Kearns Gregory J, Foster Evan W, Hutchison James E
Department of Chemistry and Materials Science Institute, University of Oregon, Eugene, Oregon 97403, USA.
Anal Chem. 2006 Jan 1;78(1):298-303. doi: 10.1021/ac051459k.
A significant challenge in materials characterization is the determination of the structure of nanoparticle assemblies that have been deposited on solid substrates, such as SiO2. The best method for obtaining quantitative information about structure, size, and spacing on the nanometer-length scale is TEM; however, commercially available TEM grids offer a limited range of substrate materials. In addition, the compositions of these grids do not permit much chemical processing. Here we describe silicon-based grids with electron-transparent SiO2 windows suitable for use as substrates for high-resolution TEM that can be easily fabricated using standard silicon microfabrication techniques. These grids are physically and chemically robust and exhibit the same surface chemistry and chemical stability as an oxide grown on a silicon wafer. Thus, the grids make possible the concurrent investigation of chemical and structural information on the same sample. Convenient modification of the surfaces of the grids provides access to a wide range of new substrates for the direct imaging of chemically modified surfaces by TEM. We demonstrate the utility of these grids by aligning DNA on the chemically modified SiO2 surface in order to direct the assembly of linear arrays of nanoparticles. Using these grids, we are able to quantify the effects of assembly conditions on nanoparticle size, spacing, and dispersity in the arrays.
材料表征中的一个重大挑战是确定沉积在诸如SiO₂等固体衬底上的纳米颗粒聚集体的结构。获取有关纳米长度尺度上的结构、尺寸和间距的定量信息的最佳方法是透射电子显微镜(TEM);然而,市售的TEM网格提供的衬底材料种类有限。此外,这些网格的成分不允许进行太多化学处理。在此,我们描述了一种基于硅的网格,其具有适合用作高分辨率TEM衬底的电子透明SiO₂窗口,该窗口可使用标准的硅微加工技术轻松制造。这些网格在物理和化学上都很坚固,并且具有与在硅片上生长的氧化物相同的表面化学性质和化学稳定性。因此,这些网格使得在同一样品上同时研究化学和结构信息成为可能。对网格表面进行便捷的修饰可为通过TEM直接成像化学修饰表面提供多种新的衬底。我们通过在化学修饰的SiO₂表面上排列DNA以指导纳米颗粒线性阵列的组装来证明这些网格的实用性。使用这些网格,我们能够量化组装条件对纳米颗粒在阵列中的尺寸、间距和分散性的影响。