Electrodeposition of hybrid organic inorganic films containing iron oxide

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1 January 2003 Materials Letters 57 (2003) Electrodeposition of hybrid organic inorganic films containing iron oxide I. Zhitomirsky *, M. Niewczas, A. Petric Department of Materials Science and Engineering, McMaster University, 1280 Main Street West Hamilton, ON, Canada L8S 4L7 Received 13 May 2002; accepted 15 May 2002 Abstract A novel method has been developed for the preparation of hybrid organic inorganic films containing iron oxide. The method is based on cathodic electrodeposition of iron oxide nanoparticles in situ in a polyelectrolyte matrix. Prepared films were studied using thermogravimetric analysis and magnetic measurements. By manipulation of deposition conditions, the amount of the deposited material, deposit composition and magnetic properties could be varied. Magnetic measurements revealed that the nanocomposite films are superparamagnetic. D 2002 Elsevier Science B.V. All rights reserved. Keywords: Electrodeposition; Iron oxide; Poly(diallyldimethylammonium chloride); Film; Hybrid; Organoceramic; Superparamagnetism 1. Introduction * Corresponding author. Fax: address: (I. Zhitomirsky). The development of nanostructured organic inorganic hybrid materials presents new challenges and opportunities for future technologies [1 6]. The nanocomposites combine the advantageous properties of organic and inorganic components. Nanostructured magnetic materials are now being extensively studied for high-capacity magnetic storage media, integrated circuits, color imaging, magnetic refrigerators and biomedical applications. Below a critical size, nanocrystalline magnetic particles may be single domain and show the unique phenomenon of superparamagnetism [7,8]. A critical obstacle in assembling and maintaining a nanoscale magnetic material is its tendency to aggregate. To overcome this, nanoparticles of magnetic materials were isolated in a polymer matrix and advanced hybrid materials were developed [7 14]. Novel applications of superparamagnetic materials are inevitably related to the development of advanced techniques for deposition of thin films. Cathodic electrolytic deposition of thin films is a new technique in ceramic processing. The feasibility of electrodeposition of various thin film materials from aqueous solutions has recently been demonstrated. Review papers describing materials science aspects, mechanisms, kinetics of deposition and applications of electrolytic films are now available [15 17]. This method brings new opportunities in electrosynthesis of nanostructured thin films and powders from aqueous solutions of metal salts [18 21]. The important discovery was the feasibility of electrochemical intercalation of water-soluble polyelectrolytes into cathodic deposits prepared by electrolytic deposition [22]. We have begun to use charged polymers for prepara X/02/$ - see front matter D 2002 Elsevier Science B.V. All rights reserved. PII: S X(02)

2 1046 I. Zhitomirsky et al. / Materials Letters 57 (2003) tion of organoceramic films [23 25]. More recent explorations have illustrated the importance of this method for various applications [26,27]. Electrolytic deposition produces nanoparticles from solutions of metals salts in electrode reactions and provides their deposition. In this work by using cationic polyelectrolytes for electrodeposition, magnetic nanoparticles were created in situ in a polymer matrix. The process of electrodeposition and the properties of hybrid iron oxide-poly(diallyldimethylammonium chloride) films are presented in this report. 2. Experimental procedures Ferric chloride hexahydrate (FeCl 3 6H 2 O), ferrous chloride tetrahydrate (FeCl 2 4H 2 O) and poly(diallyldimethylammonium chloride) (PDDA) from Aldrich were used to formulate two stock solutions for electrodeposition. Stock solution 1 contained 3.3 mm FeCl 3, 1.65 mm FeCl 2 and 1 g/l PDDA. Stock solution 2 contained 3.3 mm FeCl 3, 1.65 mm FeCl 2 and 0.5 g/l PDDA. Deionized water was de-aerated prior to solution preparation using 93% Ar 7% H 2 gas. The gas flow was maintained through the solutions during deposition and through the chamber for film drying. The electrochemical cell for deposition included a cathodic substrate centered between two parallel platinum counterelectrodes. The films were deposited on Pt foil cathodes ( mm) at a current density of 10 ma/cm 2. The Pt substrates were weighed before and after deposition experiments followed by drying at room temperature for 48 h. After drying, the electrolytic deposits were scraped from the Pt electrodes for thermogravimetric (TG) analysis and magnetic measurements. The thermoanalyzer (Netzsch STH-409) was operated in air between room temperature and 1200 jc at a heating rate of 5 jc/min. Magnetic properties were studied using a Quantum Design PPMS-9 system. DC magnetization studies were performed using the extraction magnetometer option. Magnetization hysteresis loops were measured in the field range up to 10 koe at temperatures ranging from 2 to 298 K. The external magnetic field was changed in the sweep mode at the sweep rate of 10 Oe/ min. The temperature dependence of the magnetization was studied by both zero-field- (ZFC) and field-cooled (FC) procedures. The sample was cooled down to 1.9 K in the zero external field (ZFC) and then magnetization was measured during heating to 298 K under the applied field of 200 Oe. The sample was subsequently cooled back to 1.9 K under an applied field of 200 Oe (FC) and the measurements of magnetization were carried out during heating to 298 K. 3. Results and discussion In the cathodic electrodeposition method, the high ph of the cathodic region brings about formation of colloidal particles, which precipitate on the electrode. Reduction of water is the cathodic reaction that generates OH : 2H 2 O þ 2e! H 2 þ 2OH : ð1þ In previous work [22], it was suggested that intercalation of PDDA into electrolytic deposits is achieved via heterocoagulation of oppositely charged PDDA and colloidal particles of oxides or hydroxides formed near the cathode. Electrodeposition from stock solutions 1 and 2 resulted in the formation of cathodic deposits (deposits 1 and 2, respectively). Deposit weight increased linearly with deposition time as shown in Fig. 1. Fig. 1. Deposit weight vs. deposition time for deposits 1.

