Aso Kohei, Higashimine Koichi, Miyata Masanobu, Kamio Hiroshi, Oshima Yoshifumi
School of Materials Science, Japan Advanced Institute of Science and Technology, Asahidai 1-1, Nomi, Ishikawa, Japan.
Center for Nano Materials and Technology, Japan Advanced Institute of Science and Technology, Asahidai 1-1, Nomi, Ishikawa, Japan.
Commun Chem. 2025 Apr 28;8(1):122. doi: 10.1038/s42004-025-01513-2.
Metal oxyhydroxides are essential nanomaterials for recent technologies because of their diverse applications, such as catalysis, adsorbents, and precursors of metal oxides. These applications rely on the controlled crystal structures of metal oxyhydroxides formed via hydrolyzed metal monomers' condensation. However, characterizing the atomic-scale structures of the metal oxyhydroxides has still been challenging due to their diverse structural types, nanometer-scale sizes, and beam sensitivity. Here, we developed a data-driven analysis approach for atom-resolved transmission electron microscopy images of titanium oxyhydroxide (metatitanic acid) nanoparticles. Lattice spacings and angles were measured for each of the 1300 nanoparticles with random crystal orientations, providing three-dimensional structural information. Our findings reveal their anatase-like structure with alternating layers of titanium dioxide (TiO) and titanium hydroxide (Ti(OH)) planes. The revealed structure is key to understanding their role as a precursor for metastable anatase TiO. Our approach unveils the three-dimensional structure of metal oxyhydroxides with high statistical reliability and low electron dose, paving the way for property understanding and application design.
金属羟基氧化物因其多样的应用，如催化、吸附剂以及金属氧化物的前驱体等，而成为近期技术中不可或缺的纳米材料。这些应用依赖于通过水解金属单体缩合形成的金属羟基氧化物的可控晶体结构。然而，由于金属羟基氧化物结构类型多样、尺寸在纳米级别且对电子束敏感，对其原子尺度结构进行表征仍然具有挑战性。在此，我们针对羟基氧化钛（偏钛酸）纳米颗粒的原子分辨透射电子显微镜图像开发了一种数据驱动的分析方法。对1300个具有随机晶体取向的纳米颗粒分别测量了晶格间距和角度，从而提供了三维结构信息。我们的研究结果揭示了它们具有类似锐钛矿的结构，由二氧化钛（TiO）层和氢氧化钛（Ti(OH)）层交替组成。所揭示的结构对于理解它们作为亚稳锐钛矿TiO前驱体的作用至关重要。我们的方法以高统计可靠性和低电子剂量揭示了金属羟基氧化物的三维结构，为性能理解和应用设计铺平了道路。
