Characterization of Magnetic and Non-Magnetic Iron Oxide Nanoparticles Synthesized by Different Routes

"There is an expanding interest in synthesizing high quality magnetic nanoparticles, most notably for biomedical applications. Different processing routes have been reported for the synthesis of magnetite and maghemite. However, some ambiguity remains on their precise chemistry, intermediates, and final products, due to the structural similarity of maghemite and magnetite, and the relative ease of redox transitions during synthesis. Here we present the results of TEM, x-ray and electron diffraction, and SQUID studies aimed at characterizing the products from two different reaction systems, thereby clarifying the reaction chemistry. The first system hydrolyzed aqueous FeCh and FeCb chlorides with ammonia in a micro fluidic reactor at ambient temperature; although the reaction product displayed a uniform distribution, it included non-magnetic goethite and lepidocrocite. If the aqueous solutions contained dissolved oxygen, there appeared to be extensive oxidation of Fe(II). The second system thermally decomposed iron (III) acetylacetonate in ether. In prior studies, oleylamine has been reported to serve as both a reducing agent and capping ligand to control particle characteristics; however, our studies revealed little reduction, with maghemite dominating the reaction products.IntroductionMagnetite and maghemite nanoparticles are co=only used in ferrofluids, in medical applications, and in drug delivery. Superparamagnetic properties, along with low cytotoxicity, colloid stability and bioactive molecule conjugation capability, make these nanomagnets ideal for both in-vitro and in-vivo biomedical applications [1]. One of the major constraints on widespread adoption of nanoparticles for these applications is the amount needed. Typical batch synthesis methods produce polydispersed nanoparticles, which require further size selection procedures to isolate the mono disperse nanoparticle population needed for many applications. In order to maximize the yield of usable particles from a synthesis operation, the reaction conditions must be closely controlled. This requires full knowledge of how the reaction conditions control the various aspects of nanoparticle growth. Many methods have been used to synthesize iron oxides, including sonochemical reactions, mechanochemical synthesis, hydrolysis and thermal decomposition. This work examines the latter two methods, focusing on oxidation and reduction of iron."