STEM SerialED: achieving high-resolution data for ab initio structure determination of beam-sensitive nanocrystalline materials

IF 2.9 2区 材料科学 Q2 CHEMISTRY, MULTIDISCIPLINARY IUCrJ Pub Date : 2024-01-01 DOI:10.1107/S2052252523009661
Pascal Hogan-Lamarre , Yi Luo , Robert Bücker , R. J. Dwayne Miller , Xiaodong Zou , M. Gemmi (Editor)
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Abstract

An implementation of scanning transmission electron microscopy serial electron diffraction (SerialED) through scripting is proposed. SerialED and continuous-rotation electron diffraction refinement results for the structure of zeolite Y are compared, and the structure of beam-sensitive ZSM-25 is solved by direct methods from electron diffraction data for the first time.

Serial electron diffraction (SerialED), which applies a snapshot data acquisition strategy for each crystal, was introduced to tackle the problem of radiation damage in the structure determination of beam-sensitive materials by three-dimensional electron diffraction (3DED). The snapshot data acquisition in SerialED can be realized using both transmission and scanning transmission electron microscopes (TEM/STEM). However, the current SerialED workflow based on STEM setups requires special external devices and software, which limits broader adoption. Here, we present a simplified experimental implementation of STEM-based SerialED on Thermo Fisher Scientific STEMs using common proprietary software interfaced through Python scripts to automate data collection. Specifically, we utilize TEM Imaging and Analysis (TIA) scripting and TEM scripting to access the STEM functionalities of the microscope, and DigitalMicrograph scripting to control the camera for snapshot data acquisition. Data analysis adapts the existing workflow using the software CrystFEL, which was developed for serial X-ray crystallography. Our workflow for STEM SerialED can be used on any Gatan or Thermo Fisher Scientific camera. We apply this workflow to collect high-resolution STEM SerialED data from two aluminosilicate zeolites, zeolite Y and ZSM-25. We demonstrate, for the first time, ab initio structure determination through direct methods using STEM SerialED data. Zeolite Y is relatively stable under the electron beam, and STEM SerialED data extend to 0.60 Å. We show that the structural model obtained using STEM SerialED data merged from 358 crystals is nearly identical to that using continuous rotation electron diffraction data from one crystal. This demonstrates that accurate structures can be obtained from STEM SerialED. Zeolite ZSM-25 is very beam-sensitive and has a complex structure. We show that STEM SerialED greatly improves the data resolution of ZSM-25, compared with serial rotation electron diffraction (SerialRED), from 1.50 to 0.90 Å. This allows, for the first time, the use of standard phasing methods, such as direct methods, for the ab initio structure determination of ZSM-25.

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实现光束敏感纳米晶体材料从头算结构测定的高分辨率数据。
采用连续电子衍射(SerialED)技术对每个晶体采用快照数据采集策略,解决了三维电子衍射(3DED)技术测定束敏材料结构时的辐射损伤问题。SerialED中的快照数据采集可以使用透射电镜和扫描透射电镜(TEM/STEM)来实现。然而,目前基于STEM设置的SerialED工作流程需要特殊的外部设备和软件,这限制了更广泛的应用。在这里,我们提出了一个基于stem的SerialED在赛默飞世尔科学系统上的简化实验实现,使用通用的专有软件接口,通过Python脚本来自动收集数据。具体来说,我们使用TEM成像和分析(TIA)脚本和TEM脚本来访问显微镜的STEM功能,并使用DigitalMicrograph脚本来控制相机进行快照数据采集。数据分析使用软件CrystFEL来适应现有的工作流程,该软件是为串行x射线晶体学开发的。我们的STEM串行工作流程可用于任何Gatan或赛默飞世尔科学相机。我们应用该工作流程收集了两种铝硅酸盐沸石(Y和ZSM-25)的高分辨率STEM SerialED数据。我们首次展示了通过使用STEM序列化数据的直接方法从头开始结构确定。Y型沸石在电子束下相对稳定,STEM SerialED数据延伸至0.60 Å。我们发现,用358个晶体的连续旋转电子衍射数据合并得到的结构模型与用一个晶体的连续旋转电子衍射数据得到的结构模型几乎相同。这表明从STEM SerialED中可以获得精确的结构。ZSM-25沸石对光束非常敏感,具有复杂的结构。我们发现,与串行旋转电子衍射(SerialRED)相比,STEM SerialED大大提高了ZSM-25的数据分辨率,从1.50提高到0.90 Å。这使得首次使用标准的相位方法,如直接法,来从头计算ZSM-25的结构。
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来源期刊
IUCrJ
IUCrJ CHEMISTRY, MULTIDISCIPLINARYCRYSTALLOGRAPH-CRYSTALLOGRAPHY
CiteScore
7.50
自引率
5.10%
发文量
95
审稿时长
10 weeks
期刊介绍: IUCrJ is a new fully open-access peer-reviewed journal from the International Union of Crystallography (IUCr). The journal will publish high-profile articles on all aspects of the sciences and technologies supported by the IUCr via its commissions, including emerging fields where structural results underpin the science reported in the article. Our aim is to make IUCrJ the natural home for high-quality structural science results. Chemists, biologists, physicists and material scientists will be actively encouraged to report their structural studies in IUCrJ.
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