XRD, FT-IR and SEM Study of Magnetite (Fe3O4) Nanoparticles Prepared by Hydrothermal Method

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1 NANO VISION, Vol.5(4-6), , April-June 2015 (An International Research Journal of Nano Science & Technology), ISSN (Print) ISSN (Online) XRD, FT-IR and SEM Study of Magnetite (Fe3O4) Nanoparticles Prepared by Hydrothermal Method T. Saranya 1, K. Parasuraman 1, M. Anbarasu 2 and K. Balamurugan 3 1 Department of Physics, Poompuhar College, Melaiyur, Tamilnadu, INDIA. 2 Department of Physics, Annai College of Arts and Science, Kumbakonam, Tamilnadu, INDIA. 3 Department of Physics, Annamalai University, Annamalainagar, Tamilnadu, INDIA. parasu1959@gmail.com. Presented in Second National Conference on Thin Film Science and Nano Technology (SECOND-NCTFSANT-2015) March 2-3, 2015, Rajah Serfoji Govt. College, Thanjavur, T.N. (India). ABSTRACT Nanoparticles semiconductor metal oxides achieved a great importance in Environment and industrial world today. Nanoferrite powders were prepared using a simple cost effective method at low temperature. Magnetite (Fe 3 O 4 ) nanoparticles synthesized via co-precipitation method from ferrous and ferric solutions. X-ray diffraction (XRD) was used to determine the particle size and structural properties, the microstructure, and the particle size were determined by scanning electron microscopy (SEM). FT-IR study was used to confirm the presence of functional groups in Fe 3 O 4 nanoparticles and the corresponding bands were observed. Keywords: Hydrothermal, Magnetite, X-Ray Diffraction. 1. INTRODUCTION Magnetic nanomaterials have attracted considerable attention because of their unique size-dependent properties, intriguing a variety of architectural structures and many important technological applications. Iron oxide nanomaterials have attracted great attention from many research fields. They have been found highly applicable and versatile in lithium ion batteries 1 supercapacitors 2 catalysis 3 tissue-specific releasing of therapeutic agents 4 labeling and sorting of cells 5 as well as the separation of biochemical products 6,7. Due to their super paramagnetic property and low toxicity, magnetic iron oxide (Fe 3 O 4 and Fe 2 O 3 ) nanoparticles are especially interesting to biomedical applications. However, mono disperse magnetic nanomaterials exhibit extraordinary shape dependent properties greatly different from those of their bulk nanomaterials. They have inspired scientists in recent years, in respect that the monodisperse magnetic nanoparticles not only offer better operable properties for their super paramagnetic Nano Vision Vol. 5, Issue 4-6, April-June, 2015 Pages (39-168)

