SYNTHESIS OF MAGNETITE NANO-PARTICLES BY REVERSE CO- PRECIPITATION

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1 2nd International Conference on Ultrafine Grained & Nanostructured Materials (UFGNSM) International Journal of Modern Physics: Conference Series Vol. 5 (2012) World Scientific Publishing Company DOI: /S SYNTHESIS OF MAGNETITE NANO-PARTICLES BY REVERSE CO- PRECIPITATION HAMID KAZEMZADEH School of Metallurgy and Materials Engineering, University of Tehran, Tehran, Iran hkazemzadeh@ut.ac.ir ABOLGHASEM ATAIE School of Metallurgy and Materials Engineering, University of Tehran, Tehran, Iran aataie@ut.ac.ir FERESHTEH RASHCHI School of Metallurgy and Materials Engineering, University of Tehran, Tehran, Iran rashchi@ut.ac.ir Magnetite nano-particles have been synthesized by reverse co-precipitation method using iron salts in alkaline medium in the presence of diethylene glycol (DEG). Effect of DEG on the nano-particle characteristics was investigated by XRD, FE-SEM, FTIR and VSM techniques. From XRD results it was concluded that in the presence of DEG the composition of magnetite did not change, however the mean crystallite size reduced from 10 to 5 nm. SEM micrograph showed that DEG decreased the size of spherical magnetite nano-particles from 50 to 20 nm. Fourier transform infrared spectra (FTIR) indicated that the DEG molecules chemisorbed on the magnetite nano-particles. Under the given experimental conditions, the rate of crystallization and growth reduced, which is probably due to the capping of DEG to the magnetite nano-particles. The agglomeration was also decreased which is attributed to the coating of magnetite nano-particles by DEG which prevents the formation of hydrogen bonding between magnetite and water molecules. Keywords: Nano-particles; magnetite; reverse co-precipitation; DEG. Corresponding author: Tel.: ; Fax: P.O. Box:

2 Synthesis of Magnetite Nano-Particles by Reverse Co-Precipitation Introduction Magnetite nano-particles (Fe 3 O 4 ) have been used widely for various applications such as magnetic recording media, pigment, photocatalysis, etc. 1 In recent years, magnetite nanoparticles have become attractive for biomedical applications including drug delivery, magnetic resonance imaging (MRI), hyperthermia, cell separation, etc due to their biocompatibility, magnetic properties and biodegradability. 2, 3 The magnetite nano-particles inclination to agglomeration and their oxidation in air are common problems. The colloidal stability of bare magnetite nano-particles is ensured by electrostatic repulsion. Hence, the magnetite nano-particles have been coated with appropriate organic materials to overcome these problems. Uncharged inorganic materials such as DEG adsorb on oxide surfaces due to interaction between polar functional groups of DEG molecules and hydroxylated/protonated surface sides of the oxide. 4 As a consequence the control of particles morphology and their stability in the solvent media which are all depend on the synthesis route is the key factor in the processing of magnetite nano-particles. Numerous methods such as self-propagating high-temperature synthesis (SHS) 1, thermal decomposition, micro-emulsion, hydrothermal and sonochemical synthesis 5 have been employed to synthesize magnetite nano-particles. Conventionally, magnetite nanoparticles have been prepared by co-precipitation from a solution of Fe 3+ and Fe 2+ salt in alkaline medium. Different wet-chemical synthesis parameters such as Fe 2+ /Fe 3+ ratio, ionic strength, ions concentration and ph value affect the resulting iron oxide characteristics. 6 The overall reaction equation may be indicated as follows: Fe Fe OH Fe 3 O 4 + 4H 2 O (1) In a normal co-precipitation system, an alkaline solution is dropped into the solution mixture of iron salts and ph increases gradually. After increasing ph to 3, Fe 3+ ions are immediately precipitated as ferrihydrite, which then reacts with the existing Fe 2+ ions in the solution to form magnetite. The electron transfer between Fe 2+ and Fe 3+ plays a basic role in the crystallization process and more than 10 mol% of Fe 2+ ions persuade the crystallization of all the iron into spinel. 7 In the reverse co-precipitation method, the iron salts solution is dropped into an alkaline solution. Aono et al. showed that the gradual increase in ph value would cause an increase in the mean crystallite and the particle size for the normal method as compared to the reverse method. 8 In this study, magnetite nano-particles were produced by reverse co-precipitation method and the effect of various amounts of DEG on the nano-particles characteristics was investigated.

