Kobler Aaron, Kübel Christian
Karlsruhe, Germany, private contribution.
Institute of Nanotechnology (INT), Karlsruhe Institute of Technology (KIT), Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany.
Beilstein J Nanotechnol. 2018 Feb 15;9:602-607. doi: 10.3762/bjnano.9.56. eCollection 2018.
To relate the internal structure of a volume (crystallite and phase boundaries) to properties (electrical, magnetic, mechanical, thermal), a full 3D reconstruction in combination with in situ testing is desirable. In situ testing allows the crystallographic changes in a material to be followed by tracking and comparing the individual crystals and phases. Standard transmission electron microscopy (TEM) delivers a projection image through the 3D volume of an electron-transparent TEM sample lamella. Only with the help of a dedicated TEM tomography sample holder is an accurate 3D reconstruction of the TEM lamella currently possible. 2D crystal orientation mapping has become a standard method for crystal orientation and phase determination while 3D crystal orientation mapping have been reported only a few times. The combination of in situ testing with 3D crystal orientation mapping remains a challenge in terms of stability and accuracy. Here, we outline a method to 3D reconstruct the crystal orientation from a superimposed diffraction pattern of overlapping crystals without sample tilt. Avoiding the typically required tilt series for 3D reconstruction enables not only faster in situ tests but also opens the possibility for more stable and more accurate in situ mechanical testing. The approach laid out here should serve as an inspiration for further research and does not make a claim to be complete.
为了将体积的内部结构(微晶和相界)与性能(电学、磁学、力学、热学)联系起来,需要结合原位测试进行完整的三维重建。原位测试通过跟踪和比较单个晶体及相,来监测材料中的晶体学变化。标准透射电子显微镜(TEM)通过电子透明的TEM样品薄片的三维体积提供投影图像。目前,只有借助专用的TEM断层扫描样品架,才能对TEM薄片进行精确的三维重建。二维晶体取向映射已成为晶体取向和相确定的标准方法,而三维晶体取向映射仅被报道过几次。就稳定性和准确性而言,原位测试与三维晶体取向映射的结合仍然是一个挑战。在此,我们概述一种方法,可从重叠晶体的叠加衍射图案中三维重建晶体取向,而无需样品倾斜。避免三维重建通常所需的倾斜系列,不仅能实现更快的原位测试,还为更稳定、更准确的原位力学测试开辟了可能性。这里阐述的方法应能为进一步研究提供启发,但并不宣称是完整的。