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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.

c

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

d

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

e

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, Luria–Bertani
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, sol–gel, 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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5405Ao). Fourier transform infrared (FTIR) spectra were recorded in absorption mode with Perkin Elmer FT-IR spectrometer (Spectrum 1000) along with KBr pellets. Sample Code Powder Density [gm/cc] 2 [deg] ZF 1.1a.?? are measured from the PXRD graph as shown in the Fig. preheated to 300 0 C.011 12 X Ray density g/cc 2. 544 .9 is taken for calculation. All the diffraction peaks confirmed the formation of the pure single-phase ZF with cubic spinel phase and Fdm (227) Fig. MATERIALS AND METHODS Chemicals including zinc nitrate (Zn(NO3)2. 1a PXRD pattern of the prepared ZF sample. Where ‘d’ is the average crystalline dimension perpendicular to the reflecting phases.398 2. ‘57’is the full width at half maximum intensity of a Bragg reflection excluding instrumental broadening and ‘5. RESULTS AND DISCUSSIONS 3.32 FWHM Crystal [radians] size [nm] 0. ‘k’ is Schrrer constant varies from (0. Issue 04 the cytotoxicity of the nanoparticles remain a major concern [8-10]. 3. The solution was stirred with magnetic stirrer for twenty minutes. the average value of 0. 1b PXRD pattern for (311) peak. where the smoldering type ignition took place.2 Measurements Powder X-ray diffraction (PXRD) analysis was conducted on Philips analytical X-ray diffractometer using CuKa radiation (5=1. The crystal size and the density of the ZF sample are summarized in Table-1.6H2O) ferric (III) nitrate (Fe(NO3)3. and freshly prepared oxalyl dihydrazide (ODH) (C2H6N4O2) used as starting materials without further purification. ‘5’ is the X-ray wavelength. In solution combustion method of preparation.1b.60 35.92). 22-1012). FT-IR spectra in the range 300-4000 cm-1 were recorded in order to study the nature of the chemical bonds formed. The antibacterial activity of the synthesized ZF nanopowder was done by disc diffusion assay by using standard medium. Fig. Deionized water was used to prepare all solutions. space group (JCPDS No. UV-Vis spectra of the samples were recorded with the Specord S600 .1 PXRD analysis The PXRD pattern of the as formed sample for combustion synthesis was shown in Fig. 2. 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.880.? is the Bragg’s angle. 2.1 Synthesis of zinc ferrite Zinc ferrites with stoichiometric composition were prepared by solution combustion method. 1 Powder density and crystal size. producing a zinc ferrite in froth form. Table.Inernational Journal of Science Research Volume 01. The average crystallite size of sample was estimated by employing the Debye-Scherrer formula. The stirred solution was kept in muffle furnace. Morphologies of ZF were examined by scanning electron microscope (SEM) JEOL (JSM-840A).212C205 spectrometer and the samples were obtained by dispersing the powder in liquid paraffin. ferric nitrate hydrate and freshly prepared oxalyl dihydrazide (ODH) mixture are taken in a crystalline dish and dissolved in a minimum amount of water.9H2O) were all purchased from MERCK. zinc nitrate hydrate. 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. ‘57’? and ‘5.

2a FTIR spectra of ZF sample. 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. Fig. The highest wave number is for Zn2+.3 SEM image of ZF sample. Plotting (ahc/5)2 as a function of photon energy (hc/5). SEM analysis shown in Fig. by fitting reflection data to the direct transition equation Where?545 ?5’ is the wavelength.4 UV-Vis spectra of ZF.2b Main metal-oxygen bands of FTIR spectra. Fig. the FT-IR bands of solids are usually assigned to vibration of ions in the crystal lattice. Issue 04 3.2a and 2b. i.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. Two main broad metal-oxygen bands are seen in the FT-IR spectra of spinel ferrite in particular.3 SEM analysis In the range of 4000-310 cm-1. Fig. Fig.e. whereas the lowest band observed in the range of 450-375 cm-1 is assigned to octahedralmetal stretching. gives the value of the direct band gap (Eg). 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. The inset of Figs. and extrapolating the linear portion of the curve to absorption equal to zero as shown in Fig. corresponds to intrinsic stretching vibrations of the metal at the tetrahedral site. 3/2. respectively.2 FT-IR analysis 3..stretching vibration occurring from the residual nitrate groups of metal nitrates. TEM analysis for the same is under progress. 545 . The highest one generally observed in the range of 600-540 cm-1. 2 and 3 depending on the mode of inter-band transition. The resolution used in this study cannot detect the individual crystallites. indirect allowed and indirect forbidden transition.Inernational Journal of Science Research Volume 01. which prefers tetrahedral sites because of its capability to form covalent bonds involving sp3 hybrid orbitals. The band at 1356 cm-1 is associated with the antisymmetric NO3.4 UV-Vis spectra analysis and evaluation of Energy gap (Eg) The energy gap (Eg) has been evaluated for ZF prepared by solution combustion method. ‘A’ is a constant and ‘n’ can have values 1/2. 3. 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. direct allowed and direct forbidden. 4. 4 show the UV-Vis absorption spectrum is taken in the range of 200 to 1020 nm.

