Material Discrimination in Nanoparticle Hetero-Aggregates by Analysis of Scanning Transmission Electron Microscopy Images

Hetero-contacts are interfaces between different materials at the nanoscale leading to novel functional properties. In hetero-aggregates, primary particles of at least two different materials are mixed at primary particle or cluster level. Double flame spray pyrolysis (DFSP) is a versatile technique for the controlled synthesis of such materials. Characterization of hetero-aggregates by scanning transmission electron microscopy (STEM) requires acquisition and evaluation of many aggregate images in order to derive statistically significant results. Usually, STEM energy dispersive X-ray spectroscopy (EDXS) is used to acquire elemental maps providing the material distribution of the primary particles within hetero-aggregates. However, the acquisition of a single EDXS map takes up to several minutes. For this reason, determination of material types of primary particles from the intensity in high-angle annular dark field STEM images alone is desirable. These images can be acquired within a couple of seconds. In the present work, a method is suggested which allows for achieving this objective. It can be applied to distinguish materials with a significant difference in their atomic number and hence sufficient material contrast in the STEM images.     

连续太赫兹激光透射扫描成像实验研究

太赫兹成像可用于安检、反恐和工业生产等领域,已成为研究热点。由于连续太赫兹激光源体积较小、操作简单,因此,近几年对连续太赫兹激光成像的研究越来越多。基于C02激光泵浦甲醇气体生成的118．83μm激光,采用室温单元探测器、二维位移平台、聚乙烯透镜、光阑和计算机等器件组成的扫描透射成像系统对物体进行了成像实验,比较分析了扫描步长分别为1mm和0．5mm的成像结果。实验结果表明,由于增加光阑,实际成像功率下降,但此套成像系统在激光输出功率约为20mW时,仍成像清晰,且步长为0．5mm的成像效果更好。     

Direct Synthesis of ZIF-8 on Transmission Electron Microscopy Grids Allows Structure Analysis and 3D Reconstruction

The first example of layer-by-layer growth of a metal–organic framework (MOF) directly on transmission electron microscopy (TEM) grids is described. ZIF-8 is deposited on thin amorphous carbon films and subjected to a structure analysis by (scanning) TEM ((S)TEM). This method serves as a two-in-one synthesis and TEM sample-preparation technique and allows straightforward analysis of ZIF-8 crystallites. Artifacts resulting from sample preparation are completely avoided by this approach. The morphological properties, crystal structure, and the chemical composition of the material are investigated with high spatial resolution by a variety of methods of (analytical) electron microscopy. Furthermore, the incorporation of metallic nanoparticles in ZIF-8 by integrating a corresponding step into the layer-by-layer deposition process is examined. The formation of ZIF-8 crystals on the film proceeds as under the absence of nanoparticle-forming synthesis steps. However, the nanoparticles rather cover the supporting amorphous carbon film than being incorporated in the ZIF-8 material. This information cannot be obtained from standard characterization techniques but requires the application of analytical (S)TEM techniques.     

近场显微干涉成像中的探测角度和偏振问题研究

用偶极子耦合系统来模拟近场干涉测量中的探针样品关系,并利用各电场分量之间的组合方程组精确计算出其可能探测到的强度和相位像。结果显示,近场干涉所测量到的近场像的分辨力和探测器的方位及参考光的偏振方向之间有较强的依赖关系,随着探测器位置不同或者参考光偏振方向的变化,同一样品在同一照明条件下所得到的图像也会发生明显的改变。在倏逝波照明的情况下,近场像的精确度随着探测器相对于样品视角的增大而改善,且在不同偏振方向的近场像中,只有偏振方向垂直于样品表面的像能真实反映样品的细节分布,且同时具有足够的强度分布。     

Ultrathin Sectioning Of Polymeric Materials For Low-voltage Transmission Electron Microscopy: Relief On Ultrathin Sections

Ultrathin sectioning, one of the types of specimen preparations for transmission electron microscopy (TEM), has been considered the most perfect sectioning technique leading to the thinnest sections (50–100 nm). Following a study based on a newly developed low-voltage TEM technique, a relief on the ultrathin sections of polymer blends was observed that was ascribed to substantial differences in mechanical properties of the blend constituents.[1] Lednický, F., Hromádková, J. and Pientka, Z. 2001. Ultrathin sectioning of polymeric materials for low-voltage transmission electron microscopy. Polymer, 42: 4329–4338.  [Google Scholar] In this study, an analogous relief was observed with a blend, the constituents of which are both hard in cutting.

