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Oleylamine As Both Reducing Agent and Stabilizer in a Facile Synthesis of Magnetite Nanoparticles Zhichuan Xu,†,‡ Chengmin S

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Oleylamine As Both Reducing Agent and Stabilizer in a Facile Synthesis of Magnetite Nanoparticles Zhichuan Xu,†,‡ Chengmin S 1778 Chem. Mater. 2009, 21, 1778–1780 Oleylamine as Both Reducing Agent and Stabilizer Scheme 1 in a Facile Synthesis of Magnetite Nanoparticles Zhichuan Xu,†,‡ Chengmin Shen,‡ Yanglong Hou,*,§ Hongjun Gao,*,‡ and Shouheng Sun*,† Department of Chemistry, Brown UniVersity, ProVidence, Rhode Island 02912, Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, Beijing, China 100080, and College of NPs, the mechanism leading to the chemical conversions into V Engineering, Peking Uni ersity, Beijing, China 100871 Fe3O4 is complicated by the multicomponent reactants present in the reaction mixture. To meet a demand beyond ReceiVed NoVember 1, 2008 the laboratory-scale production, a more reliable and simpli- ReVised Manuscript ReceiVed March 26, 2009 fied synthetic technique to Fe3O4 NPs with a better stoichio- metric control is still desired. Nanostructured magnetite (Fe O ) has been one of the most 3 4 Recently, we reported a chemical synthesis of FeO NPs attractive nanomaterials for various magnetic applications in the mixture of oleylamine and oleic acid.7 By varying the because of its chemical stability1 and biocompability.2 It is heating conditions and ratios of oleylamine and oleic acid, known that Fe O nanoparticles (NPs) with controlled shapes 3 4 the size of FeO NPs can be controlled from 14 to 100 nm. are appealing for information storage applications,3 and those The experiment shows that the presence of excess amount coated with hydrophilic polymers have shown great potentials of oleylamine is the key to provide a strong reductive for medical diagnosis4 and drug delivery.5 Important progress environment for the thermal decomposition of Fe(acac) .7 It has been made regarding wet chemical synthesis of Fe O 3 3 4 indicates that oleylamine acts as an alternative reducing NPs6 to meet an increasing demand for obtaining uniform agent, which is inexpensive and even stronger than the 1,2- NPs with tunable chemical and magnetic properties. Among hexadecanediol that was used previously in the Fe O NP all the sythetic procedures developed thus far, the thermal 3 4 synthesis.6a Taking advantage of multifunctional (reducing decomposition of iron acetylacetonate, Fe(acac) , in a high 3 and capping) capabilities of oleylamine, we demonstrate here boiling point organic solvent in the presence of a reducing a much simplified organic phase synthesis of Fe O NPs via reagent and surfactants was first demonstrated to be an 3 4 the thermal decomposition of Fe(acac) in benzyl ether and effective way to synthesize monodisperse Fe O NPs.6a 3 3 4 oleylamine, as illustrated in Scheme 1. By varying the Further studies showed that the thermal decomposition of volume ratio of benzyl ether and oleylamine, we can tune iron-oleate complex can produce monodiseprse Fe O NPs 3 4 the NP sizes from 7 to 10 nm, a range that shows reasonably in an ultra-large scale.6b Although this thermal decomposition large magnetization and is suitable for a CVD catalytic study. method has become the main approach to high quality Fe3O4 In a typical synthesis of ∼10 nm Fe3O4 NPs, Fe(acac)3 (3 mmol) was dissolved in 15 mL of benzyl ether and 15 mL * Corresponding authors. E-mail: [email protected]; [email protected]; [email protected]. of oleylamine. The solution was dehydrated at 110 °C for † Brown University. 1 h under N atmosphere, then quickly heated to 300 °Cat ‡ Chinese Academy of Sciences. 2 § Peking University. a heating rate of 20 °C/min, and aged at this temperature (1) (a) Zhao, M.; Beauregard, D. A.; Loizou, L.; Davletov, B.; Brindle, for 1 h. After the reaction, the solution was allowed to cool K. M. Nat. Med. 2001, 7, 1241. (b) Perez, J. M.; Josephson, L.; O’Loughlin, T.; Hogemann, D.; Weissleder, R. Nat. Biotechnol. 