Generalized Synthesis of Metal Phosphide Nanorods via Thermal Decomposition of Continuously Delivered Metal−Phosphine Complexes Using a Syringe Pump

• Published in: Journal of the American Chemical Society Vol. 127; no. 23; pp. 8433 - 8440
• Main Authors: Park, Jongnam, Koo, Bonil, Yoon, Ki Youl, Hwang, Yosun, Kang, Misun, Park, Je-Geun, Hyeon, Taeghwan
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 15.06.2005
• Subjects: Cross-disciplinary physics: materials science; rheology; Exact sciences and technology; Materials science; Nanoscale materials and structures: fabrication and characterization; Nanotubes; Physics; Nickel phosphides; Manganese phosphides; Iron phosphides; SQUID devices; Transmission electron microscopy; Cobalt phosphides; Transition elements Compounds; Nanostructures; Nanostructured materials; Magnetic properties
• ISSN: 0002-7863; 1520-5126
• DOI: 10.1021/ja0427496

We synthesized uniform-sized nanorods of transition metal phosphides from the thermal decomposition of continuously delivered metal-phosphine complexes using a syringe pump. MnP nanorods with dimensions of 8 nm × 16 nm and 6 nm × 22 nm sized were synthesized by the thermal decomposition of Mn−TOP complex, which was prepared from the reaction of Mn2(CO)10 and tri-n-octylphosphine (TOP), using a syringe pump with constant injection rates of 10 and 20 mL/h, respectively. When Co−TOP complex, which was prepared from the reaction of cobalt acetylacetonate and TOP, was reacted in a mixture solvent composed of octyl ether and hexadecylamine at 300 °C using a syringe pump, uniform 2.5 nm × 20 nm sized Co2P nanorods were generated. When cobaltocene was employed as a precursor, uniform Co2P nanorods with 5 nm × 15 nm were obtained. When Fe−TOP complex was added to trioctylphosphine oxide (TOPO) at 360 °C using a syringe pump and then allowed to age at 360 °C for 30 min, uniform-sized FeP nanorods with an average dimension of 12 nm × 500 nm were produced. Nickel phosphide (Ni2P) nanorods with 4 nm × 8 nm were synthesized successfully by thermally decomposing the Ni−TOP complex, which was synthesized by reacting acetylacetonate [Ni(acac)2] and TOP. We measured the magnetic properties of these nanorods, and some of the nanorods exhibited different magnetic characteristics compared to the bulk counterparts.