The origin of the surface relief on ultrathin sections of polymer blends was sought using low-voltage scanning TEM and atomic force microscopy. Polycarbonate/styrene-co-acrylonitrile blend was examined as a representative of blends with all components well under T _g at room temperature. A distinct surface relief was observed on both ultrathin sections and remaining cut surfaces of the blend for low-temperature and room-temperature cutting. A rougher surface relief was found on the ultrathin sections than on the remaining cut surfaces. The surface relief was assumed to occur in the course of the cutting when extensive shearing occurs. Correspondence of the surface relief with the phase structure proves the influence of different mechanical behavior of individual blend components on the resulting morphology.

     

扫描近场光学显微镜中两类光纤探针传输特性的研究

采用局域模式耦合理论，对扫描近场光学显微镜中的两类光纤探针－腐蚀锥和熔拉锥的传输特性进行了比较和分析。给出了光在探针锥中传输时耦合效率的分布情况，以及传输效率随锥长，针尖直径和光波长变化的特性。     

Nanoscale Imaging and Stabilization of Silica Nanospheres in Liquid Phase Transmission Electron Microscopy

Liquid phase transmission electron microscopy (LP‐TEM) is a novel and highly promising technique for the in situ study of important nanoscale processes, in particular the synthesis and modification of various nanostructures in a liquid. Destabilization of the samples, including reduction, oxidation, or dissolution by interactions between electron beam, liquid, and sample, is still one of the main challenges of this technique. This work focuses on amorphous silica nanospheres and the phenomena behind their reshaping and dissolution in LP‐TEM. It is proposed that silica degradation is primarily the result of reducing radical formation in the liquid phase and the subsequent accelerated hydroxylation of the silica, while alterations in silica solid structure, pH, and oxidizing species formation had limited influence. Furthermore, the presence of water vapor instead of liquid water also results in degradation of silica. Most importantly however, it is shown that the addition of scavengers for reducing radicals significantly improved amorphous silica stability during LP‐TEM imaging. Devising such methods to overcome adverse effects in LP‐TEM is of the utmost importance for further development and implementation of this technique in studies of nanoscale processes in liquid.     

GaAs/AlxGa1-xAs量子阱红外探测器微结构研究

采用金属有机物化学气相沉积法生长了两种不同结构参数GaAs/AlxGa1-xAs量子阱材料。利用傅里叶光谱仪分别对势垒中Al组分为0.20,0.30的1#,2#样品进行77 K液氮温度下光谱响应测试。结果显示:1#,2#峰值响应波长为8.38,7.59 m,而根据薛定谔方程得到峰值波长为9.694,8.134 m,二者误差分别为13.6%,6.68%。针对误差过大及吸收峰向高能方向发生漂移的现象,利用高分辨透射扫描电镜对样品微观界面结构进行分析,结果显示,样品存在不同程度的位错及不均匀性。结果表明:位错引起AlGaAs与GaAs晶格不匹配,是造成1#误差较大的主要原因;峰值响应波长随势垒中Al组分的降低而增大,说明Al组分减小致使量子阱子带间距离缩小是导致峰值响应波长红移的原因。     

GaAs/AlxGa1-xAs量子阱红外探测器微结构研究

采用金属有机物化学气相沉积法生长了两种不同结构参数GaAs/AlxGa1-xAs量子阱材料。利用傅里叶光谱仪分别对势垒中Al组分为0.20,0.30的1#,2#样品进行77 K液氮温度下光谱响应测试。结果显示：1#,2#峰值响应波长为8.38,7.59 m,而根据薛定谔方程得到峰值波长为9.694,8.134 m,二者误差分别为13.6%,6.68%。针对误差过大及吸收峰向高能方向发生漂移的现象,利用高分辨透射扫描电镜对样品微观界面结构进行分析,结果显示,样品存在不同程度的位错及不均匀性。结果表明：位错引起AlGaAs与GaAs晶格不匹配,是造成1#误差较大的主要原因;峰值响应波长随势垒中Al组分的降低而增大,说明Al组分减小致使量子阱子带间距离缩小是导致峰值响应波长红移的原因。