnetic iron oxide

nanoparticles, from preparation to in vivo MRI applicatios,
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5.

R.Weissleder, A. Bogdanov, E. A. Neuwelt, and M. Papisov,

Longcirculating iron oxides for MR imaging, Adv. Drug
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6.

Fischbach MA, Walsh CT. Antibiotics for emerging

pathogens. Science 2009; 325 (5944): 1089-93.

7.

N. Jones, B. Ray, K.T. Ranjit, A.C. Manna, Antibacterial

activity of ZnO nanoparticle suspensions on a broad spectrum
of microorganisms, FEMS Microbiology Letters 279 (2008)
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8.

U.B. Gawas etal Synthesis and characterization of

NiZnFe2O4 nano-particles obtained by auto catalytic thermal
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Y. Koseoglu et al, Magnetic and dielectric properties of

MnNiFe2O4 nanoparticles synthesized by PEG-assisted
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10.

Huseyin Kavas et al Characterization of NiFe2O4 nanoparticles synthesized by various methods, chemical papers,
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11.

Synthesis and antibacterial activity of silver nanoparticles

against gram-positive and gram-negative bacteria. Nanomedicine: Nanotechnology, Biology, and Medicine 8 (2012)
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6. ACKNOWLEDGEMENT
Dr. B.M. Nagabhushana gratefully acknowledges
Visveswaraya Technological University, Belgaum for the
support (VTU/Aca./2009-10/A-9/11714) to carry out this
research work. The authors R.S. Raveendra, P.A.
Prashanth, B. Daruka Prasad, and N.P. Bhagya thank the
management of Sai Vidya Institute of Technology,
Bangalore for their encouragement.
7.

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