3 I. Zhitomirsky et al. / Materials Letters 57 (2003) Results of thermodynamic modeling [28,29] indicate that iron species precipitate as Fe 3 O 4 under basic conditions at a molar ratio of Fe 2+ :Fe 3+ =1:2 under a nonoxidizing environment: Fe 2þ þ 2Fe 3þ þ 8OH! Fe 3 O 4 þ 4H 2 O: ð2þ Cathodic electrolytic deposition is similar to the wet chemical method of ceramic powders processing that utilizes an electrogenerated base instead of alkali. Therefore, it could be suggested that iron species in our experiments precipitate as Fe 3 O 4. However, when precipitation of iron oxide is performed in a polymer matrix, we cannot exclude the possibility of formation of other phases [29]. Indeed, the formation of Fe 2 O 3 was observed in Refs. [8,14]. Fe 2 O 3 can exist in a thermodynamically stable a- Fe 2 O 3 form and a metastable g-fe 2 O 3 form. a-fe 2 O 3 (hematite) is antiferromagnetic. Both Fe 3 O 4 (magnetite) and g-fe 2 O 3 (maghemite) are ferrimagnetics with the spinel structure. The use of these ferrimagnetic materials with high Curie points allowed formation of advanced hybrid materials, which exhibited room temperature superparamagnetism when particle size was lower than nm [7 10,14]. Some difficulties were reported [13,14] in distinguishing between nanostructured magnetite and maghemite in composite materials using X-ray diffraction. The difficulties are related to peak broadening of the two nanostructured phases having relatively close lattice constants. Magnetic properties of nanoparticles could be different from the properties of corresponding bulk materials. It is known that decrease in particle size below 20 nm results in a significant decrease of the saturation magnetization of g-fe 2 O 3 [30]. In contrast, antiferromagnetic material may acquire a net moment when particle size is sufficiently low. However, magnetization of hybrid material based on a-fe 2 O 3 [11,13] was found to be low compared to that of composites based on g-fe 2 O 3 or Fe 3 O 4. Electrolytic deposition was proven to be an important technique for synthesis of nanostructured thin films [17 21]. In the current work, electrosynthesis of iron oxide was performed in situ in a polymer matrix. The polymer matrix is necessary to prevent oxide particle agglomeration caused by Van der Waals forces and magnetostatic interparticle interactions. Organic molecules exert an influence on the size of the oxide particles [7 14,28]. We utilized TG analysis and magnetic measurements to study the composition and properties of the prepared films. Fig. 2 compares the results of TG analysis of deposits 1 and 2. The TG curves indicate that the weight loss occurs in several steps. The total weight loss in the temperature range up to 1200 jc was found to be 75.4 and 58.1 wt.% for deposits 1 and 2, respectively. We suggest that observed weight loss is mainly attributed to burning out of an organic phase. It is important to note that magnetite might be oxidized during heating in air in the TG experiments [29]. However, our TG data indicate that the amount of an inorganic phase in deposits 2 is larger than that in the deposits 1. Indeed, sample weight at 1200 jc was found to be 24.6% and 41.9% of the initial sample weight for deposits 1 and 2, respectively. Therefore, higher concentration of PDDA in stock solution 1 compared to stock solution 2 resulted in higher concentration of an organic phase and lower concentration of an inorganic phase in deposits 1 compared to deposits 2. Similar results were reported in our previous investigations of other hybrid materials [23,26]. It was demonstrated that the amount of organic phase in deposits increases with increasing PDDA concentration in solutions [23,26]. Charged PDDA particles exert a shielding effect preventing electrosynthesis of oxide or hydroxide particles [23], Fig. 2. TG data for (a) deposits 1 and (b) deposits 2.

