Surfactant-Controlled Size and Shape Evolution of Magnetic Nanoparticles (original) (raw)

2009, Crystal Growth & Design

Nanoparticle Synthesis: Large iron-manganese oxide nanoparticles were synthesized by thermal decomposition of Fe(acac) 3 and Mn(acac) 2 in the presence of 16-heptadecenoic acid that included a small amount (ca. < 4 %) of an initially unknown contaminant, which was later identified as the ester derivative, 16-heptadecenoate, arising from the acid-catalyzed hydrolysis and partial esterification of 16heptadecenitrile in the one-pot synthetic procedure. The nanoparticles were formed by mixing Fe(acac) 3 (0.40 mmol), Mn(acac) 2 (0.40 mmol), 1,2-hexadecanediol (2.0 mmol), crude 16-heptadecenoic acid (1.2 mmol) and hexadecylamine (1.2 mmol) in benzyl ether (6.0 mL). Under argon, the reaction mixture was stirred, heated, and refluxed for 1 hour. After cooling, the crude solution of iron-manganese oxide nanoparticles was mixed with absolute ethanol (30 mL). A black precipitate was isolated by centrifugation. Several post-preparative washing steps were applied to remove excess stabilizer. The precipitated nanoparticles were stored in a non-polar solution (e.g., toluene) until further study.

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