Lu Kangbo, Sourty Erwan, Loos Joachim
Department of Chemical Engineering and Chemistry, Eindhoven University of Technology, PO Box 513, 5600 MB [corrected] Eindhoven, The Netherlands.
J Electron Microsc (Tokyo). 2010 Aug;59 Suppl 1:S39-44. doi: 10.1093/jmicro/dfq048. Epub 2010 Jul 1.
We have utilized bright-field conventional transmission electron microscopy tomography and annular dark-field scanning transmission electron microscopy (ADF-STEM) tomography to characterize a well-defined carbon black (CB)-filled polymer nanocomposite with known CB volume concentration. For both imaging methods, contrast can be generated between the CB and the surrounding polymer matrix. The involved contrast mechanisms, in particular for ADF-STEM, will be discussed in detail. The obtained volume reconstructions were analysed and the CB volume concentrations were carefully determined from the reconstructed data. For both imaging modes, the measured CB volume concentrations are substantially different and only quantification based on the ADF-STEM data revealed about the same value as the known CB loading. Moreover, when applying low-convergence angles for imaging ADF-STEM tomography, data can be obtained of micrometre-thick samples.
我们利用明场传统透射电子显微镜断层扫描和环形暗场扫描透射电子显微镜（ADF-STEM）断层扫描来表征一种具有已知炭黑（CB）体积浓度的明确的CB填充聚合物纳米复合材料。对于这两种成像方法，CB与周围聚合物基体之间均可产生对比度。将详细讨论所涉及的对比度机制，尤其是ADF-STEM的对比度机制。对获得的体积重建结果进行了分析，并根据重建数据仔细确定了CB体积浓度。对于这两种成像模式，测量得到的CB体积浓度有很大差异，只有基于ADF-STEM数据的定量分析才显示出与已知CB负载量大致相同的值。此外，在对ADF-STEM断层扫描成像应用低会聚角时，可以获得微米厚样品的数据。