2 150 T. Saranya, et al., Nano Vision, Vol.5 (4-6), (2015) feature, but also have comparatively increased overall surface area and penetration for intensive performance in their application. Magnetite (Fe 3 O 4 ) is a kind of excellent magnetic material among iron oxides. It has a cubic inverse spinel structure within which oxygen forms a FCC closed packing and Fe ions occupy the interstitial tetrahedral sites and octahedral sites, and bears distinguished electric and magnetic properties on account of the hopping of electrons between Fe 2+ and Fe 3+ in the octahedral sites. Magnetite has been widely applied in numerous fields such as ferrofluid, catalysis, pigment color, magnetic storage media, environment protection, cell separation, clinic diagnosis, and therapy. Until now, various magnetite structures including nanocrystalline, particles, wires, rods, tubes, and nano sheets was successfully synthesized with diverse methods. Nevertheless, synthesis of monodisperse Fe 3 O 4 nanoparticles with uniform shape and relatively uniform size is still a challenge. The synthesis of Fe 3 O 4 particles using a variety of chemistry based synthetic strategies has been reported in the literature, for example thermal decomposition, reverse micelles, co-precipitation, sol gel processing, hydrothermal processing, sonochemical route, etc Among these synthetic methods, hydrothermal synthesis combined with organic templates for fabricating size controlled and shape controlled nanomaterials is an ideal and promising approach, because other synthetic procedures usually require expensive and some-times toxic reagents, complicated synthetic steps, and high reaction temperatures. In this article, monodisperse Fe 3 O 4 nanoparticles were synthesized via hydrothermal route. The hydrothermal reaction was operated at relatively low temperature of 120 C, which can effectively save energy. Hence, this method will be a promising strategy for large-scale production. In this study, Fe 3 O 4 nanoparticles were prepared by simple hydrothermal method. In this method to develop, a general synthetic process and explore the structural properties of the Fe 3 O 4 nanoparticles. We found that the process was convenient, environment friendly, inexpensive and efficient. 2. EXPERIMENTAL METHODS 2.1 Preparation of Magnetite (Fe 3 O 4 )nanoparticles Fe 3 O 4 nanoparticles were synthesized by the hydrothermal method. All chemical reagents used as starting materials are of analytical grade and purchased without any further purification. In a typical synthesis process, 0.05M of ferrous Chloride (Fe 2 Cl 3 ) was dissolved in 100 ml aqueous solution under vigorous stirring to form a clear solution, and then 15ml of ammonia (NH 4 ) solution were added to the above solution. This mixture was then vigorously stirred at room temperature for 1 hour to form a homogeneous solution. Finally, the mixture transferred into a 100 ml Teflon-lined autoclave, which heated at 120 o C for 3 hr. After being cooled to room temperature, the black powders were collected and washed several times with distilled water and ethanol to remove the impurities, and finally dried at 80 o C in a vacuum oven for 1 hr. Nano Vision Vol.5, Issue 4-6, April-June, 2015 Pages (39-168)

3 2.2. Characterization T. Saranya, et al., Nano Vision, Vol.5 (4-6), (2015) 151 Prepared Fe 3 O 4 nanoparticles were characterized by various techniques. The structural characterization was performed using a PhilipX PERT-PRO diffractometer system. CuK α line with wavelength of Å is generated with a setting of 30 mill amperes and 40 kv with the electrode is used for diffraction with CuKα radiation. The infrared spectra of prepared samples were recorded in the vibrational frequency ranging from 4000 to 400 cm -1 using a JASCO 460 plus FTIR spectrometer. Size and shape of the particles were determined using Scanning electron microscopy (SEM JSM-5610) analysis. 3. RESULTS AND DISCUSSION 3.1. X-ray diffraction analysis The XRD pattern of Fe 3 O 4 nanoparticles were prepared at room temperature is shown in Fig.1.The XRD data clearly confirm the crystalline phase of ferrite (Fe 3 O 4 ) to be very close to the JCPDS No For the prepared Fe 3 O 4 the most intensive lines (311) and (440) are observed the diffraction peak indicated at 2θ= and The XRD pattern shows the prepared nanoparticles are in a cubic structure of Fe 3 O 4. It can be seen that, the sites and intensity of the diffraction peaks are consistent with the standard pattern for JCPDS Card No The sample show very broad peaks, indicating the ultra-fine nature and small crystallite size of the particles. Cubic single-phase nano sized Fe3O4 powder has been obtained. The observed peaks and structure are good agreement with the reported values of Hironori Iida et al., (2007). The crystallite size of the Fe 3 O 4 product is determined by using Debye Scherrer s formula 14, D = k / β Cosθ Where, K=0.89 is the shape factor, λ is the X-ray wavelength of CuKα radiation, β is the full width at half maximum (FWHM) of the peaks and θ is the glancing angle and the average crystallite size is 13 nm. Fig.1: X-ray diffraction pattern of Fe3O4 nanoparticles synthesized by hydrothermal method Nano Vision Vol. 5, Issue 4-6, April-June, 2015 Pages (39-168)

