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通过使用注射泵对连续输送的金属膦配合物进行热分解来实现金属磷化物纳米棒的通用合成。

Generalized synthesis of metal phosphide nanorods via thermal decomposition of continuously delivered metal-phosphine complexes using a syringe pump.

作者信息

Park Jongnam, Koo Bonil, Yoon Ki Youl, Hwang Yosun, Kang Misun, Park Je-Geun, Hyeon Taeghwan

机构信息

National Creative Research Center for Oxide Nanocrystalline Materials and the School of Chemical and Biological Engineering, Seoul National University, Seoul 151-744, Korea.

出版信息

J Am Chem Soc. 2005 Jun 15;127(23):8433-40. doi: 10.1021/ja0427496.

Abstract

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 x 16 nm and 6 nm x 22 nm sized were synthesized by the thermal decomposition of Mn-TOP complex, which was prepared from the reaction of Mn(2)(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 degrees C using a syringe pump, uniform 2.5 nm x 20 nm sized Co(2)P nanorods were generated. When cobaltocene was employed as a precursor, uniform Co(2)P nanorods with 5 nm x 15 nm were obtained. When Fe-TOP complex was added to trioctylphosphine oxide (TOPO) at 360 degrees C using a syringe pump and then allowed to age at 360 degrees C for 30 min, uniform-sized FeP nanorods with an average dimension of 12 nm x 500 nm were produced. Nickel phosphide (Ni(2)P) nanorods with 4 nm x 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.

摘要

我们使用注射泵通过连续输送的金属膦配合物的热分解合成了尺寸均匀的过渡金属磷化物纳米棒。通过热分解Mn-TOP配合物合成了尺寸为8 nm×16 nm和6 nm×22 nm的MnP纳米棒,该配合物由Mn(2)(CO)(10)与三正辛基膦(TOP)反应制备,使用注射泵,注射速率分别恒定为10 mL/h和20 mL/h。当由乙酰丙酮钴与TOP反应制备的Co-TOP配合物在由辛醚和十六胺组成的混合溶剂中于300℃使用注射泵反应时,生成了尺寸均匀的2.5 nm×20 nm的Co(2)P纳米棒。当使用二茂钴作为前驱体时,获得了尺寸为5 nm×15 nm的均匀Co(2)P纳米棒。当使用注射泵在360℃将Fe-TOP配合物加入到三辛基氧化膦(TOPO)中,然后在360℃老化30分钟时,制备出了平均尺寸为12 nm×500 nm的尺寸均匀的FeP纳米棒。通过热分解由乙酰丙酮镍[Ni(acac)(2)]与TOP反应合成的Ni-TOP配合物,成功合成了尺寸为4 nm×8 nm的磷化镍(Ni(2)P)纳米棒。我们测量了这些纳米棒的磁性,其中一些纳米棒与相应的块状材料相比表现出不同的磁特性。

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