3 162 H. Kazemzadeh, A. Ataie & F. Rashchi 2. Experimental procedure Chemicals used in this study were ferric chloride (FeCl 3.6H 2 O), ferrous chloride (FeCl 2.4H 2 O), sodium hydroxide (NaOH) and diethylene glycol (DEG). All the materials used were analytical grade. The DEG-coated magnetite nano-particles were synthesized and characterized according to the flowchart shown in Fig.1. The iron salts solution was prepared by dissolving 3.24 g (0.02 moles) of FeCl 3.6H 2 O and 1.99 g (0.01 moles) of FeCl 2.4H 2 O in 20 ml de-ionized water at 25 C for 20 minutes. To prepare the 8 mol/l alkaline solution, 4.58 g of NaOH was added to 14 ml of de-ionized water and stirred for 30 minutes at 25 C. Various amounts of DEG was added to the alkaline solution. To precipitate magnetite nano-particles, iron salts solution was dropped into the NaOH solution at 80 C while it is stirring. To remove the NaCl, the co-precipitated samples were washed with distilled water and acetone. Phase composition of the samples was analyzed by Philips PW3170 XRD using Co- Kα radiation (λ= Å). The mean crystallite size of the samples was calculated by XRD line broadening technique using Scherrer formula 9. Hitachi4160 FE-SEM was used to determine the morphology of the samples. Surface structure of the samples was appraised by BRUKER-TENSOR27 Fourier transform infrared (FTIR) spectroscopy using KBr in the range of cm 1. Vibrating sample magnetometer (VSM) was employed to evaluate the magnetic properties of the samples at room temperature. Fig. 1. Experimental procedure for DEG-coated magnetite nano-particles synthesis.

4 Synthesis of Magnetite Nano-Particles by Reverse Co-Precipitation Results and discussion Fig. 2 shows the X-ray diffraction patterns of the co-precipitated samples with different DEG concentrations. Analysis of the XRD patterns confirm that magnetite has formed at all the conditions applied. Peak broadening indicating the crystallite refinement observed for samples processed in the presence of DEG. Table 1 shows the mean crystallite size of magnetite nano-particles using Scherrer formula from the XRD peak. Fig. 2. XRD patterns of the synthesized samples with various DEG amount (a) no DEG, (b) 2 ml DEG and (c) 5 ml DEG. Table 1. The mean crystallite size of magnetite nano-particles calculated from XRD patterns. Sample DEG amount (ml) Mean crystallite size (nm) a 0 10 b 2 5 c 5 7 Fig. 3 illustrates the SEM images and particle size of magnetite nano-particles. As shown in Fig. 3(a), most of the magnetite nano-particles synthesized in the absence of DEG are spherical with a mean particles size of 50 nm. The particles were severely agglomerated due to their high surface energy. Addition of 0.5 ml DEG reduces the mean particle size to about 30 nm, the rate of agglomeration is significantly increased (Fig. 3(b)). In the presence of 2ml DEG, less agglomerated and mono-dispersed nanoparticles of magnetite with mean particle size of 20 nm were obtained (Fig. 3 (c)). This is caused by the separation of nucleation and growth stages. 10 Nucleation of magnetite and its coating were carried out synchronic. In fact, DEG prevents the formation of hydrogen

5 164 H. Kazemzadeh, A. Ataie & F. Rashchi bondings between magnetite particles and water molecules, hence the particle sizes and the agglomeration reduced. The DEG amount must be adequate to acquire a uniform distribution of iron salts cations and coat the magnetite nano-particles. Also, Weak hydrogen bondings in hydrated DEG redound to homogeneous physical entrapment between hydroxyl groups and solvated cations by water molecules. 11 Fig. 3(d) indicates that the excess amount of DEG chains due to hydrogen bridging between adsorbed DEG molecules on magnetite nanoparticles surfaces tend to increasing of agglomeration above the critical concentration. In fact, in the presence of DEG, a chelating reaction occurs between iron salts cations and hydroxyl groups in the DEG. In fact, the cations are sterically entrapped in the entangled network of the DEG. The coexistence of DEG networks as nano-reactors at the moment of co-precipitation reaction slow down growth and agglomeration of the magnetite nuclei. The growth of the nuclei reaches to a limiting value at higher residence time in the enmeshed network of DEG. 11 Fig. 3. FE-SEM images of the magnetite nano-particles (a) no DEG (b) 0.5 ml DEG (c) 2ml DEG and (d) 5ml DEG.