The antibacterial activity of the prepared ZF nanopowder was tested using four common bacterial pathogens: Escherichia coli. The results are summarized in Fig. (ii) the ionic size of ZF and (iii) reactive oxygen species (ROS) formation. This may be due to the distance between the positively charged groups and the nanoparticles. Pseudomonas aeruginosa (Gram negative).Inernational Journal of Science Research Volume 01. 105 cells/ml in LuriaBertani broth (LB) were shaken (250 rpm) in light with zinc ferrite nanopowder (0.5b Comparison of efficacy of convetional antibiotics and ZF nanopowder. tuberculosis 15 6 S. 2a Antibacterial activity of ZF by Luria-Bertani broth method. 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. Pseudomonas aeruginosa) [1112].2b Antibacterial activity of conventional antibiotics.aeruginosa 17 5 M. No. 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. aureus 16 Table. Staphylococcus aureus) are more sensitive to nanoparticles than gram negative bacteria (Escherichia coli. Conventional antibiotics Zone of inhibition in diameter (mm) 1 Streptomycin 35 2 Tetracycline 40 Fig.. 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. ANTIBACTERIAL STUDIES Table. Mycobacterium tuberculosis. Controle refers to bacteria incubated without ZF nanopowder. The concentration used for test compound and that of standard remains the same. Fig.. streptomycin and tetracycline. The number of feasible bacteria was determined by plotting successive dilutions on LB agar plates and determining number of colony forming units (CFU). The presence of these helps the compound to interact or penetrate more with cell membrane of the microorganisms and there by inactivating them. Fig. The fallowing factor may be responsible for the enhancement of antibacterial activity viz.e. Sl.5a. Sl. 546 .5b and tables 2a.3%) for 24 h at 370 C. Each fragment of this compound i. Bacterial pathogens Zone of inhibition in diameter (mm) 1 Controle 80 3 E. zinc nitrate and ferric nitrate were as such tested for antibacterial activity and found inactive. Issue 04 4. No. (i) the improved colloidal aqueous stability of magnetic composite nanoparticles from the combination of zinc oxide with iron oxide. Overall it is clear that the gram positive bacteria (Mycobacterium tuberculosis. Staphylococcus aureus (Gram positive). 2b.. 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.coli 18 4 P. 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.5a Efficacy of ZF nanopowder on various bacterial pathogens. In brief.

450-455. Nanomed Nanotechnol Biol Med 2007. Huseyin Kavas et al “Characterization of NiFe2O4 nanoparticles synthesized by various methods”. K. and M. D. Appl Environ Microbiol 2007. ACKNOWLEDGEMENT Dr.. applied at higher concentrations. Y. York. 7. vol.Weissleder. 10. B. Koseoglu et al.3:168-71. Further. 321–334.Nocoara. Biology. Prashanth. Y.19. Drug Delivery Rev. no35. vol. A.” Adv. Neuwelt. Manna. Stéphane Godet.S.1 pp 145-150. published online by Springer (2010). 325 (5944): 1089-93. Issue 04 5. the study of the antibacterial activity of the ZnFe2O4 nanopowder will be extended to include other bacterial pathogens. 1995. DOI 10. Papisov./2009-10/A-9/11714) to carry out this research work. 3. CONCLUSION The present study demonstrates the facile synthesis of ZnFe2O 4 nanopowder of sizes 12 nm. 11. Gawas etal “Synthesis and characterization of NiZnFe2O4 nano-particles obtained by auto catalytic thermal decomposition of carboxylato-hydrazinate complex”. Bhagya thank the management of Sai Vidya Institute of Technology. Bangalore for their encouragement. Raveendra. Jean Dille. 879-883. “Investigation into the antibacterial behaviour of suspensions of ZnO nanoparticles” (ZnO nanofluids).M. B. G. and the utilization of this nanopowder for targeted drug delivery system will also be investigated. J Therm Anal Calorim. Nanomedicine: Nanotechnology.P. P. Pal S. MNogues et al “Ni-Zn-ferrite nanoparticles prepared by ball milling” Materials science forum. “Magnetic and dielectric properties of MnNiFe2O4 nanoparticles synthesized by PEG-assisted hydrothermal method” J. 4. Ray. Journal of Nanoparticle Research 9 (2007) 479–489.1007/s11051-010-9982-6. The authors R. Belgaum for the support (VTU/Aca. E. no.6274-6293. Jiang. Bogdanov. L.(2011). C. Walsh CT. 104. Daruka Prasad. 6. pp.Inernational Journal of Science Research Volume 01. Jones. Myong Song J. ZnFe2O4 nanopowder.73:171220. may also be used as antibacterial agents. Nagabhushana gratefully acknowledges Visveswaraya Technological University. 5.2009. 547 . “Superparamagnetic iron oxide nanoparticles. A. FEMS Microbiology Letters 279 (2008) 71–76. [11] Maribel Guzman. Shahverdi HR.B. 12. M. 9.1997. by nucleation followed by controlled growth of ZnFe2O4 nanopowder. Science 2009. Ranjit. (2009). 16. Kyung Y. Fischbach MA. from preparation to in vivo MRI applicatios”.C. R. 7. and N. Does “The antibacterial activity of silver nanoparticles depend on the shape of the nanoparticle? A study of the gram-negative bacterium Escherichia coli”. Fratiloiu. Gao. B. Fakhimi A. “Longcirculating iron oxides for MR imaging. A.T. R.Yang. 6. 63-4. Minaian MS.A. Shahverdi AR. D. “Synthesis and effect of silver nanoparticles on the antibacterial activity of different antibiotics against Staphylococcus aureus and Escherichia coli”.Nanopart Res. Antibacterial activity of ZnO nanoparticle suspensions on a broad spectrum of microorganisms. pp.Qiao. 8. Povey. “Antibiotics for emerging pathogens”. Y. “Synthesis and antibacterial activity of silver nanoparticles against gram-positive and gram-negative bacteria”. Ding. U. In the future. 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. Journal material chemistry. 2. N. and M. and Medicine 8 (2012) 37–45. chemical papers. Zhang. REFERENCES 1.