Huang Xiaohui, Tang Yushu, Kübel Christian, Wang Di
Institute of Nanotechnology, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany.
Department of Materials and Earth Sciences, Technical University of Darmstadt, Alarich-Weiss-Straße 2, 64287 Darmstadt, Germany.
Microsc Microanal. 2022 Sep 14:1-8. doi: 10.1017/S1431927622012247.
Electron tomography (ET) has gained increasing attention for the 3D characterization of nanoparticles. However, the missing wedge problem due to a limited tilt angle range is still the main challenge for accurate reconstruction in most experimental TEM setups. Advanced algorithms could in-paint or compensate to some extent the missing wedge artifacts, but cannot recover the missing structural information completely. 360° ET provides an option to solve this problem by tilting a needle-shaped specimen over the full tilt range and thus filling the missing information. However, sample preparation especially for fine powders to perform full-range ET is still challenging, thus limiting its application. In this work, we propose a new universal sample preparation method that enables the transfer of selected individual nanoparticle or a few separated nanoparticles by cutting a piece of carbon film supporting the specimen particles and mounting them onto the full-range tomography holder tip with the help of an easily prepared sharp tungsten tip. This method is demonstrated by 360° ET of Pt@TiO hollow cage catalyst showing high quality reconstruction without missing wedge.
电子断层扫描(ET)在纳米颗粒的三维表征方面越来越受到关注。然而,在大多数实验性透射电子显微镜(TEM)设置中,由于倾斜角度范围有限导致的缺失楔形问题仍然是精确重建的主要挑战。先进的算法可以在一定程度上修复或补偿缺失楔形伪影,但无法完全恢复缺失的结构信息。360°电子断层扫描提供了一种解决此问题的方法,即通过在整个倾斜范围内倾斜针状样品来填充缺失信息。然而,特别是对于细粉进行全范围电子断层扫描的样品制备仍然具有挑战性,从而限制了其应用。在这项工作中,我们提出了一种新的通用样品制备方法,该方法通过切割支撑样品颗粒的碳膜片,并借助易于制备的尖锐钨尖将选定的单个纳米颗粒或几个分离的纳米颗粒转移并安装到全范围断层扫描支架尖端。通过对Pt@TiO中空笼状催化剂进行360°电子断层扫描证明了该方法,其显示出高质量的重建且无缺失楔形。