6 Synthesis of Magnetite Nano-Particles by Reverse Co-Precipitation 165 To get further insight into the mechanism of the DEG interaction with the magnetite nano-particles surface, the FTIR spectroscopy was carried out on the synthesized magnetite nano-particles. Fig. 4 shows the typical FTIR spectrum of the magnetite nanoparticles synthesized in the presence of 2 and 5 ml of DEG. In spectra (a) the absorption at 635 cm 1 and the broad peak at about 3400 cm 1 are assigned to the Fe O and OH groups, respectively. Two bands at 2924 and 2847 cm 1 are attributed to the asymmetric CH 2 stretch and the symmetric CH 2 stretch, respectively. In spectra (b) the asymmetric CH 2 stretch and the symmetric CH 2 stretch bands shifted to 2921 and 2845 cm 1, respectively. The shifting of CH 2 characteristic bands to a lower frequency region is due to the hydrocarbon chains surrounding the nano-particles. 12 The typical band near 1520 cm 1 is related to the bending vibration of the hydroxyl bond. The absorption peaks at 1330 and 1050 cm 1 are resulted from the stretching vibration of the C O bond of the CH 2 OH group. 13 The peak at 1081 cm 1 also indicates the stretching vibration of the C O C group. These results suggest that DEG was chemisorbed onto the magnetite nano-particles. Fig. 4. FT-IR spectra of magnetite nano-particles synthesized in the presence of (a) 2 ml DEG (sample b) and (b) 5 ml (sample c) of DEG. Magnetization curves of the un-coated sample and coated samples with 2 ml DEG are shown in Fig. 5. Saturation magnetization (Ms) decreased from 54.7 in un-coated sample (a) to 29.8 emu/g in DEG coated sample (b), while the coercivity (Hc) reduced from 7.0 to 0.6 Oe. The reduction of saturation magnetization in coated sample is probably due to the smaller particles of magnetite as well as the existence of the DEG dead layer on the surface of magnetite nano-particles. Also, with a significant fraction of

7 166 H. Kazemzadeh, A. Ataie & F. Rashchi surface atoms, any crystalline disorder within the surface layer may lead to a significant decrease in the saturation magnetization of nano-particles Conclusions Fig. 5. Magnetization curves of (a) un-coated and (b) DEG coated samples. - The one-step reverse co-precipitation method was employed to synthesize DEG-coated magnetite nano-particles. - In the presence of DEG the mean crystallite size and particle size of magnetite nanoparticles reduced. - In the presence of DEG, the aggregation of the magnetite nano-particles reduced due to the partially coating of their surfaces. - The saturation magnetization and coercivity of magnetite nano-particles decreased for coated samples. 5. Acknowledgements The financial support of this work by the Research Council of the University of Tehran is gratefully acknowledged. References 1. A. Ataie, H. Kazemzadeh, R. Nikkhah-Moshaie and F. M. Ahmed, IEEE. Trans. Magn. 45(6), 2496 (2009). 2. C. Sun, J.S.H. Lee and M.Q. Zhang, Adv. Drug Delivery Rev. 60(11), 1252 (2008). 3. Y. Mizukoshi, T. Shuto, N. Masahashi and S. Tanabe, Ultrason. Sonochem. 16(4), 525 (2009). 4. M. Chastellain, A. Petri and H. Hofmannknkn, J. Colloid Interface Sci. 278(2), 353 (2004).

8 Synthesis of Magnetite Nano-Particles by Reverse Co-Precipitation W. Wu, Q. He and C. Jiang, Nanoscale Res. Lett. 3(11), 397 (2008). 6. S. C. Pang, S. F. Chin and M. A. Anderson, J. Colloid Interface Sci. 311(1), 94 (2007). 7. G. Gnanaprakash, S. Mahadevan, T. Jayakumar, P. Kalyanasundaram, John Philip and Baldev Raj, Mater. Chem. Phys. 103(1), 168 (2007). 8. H. Aono, H. Hirazawa, T. Naohara, T. Maehara, H. Kikkawa and Y. Watanabe, Mater. Res. Bull. 40(7), 1126 (2005). 9. D. Cullity, Elements of X-ray diffraction (Addison-Wesley, Massachusetts, 1978). 10. P. Tartaj, M.d.P. Morales, S. Veintemillas-Verdaguer, T. González-Carreño and C.J. Serna, J. Phys. D: Appl. Phys. 36(13), R182 (2003). 11. C. Xu and A.S. Teja, J. Supercrit. Fluids 44(1), 85 (2008). 12. L. Zhang, R. He and H.C. Gu, Appl. Surf. Sci. 253(5), 2611 (2006). 13. H. Kozuka, Handbook of sol-gel science and technology: sol-gel processing (Springer Publications, New York, 2005). 14. G.Y. Li, Y.R. Jiang, K.L. Huang, P. Ding and J. Chen, J. Alloys Compd. 466(1-2), 451 (2008).

(received: 31/7/2004 ; accepted: 25/9/2004)

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