Bell David C, Wu Yue, Barrelet Carl J, Gradecak Silvija, Xiang Jie, Timko Brian P, Lieber Charles M
Center for Imaging and Mesoscale Structures, Harvard University, Cambridge, Massachusetts 02138, USA.
Microsc Res Tech. 2004 Aug;64(5-6):373-89. doi: 10.1002/jemt.20093.
We used vapor-liquid-solid (VLS) methods to synthesize discrete single-element semiconductor nanowires and multicomposition nanowire heterostructures, and then characterized their structure and composition using high-resolution electron microscopy (HRTEM) and analytical electron microscopy techniques. Imaging nanowires requires the modification of the established HRTEM imaging procedures for bulk material to take into consideration the effects of finite nanowire width and thickness. We show that high-resolution atomic structure images of nanowires less than 6 nm in thickness have lattice "streaking" due to the finite crystal lattice in two dimensions of the nanowire structure. Diffraction pattern analysis of nanowires must also consider the effects of a finite structure producing a large reciprocal space function, and we demonstrate that the classically forbidden 1/3 [422] reflections are present in the [111] zone axis orientation of silicon nanowires due to the finite thickness and lattice plane edge effects that allow incomplete diffracted beam cancellation. If the operating conditions are not carefully considered, we found that HRTEM image delocalization becomes apparent when employing a field emission transmission electron microscope (TEM) to image nanowires and such effects have been shown to produce images of the silicon lattice structure outside of the nanowire itself. We show that pseudo low-dose imaging methods are effective in reducing nanowire structure degradation caused by electron beam irradiation. We also show that scanning TEM (STEM) with energy dispersive X-ray microanalysis (EDS) is critical in the examination of multicomponent nanowire heterostructures.
我们采用气-液-固(VLS)方法合成离散的单元素半导体纳米线和多组分纳米线异质结构,然后使用高分辨率电子显微镜(HRTEM)和分析电子显微镜技术对其结构和成分进行表征。对纳米线成像需要对用于块状材料的既定HRTEM成像程序进行修改,以考虑有限的纳米线宽度和厚度的影响。我们表明,厚度小于6 nm的纳米线的高分辨率原子结构图像由于纳米线结构二维中的有限晶格而具有晶格“条纹”。对纳米线的衍射图案分析也必须考虑有限结构产生大的倒易空间函数的影响,并且我们证明,由于有限的厚度和晶格平面边缘效应允许不完全的衍射束抵消,经典禁止的1/3 [422]反射存在于硅纳米线的[111]区轴取向中。如果不仔细考虑操作条件,我们发现当使用场发射透射电子显微镜(TEM)对纳米线成像时,HRTEM图像的离域变得明显,并且这种效应已被证明会产生纳米线本身之外的硅晶格结构的图像。我们表明,伪低剂量成像方法在减少电子束辐照引起的纳米线结构退化方面是有效的。我们还表明,配备能量色散X射线微分析(EDS)的扫描TEM(STEM)在检查多组分纳米线异质结构中至关重要。