2002, down to room temperature. The Fe3O4 NPs were extracted 20, 816. upon the addition of 50 mL of ethanol, followed by (2) (a) Tiefenauer, L. X.; Kuhne, G.; Andres, R. Y. Bioconjugate Chem. ∼ 1993, 4, 347. (b) Huh, Y. M.; Jun, Y.; Song, H. T.; Kim, S.; Choi, J.; centrifuging. The Fe3O4 NPs (yield 280 mg) were Lee, J. H.; Yoon, S.; Kim, K. S.; Shin, J. S.; Suh, J. S.; Cheon, J. dispersed in nonpolar solvents such as hexane and toluene. J. Am. Chem. Soc. 2005, 127, 12387. In the synthesis described above, the higer the ratio of (3) (a) Son, S. J.; Reichel, J.; He, B.; Schuchman, M.; Lee, S. B. J. Am. Chem. Soc. 2005, 127, 7316. (b) Zhao, W.; Gu, J.; Zhang, L.; Chen, oleylamine to benzyl ether, the smaller the Fe3O4 NPs. For H.; Shi, J. J. Am. Chem. Soc. 2005, 127, 8916. example, ∼7nmFe3O4 NPs were obtained when only (4) (a) Lee, J. H.; Huh, Y. M.; Jun, Y. W.; Seo, J. W.; Jang, J. T.; Song, ∼ ∼ H. T.; Kim, S. J.; Cho, E. J.; Yoon, H. G.; Suh, J. S.; Cheon, J. W. oleylamine was used. 8 and 9nmFe3O4 NPs were Nat. Med. 2007, 13, 95. (b) Seo, W. S.; Lee, J. H.; Sun, X. M.; Suzuki, produced with the volume ratio of oleylamine to benzyl ether Y.; Mann, D.; Liu, Z.; Terashima, M.; Yang, P. C.; Mcconnell, M. V.; of 20:10 and 18:12, respectively. If the volume ratio of Nishimura, D. G.; Dai, H. J. Nat. Mater. 2006, 5, 971. (5) (a) Son, S. J.; Reichel, J.; He, B.; Schuchman, M.; Lee, S. B. J. Am. oleylamine to benzyl ether was less than 1:1, the Fe3O4 NPs Chem. Soc. 2005, 127, 7316. (b) Zhao, W.; Gu, J.; Zhang, L.; Chen, with a broad size distribution were produced. This is probably H.; Shi, J. J. Am. Chem. Soc. 2005, 127, 8916. (6) (a) Sun, S.; Zeng, H. J. Am. Chem. Soc. 2002, 124, 8204. (b) Park, J.; due to the insufficiency of capping during the particle growth. An, K.; Hwang, Y.; Park, J. G.; Noh, H. J.; Kim, J. Y.; Park, J. H.; The transmission electron microscopy (TEM) images of Hwang, N. M.; Hyeon, T. Nat. Mater. 2004, 3, 891. (c) Yang, T.; Shen, C.; Li, Z.; Zhang, H.; Xiao, C.; Chen, S.; Xu, Z.; Shi, D.; Li, Fe3O4 NPs with different sizes are shown in Figure 1. It can J.; Gao, H. J. Phys. Chem. B 2005, 109, 23233. (d) Hui, C.; Shen, C.; be seen that the size distribution in each size group of the Yang, T.; Bao, L.; Tian, J.; Ding, H.; Li, C.; Hao, H. J. Phys. Chem. Fe3O4 NPs is very narrow. The corresponding size-distribu- C 2008, 112, 11336. (e) Park, J.; Lee, E.; Hwang, N.; Kang, M.; Kim, S. C.; Hwang, Y.; Park, J. G.; Noh, H. J.; Kim, J. Y.; Park, J. H.; Hyeon, T. Angew. Chem., Int. Ed. 2005, 44, 2872. (7) Hou, Y.; Xu, Z.; Sun, S. Angew. Chem., Int. Ed. 2007, 46, 6329. 10.1021/cm802978z CCC: $40.75 2009 American Chemical Society Published on Web 04/14/2009 Communications Chem. Mater., Vol. 21, No. 9, 2009 1779 (Figure S2, Supporting Information), indicating Fe3O4 is indeed formed during the synthesis.9d The magnetic properties of the Fe3O4 NPs were studied using a vibrating sample magnetometer (VSM) at room temperature. All the Fe3O4 NPs exhibited superparamagnetic properties with slight differences in saturation magnetization. A typical hysteresis loop of the as-synthesized Fe3O4 NPs (∼10 nm) is shown in Figure S3 (Supporting Information). The saturation moment of ∼10 nm Fe3O4 NPs (including surfactant) is about 65 emu/g. To calculate the saturation moment of pure Fe3O4 NPs, the inductively coupled plasma mass spectrometry (ICP-MS) technique was used to deter- mine the element content of Fe and Fe3O4. The ICP result showed that the weight percentage of Fe in gross particles is 58.8%, and correspondingly the weight percentage of Fe3O4 is 81.3%. It implies that the weight percentage of Figure 1. TEM images of Fe3O4 NPs: (a) 7 ( 0.5 nm, (b) 8 ( 0.4 nm, (c) surfactant is about 18.7% in the particles. On the basis of 9 ( 0.6 nm, and (d) 10 ( 0.8 nm. Scale bar is 20 nm. the ICP analysis, the caculated saturation moment of the ∼10 nm Fe3O4 NPs is ∼80 emu/g, which is very close to the previously reported values measured from the Fe3O4 NPs in the similar size.6a In a similar way, the calculated saturation moments of ∼9, ∼8, and ∼7nmFe3O4 NPs are ∼79, ∼77, and ∼76 emu/g, respectively. This is consistent with the fact that the moment is dependent on the NP size and thermal agitation has only the minor effect on the moment reduction in this 7-10 nm NP size range.9d The reductive thermal decomposition of Fe(acac)3 into 9d Fe3O4 NPs is different from that reported previously, in which a small amount of oleylamine was used with oleic acid together as surfactants and the 1,2-hexadecanediol was Figure 2. XRD patterns of Fe3O4 NPs: (a) ∼7 nm, (b) ∼8 nm, (c) ∼9 nm. used as reducing reagent. In that synthesis, the product ∼ and (d) 10 nm. (e) The standard Fe3O4 diffraction peaks (JCPDS 07- separated after a short refluxing time at reaction temperature 322). (∼300 °C) showed no magnetic response and contained tion histograms are given in Figure S1 (Supporting Informa- FeO.9d However, in our current decomposition process, we tion). found that the product separated from the reddish reaction X-ray diffraction (XRD) was used to record the crystal solution at a relatively low temperature of 170 °C had a infomation of Fe3O4 NPs. Figure 2 shows the XRD patterns magnetic response, which indicates the existence of nucleated of the Fe3O4 NPs at different sizes.
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