4 1048 I. Zhitomirsky et al. / Materials Letters 57 (2003) thus reducing the amount of inorganic phase in the hybrid materials. Room temperature magnetic measurements showed that dependence of magnetization vs. magnetic field for deposits 1 is nearly linear (Fig. 3a). However, at low temperatures, the isothermal magnetization as a function of applied field is essentially nonlinear as shown in Fig. 3b. For deposits 2, nonlinear dependence of magnetization was observed at room temperature and at lower temperatures (Fig. 4a,b). For both deposits 1 and 2, the magnetization increased with decreasing temperature (Fig. 3a,b and 4a,b). Higher magnetization was observed for deposits 2 compared to deposits 1 at the same temperatures (Fig. 3a,b vs. Fig. 4a,b). The difference is related to higher amount Fig. 3. Magnetization vs. applied field for deposits 1 at (a) 298, (b) 20 and (c) 5 K. Fig. 4. Magnetization vs. applied field for deposits 2 at (a) 298, (b) 20 and (c) 5 K.

5 I. Zhitomirsky et al. / Materials Letters 57 (2003) Fig. 5. Temperature dependence of the magnetization at for zerofield- (ZFC) and field-cooled (FC) deposits 2. of iron oxide in deposits 2 compared to deposits 1. Magnetization curves recorded in the range K showed zero remanence and zero coercivity. These data are consistent with superparamagnetic behavior of the nanoparticles. As expected, the saturation magnetization of hybrid films was found to be lower compared to that of bulk magnetite and maghemite. However, the magnetization of hybrid films was comparable to the magnetization of bulk composite materials prepared by other methods [7,9,13]. Magnetic hysteresis loops were observed at 5 K in prepared deposits as shown in Figs. 3c and 4c. Similar hysteresis loops were reported for other hybrid materials below the blocking temperature [7,9]. Zero remanence and zero coercivity are observed in the superparamagnetic state for very small particles because thermal fluctuations can prevent the existence of a stable magnetization. Below the blocking temperature, magnetic particles become magnetically frozen [31], and as a result, remanence and coercivity appear on the plot of magnetization as a function of applied field. Low field magnetization measurements in ZFC and FC modes are important for the characterization of superparamagnetic materials [9,28,31]. Results of the ZFC and FC magnetization measurements are shown in Fig. 5. The ZFC magnetization measurements show a peak at T max =25 K indicative of a characteristic blocking temperature for superparamagnetic particles. It is important to note that the T max for superparamagnetic material depends on the strength of the magnetic field and particle size distribution [9,32]. Above the blocking temperature, all the nanoparticles are at the superparamagnetic state. As a result, at temperatures higher than T max, the ZFC and FC curves are superimposed. Similar behavior was observed in other materials [28,31,33]. A separation of the ZFC and FC curves was observed at lower temperatures. This observation is consistent with the behavior of ultrafine magnetic particles below the blocking temperature [9]. Obtained experimental data indicate that superparamagnetic films based on iron oxide and PDDA could be produced by electrodeposition. However, more comprehensive investigations of magnetic properties coupled with results of electron microscopy, Mössbauer spectroscopy and other methods are necessary for characterization of the hybrid films. We cannot exclude the possibility that some weight loss in our TG experiments could also be related to the liberation of adsorbed water. Moreover, as mentioned in our previous papers, some hybrid materials cannot be considered as a simple mixture of organic and inorganic phases. It is in this regard that in our method the hybrid material is formed as a result of the interaction and heterocoagulation of polymer molecules and oxide particles formed at the electrode surface [23,26]. Work in progress deals with characterization of the composition and properties of the prepared films. One of the important possibilities provided by electrodeposition is the ability of agglomerate-free processing of nanostructured materials. It is important to note that this method has important advantages compared to other techniques, which enable synthesis of oxide particles in situ in a polymer matrix. Electrodeposition not only produces hybrid materials but also provides film deposition. In this method, the electrogenerated base is used instead of alkali, thus reducing risk of film contamination. The composition, microstructure and morphology of the films could be tailored by variation of bath composition and mass transport conditions for organic and inorganic components. There is no need to reiterate advantages of electrodeposition for formation of uniform films on substrates of complex shape and selected areas of the substrates [15,17]. Experimental results of this work open new opportunities in the formation of hybrid thin

