Gerung Henry, Boyle Timothy J, Tribby Louis J, Bunge Scott D, Brinker C Jeffrey, Han Sang M
Department of Chemical and Nuclear Engineering, University of New Mexico, 209 Farris Engineering Center, Albuquerque, New Mexico 87131, USA.
J Am Chem Soc. 2006 Apr 19;128(15):5244-50. doi: 10.1021/ja058524s.
A simple solution synthesis of germanium (Ge0) nanowires under mild conditions (<400 degrees C and 1 atm) was demonstrated using germanium 2,6-dibutylphenoxide, Ge(DBP)2 (1), as the precursor where DBP = 2,6-OC6H3(C(CH3)3)2. Compound 1, synthesized from Ge(NR2)2 where R = SiMe3 and 2 equiv of DBP-H, was characterized as a mononuclear species by single-crystal X-ray diffraction. Dissolution of 1 in oleylamine, followed by rapid injection into a 1-octadecene solution heated to 300 degrees C under an atmosphere of Ar, led to the formation of Ge0 nanowires. The Ge0 nanowires were characterized by transmission electron microscopy (TEM), X-ray diffraction analysis, and Fourier transform infrared spectroscopy. These characterizations revealed that the nanowires are single crystalline in the cubic phase and coated with oleylamine surfactant. We also observed that the nanowire length (0.1-10 microm) increases with increasing temperature (285-315 degrees C) and time (5-60 min). Two growth mechanisms are proposed based on the TEM images intermittently taken during the growth process as a function of time: (1) self-seeding mechanism where one of two overlapping nanowires serves as a seed, while the other continues to grow as a wire; and (2) self-assembly mechanism where an aggregate of small rods (<50 nm in diameter) recrystallizes on the tip of a longer wire, extending its length.
在温和条件(<400摄氏度和1个大气压)下,以锗2,6 - 二丁基苯氧化物Ge(DBP)₂(1)为前驱体,展示了一种简单的溶液法合成锗(Ge⁰)纳米线,其中DBP = 2,6 - OC₆H₃(C(CH₃)₃)₂。化合物1由Ge(NR₂)₂(其中R = SiMe₃)和2当量的DBP - H合成,通过单晶X射线衍射表征为单核物种。将1溶解在油胺中,然后在氩气气氛下快速注入加热到300摄氏度的1 - 十八烯溶液中,导致形成Ge⁰纳米线。通过透射电子显微镜(TEM)、X射线衍射分析和傅里叶变换红外光谱对Ge⁰纳米线进行了表征。这些表征表明,纳米线为立方相单晶,并包覆有油胺表面活性剂。我们还观察到,纳米线长度(0.1 - 10微米)随温度(285 - 315摄氏度)和时间(5 - 60分钟)的增加而增加。基于在生长过程中作为时间函数间歇性拍摄的TEM图像,提出了两种生长机制:(1)自种子机制,即两根重叠纳米线中的一根作为种子,而另一根继续作为线生长;(2)自组装机制,即小棒(直径<50纳米)的聚集体在较长线的尖端重结晶,延长其长度。