Daniels H R, Brydson R, Brown A, Rand B
Institute for Materials Research, The University of Leeds, Leeds, LS2 9JT, UK.
Ultramicroscopy. 2003 Sep;96(3-4):547-58. doi: 10.1016/S0304-3991(03)00115-3.
Using a series of graphitising carbons heat treated at different temperatures, the peak position of the bulk (pi+sigma) plasmon was measured using electron energy loss spectroscopy and observed to shift between 22 and 27eV. Experimental data is presented and discussed showing the effects of the collection conditions and sample orientation upon the observed spectra. We present an empirical technique by which quantitative energy filtered transmission electron microscopy (EFTEM) maps with two energy windows selected in the plasmon region can be readily acquired and processed, the results of which may be interpreted as graphitisation maps and subsequently physical property maps. An experimentally established resolution of approximately 1.6nm makes this technique a very useful tool with which to examine nanoscale properties in microstructural regions of interest in TEM specimens such as fibre/matrix interfaces within carbon-carbon composites, multi-walled carbon nanotubes and graphitic inclusions in carbon steels. Also presented is data demonstrating the unsuitability of pi(*)-related chemical EFTEM maps in both the low-loss region and at the carbon K ionisation edge for mapping bonding in such highly anisotropic media due to the strong orientation dependence of the intensity of the transitions involved. This is followed by suggestions for wider application of the plasmon mapping technique within systems other than those based upon carbon.
使用一系列在不同温度下热处理的石墨化碳,通过电子能量损失谱测量了体(π+σ)等离子体激元的峰值位置,观察到其在22至27电子伏特之间移动。给出并讨论了实验数据,展示了收集条件和样品取向对观察到的光谱的影响。我们提出了一种经验技术,通过该技术可以轻松获取和处理在等离子体激元区域选择两个能量窗口的定量能量过滤透射电子显微镜(EFTEM)图,其结果可以解释为石墨化图,进而解释为物理性质图。实验确定的约1.6纳米的分辨率使该技术成为一种非常有用的工具,可用于研究透射电子显微镜(TEM)样品中感兴趣的微观结构区域的纳米级特性,如碳-碳复合材料中的纤维/基体界面、多壁碳纳米管和碳钢中的石墨夹杂物。还展示了数据,表明由于所涉及跃迁强度的强烈取向依赖性,与π*相关的化学EFTEM图在低损耗区域和碳K电离边缘都不适用于绘制此类高度各向异性介质中的键合情况。随后提出了在基于碳以外的系统中更广泛应用等离子体激元映射技术的建议。