6 1050 I. Zhitomirsky et al. / Materials Letters 57 (2003) film materials with valuable magnetic properties. Our preliminary results indicate that other polyelectrolytes could also be used for electrodeposition of such films. 4. Conclusions We have demonstrated a new method of fabrication of superparamagnetic films. This method has the advantage of permitting nanostructured iron oxides to be synthesized in situ in a polymer matrix on an electrode to form hybrid organic inorganic films. The amount of the deposited material, film composition and properties could be varied with variation of deposition time and polymer concentration in the solutions. The method opens new opportunities in the development of hybrid nanostructured magnetic materials. References [1] J.H. Fendler, Chem. Mater. 13 (2001) [2] T. Ito, Y. Okayama, S. Shiratori, Thin Solid Films 393 (2001) 138. [3] D.B. Mitzi, Chem. Mater. 13 (2001) [4] F. Caruso, Adv. Mater. 13 (2001) 11. [5] P.G. Lacroix, Chem. Mater. 13 (2001) [6] F. Leroux, J.-P. Besse, Chem. Mater. 13 (2001) [7] R.F. Ziolo, E.P. Giannelis, B.A. Weinstein, M.P. O Horo, B.N. Ganguly, V. Mehrotra, M.W. Russell, D.R. Huffman, Science 257 (1992) 219. [8] M. Kryszewski, J.K. Jeszka, Synth. Met. 94 (1998) 99. [9] B.H. Sohn, R.E. Cohen, G.C. Papaefthymiou, J. Magn. Magn. Mater. 182 (1998) 216. [10] M. Wan, W. Zhou, J. Li, Synth. Met. 78 (1996) 27. [11] T. Yogo, T. Nakamura, K. Kikuta, W. Sakamoto, S. Hirano, J. Mater. Res. 11 (1996) 475. [12] J.L. Dormann, F. D Orazio, F. Lucari, E. Tronc, P. Prené, J.P. Jolivet, D. Fiorani, R. Cherkaoui, M. Noguès, Phys. Rev. B 53 (1996) [13] T. Yogo, T. Nakamura, W. Sakamoto, S. Hirano, J. Mater. Res. 14 (1999) [14] D.Yu. Godovsky, A.V. Varfolomeev, G.D. Efremova, V.M. Cherepanov, G.A. Kapustin, A.V. Volkov, M.A. Moskvina, Adv. Mater. Opt. Electron. 9 (1999) 87. [15] I. Zhitomirsky, L. Gal-Or, Electrochemical coatings, in: N.B. Dahotre, T.S. Sudarshan (Eds.), Intermetallic and Ceramic Coatings, Marcel Dekker, New York, 1999, pp , Chapter 3. [16] G.H.A. Therese, P.V. Kamath, Chem. Mater. 12 (2000) [17] I. Zhitomirsky, Bull. Am. Ceram. Soc. 79 (2000) 57. [18] I. Zhitomirsky, L. Gal-Or, J. Mater. Sci. 33 (1998) 699. [19] Y. Zhou, R.J. Phillips, J.A. Switzer, J. Am. Ceram. Soc. 78 (1995) 981. [20] I. Zhitomirsky, Nanostruct. Mater. 8 (1997) 521. [21] R. Chaim, Nanostruct. Mater. 1 (1992) 479. [22] I. Zhitomirsky, A. Petric, Mater. Lett. 42 (2000) 273. [23] I. Zhitomirsky, A. Petric, Mater. Lett. 46 (2000) 1. [24] I. Zhitomirsky, A. Petric, Mater. Sci. Eng., B 78 (2000) 125. [25] I. Zhitomirsky, A. Petric, Ceram. Int. 27 (2001) 149. [26] I. Zhitomirsky, A. Petric, Bull. Am. Ceram. Soc. 80 (2001) 41. [27] I. Zhitomirsky, A. Petric, JOM, Miner., Met. Mater. Soc. J. 53 (2001) 48. [28] D.K. Kim, Y. Zhang, W. Voit, K.V. Rao, M. Muhammed, J. Magn. Magn. Mater. 225 (2001) 30. [29] R.M. Cornell, U. Schwertmann, The Iron Oxides, VCH, Weinheim, [30] A.J. Koch, J.J. Becker, J. Appl. Phys. 39 (1968) [31] B.H. Sohn, R.E. Cohen, Chem. Mater. 9 (1997) 264. [32] R.W. Chantrell, M. El-Hilo, K. O Grady, IEEE Trans. Magn. 27 (1991) [33] J. Mira, J.A. López-Pérez, J. Rivas, M.A. López-Quintela, R. Caciuffo, D. Rinaldi, D. Fiorani, IEEE Trans. Magn. 33 (1997) 3724.

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