4 152 T. Saranya, et al., Nano Vision, Vol.5 (4-6), (2015) 3.2. Fourier Transform Infrared (FT-IR) spectral Analysis FT-IR spectra (Fig.3) of Fe 3 O 4 clearly shows an absorption bands around cm 1, which are characteristic stretching vibration of hydroxyl functional group (H-O-H) on the surface of nanoparticles or adsorbed water in the sample. The absorption band at 1721 cm 1 corresponds to stretching vibration of carbonyl group (C-O). The stretching vibration of the carboxylate group (C=O) is observed around cm 1. The bending vibration of H-O-H group also localized at cm 1. The absorption band around cm 1 is assigned the stretching vibration of C-C-C group. The above observed FTIR spectra confirm the presence of organic impurities in the sample during the preparation. In addition, two absorption bands at 584 cm 1 and cm 1 are corresponding to the vibration of tetrahedral and octahedral complexes respectively, which are indicative of formation of spinel ferrite structure. As can be seen from the spectra, the normal mode of vibration of tetrahedral cluster (584 cm 1 ) is higher than that of octahedral cluster (442 cm 1 ). The shouldering of the band corresponding to the tetrahedral site is observed for the sample. Fig. 2:Fourier Transform - Infrared (FTIR) spectrum of Fe3O4 nanoparticles It is attributed to the John-Teller s distortions produced by the Fe 2+ ions that causes local deformations in the lattice owing to the non-cubic component of the crystal field potential, and hence lead to the splitting of this band, corresponding to the tetrahedral site. Finally, the bands can be observed at 584 and cm -1, which corresponds to Fe 3 O 4 and due shoulders cm -1 that can be assigned to magnetite, i.e., the oxidized from of magnetite, probably present at the nanoparticle surface. X-ray spectra did not show any peak that could correspond to the presence of magnetite Surface morphology Analysis Fig.3 shows the SEM micrographs clearly show the surface features, by which it highlight that Fe 3 O 4 nanoparticle was successfully prepared. It is cleared that the tested particles are spherical in shape with a narrow size distribution and their particle sizes are nm which is approximately the size calculated by the Debye Scherrer formula. From the SEM results, the prepared crystallites are nearly spherical in shape and it can be seen that the Nano Vision Vol.5, Issue 4-6, April-June, 2015 Pages (39-168)

5 T. Saranya, et al., Nano Vision, Vol.5 (4-6), (2015) 153 particles agglomeration, indicating a good connectivity between the grains together and the size of which is about nm. The nanoparticles were agglomerated from few µm to a few tens of µm. The agglomeration was reduced with increase in grain growth. 4. CONCLUSION Fig. 3: SEM images of Fe3O4 nanoparticles Fe 3 O 4 nanoparticles with cubic structure have been successfully synthesized by hydrothermal method. From the SEM results, the prepared crystallites are nearly spherical in shape with a narrow size distribution and their particle sizes are nm which is approximately the size calculated by the Debye Scherrer formula. FT-IR study also confirm the presence of functional groups in Fe 3 O 4 nanoparticles and the bands can be observed at 584 and cm -1, which corresponds to Fe 3 O 4, and due shoulders that can be assigned to magnetite. X-ray spectra did not show any peak that could correspond to the presence of magnetite. It confirms the cubic structure of Fe 3 O 4 nanoparticles and the average particle size of the magnetite obtained from the peak broadening was 13-17nm. ACKNOWLEDGMENT The Corresponding author Dr. K. Parasuraman, would like to express his thanks to the University Grants Commission, South Eastern Region (UGC-SERO), Hyderabad, India, for sanctioning the financial assistance [F. No.6304/15 Dated:] to carry out the present research work. REFERENCES 1. Koo B, Xiong H, Slater M D, Prakapenka V B, Balasubramanian M, Podsiadlo P, Johnson C S, Rajh T and Shevchenko E V, Nano. Lett (2012) 2. Du X, WangC, Chen M, Jiao Y and Wang J. J. Phys. Chem.C (2009). 3. Lin S, Shen C, Lu D, Wang C and Gao H J. Carbon (2013) 4. Fukushima T, Sekizaqa K, Jin Y, Yamaya M, Sasaki H and Takishima T. Am. J. Physiol. 265 L67 (1993). Nano Vision Vol. 5, Issue 4-6, April-June, 2015 Pages (39-168)

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